MgAl-NH3 LDHs (layered double hydroxides), ZnAl-LDHs and ZnAl-NH3 LDHs with different molar ratio of Al/ammonia were synthesized by co-precipitation method. The synthetic LDHs samples were characterized by XRD, FT-IR, TGA-DTG and SEM techniques and tested by Congo red method. In addition, after PVC (Poly vinyl chloride) and DOP (Dioctylphthalate) were added to LDHs, the thermal stability for PVC was characterized by TGA-DTG. The results indicated that LDHs intercalated with ammonia improved thermal stability for PVC significantly, MgAl-NH3 LDHs (Mg 2+ :Al 3+ : NH3·H2O = 3:1:0.5) and ZnAl-NH3 LDHs (Zn 2+ :Al 3+ :NH3·H2O=2:1:1.5) showed the best thermal stability for PVC, interlayered space of LDHs became larger by intercalating ammonia.