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Nanomaterials (Basel)
2021 Nov 12;1111:. doi: 10.3390/nano11113034.
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Iron-Nickel Alloy with Starfish-like Shape and Its Unique Magnetic Properties: Effect of Reaction Volume and Metal Concentration on the Synthesized Alloy.
Nady N
,
Salem N
,
Mohamed MAA
,
Kandil SH
.
Abstract
Iron-nickel alloy is an example of bimetallic nanostructures magnetic alloy, which receives intensive and significant attention in recent years due to its desirable superior ferromagnetic and mechanical characteristics. In this work, a unique starfish-like shape of an iron-nickel alloy with unique magnetic properties was presented using a simple, effective, high purity, and low-cost chemical reduction. There is no report on the synthesis of such novel shape without complex precursors and/or surfactants that increase production costs and introduce impurities, so far. The synthesis of five magnetic iron-nickel alloys with varying iron to nickel molar ratios (10-50% Fe) was undertaken by simultaneously reducing Fe(II) and Ni(II) solution using hydrazine hydrate as a reducing agent in strong alkaline media for 15 min at 95-98 °C. The effect of reaction volume and total metal concentration on the properties of the synthesized alloys was studied. Alloy morphology, chemical composition, crystal structure, thermal stability, and magnetic properties of synthesized iron-nickel alloys were characterized by means of SEM, TEM, EDX, XRD, DSC and VSM. ImageJ software was used to calculate the size of the synthesized alloys. A deviation from Vegard's law was recorded for iron molar ration higher than 30%., in which superstructure phase of FeNi3 was formed and the presence of defects in it, as well as the dimensional effects of nanocrystals. The saturation magnetization (Ms), coercivity (Hc), retentivity (Mr), and squareness are strongly affected by the molar ratio of iron and nickel and reaction volume as well as the total metal concentration.
Figure 1. Photos of the prepared iron-nickel alloy during washing process (A,B).
Figure 2. SEM images of the prepared iron-nickel alloy at two magnifications; (A) ×5000 and (B) ×15,000.
Figure 3. TEM images of the prepared iron-nickel alloy at two magnifications; (A) ×5000 and (B) ×15,000.
Figure 4. The high resolution TEM images of Fe10 Ni90 molar ratio synthesized using 0.1 M metal concentration and 80 mL reaction volume carried out for 15 min at 1400 rpm and 95–98 °C.
Figure 5. Particle size as function of the molar ratio of iron using ImageJ software; 40 mL reaction volume (blue circle) and 80 mL reaction volume (green circle) with 0.1 M metal concentration, 80 mL reaction volume with 0.3 M concentration (red circle).
Figure 6. EDX analysis of the synthesized Fe10 Ni90 alloy using (A) SEM and (B) TEM. (C) TEM mapping of the alloy. Reaction reference: 0.1 M metal concentration, 80 mL reaction volume, 1400 rpm, and 95–98 °C.
Figure 7. XRD pattern of the prepared iron-nickel alloys using (A) different iron-nickel molar ratio with 0.1 M metal concentration and 80 mL reaction volume, (B) 10 to 30% iron molar ratio at both 0.1 and 0.3 M metal concentration and 80 mL reaction volume. Reference condition: 1400 rpm, and 95–98 °C.
Figure 8. The lattice parameter as function of alloy composition (% Fe molar ratio).
Figure 9. The DSC diagram of the prepared iron-nickel alloys using different iron-nickel molar ratio (10–50% Fe). Reaction reference: 0.1 M metal concentration, 80 mL reaction volume, 1400 rpm, and 95–98 °C.
Figure 10. The M-H hysteresis loops of the iron-nickel microcrystals at room temperature; (a) 0.1 M metal concentration in 40 mL reaction volume, (b) 0.1 M metal concentration in 80 mL reaction volume, and (c) 0.3 M metal concentration in 80 mL reaction solution. Reaction reference: 1400 rpm and 95–98 °C.
Figure 11. Magnetic Properties as function of Iron molar ratio in the alloys; (a) Coercivity and Magnetization, (b) Retentivity, and (c) Squareness. Reference conditions: Curve 1: 0.1 M metal concentration in 40 mL reaction volume, Curve 2: 0.1 M metal concentration in 80 mL reaction volume, and Curve 3: 0.3 M metal concentration in 80 mL reaction solution.
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