The present work is intended to pilot the possible use of ammonia precursors for the growth of III–V–N alloys with metal‐organic vapor phase epitaxy (MOVPE) as opposed to typical growth procedures using dimethylhydrazine. The GaPN alloys are grown by repeated cycles of surface nitridation and growth of a thin GaP layer with an interval separating the nitridation and growth. The effects of conditions and duration of each step on the N composition and crystallinity are systematically clarified. An N composition is controlled up to 1.6% in the current conditions, maintaining a high crystalline quality comparable to the GaP substrates, while a continuous‐supply method yields a much lower value.

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