纳米氨基酸功能化氧化铋团簇在金表面的沉积
Deposition of nanosized amino acid functionalized bismuth oxido clusters on gold surfaces
摘要：
铋化合物在催化、医学和电子学方面的潜在应用越来越受到关注，其环境友好性是其关键因素之一。最常见的起始原料是硝酸铋，它很容易水解产生大量的缩合产物。所谓的次硝酸铋是由不同组成和核的氧化铋簇组成的。然而，阻碍基于氧化铋的材料的进一步开发的一个原因是亚硝酸盐的低溶解度，这使得在基底上的靶向固定具有挑战性。我们提出了一种通过引入氨基羧酸盐作为官能团来溶解氧化铋簇的方法，并研究了这些原子精确的纳米簇在金表面上的生长模式。为此，将氧化铋簇合物[Bi 38 O 45（NO3）20（dmso）28]（NO3）4*4dmso（dmso=二甲基亚砜）与叔丁氧羰基（Boc）保护的苯丙氨酸（Phe）钠盐反应，得到可溶性手性纳米簇合物[Bi 38 O 45（Boc-Phe）24（dmso）9]。基于动态光散射（DLS），估算了簇合物的流体动力学直径，在（1.4-1.6）nm（在CH_3CN中）和（2.2 nm-2.9）nm（在乙醇中）。通过NMR和FTIR以及元素分析（EA）和XPS证明了硝酸盐被氨基羧酸盐完全交换。氧化铋团簇在质子和非质子极性有机溶剂中的溶解度和团簇在金表面上的生长模式进行了研究。通过粉末XRD、FTIR和XPS证明氧化铋簇的成功沉积，同时通过SEM、AFM和光学显微镜研究所得膜的微观结构作为沉积方法和所用溶剂的函数。
英文摘要：
Bismuth compounds are of growing interest with regard to potential applications in catalysis, medicine and electronics, for which their environmentally benign nature is one of the key factors. The most common starting material is bismuth nitrate, which easily hydrolyses to give a large number of condensation products. The so-called bismuth subnitrates are composed of bismuth oxido clusters of varying composition and nuclearity. One reason that hampers the further development of bismuth oxido-based materials, however is the low solubility of the subnitrates, which makes targeted immobilisation on substrates challenging. We present an approach towards solubilisation of bismuth oxido clusters by introducing an amino carboxylate as functional group and a study of the growth mode of these atom-precise nanoclusters on gold surfaces. For this purpose the bismuth oxido cluster [Bi38O45(NO3)20(dmso)28](NO3)4*4dmso (dmso=dimethyl sulfoxide) was reacted with the sodium salt of tert-butyloxycabonyl(Boc)-protected phenylalanine (Phe) to give the soluble and chiral nanocluster [Bi38O45(Boc-Phe)24(dmso)9]. The hydrodynamic diameter of the cluster was estimated with (1.4-1.6) nm (in CH3CN) and (2.2 nm-2.9) nm (in Ethanol) based on dynamic light scattering (DLS). The full exchange of the nitrates by the amino carboxylates was proven by NMR and FTIR as well as elemental analysis (EA) and XPS. The solubility of the bismuth oxido cluster in a protic as well as an aprotic polar organic solvent and the growth mode of the clusters on Au upon spin-, dip-, and drop-coating on gold surfaces were studied. Successful deposition of bismuth oxido cluster was proven by powder XRD, FTIR, and XPS while the microstructure of the resulting films was investigated as a function of the deposition method and the solvent used by SEM, AFM, and optical microscopy.
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