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Preparation method of silver nanoparticle dense layer on silicon wafer

A technology of silver nanoparticles and dense layer, applied in the field of nanomaterial preparation, can solve the problems of particle agglomeration, uneven distribution, sparse distribution of silver nanoparticles, etc., and achieves the effect of good repeatability and high enhancement effect.

Active Publication Date: 2019-03-19
XIAN TECH UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

It can be seen from the pictures provided that the distribution of silver nanoparticles on the surface of the silicon wafer is sparse and extremely uneven, and some particles are seriously agglomerated. Therefore, a high and uniform SERS enhancement effect cannot be obtained, and only a concentration of 10 -8 Raman Spectrum of Rodin-B Molecule in mol / L
The invention patent (CN201510973724.9) mentions that the silicon wafer treated with aminosilane is placed in the chloroauric acid solution, and the nano-gold particles are generated in situ on the surface of the silicon wafer through the weak reduction of the amino group, but the particles on the silicon wafer The distribution is still extremely sparse, resulting in an enhancement factor of only 10 for the detection of glycerol molecules 4 Magnitude

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  • Preparation method of silver nanoparticle dense layer on silicon wafer
  • Preparation method of silver nanoparticle dense layer on silicon wafer

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preparation example Construction

[0034] The preparation method of the dense layer of silver nanoparticles on the silicon chip that the present invention relates to comprises the following steps:

[0035] Step 1: Soak the silicon wafer in the alkali washing solution and the acid washing solution for 15 minutes each, so as to hydroxylate the surface of the silicon wafer;

[0036] Step 2: Place the silicon wafer obtained in Step 1 in a toluene solution of mercaptopropyltrimethoxysilane, and react at 40°C for 4-10 hours, or at room temperature for 24-40 hours, to silanize the silicon wafer;

[0037] Step 3: Soak the silicon wafer obtained in Step 2 in 0.25mM silver nitrate solution for 6-24 hours;

[0038] Step 4: Take out the silicon wafer obtained in Step 3, place it in a 5mM sodium borohydride solution, and react for 30 minutes;

[0039] Step 5: Take out the silicon chip obtained in Step 4, place it in a mixed solution of silver nitrate and polyvinylpyrrolidone, stir for 30 minutes, and then drop into 1ml, 0....

Embodiment 1

[0061] 1) Soak a silicon wafer cut to 1cm×1cm in 10ml of alkaline washing solution (ammonia: hydrogen peroxide: water = 1:1:5, volume ratio) for 15 minutes, then rinse with a large amount of deionized water, and ultrasonically clean for 2 minute;

[0062] 2) After that, soak the silicon wafer in 10ml pickling solution (hydrochloric acid: hydrogen peroxide: water = 1:1:5, volume ratio) for 15 minutes, then rinse with a large amount of deionized water and ultrasonically clean it for 2 minutes to Hydroxylation of silicon wafer surface;

[0063] 3) After the above-mentioned silicon wafer is blown dry with nitrogen, place it in 10ml of mercaptopropyltrimethoxysilane (MPTMS) toluene solution (5% volume concentration) at 40°C for 4 hours to silanize the silicon wafer;

[0064] 4) Take out the above-mentioned silicon chip, place it in toluene, toluene / ethanol mixture (volume ratio 1:1), ethanol, and deionized water for 2 minutes respectively;

[0065] 5) Soak the silicon wafers trea...

Embodiment 2

[0070] 1) Soak a silicon wafer cut to 1cm×1cm in 10ml of alkaline washing solution (ammonia: hydrogen peroxide: water = 1:1:5, volume ratio) for 15 minutes, then rinse with a large amount of deionized water, and ultrasonically clean for 2 minute;

[0071] 2) After that, soak the silicon wafer in 10ml pickling solution (hydrochloric acid: hydrogen peroxide: water = 1:1:5, volume ratio) for 15 minutes, then rinse with a large amount of deionized water and ultrasonically clean it for 2 minutes to Hydroxylation of silicon wafer surface;

[0072] 3) After the above-mentioned silicon wafer is blown dry with nitrogen, place it in 10ml of toluene solution (5% volume concentration) of mercaptopropyltrimethoxysilane (MPTMS) and keep it for 24 hours to silanize the silicon wafer;

[0073] 4) Take out the above-mentioned silicon chip, place it in toluene, toluene / ethanol mixture (volume ratio 1:1), ethanol, and deionized water for 2 minutes respectively;

[0074] 5) Soak the silicon waf...

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Abstract

The invention relates to a preparation method of a silver nanoparticle compact layer on a silicon wafer. The preparation method comprises the steps of putting the silicon wafer into an alkali wash solution and an acid wash solution for soaking in sequence, so that the surface of the silicon wafer is hydroxylated; putting the silicon wafer into a mercaptopropyltrimethoxysilane methylbenzene solution for a reaction, so that the silicon wafer is silanized; putting the silicon wafer into a silver nitrate solution and a sodium borohydride solution in sequence so that silver seed crystals can be formed; putting the silicon wafer into a mixed solution of silver nitrate and polyvinylpyrrolidone, and then dropwise adding an ascorbic acid solution so that the silver seed crystals can grow continuously; and after the process is repeated multiple times, conducting washing and ultrasonic blow-drying. According to the preparation method of the silver nanoparticle compact layer on the silicon wafer, firstly, the silver seed crystals are fixed to the silicon wafer by means of organic molecules having the dual functions; then, in-situ reduction is conducted, so that the silver seed crystals are obtained; then, the compact and uniform silver particle film layer can be obtained through multiple times of later-stage cyclic growing; when the metal particle film layer is applied to SERS, the uniform and high enhancement effect can be maintained within a large range such as the micron range; and in addition, the preparation method is good in repeatability.

Description

technical field [0001] The invention relates to the technical field of nanomaterial preparation, in particular to a method for preparing a dense layer of silver nanoparticles on a silicon wafer. Background technique [0002] In the study of surface-enhanced Raman spectroscopy (SERS), it was found that the enhancement of the light field by the substrate formed by the close arrangement of nano-metal particles would lead to the enhancement of Raman signal intensity. When the particles are in the nanometer-level gap, the electric field between the particles is coupled with each other, and the field strength is enhanced more significantly, resulting in a significant increase in the Raman signal. Therefore, for SERS substrates, it is a research hotspot in this industry to obtain a high Raman enhancement effect in order to minimize the distance between particles. [0003] The methods for preparing SERS substrates usually include etching method and colloidal particle solution metho...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C23C18/44C23C18/18B82Y40/00
CPCB82Y40/00C23C18/1658C23C18/1893C23C18/44
Inventor 吴春芳蔡长龙张进
Owner XIAN TECH UNIV