Method for preparing magnetic nano composite particles of FeCr alloy dispersed in ceramic crystal grain

A technology of ceramic crystal grains and magnetic nanometers, which is applied in the field of preparation of inorganic magnetic nanocomposite particles, can solve the problems of difficult control of particle size distribution and monodispersity, loss of special magnetic properties, easy aggregation of nanoparticles, etc., and achieve thermal stability Improvement, stability improvement, and guaranteed effect of nanostructure

Inactive Publication Date: 2009-10-28
WUHAN UNIV OF TECH
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Problems solved by technology

However, the alloy nanoparticles prepared by this method are located between or on the surface of ceramic grains, and the nanoparticles are easy to agglomerate and oxidized. At the same time, the size of the nanoparticles is easily affected by the metal oxide precursor, and the particle size distribution and monodispersity are relatively low. It is difficult to control, and the generated alloy nanoparticles often reach tens to hundreds of nanometers, which leads to the loss of its special magnetic properties

Method used

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  • Method for preparing magnetic nano composite particles of FeCr alloy dispersed in ceramic crystal grain
  • Method for preparing magnetic nano composite particles of FeCr alloy dispersed in ceramic crystal grain
  • Method for preparing magnetic nano composite particles of FeCr alloy dispersed in ceramic crystal grain

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Embodiment 1

[0032] According to the chemical formula Al 5.4 Fe 0.36 Cr 0.24 Si 2 o 13 , 0.54mol Al(NO 3 ) 3 9H 2 O, 0.036mol Fe(NO 3 ) 3 9H 2 O and 0.024mol Cr(NO 3 ) 3 9H 2 O was dissolved in 400ml of absolute ethanol to form a solution with a sum of molar concentrations of metal ions of 1.5mol / L, heated in a water bath to 60°C and vigorously stirred by magnetic force; after the solution was stirred for 6 hours, HNO with a molar concentration of 1.5mol / L was added dropwise 3 Solution, adjust the pH value of the solution to 3 and continue to stir for 3 hours; add 0.2mol tetraethyl orthosilicate (TEOS) dropwise to the solution, and add NH with a molar concentration of 15mol / L dropwise 3 ·H 2 O to adjust the pH value of the solution to 5, continue to stir for 5 hours, and then move the sol to a constant temperature water bath at 80°C for aging until a xerogel (or precursor) is formed. The xerogel was calcined at 500 °C for 5 h in flowing air to obtain amorphous oxide powder (i...

Embodiment 2

[0036] According to the chemical formula Al 5.4 (Fe 1-x Cr x ) 0.6 Si 2 o 13 , (x=0.1~0.5), with Al(NO 3 ) 3 9H 2 O, Fe(NO 3 ) 3 9H 2 O, Cr(NO 3 ) 3 ·9 H 2O and tetraethyl orthosilicate (TEOS) are carried out proportioning as raw material, according to the technique of embodiment 1, obtain and form Fe 3+ and Cr 3+ Mullite solid solution ceramic powder with complete solid solution of ions; Fe 3+ and Cr 3+ H 2 The gas was reduced at 1200°C for 1 hour, and the obtained products were magnetic nanocomposite particles of FeCr alloy dispersed in ceramic grains of different compositions. It can be affected by the composition of Fe and Cr in solid solution.

Embodiment 3

[0038] According to the chemical formula Al 5.9 Fe 0.09 Cr 0.01 Si 2 o 13 , 0.59mol Al(NO 3 ) 3 9H 2 O, 0.009mol Fe(NO 3 ) 3 9H 2 O and 0.001mol CrCl 3 9H 2 O was dissolved in 600ml of absolute ethanol to form a solution with the sum of the molar concentrations of metal ions being 1mol / L, heated in a water bath to 90°C and strongly magnetically stirred; after the solution was stirred for 1 hour, HNO with a molar concentration of 1mol / L was added dropwise 3 Solution, adjust the pH value of the solution to 3.5 and continue to stir for 3h; add 0.2mol tetraethyl orthosilicate (TEOS) dropwise to the solution, and add NH with a molar concentration of 13mol / L dropwise 3 ·H 2 O to adjust the pH value of the solution to 5.5, continue to stir for 5 hours, and then move the sol to a constant temperature water bath at 60°C for aging until a xerogel (or precursor) is formed. The xerogel was calcined at 400 °C for 5 h in flowing air to obtain amorphous oxide powder (ie precurso...

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Abstract

The invention pertains to the field of inorganic magnetic nano composite materials. A method for preparing magnetic nano composite particles of FeCr alloy dispersed in a ceramic crystal grain is characterized by comprising the following steps of: (1) raw material selection: the dosage of Al in an aluminum salt, Si in a silicon source, Fe in a ferric salt and Cr in a chromic salt meets the chemical formula of (Al6-x-yFex Cry) Si2O13 (wherein, x plus y is larger than 0 and less than or equal to 1, and x is larger than or equal to y and y is larger than 0); the aluminum salt, the silicon source, the ferric salt and the chromic salt are taken as raw materials for later use; (2) selecting one of the following two methods: (a) a sol-gel method for realizing gelatinization; (b) a coprecipitation method for realizing gelatinization; (3) preliminary roasting: xerogel is roasted for 1 to 5h in flowing air at the temperature of 400 to 600 DEG C, thus obtaining amorphous oxide powder; (4) roasting: the amorphous oxide powder is roasted for 1 to 5h in air at the temperature of 1000 to 1500 DEG C; (5) high temperature reduction: a reduction gas is used for conducting reduction for 1 to 10h at the temperature of 1200 to 1400 DEG C, thus obtaining the magnetic nano composite particles. The magnetic nano composite particles are characterized by superparamagnetic physical feature and high stability.

Description

technical field [0001] The invention belongs to the field of inorganic magnetic nano-composite materials, and specifically relates to a preparation method of an inorganic magnetic nano-composite particle formed by monodispersing high-stability FeCr alloy magnetic nano-particles inside mullite ceramic crystal grains with mullite ceramics as a matrix . Background technique [0002] Due to the potential application in magnetic recording, catalysis, magnetic fluid, magnetic resonance imaging and magnetic targeting drug carriers, the preparation and properties of Fe, Co, Ni and other magnetic metal single substance nanoparticles have attracted extensive attention in recent years. However, compared with simple metal nanoparticles, people can easily adjust the magnetic properties of alloy nanoparticles by adjusting the alloy composition, so the preparation and performance research of magnetic alloy nanoparticles has attracted more and more attention. The preparation and properties...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01F1/09B22F9/00C04B35/622
Inventor 王皓王为民傅正义
Owner WUHAN UNIV OF TECH
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