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Co–Fe–oxide nanoparticles supported on the various highly dispersed matrices: the effect of the carrier on structural and magnetic properties
Adsorption ( IF 3.3 ) Pub Date : 2023-11-06 , DOI: 10.1007/s10450-023-00417-8
Alla Dyachenko , Konrad Terpilowski , Olena Ischenko , Iryna Sulym , Dariusz Sternik , Eugen Pakhlov , Mykola Borysenko , Lyudmila Storozhuk , Lyudmila Andriyko , Olena Goncharuk

A series of mixed oxides was synthesized by deposition of the guest phase on the highly dispersed oxide matrix. Fumed nanooxides SiO2, Al2O3, SiO2/Al2O3, and SiO2/Al2O3/TiO2 with the specific surface area of 65–91 m2/g were selected as highly dispersed matrices. Co–Fe mixed oxides with the general formula Co4xFexOy (Co: Fe = 4: 1) were deposited as the guest oxides using the two-step method: (i) solvate-stimulated modification of the surface of fumed nanocarriers with the mixture of cobalt nitrate (II) and iron (III) formate and (ii) subsequent heat treatment up to 600 °C to form Co4xFexOy. The aim of this paper was to study the influence of the composition and structure of fumed oxide matrices and deposited guest phase on the morphology of the resulting composites in the gaseous and aqueous media using the XRD, XPS, FTIR, nitrogen adsorption and SEM/EDX, as well as quasi-elastic light scattering (QELS) methods. The low-temperature nitrogen adsorption isotherms have a sigmoidal shape with a narrow hysteresis loop characteristic of mesoporous materials. The specific surface area (SBET) of the composites varies from 48 to 82 m2/g, showing a tendency towards a decrease in the SBET values by 10–26% in comparison with the initial nanocarriers. The SEM data show the denser aggregate structure of nanocomposites compared to the initial carriers. The primary particle size was in the 30–60 nm range and the EDX data confirm the formation of a guest phase on the mixed aluminosilicate carriers, mainly in the surface patches corresponding to the alumina structure. According to the QELS data, there is a tendency to form aggregates of 100–10 μm in size in the aqueous media. The XRD method shows that the deposited metal oxides are in the form of crystalline phases of Co3O4 with the crystallites of 25–26 nm in size for the individual SiO2 and Al2O3 nanocarriers and 34–37 for the mixed ones, but the iron oxide reflections were not identified for the composites. XPS observation demonstrates the signal of Fe 2p electrons as the form of Fe2O3 oxide in the surface layer of nanocomposites as well as Co 2p as the Co3O4 and Co(OH)2.



中文翻译:

Co-Fe-氧化物纳米颗粒负载在各种高度分散的基质上:载体对结构和磁性的影响

通过在高度分散的氧化物基体上沉积客体相,合成了一系列混合氧化物。选择比表面积为65-91 m 2 /g的气相纳米氧化物SiO 2、Al 2 O 3、SiO 2 / Al 2 O 3和SiO 2 /Al 2 O 3 /TiO 2作为高度分散的基质。使用两步法沉积具有通式 Co 4x Fe x O y (Co: Fe = 4: 1) 的 Co-Fe 混合氧化物作为客体氧化物:(i) 气相纳米载体表面的溶剂化刺激改性与硝酸钴 (II) 和甲酸铁 (III) 的混合物,以及 (ii) 随后热处理至 600 °C 以形成 Co 4x Fe x O y。本文的目的是利用 XRD、XPS、FTIR、氮气吸附和 SEM/EDX 研究气相氧化物基体和沉积客体相的组成和结构对气态和水介质中所得复合材料形态的影响,以及准弹性光散射(QELS)方法。低温氮气吸附等温线呈S形,具有介孔材料的窄磁滞回线特征。复合材料的比表面积( S BET )在48至82 m 2 /g之间变化,与初始纳米载体相比,S BET值有下降10-26%的趋势。SEM 数据显示,与初始载体相比,纳米复合材料具有更致密的聚集结构。初级颗粒尺寸在 30-60 nm 范围内,EDX 数据证实了混合铝硅酸盐载体上客体相的形成,主要是在与氧化铝结构相对应的表面斑块中。根据 QELS 数据,在水介质中倾向于形成 100-10 μm 大小的聚集体。XRD 方法表明,沉积的金属氧化物呈 Co 3 O 4晶相形式,单个 SiO 2和 Al 2 O 3纳米载体的晶粒尺寸为 25-26 nm,混合纳米载体的晶粒尺寸为 34-37 nm。 ,但未识别出复合材料的氧化铁反射。XPS观察表明,纳米复合材料表面层中以Fe 2 O 3氧化物形式存在的Fe 2p 电子信号以及以Co 3 O 4和Co(OH) 2形式存在的Co 2p 电子信号。

更新日期:2023-11-08
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