HUO Jia, WANG Li, YU Hao-Jie, FAN Deng-Sen. SYNTHESIS AND CHARACTERIZATION OF MANGANESE-BASED FERROCENYL COORDINATION POLYMER MICROSPHERES[J]. Acta Polymerica Sinica, 2011,(9):1033-1039.
HUO Jia, WANG Li, YU Hao-Jie, FAN Deng-Sen. SYNTHESIS AND CHARACTERIZATION OF MANGANESE-BASED FERROCENYL COORDINATION POLYMER MICROSPHERES[J]. Acta Polymerica Sinica, 2011,(9):1033-1039. DOI: 10.3724/SP.J.1105.2011.10356.
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 m to 9.4 m; on the contrary
the increase of reagent concentration decreased the size of particles from 11.4 m to 9.4 m 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℃.