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While Ga and Al do not form extended solid solutions in equilibrium, metastable single phase Ga–Al alloys were prepared by rapid quenching from the melt to −1190°C (splat cooling), yielding a wide extension of the Al-rich solid solution α; at higher Ga contents, this phase is followed by a tetragonal phase α′. Another metastable phase rich in Ga was also observed. The mean atomic volumes of α and α′ permit a quadratic extrapolation to pure Ga, for which V(Ga) = 18.27 Å3 at −190°C. The solid solution formation and the structural instability of the cubic and tetragonal phases α and α′ are discussed in terms of pseudopotential theory; the analogy of α′ to a high-pressure phase of Ga has been noted.