An efficient and metal-free oxidative method was reported for synthesis of triply linked diporphyrins with 2.5 equiv of phenyliodine bis(trifluoroacetate) (PIFA). This reaction showed high selectivity for Zn(II) porphyrins and had been successfully applied in the synthesis of a novel triply-singly interlacedly linked porphyrin array with lower energy gap.
The modification before the stabilization process could tune the exothermic behavior and the structural evolution of PAN fibers during stabilization. In this study, we demonstrate that a rapid thermal pretreatment in nitrogen can effectively mitigate the exothermic behavior of PAN fibers, such as decreasing the initial temperature, broadening the exothermal peak, and decreasing the nominal heat release during heating the fibers in air. The color of fibers has shown gradual changes from white to light yellow, yellow and brown during thermal pretreatment in nitrogen with the increase of pretreating temperature and time. The differential scanning calorimetry (DSC), Fourier Transform Infrared Spectrometer (FTIR), X-ray diffraction (XRD), and Thermogravimetric Analysis (TG) characterization have been applied to analyze the thermal properties, chemical and physical structural difference between PAN, and thermally pretreated PAN fibers. The thermal pretreatment of PAN fibers in nitrogen could induce cyclization, dehydrogenation, and cross-linking reactions, in which the cyclization play an important role on improving the cyclization index of stabilized PAN fibers. Meanwhile, the pretreatment can result in noticeable changes of the aggregation structure of PAN fibers, as indicated by the increase of crystallinity and crystalline size. These structural modifications can benefit the main cyclization reaction during stabilization and enhance the carbon yield in resultant carbon fibers. The rapid thermal pretreatment in nitrogen could increase efficiency of modification on PAN fibers, and that could save much time and energy. It is beneficial to manufacture low-cost carbon fibers and to spread the applications of carbon fibers.
We have annealed Ge28.125Ga6.25S65.625 glasses doped with 0.5% Dy to create glass-ceramics in order to examine the local chemical environment of the rare earth ions (REI). More than 12 times enhancement of the emission at 2.9 and 3.5 μm was achieved in glass-ceramics produced using prolonged annealing time. Elemental mapping showed clear evidence that Ga2S3 crystalline grains with a size of 50 nm were dispersed in a Ge-S glass matrix in the glass-ceramics, and the REI could only be found near the Ga2S3 crystalline grains. From the unchanged lineshape of the emissions at 2.9 and 3.5 μm and lack of splitting of the absorption peaks, we concluded that the REI were bonded to Ga on the surface of the Ga2S3 crystals.
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