Chemistry Department, Faculty of Science, Sohag University, 82524 Sohag, Egypt.
J Colloid Interface Sci. 2012 Feb 15;368(1):56-63. doi: 10.1016/j.jcis.2011.11.027. Epub 2011 Nov 23.
Iron oxide/MCM-41 nanocomposites, Fe(2)O(3)/MCM-41, containing 5%, 10%, and 20% (w/w) iron oxide, were prepared via a direct nonhydrothermal method at room temperature. The preparations were preformed by using iron(III) nitrate, tetra-ethoxysilane (TEOS), and cetyltrimethylammonium bromide (CTAB) mixed or unmixed with dodecyltrimethylammonium bromide (DTAB). The produced materials were dried and calcined at 550 °C for 3 h. Test materials were characterized by thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), Fourier transform infrared spectroscopy (FTIR), N(2) gas adsorption/desorption isotherms, small angle and wide angle X-ray diffraction (XRD). Results indicate that mixing of CTAB with DTAB does not harm the formation of blank MCM-41 structure. For the composite Fe(2)O(3)/MCM-41 materials, results showed formation of more stable MCM-41 structure with higher surface area and improved porosity in the presence of mixed (CTAB+DTAB) than in the presence of single (CTAB) surfactants for up to 10% Fe(2)O(3)/MCM-41 (w/w). This was explained in terms of the effect DTAB on contraction of the template micellar size to compensate for the expected size expansion upon the addition of ionic iron(III) nitrate precursor. Highly dispersed Fe(2)O(3) nanoparticles were formed in all cases even with the highest iron oxide percentage. Formation of the nanocomposites was postulated to be determined by fast nucleation and slow growth of iron oxide species, which facilitated formation of well dispersed iron oxide nanoparticles inside and on the wall of the MCM-41 material.
采用室温下的直接非水热法制备了铁氧化物/MCM-41 纳米复合材料,Fe(2)O(3)/MCM-41,包含 5%、10%和 20%(w/w)的铁氧化物。通过混合或不混合使用硝酸铁、四乙氧基硅烷(TEOS)和十六烷基三甲基溴化铵(CTAB)与十二烷基三甲基溴化铵(DTAB)制备了这些材料。制备出的材料经干燥后在 550°C 下煅烧 3 小时。通过热重分析(TGA)、差示扫描量热法(DSC)、傅里叶变换红外光谱(FTIR)、N(2)气体吸附/解吸等温线、小角和宽角 X 射线衍射(XRD)对测试材料进行了表征。结果表明,CTAB 与 DTAB 的混合不会损害空白 MCM-41 结构的形成。对于复合 Fe(2)O(3)/MCM-41 材料,结果表明,在存在混合(CTAB+DTAB)表面活性剂的情况下,与仅存在单一(CTAB)表面活性剂相比,形成了更稳定的 MCM-41 结构,具有更高的表面积和改善的孔隙率,直到 10% Fe(2)O(3)/MCM-41(w/w)。这可以解释为 DTAB 对模板胶束尺寸收缩的影响,以补偿加入离子铁(III)硝酸盐前体时预期的尺寸膨胀。即使在最高氧化铁百分比的情况下,也形成了高度分散的 Fe(2)O(3)纳米颗粒。推测纳米复合材料的形成是由铁氧化物物种的快速成核和缓慢生长决定的,这有利于在 MCM-41 材料的内部和壁上形成分散良好的氧化铁纳米颗粒。