Microporous and Mesoporous Materials ( IF 4.8 ) Pub Date : 2019-11-09 , DOI: 10.1016/j.micromeso.2019.109882 Riccardo Fantini , Rossella Arletti , Simona Quartieri , Marco Fabbiani , Sara Morandi , Gianmario Martra , Francesco Di Renzo , Giovanna Vezzalini
This work studies the thermal stability, heat-induced structural deformations, and dehydration/rehydration dynamics of a synthetic high silica mordenite. It is of special interest because this particular phase has proven to be an ideal host for the encapsulation of several kinds of organic molecules making it a promising scaffold for drug delivery. The dehydration process was followed by thermal analysis, infrared spectroscopy in controlled atmosphere, in situ synchrotron XRPD, and structural refinement. Overall, all the results indicate weak interactions of H2O molecules with the silicatic mordenite framework and evidence the presence of hydroxyl groups with different condensation responses at high temperature. Infrared characterization highlighted how the desorption of adsorbed H2O molecules under degassing is already complete at rT. The unit cell parameters exhibit very slow and almost isotropic changes upon heating. Above 550 °C an increase in slope is observed for all parameters. This corresponds to the marked silanol condensation and consequent framework reassessment observed at this temperature by infrared characterization. Overall cell contractions are 0.67%, 1.18%, and 0.81% for a, b, c, respectively and 2.64% for cell volume. HS-MOR undergoes very moderate T induced deformations, indicating a very rigid and stable framework.
中文翻译:
高二氧化硅丝光沸石的热行为
这项工作研究了合成高二氧化硅丝光沸石的热稳定性,热诱导的结构变形以及脱水/再水化动力学。它具有特殊的意义,因为该特定相已被证明是封装多种有机分子的理想宿主,这使其成为有希望的药物递送支架。脱水过程之后进行热分析,受控气氛中的红外光谱,原位同步加速器XRPD和结构改进。总的来说,所有结果表明H 2 O分子与硅胶丝光沸石骨架之间的相互作用较弱,并证明了在高温下存在具有不同缩合反应的羟基。红外表征突出了吸附的H 2的解吸脱气下的O分子在r T处已经完成。晶胞参数在加热时表现出非常缓慢且几乎各向同性的变化。高于550°C,所有参数的斜率都会增加。这对应于在该温度下通过红外表征观察到的显着的硅烷醇缩合和随后的骨架重新评估。对于a,b,c,总的细胞收缩率分别为0.67%,1.18%和0.81%,而细胞体积的总收缩率则为2.64%。HS-MOR经历非常适度的T诱导变形,表明框架非常刚性和稳定。