CAJ | 학술논문

以溶胶-凝胶伴随相分离法制备的阶层多孔二氧化硅作为载体,3-氨丙基三乙氧基硅烷(APTES)为改性剂,乙醇为还原剂,在阶层多孔二氧化硅固体骨架上进行银纳米颗粒均匀负载。利用扫描电镜(SEM)、透射电镜(TEM)、X射线衍射(XRD)、汞压、N2吸附/脱附、X射线光电子能谱(XPS)等测试技术对银纳米颗粒负载阶层多孔二氧化硅进行了表征,探讨了APTES表面改性、乙醇还原机理以及银纳米颗粒负载块体的孔结构特征变化规律。结果表明：APTES表面改性将氨基接枝于阶层骨架上,氨基与银离子形成银氨离子,银氨离子经乙醇还原后将平均粒径约16 nm的银纳米颗粒成功负载于二氧化硅的大孔及介孔内部；负载后的阶层多孔块体的大孔骨架未受到破坏,但其比表面积由418 m2?g-1下降到254 m2?g-1,两次还原负载能提高银纳米颗粒的负载量。
이용효-응효반수상분리법제비적계층다공이양화규작위재체,3-안병기삼을양기규완(APTES)위개성제,을순위환원제,재계층다공이양화규고체골가상진행은납미과립균균부재。이용소묘전경(SEM)、투사전경(TEM)、X사선연사(XRD)、홍압、N2흡부/탈부、X사선광전자능보(XPS)등측시기술대은납미과립부재계층다공이양화규진행료표정,탐토료APTES표면개성、을순환원궤리이급은납미과립부재괴체적공결구특정변화규률。결과표명：APTES표면개성장안기접지우계층골가상,안기여은리자형성은안리자,은안리자경을순환원후장평균립경약16 nm적은납미과립성공부재우이양화규적대공급개공내부；부재후적계층다공괴체적대공골가미수도파배,단기비표면적유418 m2?g-1하강도254 m2?g-1,량차환원부재능제고은납미과립적부재량。
Ag nanoparticles (NPs) were uniformly immobilized in hierarchical y porous monolithic silica using γ-(aminopropyl)triethoxysilane (APTES) as a modifier and ethanol as a reductant, where the silica monolith was pre-prepared via the sol-gel accompanied by phase separation. Ag NPs embedded in the hierarchical y porous silica monoliths were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), mercury porosimetry, nitrogen adsorption/desorption analysis, and X-ray photoelectron spectroscopy (XPS). The mechanism of the modification by APTES, the reduction using ethanol, and pore structure changes of the silica monolith after immobilization of Ag NPs are discussed. The results show that APTES modifies the monolith by incorporating amino groups onto the surface of the meso-macroporous skeletons, and then amino groups react with silver ions to form a silver-amine complex. Ethanol used as an effective reductant is adopted to promote the reduction process of the silver-amine complex. Ag NPs with an average size of approximately 16 nm were homogeneously supported on both the macroporous skeletons and in the mesopores of the silica monolith with good dispersion. The embedding of Ag NPs did not spoil the macroporous skeleton of the monolithic silica, and the surface area decreased from 418 to 254 m2?g-1 after introducing Ag NPs into its macro-mesopores. It was also found that the loading amount of Ag NPs increased with repeated modification and reduction treatments.