The objective of this study was to demonstrate the potential utilization of fly ash (FA), wood ash (WA), and metakaolin (MK) in developing new alkali-activated materials (AAMs) for the removal of cadmium ions from waste water. The synthesis of AAMs involved the dissolution of solid precursors, FA, WA, and MK, by a liquid activator (Na₂SiO₃ and NaOH). In concentrated solutions of the activator, the formation of an aluminosilicate gel structure occurred. DRIFT spectroscopy of the AAMs indicated main vibration bands between 1036 cm⁻¹ and 996 cm⁻¹, corresponding to Si-O-Si/Si-O-Al bands. Shifting vibration bands were seen at 1028 cm⁻¹ to 1021 cm⁻¹, indicating that the Si-O-Si/Si-O-Al bond is elongating, and the bond angle is decreasing. Based on the X-ray diffraction results, alkali-activated samples consist of an amorphous phase and residual mineral phases. The characteristic “hump” of an amorphous phase in the range from 20 to 40° 2θ was observed in FA and in all AWAFA samples. By the XRD patterns of the AAMs obtained by the activation of a solid three-component system, a new crystalline phase, gehlenite, was identified. The efficiency of AAMs in removing cadmium ions from aqueous solutions was tested under various conditions. The highest values of adsorption capacity, 64.76 mg/g (AWAFA₆), 67.02 mg/g (AWAFAMK₆), and 72.84 mg/g mg/g (AWAMK₆), were obtained for materials activated with a 6 M NaOH solution in the alkali activator. The Langmuir adsorption isotherm and pseudo-second kinetic order provided the best fit for all investigated AAMs.