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水热微乳液法合成氧化稳定性良好的钴纳米晶,其表面被包覆有表面活性剂/聚合物复合壳。

Hydrothermal microemulsion synthesis of oxidatively stable cobalt nanocrystals encapsulated in surfactant/polymer complex shells.

机构信息

Department of Applied Biology and Chemical Technology, The Hong Kong Polytechnic University, Hung Hom, Kowloon, Hong Kong, PR China.

出版信息

Langmuir. 2010 Apr 20;26(8):6009-14. doi: 10.1021/la9045918.

Abstract

Air-stable magnetic cobalt nanocrystals have been conveniently prepared via a reverse micellar synthesis, followed by a hydrothermal treatment. The synthesis was carried out by first mixing an aqueous solution containing cobalt chloride and poly(sodium 4-styrenesulfonate) (PSS) with an organic mixture containing cetyltrimethylammonium bromide (CTAB) to form reverse micelles, followed by reducing cobalt ions with sodium borohydride. The resultant nanoparticles were then undergone a hydrothermal treatment at 165 degrees C for 8 h to generate well-dispersed CTAB/PSS-encapsulated cobalt nanocrystals with an average diameter of 3.5 +/- 0.5 nm. The nanoparticles were highly crystalline with a hexagonal close-packed crystal phase. The presence of CTAB/PSS complex coatings was identified by FT-IR and UV-vis spectroscopies as well as thermogravimetry analyses. The nanocrystals exhibited superparamagnetic property at room temperature with a saturation magnetization (M(s)) of 95 emu/g. The magnetization could be largely preserved after storage at room temperature for 4 months as the M(s) value only slightly decreased to 88 emu/g (measured at 300 K). Thus, the polymer encapsulation could not only improve thermal stability of the micelles for the growth and nucleation of Co atoms but also protect the resulting cobalt nanocrystals from oxidation through forming an oxygen impermeable sheath.

摘要

通过反胶束合成,然后进行水热处理,方便地制备了空气稳定的磁性钴纳米晶。该合成方法是通过首先将含有氯化钴和聚(4-苯乙烯磺酸钠)(PSS)的水溶液与含有十六烷基三甲基溴化铵(CTAB)的有机混合物混合,形成反胶束,然后用硼氢化钠还原钴离子。所得的纳米颗粒然后在 165℃下进行 8 小时的水热处理,以生成具有平均直径为 3.5±0.5nm 的良好分散的 CTAB/PSS 包覆的钴纳米晶。纳米颗粒具有高结晶性,具有六方密堆积的晶体相。通过傅里叶变换红外光谱(FT-IR)、紫外-可见光谱(UV-vis)以及热重分析(TGA)确定了 CTAB/PSS 复合涂层的存在。纳米晶在室温下表现出超顺磁性,饱和磁化强度(M(s))为 95 emu/g。在室温下储存 4 个月后,磁化强度可以得到很大的保留,因为 M(s)值仅略微下降至 88 emu/g(在 300 K 下测量)。因此,聚合物包封不仅可以提高用于 Co 原子生长和成核的胶束的热稳定性,而且可以通过形成不透气的护套来保护所得的钴纳米晶免受氧化。

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