The III/V semiconductor alloy GaP1−xSbx has been grown for the first time. This alloy, which has a large miscibility gap at the growth temperatures of 530–600 °C, has been grown by organometallic vapor phase epitaxy at atmospheric pressure. In spite of the miscibility gap, which is calculated to extend from x=0.01 to 0.99 at 530 °C, layers with excellent surface morphologies could be grown throughout the entire composition range. The 10 K energy band gap has been determined as a function of composition by using photoluminescence, x‐ray diffraction, and electron microprobe analysis, yielding bowing parameters of 3.8 and 2.7 eV for the Γ and X conduction band minima, respectively.

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