The mixed ligand 3-amino-1,2,4-triazole (Hatz) and terephthalic acid (H₂pta) reacted with Zn(NO₃)₂·6H₂O to synthesize a three-dimensional binuclear Zn(II) metal-organic framework: {[Zn₂·(atz)₂·(pta)]·3H₂O}_n (3D-Zn-MOF). This 3D-Zn-MOF has two different types of pores (4.5 × 4.5 Å², 5.7 × 5.7 Å²). The crystalline 3D-Zn-MOF could be prepared into nanomaterials (3D-N-Zn-MOF) with particles of approximately 100 nm by a cell fragmentation apparatus. Compared with the solid-state luminescence of Hatz and H₂pta, it was found that 3D-N-Zn-MOF exhibited strong luminescence performance and significant red-shift phenomenon. Due to the decrease in electronegativity and rigidity of ligands, as well as the effect of ligand metal charge transfer (LMCT), the fluorescence lifetime and quantum yield of 3D-ZN-N-MOF were 2.7241 ns and 3.02%, respectively. The maximum experimental adsorption capacity of 3D-N-Zn-MOF could reach 125.52 mg/g, which was superior to the majority of MOF adsorbents under the optimal adsorption conditions (25 °C, pH = 7, and the adsorbent concentration is 0.2000 g/L). The thermodynamic analysis of adsorption showed that the adsorption of Cr(VI) by 3D-N-Zn-MOF was a spontaneous (△G < 0) and exothermic (△H < 0) process. It could be found that 3D-N-Zn-MOF was a bifunctional material with potential applications by comprehensive analysis of the fluorescence and adsorption Cr(VI) performance.

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