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New Nd³⁺-doped cadmium molybdato-tungstates with the chemical formula of Cd_{1−3<i>x</i>}▯_xNd_2<i>x</i>(MoO₄)_{1−3<i>x</i>}(WO₄)_3<i>x</i> (where <i>x</i> = 0.0283, 0.0455, 0.0839, 0.1430, 0.1875, 0.2000, 0.2500, and ▯ denotes a vacant site in the crystal lattice) were successfully synthesized by the high-temperature solid state reaction method, using CdMoO₄ and Nd₂(WO₄)₃ as the initial reactants. The structure and change in their lattice parameters as a function of Nd³⁺ ion concentration were investigated by the XRD (X-ray diffraction) method. The surface morphology and grain size of the doped materials were characterized by SEM (scanning electron microscopy). Their thermal properties and initial reactants were analyzed by DTA-TG (differential thermal analysis coupled with thermogravimetry) techniques. The optical properties of the Nd³⁺-doped cadmium molybdato-tungstates, such as optical band gap, were determined by UV–vis–NIR (ultraviolet–visible–near infrared) spectroscopy. The EPR (electron paramagnetic resonance) technique provided information on the type of magnetic interactions between Nd³⁺ ions.