Synthesis of nano-sized SNO₂ by direct chemical precipitation using tin(II) chloride

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Abstract

The process of synthesizing nano-sized SNO₂ by direct chemical precipitation using tin(II) chloride and hydrogen peroxide has been investigated. The thermal behavior of the obtained powders was studied using simultaneous thermal analysis (TGA/DSC). The impact of H₂O₂ concentration in the reaction system on the set of functional groups in the materials was demonstrated using infrared spectroscopy, while X-ray diffraction analysis (XRD) was utilized to examine the crystalline structure of the powders, including the thermal transformation of tin(II) oxyhydroxide. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were employed to show the effect of the reaction system composition on the size of primary particles and the agglomerates formed. In particular, it was established that with an increase of H₂O₂ concentration, both the size of the primary particles and the agglomerates decrease. The roughness of the films formed from the obtained nanopowders was studied using atomic force microscopy (AFM). Kelvin probe force microscopy (KPFM) was used to construct surface potential distribution maps for the obtained materials and to evaluate the electron work function from their surface.

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About the authors

N. A. Fisenko

Kurnakov Institute of General and Inorganic Chemistry of the Russian Academy of Sciences

Author for correspondence.
Email: fisenkonk@yandex.ru
Russian Federation, Leninsky pr., 31, Moscow, 119991

I. A. Solomatov

Kurnakov Institute of General and Inorganic Chemistry of the Russian Academy of Sciences; National Research University “Higher School of Economics”

Email: fisenkonk@yandex.ru
Russian Federation, Leninsky pr., 31, Moscow, 119991; st. Myasnitskaya, 21, Moscow, 101000

N. P. Simonenko

Kurnakov Institute of General and Inorganic Chemistry of the Russian Academy of Sciences

Email: fisenkonk@yandex.ru
Russian Federation, Leninsky pr., 31, Moscow, 119991

Ph. Yu. Gorobtsov

Kurnakov Institute of General and Inorganic Chemistry of the Russian Academy of Sciences

Email: fisenkonk@yandex.ru
Russian Federation, Leninsky pr., 31, Moscow, 119991

T. L. Simonenko

Kurnakov Institute of General and Inorganic Chemistry of the Russian Academy of Sciences

Email: fisenkonk@yandex.ru
Russian Federation, Leninsky pr., 31, Moscow, 119991

E. P. Simonenko

Kurnakov Institute of General and Inorganic Chemistry of the Russian Academy of Sciences

Email: fisenkonk@yandex.ru
Russian Federation, Leninsky pr., 31, Moscow, 119991

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Supplementary files

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2. Fig. 1. TGA (a) and DSC (b) curves of powders obtained at different concentrations of hydrogen peroxide in the reaction system.

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3. Fig. 2. IR spectra of the obtained powders: 1 – sample 1, 2 – sample 2, 3 – sample 3, 4 – sample 1 after additional heat treatment at 300°C for 3 hours; the asterisk indicates the absorption bands from vaseline oil.

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4. Fig. 3. X-ray diffraction patterns of the obtained powders: 1 – sample 1, 2 – sample 2, 3 – sample 3, 4 – sample 1 after additional heat treatment at 300°C for 3 hours.

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5. Fig. 4. Microstructure of the obtained powders: a – sample 1, b – sample 2, c – sample 3; d – distribution of agglomerates by size according to SEM data.

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6. Fig. 5. Microstructure of the obtained powders: a – sample 1, b – sample 2, c – sample 3; d – particle size distribution according to TEM data.

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7. Fig. 6. Relief of films obtained using powders 1 (a), 2 (c) and 3 (d) and the corresponding surface potential distribution maps (b – 1, d – 2, e – 3) according to AFM and KZSM data.

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