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A kind of monodisperse and superparamagnetic gold-magnetic composite microsphere and preparation method thereof

A superparamagnetic, composite microsphere technology, applied in diamagnetic/paramagnetic materials, magnetic objects, magnetic materials, etc., can solve the problems of poor dispersion, complex process and weakening of composite materials, and achieve good stability and repeatability. Good, avoid the effect of agglomeration

Active Publication Date: 2021-07-27
SHAANXI UNIV OF SCI & TECH
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Problems solved by technology

However, during the preparation process, Fe 3 o 4 The solution is easy to oxidize, which weakens the magnetism. More importantly, the growth process of gold magnetic nanoparticles is prone to agglomeration, which is difficult to control the growth process of the material, and the resulting composite material has poor dispersion.
Later, some researchers also used the layer-by-layer assembly method and the seed crystal growth method to synthesize gold magnetic particles. First, the prepared Fe 3 o 4 The surface is modified to be positively charged, and then the negatively charged colloidal gold particles are loaded on the Fe by electrostatic adsorption force. 3 o 4 surface, with the seed as the growth center, by controlling the HAuCl 4 4H 2 The flow rate of O and reducing agent is used to obtain gold-magnetic composite materials. The particles prepared by this method have relatively uniform Au shells, but the process is more complicated and the yield is not high.

Method used

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preparation example Construction

[0036] The preparation method of the gold magnetic composite microsphere with monodisperse and superparamagnetic of the present invention comprises the steps:

[0037] (1) Preparation of mesoporous Fe by solvothermal method 3 o 4

[0038] FeCl 3 ·6H 2 O and sodium acetate are placed in a round-bottomed flask, and 1,2-propylene glycol solution is used as a solvent, stirred and ultrasonically dissolved to make it uniform, and then, the stirred mixture is heated to 90-110°C, and transferred to polytetrafluoroethylene for reaction In the kettle, react at 160-200°C for 8-10 hours. After the reaction, the black precipitate was collected by magnetic separation with a magnet, and washed several times alternately with ultrapure water and absolute ethanol until the cleaned supernatant was clear, and finally freeze-dried, and the obtained powder was mesoporous Fe 3 o 4 . where FeCl 3 ·6H 2 The molar ratio of O to sodium acetate is (0.1-0.15):1.

[0039] (2) Reducing agent on me...

Embodiment 1

[0044] (1) Preparation of mesoporous Fe by hydrothermal method 3 o 4

[0045] 5mmolFeCl 3 ·6H 2 O and 50mmol sodium acetate were placed in a round-bottomed flask, and 40ml of 1,2-propanediol solution was taken as a solvent, stirred and ultrasonically dissolved to make it uniform, and then, the stirred mixture was heated to 90°C, and transferred to polytetrafluoroethylene In the reaction kettle, react at 160°C for 8h. After the reaction, the black precipitate was collected by magnetic separation with a magnet, and washed several times alternately with ultrapure water and absolute ethanol until the cleaned supernatant was clear, and finally freeze-dried, and the obtained powder was mesoporous Fe 3 o 4 .

[0046] (2) Reducing agent on mesoporous Fe 3 o 4 surface modification

[0047] Take 0.05g of anhydrous sodium citrate and dissolve it in 100ml of ultrapure water. After the dissolution is complete, add 100mg of mesoporous Fe prepared in (1). 3 o 4 , the mixture was m...

Embodiment 2

[0051] (1) Preparation of mesoporous Fe by hydrothermal method 3 o 4

[0052] 5mmolFeCl 3 ·6H 2 O and 50mmol sodium acetate were placed in a round-bottomed flask, and 40ml of 1,2-propanediol solution was taken as a solvent, stirred and ultrasonically dissolved to make it uniform, and then, the stirred mixture was heated to 95°C, and transferred to polytetrafluoroethylene React for 10 hours at 180°C in the reactor. After the reaction, the black precipitate was collected by magnetic separation with a magnet, and washed several times alternately with ultrapure water and absolute ethanol until the cleaned supernatant was clear, and finally freeze-dried, and the obtained powder was mesoporous Fe 3 o 4 .

[0053] (2) Reducing agent on mesoporous Fe 3 o 4 surface modification

[0054] Take 0.10g of anhydrous sodium citrate and dissolve it in 100ml of ultrapure water. After the dissolution is complete, add 100mg of mesoporous Fe prepared in (1). 3 o 4 , the mixture was mech...

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Abstract

The invention provides a method for preparing monodisperse and superparamagnetic gold-magnetic composite microspheres, comprising: (1) adding ferric chloride and sodium acetate to 1,2-propylene glycol, and mixing uniformly to obtain a bright yellow mixed solution , heated to 90-110°C, after the bright yellow mixture turns into ginger yellow, the mesoporous Fe 3 o 4 Precursor solution for solvothermal reaction to obtain mesoporous Fe 3 o 4 ; (2) Dissolve anhydrous sodium citrate in water, add mesoporous Fe 3 o 4 , the resulting mixture was stirred at room temperature to obtain the surface-modified mesoporous Fe 3 o 4 solution; (3) the surface modified mesoporous Fe 3 o 4 The solution is heated, and then an aqueous solution of chloroauric acid is added, and precipitates are separated after reaction, washed and dried to obtain gold-magnetic composite microspheres. Nano Fe prepared by the present invention 3 o 4 Au / Au composites have good dispersibility in aqueous solution and have broad application prospects in the field of biomedicine.

Description

technical field [0001] The invention belongs to the technical field of inorganic nanocomposite materials, in particular to a monodisperse and superparamagnetic Fe 3 o 4 / Au composite microsphere and its preparation method. Background technique [0002] Nano-composite materials refer to the size of the material at the nanometer level. Generally, it is composed of two or more nano-materials according to a certain structure, so that the material can obtain excellent comprehensive properties. It not only has the unique quantum size effect, surface effect and Volume effect, etc., and has the synergistic effect of various nano-component structures. Due to their unique structures and composite functions, nanocomposites have gained widespread attention and applications in the fields of electronics, optics, catalysis, and biomedical technology. [0003] Au-magnetic nanocomposite material is a kind of relatively common nanocomposite structure. Generally speaking, it refers to a col...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01F41/02H01F1/00H01F1/01
CPCH01F1/0018H01F1/01H01F41/0253
Inventor 杨冬王丽霞雷蕾高可奕贾彤彤
Owner SHAANXI UNIV OF SCI & TECH
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