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Two new terbium-based metal–organic frameworks, {[Tb(ADBA)(CH3COO)(H2O)]·H2O}n(MOF 1) and [Tb(ADBA)(HCOO)(DMF)]n(MOF 2) (H2ADBA = 4,4′-(9,10-anthracenediyl) benzoic acid), were synthesized by the solvothermal method. Structural analysis indicates that the TbIIIions in MOFs 1and 2are coordinated to acetic and formic acids, respectively, leading to differences in the structures. Fluorescence measurements show that both MOFs 1and 2are fluorescence sensors for Al3+and Ga3+with fluorescence enhancement and a blue shift. The detection limits of MOF 1are 0.067 μM for Al3+and 0.093 μM for Ga3+, and the detection limits of MOF 2are 0.064 for Al3+and 0.086 μM for Ga3+. The proton conductivity measurements of MOFs 1and 2indicate that the proton conductivities of MOFs 1and 2increase in resistance with increasing humidity. MOF 1is more sensitive to humidity with a maximum conductivity of 1.07 × 10–5S·cm–1under 40 °C and 98% RH. Therefore, MOFs 1and 2are potential multifunctional MOF materials.