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The ammonium molydbate(AM) based on zinc hydroxystannate(ZHS) and AM/ZHS was coated by aluminum hydroxide (ATH) with different ratios were successfully prepared via sol-gel technique.The emphasis in this study was on the establishment of microencapsulation process by which microcapsules were formed and controlled.The clarification of the effect of preparation conditions was made on the morphology and diameter of microcapsules.The ATH/AM/ZHS microcapsules were subsequently used as filler in poly (vinyl chloride) (PVC) matrix, and flame retardancy properties of PVC composites were studied.The results revealed that LOI value of PVC/ATH/AM/ZHS microcapsule composites are higher than that of neat PVC and PVC/AM/ZHS composites.The UL 94 ratings of most of PVC/ATH/AM/ZHS microcapsule composites are V-0, whereas neat PVC gives no rating.The smoke density of PVC/ATH/AM/ZHS microcapsule composites are lower than that of neat PVC and PVC/AM/ZHS composites.