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Nano-iron powder prepn. method

A technology of nano-iron powder and iron powder, applied in the direction of coating, etc., can solve the problems of low safety, many steps, complicated operation, etc., and achieve the effect of convenient process, simple equipment, and simple post-processing

Inactive Publication Date: 2006-03-29
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The U.S. "Nano. Letters" magazine (Nano.Letters, 1393-1395, 2002) reported a method for preparing iron nanorods by reducing β-FeOOH with hydrogen. This method has many steps and complicated operations, and requires special equipment for hydrogen reduction. device, less secure

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Embodiment 1: Preparation of iron nanopowder in ethanol solvent

[0018] 4.0g FeCl 3 ·6H 2 Dissolve O in 20ml ethanol, add 15.0g NaOH and 10.0ml 80% hydrazine hydrate solution, stir until uniform; heat the above mixture at 100°C to reflux for 12h, the mother liquor becomes colorless and transparent, and the reaction can be completed; Separation, washing, and vacuum drying yielded gray-black powder.

[0019] It was proved by X-ray diffraction that the gray-black powder was pure phase α-Fe; the transmission electron microscope showed that the sample was in the shape of small squares, the particle size was uniform, and the average size was about 120nm. It can be seen that the product prepared in this example is a pure-phase α-Fe nanopowder.

[0020] Take the mother liquor after separating the iron powder, after acidification, use SCN - Color development, no Fe 3+ The characteristic color, indicating that the Fe in the mother liquor 3+ content below 10 -5 mol / l, indi...

Embodiment 2

[0022] Embodiment 2: Preparation of iron nanopowder in water solvent

[0023] 4.0g FeCl 3 ·6H 2 Dissolve O in 20ml of water, add 20.0g of NaOH and 20.0ml of 80% hydrazine hydrate solution, stir until uniform; heat the above mixture to reflux at 120°C for 12h, the mother liquor becomes colorless and transparent, and the reaction can be completed. The product was separated, washed, and dried in vacuum to obtain a gray-black powder.

[0024] The X-ray diffraction pattern of the product proves that the gray-black powder is pure phase α-Fe; the transmission electron microscope shows that the sample is in the shape of small squares, the particle size is uniform, and the size is about 250nm. It can be seen that what is prepared in this example is pure-phase nano-iron powder.

[0025] Take the mother liquor after separating the iron powder, after acidification, use SCN - Color development, no Fe 3+ The characteristic color, indicating that the Fe in the mother liquor 3+ content ...

Embodiment 3

[0028] Embodiment 3: Preparation of iron nanopowder in alcohol-water mixed solvent

[0029] Get the mother liquor 15ml that contains alkali after separating the product in Example 1, add 10ml water and 8.0g NaOH, obtain alcohol-water mixed solution; Then, add 4.0g FeCl 2 4H 2 O and 20.0ml of 50% hydrazine hydrate solution, stirred evenly; the above mixture was heated to reflux at 100°C for 11h, the mother liquor became colorless and transparent, and the reaction was completed. The product is magnetically separated, washed, and dried in vacuum to obtain a gray-black powder.

[0030] X-ray diffraction proves that the obtained product is pure-phase α-Fe; the transmission electron microscope characterizes that the sample is in the shape of small squares, with uniform particle size and an average size of about 180nm. It shows that the gray-black powder prepared in this example is nano-iron powder.

[0031] Take the mother liquor after separating the iron powder, after acidificat...

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Abstract

A process for preparing iron nanoparticles includes such steps as proportionally dissolving iron salt in alcohol, water, or their mixture, proportionally adding NaOH solution and hydrazine hydrate solution, stirring, and heating at 80-120 deg.C while refluxing until the mother liquid becomes colorless and transparent. Its advantages are high purity, adjustable granularity and high output rate (more than 99%).

Description

Technical field: [0001] The invention belongs to the technical field of preparation of metal nanomaterials, in particular to a liquid-phase chemical preparation method of nano iron powder under normal pressure. Background technique: [0002] Due to its excellent magnetic properties, large surface area and high reactivity, nano-iron powder has a very wide range of applications in the fields of catalysis, magnetic recording and electronics. At present, its main chemical preparation methods are: thermal decomposition or ultrasonic decomposition of iron-containing metal-organic compounds, borohydride reduction of iron salts, hydrogen reduction of ferric hydroxide or iron oxide, etc., but these methods have equipment to varying degrees. Expensive, complex operation process, many steps, low product purity, low yield and other disadvantages. [0003] "Journal of American Chemical Society" (Journal of American Society, 11960-11961, 1996) has reported the use of high-density ultraso...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B22F9/24B22F1/02
Inventor 倪小敏郑化桂苏晓波杨丹丹
Owner UNIV OF SCI & TECH OF CHINA
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