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
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[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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