We report the crystallographic and magnetic properties of Ni_0.3Fe_0.7Ga₂S₄ by means of X-ray diffractometer (XRD), a superconducting quantum interference device (SQUID) magnetometer, and a Mössbauer spectroscopy. In particular, Ni_0.3Fe_0.7Ga₂S₄ was studied by Mössbauer analysis for evidence of spin reorientation. The chalcogenide material Ni0.3Fe0.7Ga2S4 was fabricated by a direct reaction method. XRD analysis confirmed that Ni_0.3Fe_0.7Ga₂S₄ has a 2-dimension (2-D) triangular lattice structure, with space group P-3m1. The Mössbauer spectra of Ni_0.3Fe_0.7Ga₂S₄ at spectra at various temperatures from 4.2 to 300 K showed that the spectrum at 4.2 K has a severely distorted 8-line shape, as spin liquid. Electric quadrupole splitting, E_Q has anomalous twopoints of temperature dependence of E_Q curve as freezing temperature, T_f = 11 K, and Néel temperature, T_N = 26 K. This suggests that there appears to be a slowly-fluctuating “spin gel” state between T_f  and T_N, caused by non-paramagnetic spin state below T_N. This comes from charge re-distribution due to spin-orientation above T_f , and T_N, due to the changing E_Q at various temperatures. Isomer shift value (0.7 mm/s ≤ δ ≤ 0.9 mm/s) shows
that the charge states are ferrous (Fe²⁺), for all temperature range. The Debye temperature for the octahedral site was found to be ΘD = 260 K.