State Key Laboratory of Fine Chemicals, PSU-DUT Joint Center for Energy Research, School of Chemical Engineering, Dalian University of Technology, Dalian 116024, PR China.
Dalton Trans. 2013 Oct 7;42(37):13698-705. doi: 10.1039/c3dt51322j. Epub 2013 Aug 1.
We present here a simple solvothermal method to fabricate metal-organic framework NH2-MIL-53(Al) crystals with controllable size and morphology just by altering the ratio of water in the DMF-water mixed solvent system without the addition of any surfactants or capping agents. With increasing the volume ratio of water in the mixed solvents, a series of NH2-MIL-53(Al) crystals with different sizes and morphologies were synthesized. The average size of the smallest crystal is 76 ± 20 nm, which provides us a simple and environmentally friendly way to prepare nanoscale MOFs. The largest BET surface area of these samples is 1882 m(2) g(-1) that is mainly contributed by its micropore surface area, and its corresponding micropore volume is 0.83 cm(3) g(-1), which have greatly extended its application in the fields of gas adsorption and postsynthetic modification. All these samples were characterized by SEM, XRD, N2 adsorption/desorption, TGA and FT-IR. Then a mechanism for the impact of the water ratio on the crystal size and morphology is presented and discussed.
我们在此提出一种简单的溶剂热方法,通过改变混合溶剂中(DMF-水)水的比例,无需添加任何表面活性剂或封端剂,即可制备具有可控尺寸和形貌的金属有机骨架 NH2-MIL-53(Al)晶体。随着混合溶剂中水体积比的增加,我们合成了一系列具有不同尺寸和形貌的 NH2-MIL-53(Al)晶体。最小晶体的平均尺寸为 76 ± 20nm,这为我们提供了一种简单且环保的方法来制备纳米级 MOFs。这些样品的最大 BET 比表面积为 1882m2g-1,主要由其微孔表面积贡献,相应的微孔体积为 0.83cm3g-1,这极大地扩展了其在气体吸附和后合成修饰领域的应用。所有这些样品都通过 SEM、XRD、N2 吸附/解吸、TGA 和 FT-IR 进行了表征。然后提出并讨论了水比对晶体尺寸和形貌的影响机制。