It has been shown that the high-temperature hydrogen treatment of aluminum oxide nanowires coated with a monolayer of titanium oxide causes them to curl into nanotubes as a result of self-organization. The physicochemical properties of the nanotubes of a composite aluminum oxide aerogel coated with titanium oxide have been studied using X-ray phase analysis (XRD) and transmission electron microscopy (TEM). As a result of TiO2/Al2O3 nanofibrous aerogel treatment with hydrogen, a conversion of amorphous aluminum oxide fibers into tubes of nanocrystalline η-Al2O3 occurs, but in this case the titanium dioxide monolayer does not form a separate phase. A study of the porous structure by the low-temperature adsorption of nitrogen vapors has shown that the aerogels of TiO2/Al2O3 nanotubes have a developed mesoporous structure with a small amount of micropores and a specific surface of more than 300 m2/g. An increase in the temperature of hydrogen treatment first leads to the growth of an increase in the specific surface to 348 m2/g at 923 K, and then to a gradual decrease to 145 m2/g at 1123 K. In this case, the diameter of mesopores corresponding to a maximum on a curve of the pore size distribution decreases from 35 nm for a freshly prepared sample to 25 nm at 923 K and to 20 nm at 1123 K. The most homogeneous pores of a 25 nm diameter have the samples activated at 923 K. As a result of the high-temperature hydrogen treatment of the samples, the number of primary adsorption centers of water vapor adsorption decreases about two times. The resulting samples of TiO2/Al2O3 aerogels are close in structure to the initial aluminum oxide, whose wires just form nanotubes having a surface coated with titanium dioxide. As a result of the interaction between molecules of titanium dioxide adsorbed on the surface of aluminum oxide tubes, a substantial densification of the composite structure occurs. © 2016, Pleiades Publishing, Ltd.