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One-step statistical design of experiment for the screening and optimization of magnetite nanoparticles yields from solvothermal synthesis
Microporous and Mesoporous Materials ( IF 5.2 ) Pub Date : 2020-11-27 , DOI: 10.1016/j.micromeso.2020.110775
Sadiq Sani , Rohana Adnan , Mohammad Anwar Mohamed Iqbal

One-step custom design of experiment was employed for the simultaneous screening and optimization of raw yield (Y1) and percent yield (Y2) with heating temperature, T (190–220 °C) and reaction time, t (1.0–2.5 h) as the predictors in a conventional solvothermal magnetite nanoparticles (NPs) synthesis. Two accurate models capable of explaining 98.3% variability in the data were developed. A strong correlation exists between the actual yields (Y1, Y2) and their predicted counterparts (r = 0.99). T, t, Tt and t2 terms have a significant synergistic effect on the yields the at α = 0.05. The diagnostic plots depicted the effects in the order t > T > Tt > t2. Surface and contour plots show maximum Y1 (0.295 g) and Y2 (105%) at T = 219 °C and t = 2.5 h. The optimizer plot shows maximized Y1 (109.94%) and Y2 (0.31 g) at the highest predictor values (T = 220 °C, and t = 2.5 h) at composite desirability of 1. NPs characterization using various techniques revealed nanocubes and nanospheres with a mean diameter of 23.9 ± 7.9 nm, the crystallite size of 8.3 ± 1.4–20.4 ± 4.9 nm, a pore size of 9.07–24.47 nm, and surface area of 35.80–93.57 m2 g−1. The NPs exhibit stretching Fe–O vibrations at 571 cm−1 for tetrahedral and at 428 cm−1 for octahedral geometries in the infrared spectra and are thermally stable within the range 30–700 °C with low weight loss (8.81–32.92%) typical of mesoporous magnetite phase.



中文翻译:

溶剂热合成筛选和优化磁铁矿纳米颗粒产量的一步统计设计实验

采用一步定制的实验设计,同时筛选和优化了加热温度T(190–220°C)和反应时间t(1.0–2.5 )时的原始收率(Y 1)和百分收率(Y 2)。 h)作为常规溶剂热磁铁矿纳米颗粒(NPs)合成的预测因子。开发了两个能够解释数据中98.3%变异性的准确模型。实际收益率(Y 1,Y 2)与预测的收益率(r = 0.99)之间存在很强的相关性。T,t,Tt和t 2项对α= 0.05时的产量具有显着的协同作用。诊断图以t> T> Tt> t 2的顺序描述了这些影响。。表面和轮廓图显示了在T = 219°C和t = 2.5 h时的最大Y 1(0.295 g)和Y 2(105%)。优化器图显示了在复合期望值为1时,在最高预测值(T = 220°C,t = 2.5 h)下,Y 1(109.94%)和Y 2(0.31 g)最大化。使用各种技术对NPs的表征揭示了纳米立方体和纳米球,平均直径为23.9±7.9 nm,微晶尺寸为8.3±1.4–20.4±4.9 nm,孔径为9.07–24.47 nm,表面积为35.80–93.57 m 2  g -1。NP在四面体的571 cm -1和428 cm -1处表现出拉伸的Fe–O振动 用于红外光谱中的八面体几何形状,并且在30–700°C的温度范围内具有热稳定性,且介孔磁铁矿相的典型失重较低(8.81–32.92%)。

更新日期:2020-11-27
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