A kind of ferroferric oxide/silver composite material and its preparation method and application

A technology of ferric tetroxide and composite materials, which is applied in the field of preparation of core-shell structure composite materials, can solve the problems of reduced detection signal intensity, complicated operation, interference with detection results, etc., and achieves good SERS enhancement effect, good dispersion, and preparation. simple method effect

Inactive Publication Date: 2017-03-01
HENAN INST OF ENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The commonly used SERS substrate preparation method is to prepare gold or silver nanoparticles in the solution. In order to prevent the gold or silver nanoparticles from agglomerating during the preparation process, it is usually necessary to use surfactants to protect these nanoparticles, and then centrifuge and wash several times. Finally, these nanoparticles are collected, which is cumbersome and wastes energy; moreover, surfactants will be adsorbed on the surface of nanoparticles, interfering with the detection results or reducing the intensity of the detection signal

Method used

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  • A kind of ferroferric oxide/silver composite material and its preparation method and application
  • A kind of ferroferric oxide/silver composite material and its preparation method and application
  • A kind of ferroferric oxide/silver composite material and its preparation method and application

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Embodiment 1

[0027] Fe 3 o 4 Particle preparation method: in 1.35g FeCl 3 •6H 2 Add 40 mL of ethylene glycol to O and stir magnetically until FeCl 3 •6H 2 O was completely dissolved, then added 3.6 g NaAc and 1.0 g polyethylene glycol, and stirred for 1 h to obtain a homogeneous mixture. Then the mixture was transferred to a 50 mL stainless steel reaction kettle with a polytetrafluoroethylene liner, and the reaction kettle was heated to 200 °C in a blast drying oven, kept for 8 h, and then naturally cooled to room temperature. The obtained product was collected by a magnet, washed three times with distilled water, then washed three times with absolute ethanol, collected by a magnet, and then dried in a vacuum oven at 60 °C for 6 h to obtain a black powder.

[0028] Take a small amount of the above-mentioned black powder, add distilled water and ultrasonically disperse it, drop the dispersion onto a silicon wafer, and test it on a scanning electron microscope after natural drying to ob...

Embodiment 2

[0030] Fe 3 o 4 The preparation method of / Ag composite material: get the Fe in embodiment 1 3 o 4 Add 8 mL of distilled water to 40 mg of particles, and ultrasonically disperse for 5 min to obtain Fe 3 o 4 Dispersion A. Take 100 μL of dispersion A and add it to 195 mL of distilled water, stir evenly to obtain dispersion B, add 4 mL of 0.1 mol / L ascorbic acid aqueous solution under constant stirring, and then add 0.1 mol / L of [Ag(NH 3 ) 2 ]OH 0.4 mL. In dispersion C, Fe 3 o 4 The particle concentration is 2.5 mg / L, the ascorbic acid concentration is 2 mmol / L, [Ag(NH 3 ) 2 ]OH concentration is 0.2 mmol / L. At a temperature of 25°C, the dispersion C was reacted for 30 minutes under constant stirring. After the reaction, the product was collected with a magnet and washed three times with distilled water to obtain a spherical core-shell structure Fe 3 o 4 / Ag composites.

[0031] The aforementioned stirring refers to mechanical stirring using a propeller stirrer.

[0...

Embodiment 3

[0037] According to the invention patent "a magnetic surface-enhanced Raman spectroscopy substrate and its preparation method" (application publication number: CN104034715A), the surface-enhanced Raman spectroscopy substrate is prepared. The substrate is made of Fe with a core-shell structure 3 o 4 / Ag particles are piled up and have a flower-like structure. The optimized preparation method is as follows: dissolve 0.54 g of ferric chloride hexahydrate, 1.176 g of sodium citrate dihydrate, and 0.36 g of urea in 40 mL of distilled water, and then add 0.3 g polyacrylamide, stir until it is completely dissolved; transfer the above solution to a 50 mL reaction kettle lined with polytetrafluoroethylene, seal it and place it in a blast drying oven, and react at 200°C for 8 h; Cool to room temperature, collect the black precipitate with a magnet, wash with distilled water for 3 times, then wash with absolute ethanol for 3 times, and dry in a vacuum oven at 60°C for 8 hours to obtain F...

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Abstract

The invention discloses a ferroferric oxide / silver composite material and a manufacturing method and application of the ferroferric oxide / silver composite material. The composite material is composed of a ferroferric oxide particle and a silver layer which wraps the ferroferric oxide particle, and is of a spherical core-shell structure with the ferroferric oxide particle as a core and the silver layer as a shell. The manufacturing method includes the following steps: the ferroferric oxide particle is dispersed in distilled water; ascorbic acid and a silver-ammonia solution are sequentially added into the dispersion liquid after ultrasound processing is carried out; a reaction is made for 10-80 min at the temperature ranging from 20 DEG C to 50 DEG C so as to obtain the ferroferric oxide / silver composite material of the spherical core-shell structure. The manufacturing method of the ferroferric oxide / silver composite material is simple; the surface of the ferroferric oxide particle can be wrapped with the even silver layer without modifying the ferroferric oxide particle, the speed for restoring silver-ammonia with the ascorbic acid is low, and an even silver shell can be slowly and evenly formed on the surface of the ferroferric oxide particle through silver. The ferroferric oxide / silver composite material can serve a surface strengthening Raman spectrum substrate, and the strengthening effect is good.

Description

technical field [0001] The invention relates to a preparation method and application of a core-shell structure composite material, in particular to a preparation method of a spherical core-shell structure ferric oxide / silver composite material and its application in surface-enhanced Raman spectroscopy. Background technique [0002] In 1977, Van Duyne and Jeanmaire found that pyridine adsorbed on a rough silver electrode could measure a huge Raman signal, and the signal enhancement could not be caused by more pyridine molecules adsorbed on the rough silver electrode surface. Subsequently, on rough noble metal surfaces, many different molecules were confirmed to have strong Raman signals. This Raman enhancement effect associated with rough noble metal surfaces is called Surface Enhanced Raman Scattering (Surface Enhanced Raman Scattering, SERS). )effect. The substrate material to which these molecules are attached is called a surface-enhanced Raman spectroscopy substrate. SE...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B22F1/02B22F9/24G01N21/65B82Y30/00B82Y40/00
Inventor 郭怡叶英杰毕建平王新莉吴素珍
Owner HENAN INST OF ENG
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