Abstract: NH₄ZnPO₄ powders were synthesized using a simple precipitation method at room temperature. The effects of polyvinyl pyrrolidone (PVP), polyvinyl alcohol (PVA), glucose, and hexadecyltrimethylammonium bromide (CTAB) solutions on the morphology and structure of the prepared samples were investigated. The phase composition and morphology of the prepared samples were characterized using X-ray diffraction and scanning electron microscopy, respectively. Depending on the polymer sources, the hexagonal structure prepared using non-surfactant of water completely changed to monoclinic structure when CTAB was added. X-ray absorption near-edge structure (XANES) and X-ray photoelectron spectroscopy (XPS) were performed to study the local structure and surface electronic structure of the prepared samples, confirming that the oxidation states of P and Zn ions are 5+ and 2+, respectively. On the basis of the results of inductively coupled plasma atomic emission spectroscopy (ICP-OES), the NH₄ZnPO₄ powders can be classified as a slow-release fertilizer where less than 15% of the ions were released in 24 h. A simple precipitation method using water, PVP, PVA, sucrose, and CTAB as a template can be used to synthesize NH₄ZnPO₄ powders. In addition, this method may be extended for the preparation of other oxide materials.