Layered double hydroxides are composed by substitution of metal cation divalent and trivalent. Metal cation divalent and trivalent can be changed. In this work, effect metal cation trivalent (M3+) toward layer formation were studied. Synthesis of LDHs has used co-precipitation methods with molar ratio 3:1 and kept pH at 10. The result of synthesis was characterized by X-ray Diffraction (XRD) and Fourier Transform Infrared (FT-IR) analyses.