The aim of the present work was to investigate the formation of nanostructured alumina, zirconia, magnesia, titanium oxide, etc. powders and fibers as well as to research their crystal and microstructure.

The initial preform for oxide nanostructured fibrous materials preparation were hydrated cellulose filaments, felt and fabrics. They were impregnated with aqueous metal salt solutions and then were dried. The hydrated cellulose was chosen because it was a polysaccharide of complex architecture: the latter consisted of crystallites – microfibrilles surrounded by amorphous and crystal fields with microcapillaries and micropores. In the act of being adsorbed, the solutions were elevated via the capillary channels into the interfibrillar space and penetrated first into an amorphous, then into a crystal component of polysaccharide macromolecules. In this case, the impregnating liquid was kept by cellulose at the capillary expense, absorbing forces and chemical bond energy.

The complex processes proceed at heating of cellulose fibers containing metal salts. The adsorbed water was first removed near 100⁰C. Then there took place hydrolysis of crystal hydrated salts and thermolysis of hydrated cellulose fibers, followed by the loss of chemically bound water. As a result, cellulose fibers  lost gaseous and liquid organic substances, and transformed into carbon filaments, containing high-dispersed metal hydroxide and oxide grains. At temperatures 300-500⁰C carbon burnt out, metal hydroxide transformed into oxide grains that were annealed each other at their contact place to form a nanostructured fibers. It should be noticed, a macrostructure of oxide fiber was similar to the initial polymer architecture (bio-mimetic phenomenon). This investigation permit purposefully develop technologies of nanostructured inorganic fibers and powders.

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