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Controllable preparation method of micron-order Fe3O4

A micron-scale, solution technology, applied in ferrous oxides, iron oxides/iron hydroxides, etc., can solve the problems of uncontrollable nucleation and growth, narrow particle size distribution of micron-sized particles, and high phase purity. The effects of controllable nucleation and growth processes, high particle crystallinity, and high sample phase purity

Inactive Publication Date: 2013-07-17
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The object of the invention is to provide a micron-scale Fe 3 o 4 The controllable preparation method solves the problem of uncontrollable nucleation and growth, and the prepared micron-sized particles have a very narrow particle size distribution and high phase purity

Method used

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  • Controllable preparation method of micron-order Fe3O4
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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 1) FeSO 4 ·7H 2 O and NaOH are dissolved in distilled water respectively, and form FeSO with a concentration of 2.0mol / L after dissolution 4 Solution and concentration are the NaOH solution of 16.80mol / L;

[0028] 2) FeSO configured in step 1 4 The solution is dissolved in the NaOH solution configured in step 1, and the FeSO 4 The volume ratio of the solution to the NaOH solution is 2:5, stir to fully dissolve it;

[0029] 3) The mixed solution obtained in step 2 was assisted with low-frequency ultrasonic treatment, the ultrasonic power was 40W, and the ultrasonic time was 8min, until the mixed solution was light green;

[0030] 4) Transfer the solution obtained in step 3 into a Teflon hydrothermal kettle with a volume of 60%, and keep it warm for 10 hours at a temperature of 160°C;

[0031] 5) Add 200ml of distilled water to the precipitate obtained in step 4 to rinse, and perform centrifugation. The centrifuge speed is 12000r / min, and the centrifugation time is 5...

Embodiment 2

[0035] 1) FeSO 4 ·7H 2 O and NaOH are dissolved in distilled water respectively, and form FeSO with a concentration of 3.50mol / L after dissolution. 4 solution and a NaOH solution with a concentration of 11.00mol / L;

[0036] 2) FeSO configured in step 1 4 The solution is dissolved in the NaOH solution configured in step 1, and the FeSO 4 The volume ratio of the solution to the NaOH solution is 2:5, stir to fully dissolve it;

[0037] 3) The mixed solution obtained in step 2 was assisted with low-frequency ultrasonic treatment, the ultrasonic power was 70W, and the ultrasonic time was 12min, until the mixed solution was light green;

[0038] 4) Transfer the solution obtained in step 3 into a Teflon hydrothermal kettle with a volume of 80%, and keep it warm for 15 hours at a temperature of 200°C;

[0039] 5) Add 200ml of distilled water to the precipitate obtained in step 4 to rinse, and perform centrifugation. The centrifuge speed is 12000r / min, and the centrifugation time ...

Embodiment 3

[0043] 1) FeSO 4 ·7H 2 O and NaOH are dissolved in distilled water respectively, and form FeSO with a concentration of 5.0mol / L after dissolution. 4 solution and a NaOH solution with a concentration of 20.00mol / L;

[0044] 2) FeSO configured in step 1 4 The solution is dissolved in the NaOH solution configured in step 1, and the FeSO 4The volume ratio of the solution to the NaOH solution is 2:5, stir to fully dissolve it;

[0045] 3) The mixed solution obtained in step 2 was assisted with low-frequency ultrasonic treatment, the ultrasonic power was 70W, and the ultrasonic time was 10min, until the mixed solution was light green;

[0046] 4) Transfer the solution obtained in step 3 into a Teflon hydrothermal kettle with a volume of 90% at a filling ratio of 90%, and keep it warm for 10 hours at a temperature of 280°C;

[0047] 5) Add 200ml of distilled water to the precipitate obtained in step 4 to rinse, and perform centrifugation. The centrifuge speed is 12000r / min, and ...

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Abstract

The invention provides a controllable preparation method of micron-order Fe3O4. The controllable preparation method comprises the following steps of: mixing an FeSO4 solution with a sodium hydroxide solution according to a volume ratio of 2:5, fully dissolving, and performing low-frequency ultrasonic auxiliary processing until the mixed liquor is light green; then transferring the solution into a Teflon hydrothermal kettle, wherein the packing ratio in reaction kettle is 60-90%; and preserving heat at 160-280 DEG C for 10-15 hours, taking out precipitate, washing and then centrifugalizing, and drying at 120 DEG C under an air atmosphere. The method provided by the invention solves the problem that nucleation and growth are uncontrollable, and the prepared micron-sized grains are very narrow in size distribution and have high phase purity.

Description

【Technical field】 [0001] The invention belongs to the technical field of preparing nano powder by wet chemical method, and in particular relates to a controllable preparation method of micron-sized iron ferric oxide. 【Background technique】 [0002] Fe 3 o 4 It is a ferrimagnetic material with good performance. Due to its biocompatibility, it can be used in biomedical fields such as gene separation and directional drug delivery. It also has unique electrical and magnetic properties. It is used in magnetic devices, microwave materials, etc. , Magnetic ink and so on have a wide range of applications. The currently reported Fe 3 o 4 The preparation methods can obtain finer particles, but still cannot obtain satisfactory results in terms of particle size and controllability of nucleation and growth. For example, Chinese Patent Announcement No. CN102502877A reports a method for synthesizing porous ferroferric oxide magnetic microspheres. The method uses ferrous ions and ferr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G49/08
Inventor 于成龙高丹鹏郝欣王斐乔畅君郝晓明霍仁杰王志刚
Owner SHAANXI UNIV OF SCI & TECH
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