Composition and morphology of thin transparent films obtained from sols based on TiN(IV) compounds

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Abstract

The results of a comparative study of the composition and structure of thin films formed from film-forming sol-gel compositions based on SnCl4/EtOH/H2O and SnCl4/EtOH/H2O/NH4ОН precursors are presented. The features of the morphology and distribution of Sn, N and Cl atoms over the surface of the films were analyzed, as well as the transparency of the films depending on the amount of ammonium hydroxide introduced into the sol-gel composition. Possible chemical processes and reaction products underlying film formation and crystallization of film surfaces are considered. It was shown that the size and shape of the resulting skeletal crystals depend on the amount of ammonium hydroxide introduced into the sol-gel system. Formation of SnO2 crystals and crystals containing NH4Cl was studied in the films at the nano- and micro scales by using optical and electron microscopy and X-ray phase analysis. The new data obtained make it possible to control the morphology and composition of the synthesized thin films by changing the ratio of sol-gel synthesis precursors.

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About the authors

Е. A. Bondar’

Satpayev University

Email: floijan@gmail.com

Institute of Physics and Technology

Kazakhstan, Almaty, 050013

О. А. Shilova

Satpayev University; Institute of Silicate Chemistry of the Russian Academy of Sciences

Email: floijan@gmail.com

Institute of Physics and Technology

Kazakhstan, Almaty, 050013; St. Petersburg, 199034, Russia

I. А. Lebedev

Satpayev University

Email: floijan@gmail.com

Institute of Physics and Technology

Kazakhstan, Almaty, 050013

Е. А. Dmitrieva

Satpayev University

Email: floijan@gmail.com

Institute of Physics and Technology

Kazakhstan, Almaty, 050013

A. I. Fedossimova

Satpayev University

Email: floijan@gmail.com

Institute of Physics and Technology

Kazakhstan, Almaty, 050013

A. S. Kovalenko

Institute of Silicate Chemistry of the Russian Academy of Sciences

Email: floijan@gmail.com
Russian Federation, St. Petersburg, 199034

A. M. Nikolaev

Institute of Silicate Chemistry of the Russian Academy of Sciences

Author for correspondence.
Email: floijan@gmail.com
Russian Federation, St. Petersburg, 199034

S. А. Ibraimova

Satpayev University

Email: floijan@gmail.com

Institute of Physics and Technology

Kazakhstan, Almaty, 050013

A. K. Shongalova

Satpayev University

Email: floijan@gmail.com

Institute of Physics and Technology

Kazakhstan, Almaty, 050013

U. B. Issayeva

Satpayev University

Email: floijan@gmail.com

Institute of Physics and Technology

Kazakhstan, Almaty, 050013

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2. Fig. 1. Surface morphology of films obtained from film-forming sol-gel systems SnCl4/EtOH/H2O (a) and SnCl4/EtOH/H2O/NH4OH (b-e) with calculated NH4+/Sn4+ ratio (wt%) = 0.1 (b); 0.2 (c); 0.45 (d); 0.9 (e); 1.8 (f). The insets (c-e) show the surface fragments of the films at higher magnification.

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3. Fig. 2. Distribution of Sn, N, Cl elements in the structure of thin films obtained from the film-forming sol-gel system SnCl4/EtOH/H2O without the addition of ammonium hydroxide (a) and from the sol-gel systems SnCl4/EtOH/H2O/NH4OH with the addition of ammonium hydroxide at different NH4 +/Sn4+ ratios: 0.2 (c); 0.45 (d); 0.9 (e); 1.8 (f).

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4. Fig. 3. X-ray crystalline structure of the film obtained from the film-forming system SnCl4/EtOH/H2O/NH4OH at mass ratio NH4+/Sn4+ = 1.8 (a); b - enlarged fragment. Signals from crystallographic surfaces of SnO2 and NH4Cl are marked.

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5. Fig. 4. Transmission spectra of a glass substrate (0) and films deposited on this substrate by centrifugation from sols based on aqueous-alcoholic solution of SnCl4 - 5H2O without addition of ammonium hydroxide (a) and with addition of ammonium hydroxide at different NH4+/Sn4+ ratios: 0.2 (c); 0.45 (d); 0.9 (e); 1.8 (f).

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