Кинетические закономерности синтеза наночастиц диоксида кремния при гетерогенном гидролизе тетраэтоксисилана с использованием L-аргинина в качестве катализатора

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Abstract

В работе исследована кинетика синтеза наночастиц кремнезема (< 50 нм) в условиях гетерогенного гидролиза тетраэтоксисилана (ТЭОС) с использованием L-аргинина в качестве щелочного катализатора. Определены скорости процесса образования диоксида кремния в диапазоне температур 10–95°C при концентрациях катализатора 6–150 мМ. Показано, что энергия активации процесса зависит от концентрации катализатора и изменяется в диапазоне 21.5–13.9 кДж/моль, линейно уменьшаясь с ростом концентрации L-аргинина в системе. Проведена оценка критерия сохранения монодисперсности частиц SiO2 при их доращивании “на затравку”. Экспериментально установлена зависимость плотности кремнеземных частиц субмикронных размеров от температуры отжига. В диапазоне температур 200–1000°C плотность частиц меняется от 2.04 до 2.20 г/см3.

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About the authors

В. М. Масалов

Институт физики твердого тела имени Ю.А. Осипьяна РАН

Email: sovyk@inbox.ru
Russian Federation, ул. Академика Осипьяна, 2, Черноголовка, Московская обл., 142432

Н. С. Сухинина

Институт физики твердого тела имени Ю.А. Осипьяна РАН

Email: sovyk@inbox.ru
Russian Federation, ул. Академика Осипьяна, 2, Черноголовка, Московская обл., 142432

Д. Н. Совык

Институт общей физики им. А.М. Прохорова РАН

Author for correspondence.
Email: sovyk@inbox.ru
Russian Federation, ул. Вавилова, 38, Москва, 119991

В. Г. Ральченко

Институт общей физики им. А.М. Прохорова РАН

Email: sovyk@inbox.ru
Russian Federation, ул. Вавилова, 38, Москва, 119991

Г. А. Емельченко

Институт физики твердого тела имени Ю.А. Осипьяна РАН

Email: sovyk@inbox.ru
Russian Federation, ул. Академика Осипьяна, 2, Черноголовка, Московская обл., 142432

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2. Fig. 1. Change in the concentration of silicon dioxide during the hydrolysis of TEOS at a temperature of 60 °, The concentration of L-arginine is 6 mM and the mixing intensity of the reaction mixture is different: 1 ‑ the rotation speed of the agitator is 200 rpm, 2 – 600 rpm. On the right axis of the ordinate, the veli is postponed‑ the rank of the degree of conversion of the TEOS.

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3. Fig. 2. Kinetic lines of the heterogeneous hydrolysis-condensation of TEOS at different temperatures and concentrations of L-arginine.

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4. Fig. 3. The dependence of the speed of the formation process SiO2 from temperature for different concentrations L-arginine.

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5. Fig. 4. Temperature dependences of the process rate constant at different concentrations of the L-arginine catalyst.

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6. Fig. 5. Dependence of the activation energy of the process on the concentration of L-arginine.

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7. 6. Silicon dioxide particles obtained by heterogeneous hydrolysis of TEOS in the presence of L-arginine. Silicon dioxide particles D = 132.7 ± 2.1 nm (b) obtained by incrementing particles with a diameter D = 42.9 ± 2.5 nm (a). The inserts show normal particle size distributions.

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8. Fig. 7. SEM images of SiO2 particles obtained by seed growth: (a) bimodal particle size distribution; (b) monodisperse particles.

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9. Figure 8. Dependence of the density of silicon dioxide particles with a diameter of ~ 300 nm obtained under conditions of heterogeneous hydrolysis of TEOS in the presence of L-arginine on the annealing temperature. The duration of annealing was 24 hours.

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