An MOF-precious metal composite SERS substrate and a preparing method thereof
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A precious metal, MOF technology, applied in the field of MOF-precious metal composite SERS substrate and its preparation, can solve the problems of poor detection signal, large specific surface area, large porosity, weak binding ability, etc., and achieve high repetition rate, high porosity, and specific surface area. falling effect
Active Publication Date: 2017-12-15
ZHONGBEI UNIV
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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 det
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[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.
[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 32mL ultrapure water in turn to prepare a gold seed growth solution (49 mL).
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Abstract
The invention relates to the field of MOF-precious metal nanocomposites, and particularly relates to an MOF-precious metal composite SERS substrate and a preparing method thereof. In an alcohol solution, CTAB modified positive-charged precious metal nanoparticles are loaded onto the surface of an MOF material through electrostatic functions to form the MOF-precious metal composite SERS substrate. Compared with in-situ growth methods, the precious metal nanoparticles are loaded onto the surface of the MOF material through electrostatic functions in the method, a high porosity, a high specific surface area and excellent adsorption capability of the MOF material are maintained, morphology, the size and density of the metal nanoparticles on the surface of the MOF can be accurately controlled, and a large amount of Raman active sites are prepared, thus further effectively improving properties of the composite substrate SERS. The MOF-AuNPs composite SERS substrate prepared by the method has double functions including adsorption enrichment and Raman enhancement, does not need surface modification and can achieve 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...
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