Structure and preparation method for magnetic sliver-flower nano-particles

A magnetic nanoparticle and nanoparticle technology, applied in the field of nanomaterials and photonic materials, can solve the problems of unsatisfactory SERS performance, large surface roughness, large specific surface area, etc., and achieve convenient chemical modification, simple synthesis method, and good dispersion Effect

Inactive Publication Date: 2017-06-23
ACADEMY OF MILITARY MEDICAL SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These silver-modified magnetic nanocomposite particles do not provide enough hot spots for SERS detection, and the SERS performance is not ideal.
The magnetic silver flower nanostructure with large specific surface area, large surface roughness and flower-like structure with nano-tips has not yet been obtained.

Method used

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  • Structure and preparation method for magnetic sliver-flower nano-particles
  • Structure and preparation method for magnetic sliver-flower nano-particles
  • Structure and preparation method for magnetic sliver-flower nano-particles

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] A preparation of high-performance magnetic silver flower nanoparticles:

[0032] figure 1 A schematic diagram of the preparation process of magnetic silver flower nanoparticles is given. Its concrete preparation method is divided into the following five steps: the first step, adopts solvothermal synthesis method to synthesize the Fe of 100-600 nanometers 3 o 4 magnetic nanoparticles. Dissolve 1.35 g of ferric chloride hexahydrate in 40 ml of ethylene glycol, and stir magnetically for 30 minutes. Next, 2.7 g of sodium acetate and 1 g of polyethylene glycol 20000 were added to the solution and stirred until the reactants were completely dissolved, then the mixture was transferred to an autoclave (50 ml capacity) with a polytetrafluoroethylene liner and heated to 200 degrees Celsius reaction for 6-24 hours. The product was collected with a magnet, washed twice with deionized water and ethanol respectively, and finally the product was vacuum-dried at 60 degrees Celsius...

Embodiment 2

[0042] The SERS enhancement ability of magnetic silver flower nanoparticles was characterized by Raman labeling molecule p-aminothiophenol (PATP):

[0043] PATP is a commonly used sulfhydryl Raman marker, and it will produce significant chemically enhanced Raman characteristic peaks when combined with gold or silver. Configure different concentrations of PATP ethanol solutions (10 -5 -10 -12 mol), 1 ml per tube. Add magnetic silver flower nanoparticles to the above solution, and react with ultrasound for 30 minutes to fully combine PATP on the surface of magnetic silver flower nanoparticles. After magnetic separation, add the particle concentrate to a clean silicon chip, and perform Raman after drying. detection.

[0044] Figure 6 It is the experimental result of Example 2. Figure 6 Shown is the Raman map of PATP excited by magnetic silver flower nanoparticles, and the abscissa is the Raman shift, of which 1078, 1576cm -1 The peak is the main peak among the characteris...

Embodiment 3

[0046] Detection of Dithiocarbamate Pesticide Thiram Using Magnetic Silver Flower Nanoparticles:

[0047] Thiram is a commonly used dithiocarbamate pesticide with strong Raman characteristic peaks. The magnetic silver flower nanoparticles were added to different concentrations of thiram aqueous solution, incubated with ultrasound for 15 minutes, and the particles were magnetically enriched and directly detected by a portable Raman spectrometer.

[0048] Figure 7 It is the experimental result of embodiment 3. Figure 7 Shown is the Raman spectrum of the thiram bimolecule excited by the magnetic silver flower nanoparticles, and the abscissa is the Raman shift, of which 561, 1385cm -1 The peak is the main peak among the characteristic peaks of thiram bimolecules. Raman detection conditions are excitation time 5 seconds, excitation power 20%. The experimental results show that the detection limit of thiram by magnetic silver flower nanoparticles is 1×10 -10 Moore, with very ...

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Abstract

The invention discloses a structure and a preparation method for magnetic sliver-flower nano-particles. The structure takes magnetic nano-particles (Fe3O4) as the core and takes a silicon dioxide shell layer (SiO2) as a multi-functional layer. By formaldehyde reduction, flower-shaped sliver shells similar to needle points rapidly grow. The preparation method comprises the following steps: wrapping surfaces of 100-6000 nano Fe3O4 magnetic nanoparticles with an SiO2 layer and improving dispersion of magnetic nano-particles and providing position points of sliver seed growth; utilizing a chemical electroplating method with the assistance of ultrasonic wave to grow the surfaces of the Fe3O4@SiO2 magnetic particles with uniform and dense sliver particles as seeds for growth of flower-shaped sliver shells; finally, utilizing formaldehyde as a reduction agent and ammonium hydroxide as a catalyst to rapidly reduce magnetic sliver-flower nano-particles on the ultrasonic condition. The invention further discloses a magnetic SERS substrate prepared by the above method. The magnetic SERS substrate is made from magnetic sliver-flower nano-particles and is good in dispersion, high in magnetic induction, stable in structure and great in heart and can be directly used for SERS detection of small molecule pollutants, pesticide residuals and illegal additives of food.

Description

technical field [0001] The invention relates to a structure and a preparation method for preparing magnetic silver flower nanoparticles, belonging to the fields of photonic materials and nanometer materials. Background technique [0002] Magnetic nanoparticles can quickly enrich and capture target samples under the action of an external magnetic field. They are easy to operate and easy to modify. They have been widely used in various biochemical experiments. Bare magnetic beads are easily oxidized, dissolved in an acidic environment, and lack active groups on the surface. Therefore, a variety of materials are used to encapsulate or modify magnetic nanoparticles to make them have better stability, biocompatibility and multifunctionality, such as SiO 2 、TiO 2 , Au, Ag, Al 2 o 3 Wait. Among them, silver has catalytic, bactericidal and optical properties, and is an ideal material for modifying magnetic beads. In particular, precious metals such as gold and silver can signi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01F1/11C01G49/08B22F1/02C23C18/44
CPCB22F1/0007H01F1/112C23C18/44C01G49/08B22F2207/07C01P2004/84B22F1/07B22F1/065B22F1/17
Inventor 王升启汪崇文肖瑞李敏李萍荣振蒋娜曲新艳郭晶徐胜平
Owner ACADEMY OF MILITARY MEDICAL SCI
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