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Colloidal silver iodide: synthesis by a reverse micelle method and investigation by a small-angle neutron scattering study

机译:胶态碘化银:反胶束法合成和小角中子散射研究

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摘要

Silver iodide nanoparticles were prepared by mixing two microemulsions containing the precursor salts, silver nitrate and potassium iodide. Five values of w=[water]/[surfactant] were used, namely 2, 4, 8, 16, and 32. Transmission electron microscopy (TEM) showed that the nanoparticle diameters were 4–240 nm and increased proportionally with w. The nanoparticles prepared from a microemulsion of w=2 and 8 showed brown and ocherous colors respectively, while bulk silver iodide powder is pale yellow. The crystal structure was determined by neutron powder diffraction. The composition was estimated to be 25% β-AgI and 75% β-AgI. The super-ionic conductor phase could not be detected at room temperature. The w=8 microemulsion was examined with small-angle neutron scattering (SANS) in order to study the core-shell structure of the reverse micelles at various temperatures. Measurements were carried out at 20 and 9 ℃ and then at 70 ℃ and finally at 28 ℃, in order to investigate whether the structural changes were reversible with temperature. The total radius of the micelles, surfactant shell thickness and water core radius decreased with increasing temperature and the changes were reversible with temperature. The particle diameters derived by TEM were generally larger than those estimated from the SANS measurements. This suggested that the silver iodide nuclei formed initially grew to reach a certain size, corresponding to the most thermodynamically stable species in the microemulsion, because of the fast exchange between the water cores.
机译:通过混合两种包含前体盐,硝酸银和碘化钾的微乳液来制备碘化银纳米颗粒。 w的五个值= [水] / [表面活性剂],即2、4、8、16和32。透射电子显微镜(TEM)显示纳米粒子的直径为4–240 nm,并且与w成正比。由w = 2和8的微乳液制备的纳米颗粒分别显示棕色和and色,而大块碘化银粉末为浅黄色。通过中子粉末衍射确定晶体结构。组成估计为25%β-AgI和75%β-AgI。在室温下无法检测到超离子导体相。为了研究在不同温度下反胶束的核-壳结构,使用小角中子散射(SANS)检查了w = 8的微乳液。为了研究结构变化是否随温度可逆,在20和9℃,然后在70℃,最后在28℃进行了测量。胶束的总半径,表面活性剂壳的厚度和水核半径随温度的升高而减小,并且其变化随温度可逆。通过TEM得出的粒径通常大于根据SANS测量得出的粒径。这表明由于水核之间的快速交换,最初形成的碘化银核开始生长到一定大小,与微乳液中最热力学稳定的物种相对应。

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