| Summary: | A cost-effective solution for the synthesis of high-porosity TiO<sub>2</sub> aerogels, which can be used as a mesoporous perovskite network charge-carrier material during the manufacture of solar cells, is described. The effects of the synthesis parameters (precursor (titanium (IV) isopropoxide (TIP) and tetrabutyl orthotitanate (TBOT)), additional solvent exchange (n-hexane (nH), cyclohexane (CH), and diethyl ether (DE)), subcritical drying (800 mbar vacuum, 70 °C, 8 h), aging, and calcination on the aerogel’s structure have been investigated. Methods of XRD, FT-IR, BET, Raman, STA, SEM, UV–vis, and thermal conductivity measurements were applied to find out the relation between the synthesis conditions and the properties of the synthesized aerogels. Amorphous aerogels are polydispersed systems with the highest probability of pore diameter from 0.5 to 15 nm. An nH-exchanged, aged aerogel synthesized from the precursor TIP shows the highest diameter of pores. After calcination, the aerogels tend to crystallize into an anatase phase and the size of the crystallites depends on the precursor’s nature. Calcination leads to a significant increase in both the apparent and true density of the aerogels, and it also results in an increase in porosity and thermal conductivity.
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