The measurement of proton-enhanced carbon-13 T1 values by a method which suppresses artifacts

结晶度 无定形固体 聚合物 材料科学 催化作用 质子化 碳-13核磁共振 聚乙烯 化学 化学工程 结晶学 有机化学 复合材料 工程类 离子
作者
Dennis A. Torchia
出处
期刊:Journal of magnetic resonance [Elsevier]
卷期号:30 (3): 613-616 被引量:709
标识
DOI:10.1016/0022-2364(78)90288-3
摘要

In this study, polyethylene terephthalate (PET) textiles were metallized with Pt via supercritical carbon dioxide (sc-CO2) catalyzation, using palladium(II) hexafluoroacetylacetonate (Pd(hfac)2) as the Pd catalyst source. The effects of the treatments on the structural changes and molecular mobility of PET were elucidated by solid-state 13C nuclear magnetic resonance (NMR) spectroscopy. The carbonyl and nonprotonated aromatic carbons and the methylene and protonated aromatic carbons were analyzed from the NMR spectra using a three-component model (crystalline, rigid amorphous, and mobile amorphous components), which inferred that the PET polymer textile comprised one crystalline and two amorphous regions. Additionally, when Pd catalyzation was performed on the textile under sc-CO2 conditions, the crystalline peak of the carbonyl carbon exhibited a chemical shift into a higher magnetic field, and the spin–lattice relaxation time increased. These results implied that Pd could exist in the vicinity of the CO carbon. The X-ray diffraction studies also showed crystallinity of PET increased by sc-CO2 catalyzation, while sc-CO2 annealing without Pd(hfac)2 did not increase it. Therefore, Pt films were successfully coated on the PET via catalytic plating using sc-CO2. The catalyzation reduced the molecular mobility of the PET polymer, indicating the incorporation of the catalytic metal into the polymer chain. The carbonyl carbon peak simultaneously shifted to a higher field, implying that the catalytic Pd could approach the carbonyl groups. The detailed analysis of the structure and molecular mobility provides valuable information that can contribute to the development of novel conductive materials.
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