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Structural, magnetic, and acidic properties of cobalt ferrite nanoparticles synthesised by wet chemical methods

机译:湿化学法合成的钴铁氧体纳米颗粒的结构,磁性和酸性

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A detailed investigation on the effect of preparation method on the structural, magnetic, and acidic properties of cobalt ferrite nanoparticles prepared by sol–gel and co-precipitation is presented. Citric acid and ethylene glycol were used as gelling agents, while sodium hydroxide and aqueous ammonia were used as precipitating agents. The resulting ferrites were calcined at 450°C and 750°C. Sharper X-ray diffraction (XRD) peaks were observed for the samples calcined at 750°C, indicating greater crystallinity of the samples calcined at higher temperature. Average crystallite sizes fell in the ranges of 7.1–21.1 nm and 30.4–42.1 nm for the samples calcined at 450°C and 750°C, respectively. The infrared spectra revealed two main absorption bands, the high frequency band ν1 around 600 cm-1 and the low frequency band ν2 around 400 cm-1 arising from stretching vibrations of the oxygen bond with the metal in the tetrahedral (A) and octahedral (B) sites in the spinel lattice. Agglomeration of particles was observed in the scanning electron microscopy (SEM) images. Magnetic parameters of CoFe2O4 nanoparticles greatly depended on calcination temperature and preparation techniques. Ammonia temperature programmed desorption (TPD) measurements indicated that weak acid sites predominate medium strength sites, while the number of strong acid sites is the least. Cumulative acidity decreased for the samples calcined at higher temperature. The results underline the effect of preparation conditions on the morphology, crystallite size, and magnetic properties of nano ferrites.
机译:详细介绍了制备方法对溶胶-凝胶法和共沉淀法制备的钴铁氧体纳米粒子的结构,磁性和酸性的影响。柠檬酸和乙二醇用作胶凝剂,而氢氧化钠和氨水用作沉淀剂。将所得的铁氧体在450℃和750℃下煅烧。在750°C煅烧的样品中观察到更清晰的X射线衍射(XRD)峰,表明在高温下煅烧的样品具有更大的结晶度。在450°C和750°C下煅烧的样品的平均微晶尺寸分别在7.1–21.1 nm和30.4–42.1 nm范围内。红外光谱显示出两个主要吸收带,在600 cm-1附近的高频段ν1和在400 cm-1附近的低频段ν2(由于四面体(A)和八面体( B)尖晶石晶格中的位点。在扫描电子显微镜(SEM)图像中观察到颗粒的团聚。 CoFe2O4纳米粒子的磁性参数很大程度上取决于煅烧温度和制备技术。氨温度程序解吸(TPD)测量表明,弱酸位点占中等强度位点的主导,而强酸位点的数量最少。在较高温度下煅烧的样品的累积酸度降低。结果强调了制备条件对纳米铁氧体的形貌,微晶尺寸和磁性的影响。

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