Zn-doped InGaN thin films were deposited on GaN/sapphire by metalorganic chemical vapor deposition, and studied by a combination of high-resolution X-ray diffraction (HR-XRD), micro-photoluminescence (PL) and secondary ion mass spectrometry (SIMS). Indium phase separation is studied comparatively. HR-XRD exhibits a GaN band and a single band from InGaN for samples without phase separation, but two InGaN bands corresponding to different x(In) for samples with phase separation. PL excitation power dependence measurements reveal 2 sets of InGaN PL emissions for samples with phase separation, but only 1 set for samples without phase separation. SIMS data showed that phase separated InGaN:Zn films possess a high Zn concentration near the InGaN–GaN interface and non-uniform distributions of In and Zn contents, which are in contrast with data from InGaN:Zn films with no In-phase separation.