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Method for ultrasonically preparing Fe3O4 nano-particle through ammonia dispersion

A nanoparticle and ammonia technology, applied in the field of nanomaterials, can solve the problem of not being able to disperse quickly, and achieve the effects of low cost, mild reaction conditions, and prevention of uneven particle size distribution.

Inactive Publication Date: 2011-01-05
NORTHWEST NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Preparation of Fe by Dropping Ammonia under Ultrasonic Condition 3 o 4 Magnetic particles cannot be dispersed quickly after the liquid is added dropwise, and can only react in a small local area. The generated magnetic particles are easy to attract each other, resulting in serious agglomeration

Method used

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  • Method for ultrasonically preparing Fe3O4 nano-particle through ammonia dispersion
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  • Method for ultrasonically preparing Fe3O4 nano-particle through ammonia dispersion

Examples

Experimental program
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Effect test

Embodiment 1

[0034] In the reaction vessel, prepare FeCl 3 ·6H 2 O and FeSO 4 ·7H 2 A mixed solution of O. FeCl in the mixed solution 3 ·6H 2 O and FeSO 4 ·7H 2 The molar ratio of O is 1.75:1, and the concentrations of ferric ions and ferrous particles are 0.044M and 0.025M, respectively.

[0035] Seal the reaction vessel, evacuate it, and fill it with nitrogen, so that the reaction vessel is under nitrogen protection; place the reaction vessel in a 200W ultrasonic instrument, adjust the temperature of the ultrasonic wave to 25°C, and radiate the intensity to 40KHZ; at the same time, mix the reaction vessel with Feed ammonia gas in the solution, the feed amount of ammonia gas is 17% of solution quality; Control the feed speed of ammonia gas 0.4g / min; Ultrasonic radiation 30 minutes, reaction solution presents dark brown precipitation; Cool to room temperature, use respectively Wash the product with distilled water and ethanol; then dry it in a vacuum oven at 25°C for 12 hours to ob...

Embodiment 2

[0037] In the reaction vessel, prepare FeCl 3 ·6H 2 O and FeSO 4 ·7H 2 A mixed solution of O. FeCl in the mixed solution 3 ·6H 2 O and FeSO 4 ·7H 2 The molar ratio of O is 2:1, and the concentrations of ferric ions and ferrous particles are 0.05M and 0.025M, respectively.

[0038] Seal the reaction vessel, vacuumize it, and fill it with nitrogen, so that the reaction vessel is under nitrogen protection; place the reaction vessel in a 200W ultrasonic instrument, adjust the temperature of the ultrasonic wave to 35°C, and radiate at 40KHZ; at the same time, mix the reaction vessel with Feed ammonia gas in the solution, and the feeding amount of ammonia gas is 17% of solution quality; Control the feeding speed of ammonia gas 0.4g / min; Ultrasonic radiation 50 minutes, reaction solution presents pitchy precipitation; Cool to room temperature, use respectively Wash the product with distilled water and ethanol; then dry it in a vacuum oven at 25°C for 12 hours to obtain Fe 3 ...

Embodiment 3

[0040] In the reaction vessel, prepare FeCl 3 ·6H 2 O and FeSO 4 ·7H 2 A mixed solution of O. FeCl in the mixed solution 3 ·6H 2 O and FeSO 4 ·7H 2 The molar ratio of O was 1.75:1, and the concentrations of ferric ions and ferrous particles were 0.035M and 0.02M, respectively.

[0041] Seal the reaction vessel, vacuumize it, and fill it with nitrogen, so that the reaction vessel is under nitrogen protection; place the reaction vessel in a 200W ultrasonic instrument, adjust the temperature of the ultrasonic wave to 35°C, and radiate at 40KHZ; at the same time, mix the reaction vessel with Feed ammonia gas in the solution, the feed amount of ammonia gas is 20% of solution quality; Control the feed speed of ammonia gas 0.4g / min; Ultrasonic radiation 50 minutes, reaction solution presents pitchy precipitation; Cool to room temperature, use respectively Wash the product with distilled water and ethanol; then dry it in a vacuum oven at 25°C for 12 hours to obtain Fe 3 o 4 ...

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Abstract

The invention provides a method for ultrasonically preparing a Fe3O4 nano-particle in the condition of ammonia dispersion, comprising the following steps of: under protection of nitrogen, leading ammonia into a solution dissolved with iron ions and ferrous iron particles, ultrasonically dispersing for 30-70 mins at the temperature of 25-45 DEG C, and producing a pitchy sediment product in the solution; cooling to the room temperature, washing respectively with distilled water and ethanol and vacuum drying to finally obtain the Fe3O4 nano-particle. Discovered by analyzing the magnetic performance of the product by a vibrating sample magnetometer that, in the condition without an external magnetic field, the remanence and the coercivity of the particle can both be neglected, the saturation magnetization is 62-75 emu / g, and the particle shows superparamagnetism at the room temperature, also has higher magnetic responsiveness and has potential application prospect in a drug delivery system and the catalysis field.

Description

technical field [0001] The invention belongs to the technical field of nanomaterials and relates to a Fe 3 o 4 The preparation method of nanoparticle, especially relates to a kind of under the protection of nitrogen, utilize ammonia diffusion ultrasonic to prepare Fe 3 o 4 nanoparticle approach. Background technique [0002] Magnetic nanoparticles exhibit an unusual variety of magnetic behaviors due to their surface / interface effects. Ferroferric oxide nanoparticles are a kind of high Curie temperature (850K) and high saturation magnetization (92Am at 300K). 2 / kg) of magnetic oxides are widely used in magnetic resonance imaging, catalytic materials, magnetic data storage devices and clinical targeted drug delivery, etc. At present, the preparation of Fe reported in the literature 3 o 4 There are many methods for nanoparticles, such as using CO / CO 2 Gas reduction hematite method, hydrothermal method, microwave-assisted method, sol-gel method, γ-ray radiation method, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G49/08
Inventor 莫尊理张春冯超郭瑞斌孟淑娟张俊晓
Owner NORTHWEST NORMAL UNIVERSITY
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