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A kind of MOF-noble metal composite SERS substrate and preparation method thereof

A MOF-, precious metal technology, applied in the field of MOF-precious metal composite SERS substrate and its preparation, can solve the problems of large specific surface area, large porosity, weak binding ability, poor detection signal, etc., and achieve high porosity, high repetition rate, specific The effect of surface area reduction

Active Publication Date: 2020-09-04
ZHONGBEI UNIV
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  • Application Information

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Problems solved by technology

The composite particles combine the large specific surface area and high porosity of MOF materials, which can effectively adsorb and enrich the analyte molecules and the excellent surface plasmon properties of gold nanoparticles, which significantly improves the sensitivity of the composite SERS substrate for the detection of organic pollutants and solves the problem At present, the weak binding ability between polycyclic aromatic hydrocarbons and traditional precious metal materials and the poor detection signal have successfully realized the rapid, direct and highly sensitive SERS detection of polycyclic aromatic hydrocarbons.

Method used

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  • A kind of MOF-noble metal composite SERS substrate and preparation method thereof
  • A kind of MOF-noble metal composite SERS substrate and preparation method thereof
  • A kind of MOF-noble metal composite SERS substrate and preparation method thereof

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preparation example Construction

[0029] The preparation method of described MOF-AuNPs composite SERS substrate, comprises the steps:

[0030] ① Preparation of MIL-101: Add 5mmol of chromium nitrate nonahydrate, hydrofluoric acid, terephthalic acid and 24mL of deionized water into the reaction kettle, keep the temperature at 220°C for 12h, then gradually cool down to 150°C within 1h, Slowly drop to room temperature within 12h. The product was centrifuged to obtain MIL-101(Cr) powder. Disperse 1 mg of MIL-101(Cr) powder in 10 mL of methanol to obtain a MIL-101(Cr) methanol dispersion with a concentration of 0.1 mg / mL.

[0031] (1) Preparation of AuNPs: Rapidly add sodium borohydride (0.01M, 0.6mL) solution at 2-4°C to tetrachloroauric acid (0.01M, 0.25mL) and CTAB (0.1M, 7.5mL) by seed growth method ) in the mixed solution, vigorously stirred for 1 min, and stood at room temperature for 1 h to obtain gold seeds.

[0032] Add CTAB (0.1M, 6.4mL), tetrachloroauric acid (0.01M, 6.8mL), and ascorbic acid (0.1M, 3...

Embodiment 1

[0040] The preparation of gold seed, its step is:

[0041] Quickly add sodium borohydride (0.01M, 0.6mL) solution at 2-4°C to a mixed solution of tetrachloroauric acid (0.01M, 0.25mL) and CTAB (0.1M, 7.5mL), stir vigorously for 1min, and After standing for 1 h, gold seeds (8.35 mL) were obtained.

Embodiment 2

[0043] The preparation of gold seed growth solution, its step is:

[0044] Add CTAB (0.1M, 6.4mL), tetrachloroauric acid (0.01M, 6.8mL), and ascorbic acid (0.1M, 3.8mL) to 32 mL of ultrapure water in sequence to prepare a gold seed growth solution (49 mL).

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Abstract

The invention relates to the field of MOF-noble metal nanocomposite materials, in particular to a MOF-noble metal composite SERS substrate and a preparation method thereof. In the alcohol solution, the CTAB-modified positively charged noble metal nanoparticles were supported on the surface of the MOF material through electrostatic interaction to form a MOF-noble metal nanocomposite SERS substrate. Compared with the in-situ growth method, the present invention loads noble metal nanoparticles on the surface of MOF through electrostatic interaction, while maintaining the high porosity, specific surface area and excellent adsorption capacity of MOF materials, it can achieve the metal nanoparticles on the surface of MOF. The shape, size and density can be precisely controlled to prepare a large number of Raman active sites, which can further effectively improve the SERS performance of the composite substrate. The MOF-AuNPs composite SERS substrate prepared by the present invention has dual functions of adsorption enrichment and Raman enhancement, without surface modification, and can realize direct and highly sensitive detection of molecules such as fluoranthene.

Description

technical field [0001] The invention relates to the field of MOF-noble metal nanocomposite materials, in particular to a MOF-noble metal composite SERS substrate and a preparation method thereof. Background technique [0002] Surface-enhanced Raman scattering technology is an ultrasensitive and non-destructive molecular detection technology, which is widely used in chemical sensing, biomedicine, environmental pollutant detection and other fields. Nowadays, it is still an important challenge to prepare SERS substrates with high sensitivity, good reproducibility and high stability to realize rapid, direct and highly sensitive detection of environmental organic pollutants. Polycyclic aromatic hydrocarbons, a product of petroleum combustion, have poor adsorption to the surface of traditional noble metal SERS substrates, and it is difficult to reach the local surface plasmon resonance region, and the SERS effect is weak. At present, surface modification-the method of introducing...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/65B22F9/24B22F1/00B82Y30/00B82Y40/00
CPCG01N21/658B82Y30/00B82Y40/00B22F9/24B22F1/07B22F1/054
Inventor 刘亚青张丛筠刘晓宇赵贵哲
Owner ZHONGBEI UNIV
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