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The aluminum-containing polycarbosilane (Al-PCS) with various quantities of aluminum was obtained by adding aluminium acetylacetonate (Al(AcAc)3) as an aluminum source to polysilacarbosilane (PSCS). Subsequently, thermal decomposition and condensation at various conditions were carried out. The molecular weight $$ \left( {\overline{\text{Mn}} } \right),\,\overline{\text{Mn}} $$ distribution, yield and softening point of the resulting Al-PCS differ with the Al(AcAc)3:PSCS weight ratio, the thermolysis temperature and the reaction time. The larger the Al(AcAc)3:PSCS weight ratio, the higher the thermolysis temperature and the longer the reaction time, the greater the $$ \overline{\text{Mn}} , $$ yield and softening point of Al-PCS. In addition, the oxygen and aluminum contents of Al-PCS increase at higher Al(AcAc)3:PSCS weight ratios. As the mixing weight ratio of Al(AcAc)3:PSCS increased, additional oxygen was introduced into Al-PCS with the increased Al content. The structure of Al-PCS was characterized by the FT-IR. These results show that Al-PCS is very similar to polycarbosilane in structure.