SiO2@Ag@ZrO2 nano material with multilayer core-shell structure, and preparation method and application thereof

A multi-layer core-shell structure and nano-material technology, applied in the field of SERS detection, can solve the problems of uneven distribution of analytes, reduction of Raman signal, and limitation of SERS application range, etc., achieve uniform Raman signal enhancement effect, improve Raman Man enhancement effect, the effect of enhancing SERS signal

Active Publication Date: 2019-10-01
CHINA JILIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] However, there are still obvious technical defects in the SERS active substrate materials used at this stage. On the one hand, the distribution of noble metal nanoparticles in the existing SERS active substrate materials is poor, resulting in the distribution of analytes adsorbed on the SERS active substrate. inhomogeneous, making it difficult to obtain reproducible signals using surface-enhanced Raman scattering
On the other hand, noble metal nanoparticles represented by silver are easily affected by the environment, which leads to a decrease in Raman signal; and when silver nanoparticles are used as the substrate, the silver nanoparticles are easily oxidized in the air, resulting in the destruction of the substrate structure.
Therefore, when using silver nanoparticles as a SERS substrate for Raman detection, the actual test environment needs to be considered, which severely limits the practical application range of SERS.

Method used

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  • SiO2@Ag@ZrO2 nano material with multilayer core-shell structure, and preparation method and application thereof
  • SiO2@Ag@ZrO2 nano material with multilayer core-shell structure, and preparation method and application thereof
  • SiO2@Ag@ZrO2 nano material with multilayer core-shell structure, and preparation method and application thereof

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preparation example Construction

[0053] The embodiment of the present invention provides a SiO 2 @Ag@ZrO 2 The preparation method of multilayer core-shell structure nanomaterial is characterized in that it comprises the following steps:

[0054] (1) Preparation of SiO 2 Microspheres:

[0055] (11) Add TEOS to ethanol at a volume ratio of 1.5:15-16 to prepare A solution, and set aside; add ammonia water with a mass concentration of 25%-28% to ethanol at a volume ratio of 3:(13-14) Prepare B solution in, standby;

[0056] (12) Mix the above-mentioned A solution and B solution according to the volume ratio of (16.7-17): (16.7-17) under the stirring condition of rotation speed ≥ 10000rpm, stir and react at 15-25°C and 250-300rpm for 2h, The product was washed by centrifugation at 6000~8000rpm, then dissolved in ethanol, and ultrasonicated for 20min~30min to obtain monodisperse SiO 2 nanoparticles;

[0057] (13) Monodisperse SiO 2 The nanoparticles are centrifuged and dried under vacuum at 60-70°C for 1.5-2...

Embodiment 1

[0076] Embodiment 1 of the present invention provides a SiO 2 @Ag@ZrO 2 The preparation method of multilayer core-shell structure nanomaterial is characterized in that it comprises the following steps:

[0077] (1) Preparation of SiO 2 Microspheres:

[0078] (11) Add 1.5mLTEOS to 15.2mL ethanol to prepare A solution, and set aside; add 3mL of 25% ammonia water with a mass concentration of 0.5% to 13.7mL ethanol to prepare B solution, set aside;

[0079] (12) Mix the above-mentioned 16.7mL A solution and 16.7mL B solution evenly under the stirring condition of rotation speed ≥ 10000rpm, stir and react at 15°C and 250rpm for 2h, centrifuge and wash the product at 6000rpm, then dissolve it in 10ml of ethanol, and ultrasonicate for 20min to obtain monodisperse SiO 2 nanoparticles;

[0080] (13) Monodisperse SiO 2 The nanoparticles were centrifuged and dried under vacuum at 70°C for 2 hours to obtain SiO 2 Microspheres.

[0081] (2) Preparation of modified SiO 2 Microspher...

Embodiment 2

[0099] Embodiment 2 of the present invention provides a SiO 2 @Ag@ZrO 2 The preparation method of multilayer core-shell structure nanomaterial is characterized in that it comprises the following steps:

[0100] (1) Preparation of SiO 2 Microspheres:

[0101] (11) Add 1.5mLTEOS to 15mL ethanol to prepare A solution, and set aside; add 3mL of 25% ammonia water with a mass concentration of 0.5% to 13mL ethanol to prepare B solution, set aside;

[0102] (12) Mix the above-mentioned A solution and B solution evenly under the stirring condition of rotating speed ≥ 10000rpm, stir and react at 15°C and 250rpm for 2h, and centrifuge wash the product at 6000pm, then dissolve it in 10ml of ethanol, and ultrasonicate for 20min to obtain a single Dispersed SiO 2 nanoparticles;

[0103] (13) Monodisperse SiO 2 The nanoparticles were centrifuged and dried under vacuum at 60°C for 1.5h to obtain SiO 2 Microspheres.

[0104] (2) Preparation of modified SiO 2 Microspheres

[0105] (21...

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Abstract

The invention discloses a preparation method of a SiO2@Ag@ZrO2 nano material with a multilayer core-shell structure for SERS detection, and method has simple steps and convenient operation. In the prepared SiO2@Ag@ZrO2 nano material with a multilayer core-shell structure, Ag nano particles are uniformly adsorbed on the surface of a SiO2 microsphere, and SERS signals with high repeatability and strong stability can be generated, thereby having excellent Raman enhancement effect; and ZrO2 is wrapped outside, so that the stability is high, the environmental adaptability can be improved, and the Ag nano particles are protected from being damaged.

Description

technical field [0001] The invention relates to the technical field of SERS detection, more specifically to a SiO 2 @Ag@ZrO 2 Multilayer core-shell structure nanomaterials and their preparation methods and applications. Background technique [0002] Surface-enhanced Raman scattering (SERS) is a powerful vibrational spectroscopy technique that can provide non-destructive and ultrasensitive characterization at the surface of plasmonic nanostructures or at the single-molecule level The information in the wavenumber region has fingerprints, sensitivity at the single molecule level, and non-destructive data acquisition capabilities, and has broad application prospects in the fields of agricultural production, environmental monitoring, chemical analysis, and food safety. At present, noble metal nanoparticles are widely used as SERS active substrates due to their broad plasmon resonance region and the Raman signal amplification effect of surface plasmon resonance, which exhibit s...

Claims

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Application Information

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IPC IPC(8): G01N21/65B22F9/24B22F1/02B82Y30/00B82Y40/00
CPCG01N21/658B22F9/24B82Y30/00B82Y40/00B22F1/16B22F1/17
Inventor 梁培周勇峰倪德江余志张德叶嘉明
Owner CHINA JILIANG UNIV
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