Sterczyńska Angelina, Śliwińska-Bartkowiak Małgorzata, Zienkiewicz-Strzałka Małgorzata, Deryło-Marczewska Anna
Faculty of Physics, Adam Mickiewicz University.
Faculty of Physics, Adam Mickiewicz University; NanoBioMedical Centre;
J Vis Exp. 2019 Mar 27(145). doi: 10.3791/58395.
In this work, we report the synthesis and characterization of ordered nanoporous carbon material (also called ordered mesoporous carbon material [OMC]) with a 4.6 nm pore size, and ordered silica porous matrix, SBA-15, with a 5.3 nm pore size. This work describes the surface properties of nanoporous molecular sieves, their wettability, and the melting behavior of D2O confined in the differently ordered porous materials with similar pore sizes. For this purpose, OMC and SBA-15 with highly ordered nanoporous structures are synthesized via impregnation of the silica matrix by applying a carbon precursor and by the sol-gel method, respectively. The porous structure of investigated systems is characterized by an N2 adsorption-desorption analysis at 77 K. To determine the electrochemical character of the surface of synthesized materials, potentiometric titration measurements are conducted; the obtained results for OMC shows a significant pHpzc shift toward the higher values of pH, relative to SBA-15. This suggests that investigated OMC has surface properties related to oxygen-based functional groups. To describe the surface properties of the materials, the contact angles of liquids penetrating the studied porous beds are also determined. The capillary rise method has confirmed the increased wettability of the silica walls relative to the carbon walls and an influence of the pore roughness on the fluid/wall interactions, which is much more pronounced for silica than for carbon mesopores. We have also studied the melting behavior of D2O confined in OMC and SBA-15 by applying the dielectric method. The results show that the depression of the melting temperature of D2O in the pores of OMC is about 15 K higher relative to the depression of the melting temperature in SBA-15 pores with a comparable 5 nm size. This is caused by the influence of adsorbate/adsorbent interactions of the studied matrices.
在本研究中,我们报道了孔径为4.6 nm的有序纳米多孔碳材料(也称为有序介孔碳材料[OMC])以及孔径为5.3 nm的有序二氧化硅多孔基质SBA - 15的合成与表征。本工作描述了纳米多孔分子筛的表面性质、它们的润湿性以及限制在具有相似孔径的不同有序多孔材料中的D2O的熔化行为。为此,通过分别应用碳前驱体浸渍二氧化硅基质和采用溶胶 - 凝胶法,合成了具有高度有序纳米多孔结构的OMC和SBA - 15。通过在77 K下进行N2吸附 - 脱附分析来表征所研究体系的多孔结构。为了确定合成材料表面的电化学特性,进行了电位滴定测量;相对于SBA - 15,OMC的测量结果显示其零电荷点pH(pHpzc)显著向更高的pH值偏移。这表明所研究的OMC具有与氧基官能团相关的表面性质。为了描述材料的表面性质,还测定了渗透到所研究多孔床中的液体的接触角。毛细管上升法证实了二氧化硅壁相对于碳壁润湿性的增加以及孔隙粗糙度对流体/壁相互作用的影响,这在二氧化硅中比在碳介孔中更为明显。我们还通过介电方法研究了限制在OMC和SBA - 15中的D2O的熔化行为。结果表明,相对于具有可比5 nm尺寸的SBA - 15孔中熔化温度的降低,OMC孔中D2O熔化温度的降低约高15 K。这是由所研究基质的吸附质/吸附剂相互作用的影响引起的。