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不同反应时间下水热合成的FeO@C纳米复合材料的表面性质比较

Comparison of the Surface Properties of Hydrothermally Synthesised FeO@C Nanocomposites at Variable Reaction Times.

作者信息

Sani Sadiq, Adnan Rohana, Oh Wen-Da, Iqbal Anwar

机构信息

School of Chemical Sciences, Universiti Sains Malaysia (USM), Penang 11800, Malaysia.

Department of Applied Chemistry, Federal University Dutsin-Ma, Dutsinma P.M.B. 5001, Nigeria.

出版信息

Nanomaterials (Basel). 2021 Oct 16;11(10):2742. doi: 10.3390/nano11102742.

Abstract

The influence of variable reaction time (t) on surface/textural properties (surface area, total pore volume, and pore diameter) of carbon-encapsulated magnetite (FeO@C) nanocomposites fabricated by a hydrothermal process at 190 °C for 3, 4, and 5 h was studied. The properties were calculated using the Brunauer-Emmett-Teller (BET) isotherms data. The nanocomposites were characterised using Fourier transform infrared spectroscopy, X-ray diffraction analysis, thermogravimetry, and scanning and transmission electron microscopies. Analysis of variance shows t has the largest effect on pore volume (F value = 1117.6, value < 0.0001), followed by the surface area (F value = 54.8, value < 0.0001) and pore diameter (F value = 10.4, value < 0.001) with R-adjusted values of 99.5%, 88.5% and 63.1%, respectively. Tukey and Fisher tests confirmed t rise to have caused increased variations in mean particle sizes (11-91 nm), crystallite sizes (5-21 nm), pore diameters (9-16 nm), pore volume (0.017-0.089 cm g) and surface area (7.6-22.4 m g) of the nanocomposites with individual and simultaneous confidence limits of 97.9 and 84.4 (p-adj < 0.05). The nanocomposites' retained Fe-O vibrations at octahedral (436 cm) and tetrahedral (570 cm) cubic ferrite sites, modest thermal stability (37-60 % weight loss), and large volume-specific surface area with potential for catalytic application in advanced oxidation processes.

摘要

研究了在190℃水热条件下反应3、4和5小时制备碳包覆磁铁矿(FeO@C)纳米复合材料时,可变反应时间(t)对其表面/纹理性质(表面积、总孔体积和孔径)的影响。使用布鲁诺尔-埃米特-特勒(BET)等温线数据计算这些性质。通过傅里叶变换红外光谱、X射线衍射分析、热重分析以及扫描和透射电子显微镜对纳米复合材料进行表征。方差分析表明,t对孔体积影响最大(F值 = 1117.6,p值 < 0.0001),其次是表面积(F值 = 54.8,p值 < 0.0001)和孔径(F值 = 10.4,p值 < 0.001),调整后的R值分别为99.5%、88.5%和63.1%。Tukey和Fisher检验证实,t的增加导致纳米复合材料的平均粒径(11 - 91 nm)、微晶尺寸(5 - 21 nm)、孔径(9 - 16 nm)、孔体积(0.017 - 0.089 cm³/g)和表面积(7.6 - 22.4 m²/g)的变化增加,个体和同时置信限分别为97.9和84.4(p调整 < 0.05)。纳米复合材料在八面体(436 cm⁻¹)和四面体(570 cm⁻¹)立方铁氧体位点保留了Fe - O振动,具有适度的热稳定性(37 - 60%重量损失),并且具有较大体积比表面积,在高级氧化过程中具有催化应用潜力。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/76dc/8537566/6b68b2b776af/nanomaterials-11-02742-g001.jpg

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