[en] Nd_2-xLi_xTi₂O_7-δ where x = 0, 0.2, 0.3 and 0.4 was synthesized by Gel Entrapment Technique (GET). Hexamethylenetetramine (HMTA) was used as the gelation agent. For the preparation of the compound, appropriate amounts of Nd(NO₃)₃, TiOCI₂, LiNO₃ and 0.2 moles of NH₄NO₃ were mixed in a 500 ml beaker. To this mixture, desired amount of 3M HMTA solution was added at room temperature. On heating the solution turned into a hard gel. The gel was dried at 180 deg C and then ignited at 250 deg C, leaving behind a fluffy-mass. This precursor powder was further heated to 500 deg C in flowing O₂ atmosphere to remove any leftover organic matter and finally to 800 deg C for 10 h to get phase-pure compound. The compounds were characterized by room temperature XRD for phase purity and Dynamic Light Scattering (DLS) for particles size analysis. The particle size distribution studied by DLS showed that particles were present in the size range of 35-400 nm with an average particle size of ∼130 nm. Reducibility of the Ti⁴⁺ was studied by Temperature Programmed Reduction (TPR)