Preparação, análise microestrutural e propriedades magnéticas de nanocompósitos de CoFe2O4/CoFe2

Abstract

In this study, the preparation process of 𝐶𝑜𝐹𝑒2𝑂4/𝐶𝑜𝐹𝑒2 nanocomposites will be carried out, followed by a detailed analysis of their internal structure. In addition, the magnetic properties will be investigated to optimise these characteristics in the samples. The synthesis of 𝐶𝑜𝐹𝑒2𝑂4 was carried out using the gel-combustion method, and the substance was subjected to different calcination temperatures for a period of 2 hours under normal atmospheric conditions. Subsequently, the samples were submitted to milling processes at different periods to induce a high residual micro deformation inside the particles and increase the coercivity. After the synthesis of the cobalt ferrite nanocomposite, the next step is the reduction using hydrogen. In this process, the nanocomposite is exposed to a controlled environment containing gaseous hydrogen. At a temperature of 350°C and in time intervals of 10, 15, 20, 25 and 30 minutes, the chemical reduction reaction occurs, in which the hydrogen reacts with the oxides present in the nanocomposite. In addition to the 𝐶𝑜𝐹𝑒2𝑂4/𝐶𝑜𝐹𝑒2 nanocomposite synthesis method with 𝐻2 gas, it is possible to obtain it with the high-energy milling method. In this way, ground cobalt ferrite is mixed with different concentrations of cobalt iron. Then, the sample is subjected to a ball mill for 1 minute to obtain a uniform mixture and a magnetic coupling between both phases, thus forming the 𝐶𝑜𝐹𝑒2𝑂4/𝐶𝑜𝐹𝑒2 nanocomposite. In samples calcined at different temperatures, agglomeration of nanoparticles forms during heating at high temperatures, which contributes to the growth of crystallites and, consequently, to an increase in saturation magnetization. The redistribution of cations, specifically the 𝐹𝑒3+ ions, in octahedral sites is also responsible for the increase in saturation magnetization. Furthermore, the reduction in the magnetic coercivity of cobalt ferrite with increasing calcination temperature is caused by changes in the microstructure and distribution of cations in the ferrite crystal lattice. .The unground sample has the following characteristics: magnetic coercivity (𝐻𝑐) of 0.4 KOe, magnetic saturation 𝑀𝑠 of 75 emu/g, remanence rate 𝑀𝑅⁄𝑀𝑆 of 0.38 and maximum magnetic energy (𝐵𝐻)𝑚𝑎𝑥 of 2.0 𝑘𝐽 𝑚3 ⁄ . After grinding, there was a considerable increase in almost all attributes, which became 𝐻𝑐 = 3.7 kOe, 𝑀𝑠 = 66 emu/g, 𝑀𝑅⁄𝑀𝑆 = 0.56, and (𝐵𝐻)𝑚𝑎𝑥 = 9.6 𝑘𝐽 𝑚3 ⁄ . The results indicate that this increase is related to the addition of stress and the density of microstructural defects. An increase in magnetic anisotropy is also observed with milling, which is attributed to anisotropic stress. Thus, it is concluded that ultrafast grinding brings several advantages over conventional grinding, especially in terms of efficiency, where you have a tenfold reduction in grinding time and a considerable increase in magnetic properties. Heat treatment in a hydrogen atmosphere is effective in transforming cobalt ferrite into cobalt iron. This process is fast and efficient, reducing cobalt ferrite by approximately 90% in just 20 minutes. Additionally, heat treatment increases the saturation magnetization of cobalt ferrite, making it more magnetic. On the other hand, the magnetic coercivity of cobalt ferrite decreases when reduced in iron-cobalt, which is expected since iron-cobalt is magnetically soft. The method of producing 𝐶𝑜𝐹𝑒2𝑂4/𝐶𝑜𝐹𝑒2 nanocomposite through high-energy ball mill has several advantages. The high efficiency and speed of the process stands out, which is 60 times faster compared to other techniques.