Preparation method and application of silver nano flower clusters/silver micro pieces of graded structures

A hierarchical structure, silver nanotechnology, applied in the field of analysis, can solve the problems that the structure uniformity of branches or flower clusters cannot be guaranteed, the density of silver nanosheets is small, and the silver nanostructure is not conducive to the detection of SERS technology, so as to achieve good SERS signal uniformity Reproducibility and repeatability, the effect of strong surface-enhanced Raman scattering

Active Publication Date: 2016-11-09
HEFEI GUOXUAN HIGH TECH POWER ENERGY
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Researchers have used metals such as zinc, copper, and iron to prepare silver micro-nano-structured SERS substrates with various morphologies, such as replacing silver nitrate with zinc flakes or copper flakes, without adding surfactants. Silver dendrites or flower cluster micro-nano structures were prepared (Appl. Phys. Lett. 89 (2006) 173104-173103; Chem. Commun. (2008) 2692-2694), although these dendrite or flower cluster structures have good SERS activity, but the homogeneity of the structure of silver branches or flower clusters cannot be guaranteed, so the repeatability of the SERS signal cannot be guar...

Method used

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  • Preparation method and application of silver nano flower clusters/silver micro pieces of graded structures
  • Preparation method and application of silver nano flower clusters/silver micro pieces of graded structures
  • Preparation method and application of silver nano flower clusters/silver micro pieces of graded structures

Examples

Experimental program
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Effect test

Embodiment 1

[0027] (1) Pretreatment of aluminum flakes: Cut the aluminum flakes into circular pieces with a diameter of 3 cm, first ultrasonically clean them in acetone for 40 minutes, then wash them several times with distilled water; then ultrasonically clean them in ethanol for 40 minutes, and then wash them with distilled water Several times, a clean aluminum sheet is obtained.

[0028] (2) Preparation of silver seed crystals: configure 5×10 -4 M Sodium borohydride (NaBH 4 ) solution, stand for 2 hours before use; take 0.005 g of silver nitrate and 0.04 g of PVP into 80 mL of deionized water, stir until completely dissolved; take 20 mL of 5×10 -4 M NaBH 4 The solution was quickly added to the mixed solution of silver nitrate and PVP, stirred at 800rpm for 10 minutes, and then left to stand for 24 hours to obtain silver seed crystals.

[0029] Such as figure 2 It can be seen that the size of the seed crystal is relatively uniform, and the average diameter is about 15nm.

[0030...

Embodiment 2

[0042] (1) Pretreatment of aluminum flakes: cut the aluminum flakes into circular slices with a diameter of 5 cm, first ultrasonically clean them in acetone and then wash them with distilled water for 3 times; then wash them with distilled water for 5 times after ultrasonic cleaning in ethanol, Clean aluminum flakes.

[0043] (2) Preparation of silver seed crystals: the concentration is 5×10 in an ice-water bath -4 Sodium borohydride solution of M (NaBH 4 ), stand still for 2 hours; get 0.005 grams of silver nitrate and 0.03 grams of PVP into deionized water, stir until completely dissolved; then quickly add sodium borohydride solution, so that the mass ratio of sodium borohydride to silver nitrate is 0.5:13, then stirred at 800 rpm for 10 minutes, and stood still for 24 hours to obtain silver seed crystals.

[0044] (3) Spin coating: drop 200 µL of silver seed crystal colloidal solution onto an aluminum sheet fixed on a spin coater, spin coat at a speed of 1000 rpm for 3 m...

Embodiment 3

[0048] (1) Pretreatment of aluminum flakes: cut the aluminum flakes into circular slices with a diameter of 4 cm, first ultrasonically clean them in acetone and then wash them with distilled water for 5 times; then ultrasonically clean them in ethanol and wash them with distilled water for 4 times, Clean aluminum flakes.

[0049] (2) Preparation of silver seed crystals: the concentration is 5×10 in an ice-water bath -4 Sodium borohydride solution of M (NaBH 4 ), stand still for 2 hours; get 0.005 gram of silver nitrate and 0.1 gram of PVP into deionized water, stir until completely dissolved; then quickly add sodium borohydride solution, so that the mass ratio of sodium borohydride to silver nitrate is 2:13, then stirred at 800rpm for 10 minutes, and left to stand for 24 hours to obtain silver seed crystals.

[0050] (3) Spin coating: drop 300 µL of silver seed crystal colloidal solution onto an aluminum sheet fixed on a spin coater, spin coat at a speed of 1500 rpm for 5 m...

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Abstract

The invention relates to a preparation method and application of silver nano flower clusters/silver micro pieces of graded structures. The preparation method comprises the steps that silver nitrate and polyvinylpyrrolidone are added into deionized water according to the mass ratio of 0.5:(3-10) and then stirred till the silver nitrate and the polyvinylpyrrolidone are completely dissolved; then a sodium borohydride solution is added rapidly, and stirring and standing are conducted, so that silver seed crystals are obtained; and the clean surface of an aluminum sheet is spin-coated with the silver seed crystals through a spin coating instrument; and the aluminum sheet spin-coated with the silver seed crystals is placed in a mixed deposition solution for a standing reaction for at least 120 minutes, then in-situ growth of the silver nano flower clusters/silver micro pieces of the graded structures on the surface of the aluminum sheet is achieved, and the aluminum sheet with the silver nano flower clusters/silver micro pieces of the graded structures can serve as a substrate for surface enhanced raman scattering spectrum detection of a low-concentration electrolyte additive, namely 1,3-propane sultone. The preparation method is simple, the cost is low, and the preparation cycle is short; and in addition, the silver nano flower clusters/silver micro pieces with the same morphology are evenly distributed on the surface of the aluminum sheet, and the good SERS signal uniformity and repeatability of the substrate are guaranteed.

Description

technical field [0001] The invention relates to the field of analysis technology, in particular to a preparation method of hierarchically structured silver nanoflower clusters / silver microsheets and its application to low-concentration detection of electrolyte additive 1,3-propane sultone. Background technique [0002] At present, the component analysis of lithium-ion battery electrolyte additives is mainly based on traditional gas chromatography, gas chromatography / mass spectrometry, and high performance liquid chromatography. Although these detection methods can realize the detection of electrolyte additives in the laboratory, the extraction and pretreatment process of the sample is relatively cumbersome, the detection time is long, and it is not suitable for in-situ and on-site rapid analysis. Surface-enhanced Raman scattering spectroscopy (SERS) technology is one of the most sensitive analytical techniques with rapid, high-sensitivity, and fingerprint-identifying detec...

Claims

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Application Information

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IPC IPC(8): B22F9/24B22F1/00G01N21/65B82Y40/00B82Y30/00
CPCG01N21/658B82Y30/00B82Y40/00B22F9/24B22F1/0553B22F1/054
Inventor 李中波夏劲
Owner HEFEI GUOXUAN HIGH TECH POWER ENERGY
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