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Synthesis and characterization of the interpenetrated MOF-5

热重分析 金属有机骨架 扫描电子显微镜 吸附 材料科学 粉末衍射 比表面积 分解 化学工程 核化学 化学 结晶学 物理化学 有机化学 复合材料 催化作用 工程类
作者
Bi Chen,Xiu‐Jian Wang,Qian‐Feng Zhang,Xiaoyong Xi,Jingjing Cai,Qi Huang,Si Shi,Jie Wang,Dan Yuan,Min Fang
出处
期刊:Journal of Materials Chemistry [Royal Society of Chemistry]
卷期号:20 (18): 3758-3758 被引量:176
标识
DOI:10.1039/b922528e
摘要

MOF-5 is an important metal–organic framework and has been intensely studied, especially in its hydrogen storage properties. In this study, we obtained the interpenetrated MOF-5 materials (MOF-5-int) using N,N′-dimethylformamide (DMF) or N,N′-diethylformamide (DEF) as solvents. The Langmuir surface area of MOF-5-int determined by N2 adsorption is 950–1100 m2 g−1, much lower than the non-penetrated MOF-5 (3000 m2 g−1). However, it can store 1.54–1.82 wt% by volumetric method hydrogen at 77 K and 1 atm, which is higher than the amount stored by the non-penetrated MOF-5. The MOF-5-int was also characterized by XRD-powder diffraction, thermogravimetric analysis (TGA), nitrogen adsorption/desorption analysis, scanning electron microscope (SEM) and X-ray single-crystal structure diffraction. In addition, we found grinding greatly facilitates the decomposition of the MOF-5-int material by H2O to a nonporous phase ZnBDC·xH2O (within 2–5 min, BDC = 1,4-benzenedicarboxylate), even under low humidity (30%), which calls for careful handling of the MOF-5 material. The effects of the water content, reaction time, reaction temperature, molar ratio of Zn(NO3)2 to H2BDC, addition of H2O2, rapid stirring and dilution on the synthesis of MOF-5-int were studied and the synthetic conditions were optimized. Moreover, Hafizovic et al. (J. Am. Chem. Soc., 2007, 129, 3612) found the intensity ratio of the powder XRD peak at 9.7° to that at 6.8° (referred to as the R1 value) of MOF-5 can be used to predict its porosity. The lower the intensity ratio, the more porous it is. In this study, we showed that MOF-5-int can have a very low R1 value but also a low porosity. The low specific surface area (SSA) is mainly due to its interpenetrated structure instead of the entrapped zinc species or the mesopores in the material, as previously proposed in the literature, and associated with the characteristic, very strong peak at 13.8° in its XRD-powder diffraction pattern. A high R2 value (the ratio of the intensity of the peak at 13.8° to that at 6.8°) suggests an interpenetrated structure, especially when the R1 value is low. In addition, we found that although entrapped ZnO or solvent molecules can increase the R1 value, and a low R1 value implies no zinc species or solvent molecules entrapped in the MOF-5 framework, a high R1 value does not necessarily suggest the presence of entrapped molecules.
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