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.