Sol–gel–xerogel transformations in the thin layer at the salt solution–gaseous reagent interface and the synthesis of new materials with microtubular morphology

  • Vladislav Gurenko
  • Larisa GulinaEmail author
  • Valeri Tolstoy
Original Paper: Functional coatings, thin films and membranes (including deposition techniques)


In this report, we consider the peculiarities of sol–gel–xerogel transformations, which occurs in the thin layer at the FeCl2/FeCl3 water solution and gaseous NH3 interface. A thin layer consisting of nanoparticles of Fe(OH)3 and Fe3O4 is formed as a result of interfacial reaction. Depending on the time of treatment with gaseous ammonia, it was possible to obtain either a freestanding layer with a thickness of 1 μm or microtubular structures (scrolls). Synthetic conditions, under which a large number of preferentially oriented microtubes are formed with diameters of about 10 and up to 200-μm long, were determined. The synthesized structures consisted of crystalline Fe3O4 nanoparticles with an average diameter of about 5–10 nm incorporated in an amorphous matrix. Layers and tubes were characterized by X-ray diffraction analysis, scanning and transmission electron microscopy (SEM and TEM), and X-ray photoelectron spectroscopy. The model, concerning sol–gel–xerogel transformations in the thin layer, formed after interaction at the salt solution–gaseous reagent interface, was suggested. The magnetic properties of the products were studied.


  • A sol–gel–xerogel transformation in the thin layer at the gas–solution interface has been studied.

  • Tubular or planar morphology of the products depended on synthesis conditions.

  • The opportunity to obtain an array of oriented microtubes was demonstrated for the first time.

  • The layers and tubes based on Fe3O4 demonstrated superparamagnetic properties.


Sol–gel process Interface Thin films Microtubes Magnetite 



This work was supported by the Russian Science Foundation (grant No. 16-13-10223). We are grateful to the Research Park of St. Petersburg State University for assistance in studies of our samples: Nanotechnology Center, Centre for Innovative Technologies of Composite Nanomaterials, and Centre for X-Ray Diffraction Studies.

Compliance with ethical standards

Conflict of interest

The authors declare that they have no conflict of interest.


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© Springer Science+Business Media, LLC, part of Springer Nature 2019

Authors and Affiliations

  1. 1.Institute of ChemistrySaint Petersburg State UniversitySt. PetersburgRussia

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