Facile Green Synthesis of Magnetic Fe$ _\textbf{3} $C@C Nanocomposite using Natural Magnetite
doi: 10.1063/1674-0068/cjcp1907142
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摘要: 采用改进的溶胶凝胶法，以天然磁铁矿为铁源，开发出一种制备过程简单且环境友好且低成本的磁性Fe$ _3 $C$ @ $C纳米材料制备策略.其中，柠檬酸作为多元羧酸络合剂，不但可以有效地溶解不同铁源，例如Fe、Fe$ _3 $O$ _4 $或天然磁铁矿，形成柠檬酸铁盐络合物；还可以在热解过程中作为碳源，形成包裹碳层.通过控制高温热解过程可以直接形成特殊的核-壳结构形态. Fe$ _3 $C$ @ $C纳米材料具有超顺磁性特性(38.09 emu/mg).
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关键词:
- 磁性材料 /
- 天然铁矿石 /
- Fe$ _3 $C$ @ $C /
- 柠檬酸络合
Abstract: One simple and environmental friendly synthesis strategy for preparing low-cost magnetic Fe$ _3 $C@C materials has been facilely developed using a modified sol-gel approach, wherein natural magnetite acted as the iron source. A chelating polycarboxylic acid such as citric acid (CA) was employed as the carbon source, and it dissolved Fe very effectively, Fe$ _3 $O$ _4 $ and natural magnetite to composite an iron-citrate complex with the assistance of ammonium hydroxide. The core-shell structure of the as-prepared nanocomposites was formed directly by high-temperature pyrolysis. The Fe$ _3 $C@C materials exhibited superparamagnetic properties (38.09 emu/mg), suggesting potential applications in biomedicine, environment, absorption, catalysis, etc.-
Key words:
- Magnetic material, Natural magnetite /
- Fe$ _3 $C@C /
- Citric acid complexation /
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Figure 1. XRD patterns of the Fe$ _3 $C@C samples from (A) Fe$ _3 $O$ _4 $ and (B) after acid-treatment, and (C, D) from different iron sources with (D) after acid-treatment calcined at 700 $ ^{\circ} $C.
Figure 2. Typical SEM images of the Fe$ _3 $C@C samples obtained at 700 $ ^{\circ} $C from (A) Fe$ _3 $O$ _4 $ and (B) natural magnetite
Figure 3. TEM images of the Fe$ _3 $C@C samples obtained at 500 $ ^{\circ} $C from Fe$ _3 $O$ _4 $ A(a) before and A(b) after acid-treatment, at 700 $ ^{\circ} $C from Fe$ _3 $O$ _4 $; B(a) before, B(b) and B(c) after acid washing, at 700 $ ^{\circ} $C with natural magnetite; C(a) before, C(b) and C(c) after acid washing.
Figure 4. The magnetic hysteresis loop of the Fe$ _3 $C@C samples prepared from different iron sources at 700 $ ^{\circ} $C (a) before and (b) after acid washing.
Figure 5. Schematic of the synthesis process of the Fe$ _3 $C@C samples modified by sol-gel method.
Supplementary Fig. 1. TG and DTG profiles of the fully dried gel precursor from natural magnetite (10 ℃/min in N2)
Supplementary Fig 2. The magnetic hysteresis loop of the Fe3C@C samples prepared from pure Fe3O4 and Fe at 700 ℃ (a) before and (b) after acid washing.
Supplementary Table 1. The element composition of the natural magnetite and the as-prepared Fe3C@C sample.
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