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As a typical Aurivillius-type compound, CaBi4Ti4O15 (CBT) is considered a strong competitor among high-temperature piezoelectric materials, but it is difficult to achieve both high piezoelectric activity and a high Curie temperature for CBT. In this work, the method of double-ion co-substituting at different crystalline sites was used to modify the electrical properties of CBT. The Gd/Mn co-doped CBT ceramics with the chemical formula of Ca1−xGdxBi4Ti4O15+0.2 wt% MnO2 (CBT–100xGM, x = 0–0.11) were prepared via the conventional sintering process. The phase and valence band structures, chemical compositions and microstructures, dielectric and ferroelectric properties, electrical conduction behaviors, and electroelastic and piezoelectric properties of the ceramics were characterized. The doping concentration effects of Gd3+ were analyzed according to the composition-dependent structures and properties of CBT–100xGM. The donor substitution of Gd3+ for Ca2+ at the A-site reduced the tolerance factor of the perovskite-like structure and decreased the concentration of intrinsic oxygen vacancies. While Mn3+ tended to substitute for Ti4+ at the B-site, the extrinsic oxygen vacancies are limited near the defect center of Ti(Mn) because of the formation of (
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