We studied a combination of supercritical CO2, water and ethanol for the preparation of crystalline and pure nanostructured TiO2 without any thermal processing. The effect of temperature (40-150 °C) and sequence on structural and textural properties was investigated at constant pressure of 30 MPa. The prepared aerogels were characterized with respect to the (micro)structural properties by Raman spectroscopy and X-ray diffraction. The textural properties such as specific surface area, content of mesoporous and volume of microporous were determined from nitrogen physisorption and skeletal density by helium pycnometry measurements.