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Controllable preparation method of monodisperse nano alpha-phase ferric oxide monocrystal

A ferric oxide, monodisperse technology, applied in chemical instruments and methods, single crystal growth, single crystal growth, etc., to achieve the effects of low preparation cost, low energy consumption, and simple equipment

Inactive Publication Date: 2014-12-10
NANCHANG HANGKONG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, up to now, no monodisperse α-phase ferric oxide nanomaterials with controllable particle size distribution / morphology have been prepared by an atmospheric pressure and mild wet chemical method.

Method used

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  • Controllable preparation method of monodisperse nano alpha-phase ferric oxide monocrystal
  • Controllable preparation method of monodisperse nano alpha-phase ferric oxide monocrystal
  • Controllable preparation method of monodisperse nano alpha-phase ferric oxide monocrystal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Example 1: Add 400 ml of ferric chloride aqueous solution with a mass ratio of 0.8% to a 500 ml round bottom flask, heat the ferric chloride aqueous solution with an oil bath at 80°C, and keep it warm for 0.5 h; then, add 2 ml of ferric chloride under stirring conditions With 80% hydrazine hydrate aqueous solution, the oil bath was heated to 105°C at a rate of 5°C / min and refluxed for 6 h; the obtained brick red precipitate was collected and dried at 80°C for 6 h. Scanning electron microscope observation found that the prepared α-phase ferric oxide was spindle-shaped, with a main size of 300 nm × 90 nm, presenting a monodisperse state (see figure 2 ); the morphology observed by the transmission electron microscope is consistent with that of the scanning electron microscope, and the selected electron diffraction of a single nanomaterial confirms that the material is a single crystal.

Embodiment 2

[0030] Example 2: Add 800 ml of ferric chloride aqueous solution with a mass ratio of 4% to a 1000 ml round bottom flask, heat the ferric chloride aqueous solution with an oil bath at 80°C, and keep it warm for 2 h; then, add 18 ml of ferric chloride under stirring conditions With 80% hydrazine hydrate aqueous solution, the oil bath was heated to 105°C at a rate of 5°C / min and refluxed for 6 h; the obtained brick red precipitate was collected and dried at 80°C for 6 h. Observation by scanning electron microscopy revealed that the prepared α-phase ferric oxide was ellipsoidal, with a main size of 200 nm×120 nm, presenting a monodisperse state (see image 3 ).

Embodiment 3

[0031] Example 3: Add 4000 ml of ferric chloride aqueous solution with a mass ratio of 8% to a 5000 ml round bottom flask, heat the ferric chloride aqueous solution with an oil bath at 80°C, and keep it warm for 2 h; subsequently, add 168 ml of ferric chloride under stirring conditions With 80% hydrazine hydrate aqueous solution, the oil bath was heated to 105°C at a rate of 5°C / min and refluxed for 6 h; the obtained brick red precipitate was collected and dried at 80°C for 6 h. Scanning electron microscope observation found that the prepared α-phase ferric oxide was ellipsoidal, with a main size of 100 nm×100 nm, showing a monodisperse state (see Figure 4 ).

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Abstract

The invention relates to a controllable preparation method of a monodisperse nano alpha-phase ferric oxide monocrystal, which comprises the following steps: preparing a 0.8-8 wt% soluble ferric iron brine solution; heating the water solution in an oil bath, and keeping the temperature for 0.5-2 hours; adding a certain amount of hydrazine hydrate into the water solution while stirring, heating the oil bath to 100-120 DEG C, and keeping the temperature for 4-12 hours; and drying the obtained precipitate at certain temperature for 3-12 hours. The soluble ferric iron salt and hydrazine hydrate used as the raw materials react in a water system by a one-pot process to obtain the alpha-phase ferric oxide nano material; and by changing the mole ratio of the ferric iron to the hydrazine hydrate within the range of 1:(2-1.6), the monodisperse alpha-phase ferric oxide nano material, which has the advantages of uniform particles, controllable particle size distribution and controllable shape, can be prepared. The nano material preparation technique has the advantages of low preparation cost, low energy consumption, simple equipment and the like, and can easily implement industrialized production.

Description

technical field [0001] The invention belongs to the technical field of nanomaterial preparation, relates to a controllable preparation method of monodisperse nano-α-phase ferric oxide single crystal, and belongs to the technology of preparing alpha-phase ferric oxide nano-material by wet chemical method. technical background [0002] Nanocrystals are the foundation of modern science and technology. Generally speaking, the properties of nanocrystals and their range of applications are affected by their shape and size, which is mainly due to the fact that the shape and size of nanocrystals determine the coordination and arrangement of surface atoms and the surface crystal structure (Hu J, et al. al. Science , 2001, 292(5524): 2060-2063.). Therefore, a lot of work has been put into how to precisely control the geometry and size of nanocrystals. α-phase ferric oxide (α-Fe 2 o 3 ) as an important thermally stable semiconductor ferrite (its bandwidth Eg = 2.1–2.2 eV), has t...

Claims

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Application Information

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IPC IPC(8): C30B7/14C30B29/16
Inventor 陈德志权红英曹群罗旭彪罗胜联
Owner NANCHANG HANGKONG UNIVERSITY