锰-二茂铁基配位聚合物微球的制备与表征

采用溶剂热法制得了一系列锰-二茂铁基配位聚合物微球,系统研究了反应时间、反应物浓度等因素对配位聚合物微球的形貌和尺寸的影响规律,采用SEM、TEM、PXRD、EDX和FTIR等方法研究了微球的形貌、尺寸和结构等.发现通过调节反应时间,可使微球的尺寸约在4 ～9 μm范围内变化,提高反应物浓度可使微球从光滑的球形结构向核...

SYNTHESIS AND CHARACTERIZATION OF MANGANESEBASED FERROCENYL COORDINATION POLYMER MICROSPHERES

A series of manganese-based ferrocenyl coordination polymer microspheres were prepared by solvothermal reactions,the influence of reaction time and reagent concentration on the morphology and diameters of microspheres was investigated systematically,and the morphology,diameters and crystal structure of manganese-based ferrocenyl coordination polymer microspheres were characterized by scanning electron microscopy(SEM),transmission electron microscopy(TEM),powder X-ray diffraction(PXRD),energy dispersive X-ray spectrometry(EDX) and Fourier-transform infrared spectroscopy(FT-IR).By adjusting the reaction time from 8 h,12 h to 24 h,the diameters of microspheres increased from 4 μm to 9.4 μm;on the contrary,the increase of reagent concentration decreased the size of particles from 11.4 μm to 9.4 μm at the tested range,and,at the same time,spheres were transformed from smooth spherical structures into core-shell structures.PXRD showed that manganese-based ferrocenyl coordination polymers crystallized into sandwich layered crystal structure with the possible formula of Mn4(OH)4(OOCC5H4FeC5H4COO)2.Within the framework,two kinds of different manganese atoms in a distorted octahedral geometry were incorporated into the layers and the ferocenedicarboxylato group existed as a synperiplanar conformation and tridentate-bridging mode connecting three manganese atoms.Manganese atoms were connected with oxygen atoms to form a two-dimensional inner layer with the ferrocenyl groups arranged along two sides of the inner layer,thus forming the sandwich-like coordination polymers.EDX indicated the microspheres contained Mn,Fe,C and O,and C-O stretching frequency shifting from 1687 cm-1 for the precursor to 1581.7 cm-1 for the product from FT-IR spectra confirmed the formation of coordination polymer.TGA showed the coordination polymer microspheres had good thermal stability up to at least 319℃.