Department of Materials Science and Technology, University of Crete , Heraklion 71003, Crete, Greece.
J Am Chem Soc. 2015 Nov 4;137(43):13943-8. doi: 10.1021/jacs.5b09110. Epub 2015 Oct 22.
We report the synthesis of ion-exchangeable molybdenum sulfide chalcogel through an oxidative coupling process, using (NH4)2MoS4 and iodine. After supercritical drying, the MoS(x) amorphous aerogel shows a large surface area up to 370 m(2)/g with a broad range of pore sizes. X-ray photoelectron spectroscopic and pair distribution function analyses reveal that Mo(6+) species undergo reduction during network assembly to produce Mo(4+)-containing species where the chalcogel network consists of [Mo3S13] building blocks comprising triangular Mo metal clusters and S2(2-) units. The optical band gap of the brown-black chalcogel is ∼1.36 eV. The ammonium sites present in the molybdenum sulfide chalcogel network are ion-exchangeable with K(+) and Cs(+) ions. The molybdenum sulfide aerogel exhibits high adsorption selectivities for CO2 and C2H6 over H2 and CH4. The aerogel also possesses high affinity for iodine and mercury.
我们通过氧化偶联过程报告了离子交换型硫化钼杂化凝胶的合成，使用(NH4)2MoS4和碘。经过超临界干燥后，MoS(x)非晶态气凝胶表现出高达 370 m2/g 的大表面积和宽范围的孔径。X 射线光电子能谱和配对分布函数分析表明，Mo(6+)物种在网络组装过程中经历还原，生成含有 Mo(4+)的物种，其中杂化凝胶网络由包含三角形 Mo 金属簇和 S2(2-)单元的[Mo3S13]构建块组成。棕色-黑色杂化凝胶的光学带隙约为 1.36 eV。存在于钼硫化物杂化凝胶网络中的铵位点可与 K(+)和 Cs(+)离子进行离子交换。钼硫化物气凝胶对 CO2 和 C2H6 相对于 H2 和 CH4 表现出高吸附选择性。气凝胶对碘和汞也具有高亲和力。
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