We herein demonstrate the intercalation of several organic benzenepolycarboxylic compounds, terephthalic acid (TC), 1,3,5-benzenetricarboxylic acid (BTC) and 1,2,4,5-benzenetetracarboxylic acid (BTCC), into the layered terbium hydroxide (LTbH) and the sensitized luminescence of these organic species for the layer Tb 3+. All of the as-prepared products demonstrated characteristic XRD diffractions attributed to layered materials. Compared with the NO 3-LTbH precursor, efficient energy transfer from intercalated organic anions to Tb 3+ centers in LTbH layers took place, thus markedly enhancing the Tb 3+ luminescence. The relationship between the triplet energy levels of the organic guests and the energy level of Tb 3+ was analyzed to explain the sensitization effect and energy transfer from the gallery sensitizers to the layer Tb 3+ ions. The fluorescence lifetimes of NO 3-LTbH, TC-LTbH, BTC-LTbH and BTCC-LTbH were determined to be 0.131, 0.315, 0.579 and 0.642 ms, respectively, indicating significantly increased lifetimes of the LTbH composites intercalated with the organic species.