利用液相还原与改进的Stbr法相结合,在不使用表面改性剂和氨水的条件下,通过向原硅酸乙酯(TEOS)和氯化铁混合溶液直接添加硼氢化钾,一步合成了二氧化硅包覆的纳米铁复合材料(Fe@SiO_2).通过X射线粉末衍射(XRD)仪、能量色散X射线仪(EDAX)、透射电子显微镜(TEM)、紫外-可见(UV-Vis)吸收分光光度计、傅里叶红外(FTIR)光谱仪、X射线光电子能谱仪(XPS)等对所得样品的形貌、结构和组成进行表征.将制备的Fe@SiO_2用于水体中Cr(Ⅵ)还原去除并考察了TEOS添加量对其去除能力的影响.结果表明Fe@SiO_2具有清晰的核壳结构,多孔的SiO_2包裹1-2个球形纳米铁粒子.纳米铁粒径主要分布在20-30 nm之间,随着TEOS投加量的增加,SiO_2层变厚,纳米铁核具有更好的分散性.与未包覆型纳米铁相比,Fe@SiO_2对Cr(Ⅵ)的去除能力显著提高.TEOS投加量为0.1 mL所制备的Fe@SiO_3对Cr(Ⅵ)去除能力(以Fe的质量计算)达到量大,为466.67 mg·g~(-1),而未包覆型纳米铁仅为76.35 mg·g~(-1).
Without using aqueous ammonia and a surface modifier,a facile one-step method was developed to fabricate Fe nanoparticles coated with a SiO_2 shell(Fe@SiO_2) by a modified Stober method combined with an aqueous reduction method.The Fe@SiO_2 was prepared by directly adding potassium borohydride to a mixed solution of tetraethylorthosilicate(TEOS) and anhydrous ferric chloride.The structure and morphology of the as-synthesized powders were investigated by X-ray powder diffraction (XRD),energy dispersion analysis of X-ray(EDAX),transmission electron microscopy(TEM), ultraviolet-visible(UV-Vis) absorption spectroscopy,Fourier-transform infrared(FTIR) spectrometry and X-ray photoelectron spectroscopy(XPS).The feasibility of using the prepared Fe@SiO_2 for the reductive immobilization of Cr(VI) in water was studied.The influence of TEOS addition on Cr(VI) removal by Fe@SiO_2 was investigated.The results showed that the prepared Fe@SiO_2 had a distinct core-shell structure.One or two Fe nanoparticles(20-30 nm in diameter) were homogeneously coated by a porous SiO_2 shell.With an increase in the amount of added TEOS the Fe nanoparticles had better dispersion and the thickness of the SiO_2 coating increased gradually.Compared with uncoated Fe nanoparticles,Cr(Ⅵ) removal by Fe@SiO_2 increased greatly.At a TEOS dosage of 0.1 mL the removal ability of the prepared Fe@SiO_2 was the highest.The highest removal ability of Fe@SiO_2 was 466.67 mg·g~(-1) and it was only 76.35 mg·g~(-1) for uncoated Fe nanoparticles.