Conversion of N ‐Methylpolyborosilzane to Amorphous Siliconboroncarbonitride The amorphous ceramic ‘SiBN3C' has been synthesized starting from 1,1‐dichloro‐N‐(trichlorosilyl)‐boranamine (TADB) with N‐methylpolyborosilazane as a polymeric intermediate. On heating the ceramic up to 1900 °C no microstructural changes occur. The thermal conversion of the preceramic polymer was investigated by thermal analysis, infrared spectroscopy and nuclear magnetic resonance spectroscopy. Surprisingly, the pyrolysis proceeds in three clearly divided steps which can be assigned to completion of the polycondensation (200–350 °C), fragmentation (580–620 °C) and elimination of residual hydrogen (1000–1400 °C). 相似文献
Zirconium carbide (ZrC) was synthesized from inorganic–organic hybrid precursor’s pyrolysis by solution-based processing. Zirconium-containing complexes, which were obtained by chelation of oxide bidentate ligands to zirconium, were used to combine with phenolic resin to form precursors for ZrC. The precursors using specific ligands including acetylacetone, ethyleneglycol, and salicylic acid transformed into pure ZrC at a relatively low temperature (1,550 °C) in addition to that using lactic acid. As a comparison, synthesis of ZrC only using zirconium oxychloride octahydrate (ZrOCl2·8H2O) and phenolic resin was also conducted. The synthesized powders had a small average crystallite size (~300 nm), and a low oxygen content (~2.5 at.%). The conversions from as-synthesized preceramic precursors to ceramics were studied by means of FTIR, SEM, EDS, XRD, and XPS. The oxidation behavior of the synthesized ZrC in air was studied by DSC-TG analysis. 相似文献
Solid composite polymer electrolytes consisting of polyethylene oxide (PEO), LiClO4, and porous inorganic–organic hybrid poly (cyclotriphosphazene-co-4, 4′-sulfonyldiphenol) (PZS) nanotubes were prepared using the solvent casting method. Differential scanning calorimetry
and scanning electron microscopy were used to determine the characteristics of the composite polymer electrolytes. The ionic
conductivity, lithium ion transference number, and electrochemical stability window can be enhanced after the addition of
PZS nanotubes. The electrochemical impedance showed that the conductivity was improved significantly. Maximum ionic conductivity
values of 1.5 × 10−5 S cm−1 at ambient temperature and 7.8 × 10−4 S cm−1 at 80 °C were obtained with 10 wt.% content of PZS nanotubes, and the lithium ion transference number was 0.35. The good
electrochemical properties of the solid-state composite polymer electrolytes suggested that the porous inorganic–organic hybrid
polyphosphazene nanotubes had a promising use as fillers in SPEs and the PEO10–LiClO4–PZS nanotube solid composite polymer electrolyte might be used as a candidate material for lithium polymer batteries. 相似文献
Fully crosslinked, stable poly[cyclotriphosphazene‐co‐(4,4′‐sulfonyldiphenol)] (PZS) microspheres have been prepared via the polycondensation between hexachlorocyclotriphosphazene and 4,4′‐sulfonyldiphenol by precipitation polymerization. The diameter of the PZS microspheres ranged from 0.6 to 1.0 µm with the specific surface area of the microspheres ranging from 11.7 to 10.1 m2 · g?1. The formation of the non‐porous microspheres was observed to obey an oligomeric species absorbing mechanism. The fully crosslinked chemical structure of the PZS microspheres were determined by IR, CP/MAS NMR, XRD, and EDX. No glass‐transition temperature was observed and the onset of the thermal‐degradation temperature was 542 °C. Thermal stability of the PZS microspheres by the precipitation polycondensation was significantly improved as compared with crosslinked microspheres produced by addition polymerizations.
The phenylmethacrylamide monomer, 1‐(4‐methacrylamidophenyl)‐1‐(4‐nitrophenyl)prop‐1‐en‐3‐one (MPNP) containing a photosensitive group was synthesized by reacting 4‐nitrocinnamoylaniline with methacryloyl chloride in the presence of triethylamine at 0–5°C. The functional monomer, MPNP was polymerized in ethyl methyl ketone (EMK) under nitrogen atmosphere at 70°C using benzoyl peroxide (BPO) as the initiator. The synthesized polymer was characterized by UV, IR, 1H‐NMR and 13C‐NMR spectroscopy. The molecular weight data of the polymer as obtained from gel permeation chromatography suggests a higher tendency for chain termination by radical recombination than disproportionation. The thermal studies of the polymer were obtained from thermogravimetric analysis. The glass transition temperature of the polymer was determined by differential scanning calorimetry. The solubility of the polymer was tested in various organic solvents at room temperature. The photosensitivity of the polymer was investigated in various solvents in the presence and absence of triplet photosensitizers. The effect of the different solvents nature and concentration on the rate of photocrosslinking of the polymer were also examined for using the polymer as negative photoresist materials. 相似文献
Allyl methacrylate was polymerized in CCl4 solution by α,α′‐azoisobutyronitrile at 50, 60, and 70°C. The kinetic curves were auto‐accelarated types at 60 and 70°C, but almost linear at 50°C. Arrhenius activation energy was 77.5 kJ/mol. The polymer was insoluble in common organic solvents. It was characterized by FT‐IR, NMR, DSC, TGA and XPS methods. About 98–99% of allyl side groups were remained as pendant even after completion of the polymerization. The spectroscopic and thermal results showed that polymerization is not a cyclopolymerization type, but may have end group cyclization. The high molecular weight is the main cause of a polymer being insoluble even in the early stage of the polymerization. Molecular weight of 1.1×106 for a soluble polymer fraction was measured by light scattering method. The Tg of polymer was 94°C, and after curing at 150–200°C, increased to 211°C. The thermal pyrolysis of polymer at about 350°C gave an anhydride by linkage type degradation, and side group cyclization. The XPS analysis showed the presence of radical fragments of AIBN (initiator) and CCl4 (solvent) associated with oligomers. 相似文献
New methacrylic monomer having free radical polymerizable methacryloyl group and photocrosslinkable functional group was synthesized by reacting hydroxyl chalcone with methacryloyl chloride. The monomer was homopolymerized in methyl ethyl ketone solvent using benzoyl peroxide as an initiator at 70°C. The prepared homopolymer was characterized by UV, FT‐IR, 1H‐NMR and 13C‐NMR spectra. The molecular weights (Mw and Mn) were estimated by gel permeation chromatography. The thermal stability of the polymer was measured by thermogravimetric analysis. The glass transition temperature of the polymer was determined by differential scanning calorimetry. The photocrosslinking property of the polymer was also studied. 相似文献