This study continues the investigation into the ash cenosphere formation mechanism using a series of narrow size-fractioned ash cenosphere samples separated from the fly ash of an Australian coal-fired power station. The gas products locked inside various ash cenosphere size fractions are dominantly CO 2 and some N 2 . With increasing ash cenosphere particle size from 63–75 μm to 150–250 μm, the average gas pressure decreases from 0.227 atm (at normal temperature and pressure, NTP) to 0.172 atm while the amount of CO 2 and N 2 locked in ash cenospheres increases significantly. The SiO 2 /Al 2 O 3 ratio decreases with increasing ash cenosphere size, accompanied with an increase in the sum of TiO 2 and Fe 2 O 3 contents. Thermomechanical analysis further shows that ash cenospheres of different size fractions cannot achieve full melting at 1600 °C, suggesting that the formation of these ash cenospheres requires higher temperatures. Further analysis based on ash chemistry of individual cenospheres suggests that the optimum particle temperature for cenosphere formation is ∼1640–1850 °C. The growth of cenosphere precursors is governed by a wide range of viscosity of molten cenosphere precursors together with the force of surface tension, which is inversely proportional to the viscosity of molten droplets, producing ash cenospheres with various wall thicknesses. The data suggest that, apart from Fe 2 O 3, TiO 2 may play an important role in the formation of ash cenospheres.