Механохимический синтез нанокомпозитов с заданным составом добавкой растворителя прекурсоров

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Abstract

Задача данной работы состоит в попытке внедрения в научную практику метода “механохимической перекристаллизации” в твердофазных системах с малыми добавками жидкого растворителя. В качестве такового использовался диметилсульфоксид (ДМСО) – универсальный биполярный апротонный растворитель. Как пример, была изучена механическая активация реакционного процесса AgNO3 + NH4I + zNH4NO3 (разбавитель) + yS + xДМСО = AgI + yS* + (z + 1)NH4NO3 + + xДМСО, где z ≈ 5, y ≈ 1, x << 1 – мольные доли. Было установлено образование наночастиц серы (S*) и йодида серебра (AgI), а по сути, сделан синтез нанокомпозитов S*/AgI с контролируемым содержанием компонентов. Применение разбавителя NH4NO3 – нецелевого продукта механосинтеза – обеспечивало стабилизацию размеров наночастиц. Получение наночастиц в среде ДМСО достигается не прямой механической активацией, а в результате обычной перекристаллизации (непрерывный процесс растворения-кристаллизации серы) или реакционной перекристаллизации (непрерывный процесс растворения AgNO3, NH4I и их реакция с кристаллизацией AgI). Первый вариант реализуется при получении S*, а второй – AgI. Целевые продукты (S*, AgI и S*/AgI) отмывались от водорастворимых компонентов (NH4NO3, ДМСО) с применением ультразвуковой бани. Предложенное техническое решение было осуществлено в шаровых планетарных мельницах с различной фурнитурой.

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About the authors

Ф. Х. Уракаев

Институт геологии и минералогии им. В. С. Соболева СО РАН

Author for correspondence.
Email: urakaev@igm.nsc.ru
Russian Federation, пр. Академика Коптюга, 3, Новосибирск, 630090

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Supplementary files

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2. Fig. 1. Micrographs of TEM of washed sulfur particles from samples of experiments on mechanochemical recrystallization of sulfur with the addition of 1 ml (a) and 5 ml (b) DMSO.

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3. Fig. 2. XRD data of the sulfur sample obtained by washing and drying the MA product according to scheme (1) with the addition of 2 ml DMSO.

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4. Fig. 3. The result of Raman spectroscopy of a sulfur sample obtained by washing and drying the MA product according to scheme (1) with the addition of 2 ml DMSO.

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5. Fig. 4. SEM-EMF data of a sulfur sample obtained by washing and drying the MA product by reaction (1) with the addition of 3 ml DMSO. The inserts provide a microphotography of the SEM of the analysis area (a) and a table of elemental composition (b).

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6. Fig. 5. Diffractograms of S*/AgI samples with the addition of 5 ml (a) and 1 ml (b) DMSO.

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7. Fig. 6. Raman spectroscopy data for S*/AgI nanocomposites prepared by mechanochemical recrystallization with additives of 5 ml (a) and 1 ml (b) DMSO.

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8. Fig. 7. SEM micrography of the S*/AgI sample obtained with the addition of 1 ml DMSO.

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9. Fig. 8. SEM-EMF data for the S*/AgI sample obtained with the addition of 5 ml DMSO: (a) SEM micrograph with an EMF application area marked with a cross; (b) the result of the EMF determination of the elemental composition; (c) the blitz of the content of the elements.

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10. Fig. 9. XRD results of nanocomposite samples S*/AgI obtained in a Pulverizette 5 mill with additives of 1, 2, 3 and 5 ml DMSO.

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11. Fig. 10. Raman spectroscopy data for S*/AgI nanocomposites obtained at the Pulverizette 5 mill with additives of 1, 2, 3 and 5 ml DMSO.

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