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Synthesis method and application of nano-silver/silica Raman surface enhanced thin film

A silicon dioxide and surface-enhanced technology, applied in Raman scattering, filament/wire forming, single-component synthetic polymer rayon, etc., can solve the problem of poor repeatability of results, unfavorable popularization and application, and complicated preparation process, etc. Problems, to achieve good experimental repeatability, wide application, easy to remove the effect

Active Publication Date: 2018-12-25
SUZHOU UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Si Minzhen et al. used microwave heating to quickly prepare nano-silver with mostly spherical particles, but the influence of microwave heating time and heating method on the morphology of nano-silver needs to be further studied
Silver sol is a frequently used SERS substrate, but it is easy to cause agglomeration and sedimentation of the system after adding the corresponding probe molecules, which makes the repeatability of the results poor and limits its application in SERS substrates. The active metal silver film layer There are many preparation methods, including spin coating method, vacuum evaporation method, self-assembled nano-metal colloid method, lithography method and silver mirror surface reduction method, etc. However, most of these methods have complicated preparation process, time-consuming and uneconomical, which are not conducive to popularization. application

Method used

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  • Synthesis method and application of nano-silver/silica Raman surface enhanced thin film
  • Synthesis method and application of nano-silver/silica Raman surface enhanced thin film
  • Synthesis method and application of nano-silver/silica Raman surface enhanced thin film

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] The synthesis method of nano silver / silicon dioxide Raman surface enhanced film is:

[0019] Step 1: Preparation of spinning solution: Weigh 2g of PVP with a molecular weight of 1.3 million and dissolve it in 30mL of ethanol, stir magnetically for 2 hours, slowly add 2.23mL tetraethyl orthosilicate dropwise, stir for 4 hours to obtain solution A, and then Dissolve 0.085g of silver nitrate in 5mL of water, then slowly add it dropwise to solution A, and stir for 24 hours;

[0020] The second step: at a temperature of 20°C and a humidity of 55%, the positive voltage of the electrospinning is controlled to be 16KV, the negative voltage is -3KV, the spinning distance is 20cm, and the spinning speed is 0.4mm / min. Liquid spinning is made into thin film material, irradiated by fluorescent lamp, and left to stand for 6 hours;

[0021] Step 3: Remove the film, put it in a vacuum drying oven, dry at 30°C for 24 hours, then calcinate at 550°C for 3 hours, and cool naturally.

[0...

Embodiment 2

[0024] The synthesis method of nano silver / silicon dioxide Raman surface enhanced film is:

[0025] Step 1: Preparation of spinning solution: Weigh 2g of PVP with a molecular weight of 2 million and dissolve it in 50mL of ethanol, stir magnetically for 2 hours, slowly add 6mL tetraethyl orthosilicate dropwise, stir for 4 hours to obtain solution A, then take Dissolve 0.6g of silver nitrate in 6mL of water, then slowly add it dropwise to solution A, and stir for 24 hours;

[0026] The second step: at a temperature of 22°C and a humidity of 60%, control the positive voltage of electrospinning to 16KV, the negative voltage to -3KV, the spinning distance to 20cm, and the spinning speed to 0.6mm / min. Liquid spinning is made into thin film material, irradiated by fluorescent lamp, and left to stand for 6 hours;

[0027] Step 3: Remove the film, put it in a vacuum drying oven, dry it at 30°C for 24 hours, then calcinate it at 500°C for 3 hours, and cool it naturally.

[0028] The d...

Embodiment 3

[0030] The synthesis method of nano silver / silicon dioxide Raman surface enhanced film is:

[0031] Step 1: Preparation of spinning solution: Weigh 2g of PVP with a molecular weight of 500,000 and dissolve it in 20mL of ethanol, stir magnetically for 2 hours, slowly add 2mL tetraethyl orthosilicate dropwise, stir for 4 hours to obtain solution A, then take Dissolve 0.3g of silver nitrate in 5mL of water, then slowly add it dropwise to solution A, and stir for 24 hours;

[0032] The second step: at a temperature of 18°C ​​and a humidity of 50%, control the positive voltage of electrospinning to 8KV, the negative voltage to -3KV, the spinning distance to 20cm, and the spinning speed to 0.6mm / min. Liquid spinning is made into thin film material, irradiated by fluorescent lamp, and left to stand for 6 hours;

[0033] Step 3: Remove the film, put it in a vacuum drying oven, dry it at 30°C for 24 hours, then calcinate it at 700°C for 3 hours, and cool it naturally.

[0034] The di...

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Abstract

The invention provides a synthesis method and application of a nanometer silver / silicon dioxide Raman surface enhanced thin film. The thin film is prepared from the following steps of: taking PVP (polyvinyl pyrrolidone) to dissolve into ethanol; performing magnetic stirring for 2 hours; slowly dripping tetraethoxysilane; performing stirring for 4 hours to obtain a solution A; then, taking and dissolving silver nitrate into water; then, slowly dripping the silver nitrate into the solution A to be stirred; then, performing static spinning at the temperature being 18 to 22 DEG C and the humidity being 50 percent to 60 percent; preparing spinning liquid into a thin film material on a receiving plate; performing illumination by a fluorescent lamp; standing for 6 hours; taking down the thin film; putting the thin film into a vacuum drying box to be dried for 24 hours at the temperature being 25 to 30 DEG C; then, performing calcinations for 3 to 5 hours; performing natural cooling; thereby obtaining the nanometer silver / silicon dioxide Raman surface enhanced thin film. The material can be used as a Raman enhanced material with the advantages of high stability, high repeatability, high universality, high activity and simple and cheap preparation method; good application prospects are realized in the aspect of antibiotic pollution monitoring.

Description

technical field [0001] The invention relates to the field of detection materials, in particular to the synthesis and application of nano-silver / silicon dioxide Raman surface enhanced thin films. Background technique [0002] With the rapid development of nanotechnology, the surface-enhanced Raman effect (Surface-Enhanced Raman Scattering, SERS) has the ability to detect trace organic substances, and can obtain high sensitivity to provide rich interface information, while the detection time is short (tens seconds), the cost is much lower than that of chromatographic methods. [0003] Through in-depth research on surface-enhanced Raman, people have increasingly realized that the further development of surface-enhanced Raman is mainly limited by the preparation technology of active substrates. Silver nanoparticles have attracted much attention due to their excellent biocompatibility and unique antibacterial, catalytic, electronic and other properties. Compared with other metal...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D04H1/728D01D5/00D01F6/44D01F1/10G01N21/65
CPCD01D5/003D01D5/0069D01D5/0092D01F1/10D01F1/103D01F6/44D04H1/728G01N21/658
Inventor 刘成宝陈丰吕岩陈志刚钱君超吴正颖唐远征陈晓
Owner SUZHOU UNIV OF SCI & TECH
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