Синтез ZnGa2Se4 взаимодействием GaI3 и ZnI2 с селеном

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Проведено термодинамическое моделирование систем GaI3–Se и ZnI2–Se методом констант равновесия в температурном интервале 200–500°С. Показано, что равновесная степень превращения йодидов в Ga2Se3 и ZnSe составляет 21 и 0.7٪ соответственно. Основным компонентом паровой фазы в обеих системах является молекулярный йод. Разработан способ получения Ga2Se3, ZnSe, ZnGa2Se4 взаимодействием GaI3 и ZnI2 с селеном в вакуумированном кварцевом реакторе с двумя температурными зонами. Селективное выведение йода из реакционного расплава позволило достичь практического выхода селенидов на уровне 86–90٪ при температуре 450°С. Остаточное содержание йода в полученных соединениях составило 0.2–1 ат.%.

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Sobre autores

А. Вельмужов

Институт химии высокочистых веществ им. Г.Г. Девятых Российской академии наук

Autor responsável pela correspondência
Email: velmuzhov.ichps@mail.ru
Rússia, ГСП-75, ул. Тропинина, 49, Нижний Новгород

Е. Тюрина

Институт химии высокочистых веществ им. Г.Г. Девятых Российской академии наук

Email: velmuzhov.ichps@mail.ru
Rússia, ГСП-75, ул. Тропинина, 49, Нижний Новгород

М. Суханов

Институт химии высокочистых веществ им. Г.Г. Девятых Российской академии наук

Email: velmuzhov.ichps@mail.ru
Rússia, ГСП-75, ул. Тропинина, 49, Нижний Новгород

А. Сучков

Институт химии высокочистых веществ им. Г.Г. Девятых Российской академии наук

Email: velmuzhov.ichps@mail.ru
Rússia, ГСП-75, ул. Тропинина, 49, Нижний Новгород

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2. Fig. 1. Thermodynamically determined composition of the vapor (a), condensed (b) phases and the equilibrium degree of transformation of GaI3 into Ga2Se3 in the GaI3–Se system.

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3. Fig. 2. Thermodynamically determined composition of the vapor (a), condensed (b) phases and the equilibrium degree of conversion of ZnI2 to ZnSe in the ZnI2–Se system.

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4. Fig. 3. The setup for loading components into the reactor (stage 1) and synthesizing Ga2Se3, ZnSe and ZnGa2Se4 (stage 2): 1, 2, 3 – ampoules with reagents; 4 – tubular furnaces; 5 – programmable thermostats; 6 – breakable partitions; 7 – magnetic strikers; 8 – outlet tube; 9 – reactor; 10 – iodine receiver; A, B, C – constrictions.

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5. Fig. 4. X-ray diffraction patterns of the products of the interaction of gallium(III) iodide (a) and zinc(II) iodide (b) with selenium (the dashes correspond to the position of the reflections Ga2Se3 (05-0724) and ZnSe (80-0021) [23]).

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6. Fig. 5. X-ray diffraction patterns of the products of the combined interaction of gallium(III) iodide and zinc(II) iodide with selenium at 450°C for 1 (1), 2 (2) and 3 (3) h (the dotted lines correspond to the position of the ZnGa2Se4 reflections (PDF 47-1590) [23]).

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