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A benzophenone-bearing acid oligodimethacrylate and its application to the preparation of silver/gold nanoparticles/polymer nanocomposites

机译:含苯甲酮的酸低聚二甲基丙烯酸酯及其在制备银/金纳米颗粒/聚合物纳米复合材料中的应用

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The synthesis of photosensitive urethane dimethacrylate that contains poly(ethylene oxide) sequence (PEG, M_w: 400), carboxylic and benzophenone moieties, and its characterization by specific methods (~1H and ~(13)C NMR, FTIR, UV and electrospray ionization-mass spectroscopy) are reported. UV curing parameters of this macromer (BP-UDMA) alone and in monomer combinations was evaluated through FTIR spectroscopy and photo-differential scanning calorimetry using 1 wt% 4-(dimethylamino) phenylacetic acid as co-initiator or Irgacure 819 (Irg819). The results show that the photopolymerization rates of the BP-UDMA are higher in the case of Irg819 (R _(max) ~P: 0.108 s~(-1)) due to its synergic action, whereas the degree of conversion of C=C double bond (DC, after 120 s of UV irradiation) is over 77 %. When other co-monomers (non-acid urethane dimethacrylate and silyl urea methacrylate) are incorporated into the formulation, the photopolymerization rate (0.095-0.132 s~(-1)) and DC (84.59-79.69 %) varied in reasonable limits. Depending of the photoinitiator type, as well as the monomer composition, the addition of 0.5, 1 and 3 wt% noble metal precursors (AgNO_3 and AuBr_3) led to the formation of hybrid composites with in situ-synthesized nanoparticles (NPs), where the variations in the intensity of the surface plasmon absorption bands appeared in the range 400-456 nm (Silver) or 500-553 nm (Gold), better results being obtained in the first initiating system. Homogeneous dispersion of nanoparticles into the polymer matrix was evidenced by EDX and TEM analysis, the last proving the existence of nanoparticles with sizes around 10 nm and variable morphologies. X-ray diffraction analysis complemented these results.
机译:包含聚(环氧乙烷)序列(PEG,M_w:400),羧基和二苯甲酮部分的光敏氨基甲酸酯二甲基丙烯酸酯的合成及其通过特定方法进行表征(〜1H和〜(13)C NMR,FTIR,UV和电喷雾电离-质谱法)。使用1 wt%的4-(二甲氨基)苯乙酸作为共引发剂或Irgacure 819(Irg819),通过FTIR光谱和光差扫描量热法评估了这种大分子单体(BP-UDMA)的紫外固化参数。结果表明,由于Irg819的协同作用,BP-UDMA的光聚合速率较高(R _(max)〜P:0.108 s〜(-1)),而C = C双键(DC,UV照射120 s后)超过77%。当将其他共聚单体(非酸性氨基甲酸酯二甲基丙烯酸酯和甲基丙烯酸甲硅烷基脲)掺入配方时,光聚合速率(0.095-0.132 s〜(-1))和DC(84.59-79.69%)在合理的范围内变化。根据光引发剂类型以及单体组成的不同,添加0.5、1和3 wt%的贵金属前体(AgNO_3和AuBr_3)导致形成具有原位合成纳米颗粒(NPs)的杂化复合材料。在400-456 nm(银)或500-553 nm(金)范围内,表面等离激元吸收带的强度发生了变化,在第一个启动系统中获得了更好的结果。通过EDX和TEM分析证明了纳米颗粒均匀分散在聚合物基质中,最后证明了存在尺寸约10 nm的纳米颗粒和形态可变的纳米颗粒。 X射线衍射分析补充了这些结果。

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