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Preparation method of SERS substrate of Ti/TiOx/Ag hybrid composite material

A composite material and substrate technology, which is used in analytical materials, material excitation analysis, metal material coating processes, etc., can solve the problems of cumbersome substrate solutions, low detection sensitivity, and low detection sensitivity of SERS substrates.

Inactive Publication Date: 2020-10-27
言谱物(杭州)智能科技有限责任公司
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Problems solved by technology

For example, the Chinese patent number is 201510693040.3, and the patent name is "A kind of Ag / TiO 2 Flexible, reusable SERS substrate and its preparation method", specifically proposed a preparation of Ag / TiO 2 Flexible, reusable SERS substrates, but experimentally prepared Ag / TiO 2 The substrate scheme is cumbersome; the light source used for nano-silver modification is a xenon arc lamp, and the intrinsic stability of the spectrum of the xenon arc light source is worse than that of the ultraviolet light; and the actual detection sensitivity of the SERS substrate is not high
Another example is that the Chinese patent number is 201810556666.3, and the patent name is "Nano-Silver Modified Titanium Dioxide Nanosheet Array SERS Substrate Material and Its Preparation Method and Application", which specifically prepared TiO grown on the surface of carbon paper. 2 Although the SERS substrate of the ordered nanosheet array also uses titanium foil as the titanium source for the hydrothermal synthesis reaction, there are problems of cumbersome preparation for subsequent experiments and low actual detection sensitivity.
Therefore, the SERS active substrate based on rough noble metal and semiconductor composites remains to be studied.

Method used

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  • Preparation method of SERS substrate of Ti/TiOx/Ag hybrid composite material
  • Preparation method of SERS substrate of Ti/TiOx/Ag hybrid composite material
  • Preparation method of SERS substrate of Ti/TiOx/Ag hybrid composite material

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preparation example Construction

[0030] A preparation method of a SERS substrate of a Ti / TiOx / Ag hybrid composite material, comprising the following steps:

[0031] Step 1: Weigh the NaOH solid in a beaker, and configure an aqueous NaOH solution with a concentration of 0.5mol / L-5mol / L;

[0032] Step 2: Place the cleaned and dried titanium foil with a size of 0.5cm*0.5cm*0.1mm in a Teflon-lined stainless steel autoclave pre-filled with a volume of 30mL NaOH aqueous solution;

[0033] Step 3: Place the Teflon-lined stainless steel autoclave in step 2 in a blast drying oven for hydrothermal synthesis reaction. The temperature of the hydrothermal synthesis reaction is set at 200°C for 6 hours to obtain Ti / TiOx nano membrane;

[0034] Step 4: Take out the Ti / TiOx nano-membrane and immerse it in 30mL, 0.1mol / L HNO 3 Acid-base neutralization reaction in the solution for 2 hours;

[0035] Step 5: Repeat step 4 1-2 times until the acid-base neutralization reaction is completed, clean the Ti / TiOx nano-film with deio...

Embodiment 1

[0042] Weigh the NaOH solid powder in a beaker, and configure a NaOH aqueous solution with a concentration of 0.5mol / L; place the cleaned and dried titanium foil with a size of 0.5cm*0.5cm*0.1mm in the pre-filled NaOH with a volume of 30mL A Teflon-lined stainless steel autoclave for aqueous solution; place the Teflon-lined stainless steel autoclave in a blast drying oven, the reaction time is 6 hours, and the reaction temperature is 200 ° C; the Ti / TiOx nano-film obtained by the reaction is immersed in to a volume of 30mL and a concentration of 0.1mol / L of HNO 3 In the solution for 2 hours, and repeat 1-2 times until the acid-base neutralization reaction is completed. Then it was washed with deionized water and dried in a vacuum oven at a drying temperature of 70° C. and a drying time of 20 minutes to obtain a neutral Ti / TiOx nano film.

[0043] figure 1 It is the SEM image of the Ti / TiOx nano-film under the condition of NaOH concentration 0.5mol / L, from which the structure...

Embodiment 2

[0045] Weigh the NaOH solid powder in a beaker, and configure a NaOH aqueous solution with a concentration of 3mol / L; place the cleaned and dried titanium foil with a size of 0.5cm*0.5cm*0.1mm in a pre-filled NaOH aqueous solution with a volume of 30mL The Teflon-lined stainless steel high-pressure reactor; the Teflon-lined stainless steel high-pressure reactor was placed in a blast drying oven, the reaction time was 6 hours, and the reaction temperature was 200 ° C; the Ti / TiOx nano-film obtained by the reaction was immersed in HNO with a volume of 30mL and a concentration of 0.1mol / L 3 In the solution for 2 hours, and repeat 1-2 times until the acid-base neutralization reaction is completed. Then it was washed with deionized water and dried in a vacuum oven at a drying temperature of 70° C. and a drying time of 20 minutes to obtain a neutral Ti / TiOx nano film.

[0046] figure 2 It is the SEM image of the Ti / TiOx nano-film under the condition of NaOH concentration 3mol / L, ...

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Abstract

The invention provides a preparation method of an SERS substrate of a Ti / TiOx / Ag hybrid composite material. The preparation method comprises the following steps of: firstly, preparing a Ti / TiOx nano-film from a titanium foil and a NaOH solution through a hydrothermal synthesis reaction at 200 DEG C for 6 hours; immersing the Ti / TiOx film into an AgNO3 solution and carrying out redox reaction for 2hours under the irradiation of an ultraviolet lamp of a three-purpose ultraviolet analyzer with the wavelength of 365nm, so as to enable nano-silver to modify in the interior of the Ti / TiOx nano-film, thereby obtaining the SERS substrate of the Ti / TiOx / Ag hybrid composite material. The SERS substrate of the Ti / TiOx / Ag hybrid composite material prepared by the invention is simple in preparation method and low in equipment requirement, and has relatively good sensitivity and relatively good uniformity and stability in real object detection.

Description

technical field [0001] The invention relates to the preparation of a SERS substrate, in particular to the preparation of a SERS substrate of a Ti / TiOx / Ag hybrid composite material, and belongs to the technical field of surface-enhanced Raman scattering spectroscopy. Background technique [0002] Over the past decades, surface-enhanced Raman scattering (SERS) has been widely used in many fields such as chemistry, pharmaceuticals, biosensing, and food safety due to its high sensitivity and fast response. At present, the SERS mechanisms generally accepted by the academic circle mainly include physical enhancement mechanism and chemical enhancement mechanism. One is the electromagnetic field enhancement (EM) mechanism: that is, when a beam of light is incident on a rough metal surface, the free electrons on the metal surface produce a surface plasmon resonance effect (LSPR) that causes the enhancement of the local electric field, making the distance from the rough metal surface ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/65C23C26/00B22F9/24
CPCG01N21/658C23C26/00B22F9/24
Inventor 张秀斌梁培黄杰
Owner 言谱物(杭州)智能科技有限责任公司
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