The synthesis of layered double hydroxide Mg/Fe and polyoxometalate H3[aPW12O40]•nH2O has been done. The intercalation compounds were characterized using XRD and spectrophotometer FT-IR. The result of characterization using XRD shows the successful intercalation of layered double hydroxide with polyoxometalate H3[a-PW12O40]•nH2O compound, there is an increase of the interlayer spasing of 4.…