The reactivity of LiNO₃ and Al(NO₃)₃ with respect to urea and β-alanine was investigated. Experimental results proved that β-alanine is a more suitable fuel for LiNO₃, whereas urea seems to be more adequate for Al(NO₃)₃. Based on the different metal nitrate/fuel mixture reactivity, nanocrystalline γ-LiAlO₂ powders were prepared by solution combustion synthesis using a fuel mixture of urea and β-alanine. This fuel mixture yielded single-phase nanocrystalline γ-LiAlO₂ (32.6 nm) directly from the combustion reaction. The resulted powder had a specific surface area of 3.2 m²/g and no supplementary annealing was required. On the other hand, pure γ-LiAlO₂ could not be obtained by using a single fuel (urea, β-alanine) unless annealing at 900 °C for 1 h was performed.