CN108802007B - Surface enhanced Raman substrate with large-area nano-film structure and preparation method thereof - Google Patents

Surface enhanced Raman substrate with large-area nano-film structure and preparation method thereof Download PDF

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CN108802007B
CN108802007B CN201810626868.0A CN201810626868A CN108802007B CN 108802007 B CN108802007 B CN 108802007B CN 201810626868 A CN201810626868 A CN 201810626868A CN 108802007 B CN108802007 B CN 108802007B
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汤俊琪
石俊生
满石清
欧全宏
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Yunnan Normal University
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Abstract

The invention belongs to the technical field of Raman scattering, and discloses a surface-enhanced Raman substrate with a large-area nano-film structure and a preparation method thereof, wherein a polylysine modified glass slide is used as an initial substrate, and is placed in a chloroauric acid solution with a certain concentration after being soaked and activated in a gold seed solution; and dropwise adding a mixed solution of ascorbic acid and sodium citrate with a certain concentration ratio, so that chloroauric acid radical ions are continuously reduced into gold atoms on the polylysine modified glass slide and are aggregated and adsorbed on the glass slide to form nano gold particles, and a nano film structure with a certain surface roughness is formed. The method has the advantages of low cost, simple operation, adjustable process, good repeatability, stability and reliability.

Description

Surface enhanced Raman substrate with large-area nano-film structure and preparation method thereof
Technical Field
The invention belongs to the technical field of Raman scattering, and particularly relates to a surface enhanced Raman substrate with a large-area nano-film structure and a preparation method thereof.
Background
Currently, the current state of the art commonly used in the industry is such that:the surface-enhanced Raman spectroscopy (SERS) technology has the characteristics of simplicity, rapidness, less interference, no damage and low cost, and has been widely and deeply researched in the fields of analytical chemistry, inspection medicine, food safety, surface science and the like. One of the keys of the application of the SERS technology to the substance measurement and analysis is the preparation of a substrate, and how to prepare a substrate with a large area, stability, repeatability and uniform morphology has been a focus and focus of research. At present, although a highly repetitive SERS active substrate with a large area can be prepared by a top-down (top-down) etching technique such as photolithography and casting, the method has problems of high cost, low yield, low hot spot density, and the like, compared with a chemical self-assembly technique.
In summary, the problems of the prior art are as follows:the large-area ordered nanostructure film is prepared by technical methods of photoetching, electron beam etching, sputtering or plasma deposition, vapor deposition and the like from top to bottom, on one hand, expensive instruments and equipment and trained operation technicians are needed; on the other hand often existThe working time is long, the processing efficiency is low, and a series of problems such as micron-scale and the like are difficult to break through. Therefore, it is necessary to adopt a suitable technical means to improve the preparation efficiency of the large-area nano-film and improve the uniformity of the nano-film. The problems of high cost, low yield, low hot spot density and the like of preparing the SERS active substrate with high repeatability and large area are solved.
The difficulty and significance for solving the technical problems are as follows:
the large-area nano-film structure is prepared by the self-assembly technology, the operation equipment is simple, the preparation process is simple and controllable, and the obtained nano-film structure is stable and has high close packing degree. The application of the nano film in the fields of optics, catalysis, sensing analysis and the like is promoted.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a surface enhanced Raman substrate with a large-area nano-film structure and a preparation method thereof.
The invention is realized in such a way that the preparation method of the surface enhanced Raman substrate with the large-area nano-film structure comprises the following steps: adopting a polylysine modified glass slide as an initial substrate, soaking and activating the glass slide in a certain volume of nano-gold seed solution, and then placing the glass slide in a chloroauric acid solution with a certain concentration; and dropwise adding a mixed solution of ascorbic acid and sodium citrate with a certain concentration ratio, so that chloroauric acid radical ions are continuously reduced to form nanogold on the polylysine modified glass slide and adsorbed on the glass slide to form a nanomembrane structure with a certain surface roughness.
The method comprises the following specific steps:
1) cutting the common polylysine modified carrier into 2 × 2cm pieces with a glass knife2The left and right small blocks are reserved.
2) 0.025mM chloroauric acid (HAuCl) in 10mL4) To the solution was added 100. mu.L of 1% (w/v mass/volume concentration) sodium citrate (Na)3Cit) solution and stirring well, then 500. mu.L of 10mM ice-bath sodium borohydride (NaBH) was added rapidly4) The solution is added after 30min of reactionSoaking the small polylysine modified slide in a refrigerator at 6 ℃ overnight to promote the surface amino group (-NH) of the polylysine modified slide2) Activation and hydrophilic properties of (a).
3) The soaked slide glass was rinsed with pure water and immersed in 10mL of 10-4M in chloroauric acid, and 10mL of a mixed solution of ascorbic acid and sodium citrate was added dropwise at the same time using a micro syringe pump. Wherein the dropping speed of the micro-injection pump is 20mL/h, and Ascorbic Acid (AA) and sodium citrate (Na)3Cit) at a concentration of 0.05% and 0.025%, respectively (both in mass volume percent, w/v). After the dropwise addition is finished, standing the solution for a certain time to finish the in-situ reduction self-assembly process of the gold nanoparticles to obtain a large-area nano-film structure, taking out the slide covered with the large-area nano-film structure, washing the slide with ultrapure water, drying the slide with nitrogen, and hermetically storing the slide for later use.
4) Placing the glass slide plated with the large-area nano structure at 10-5And soaking the crystal violet solution of M in the crystal violet solution for 15min, taking out, washing with ultrapure water, drying with nitrogen, and testing by integrating for 5s under a laser Raman spectrometer with the wavelength of 532nm to obtain a Surface Enhanced Raman Spectrum (SERS).
In summary, the advantages and positive effects of the invention are:the method has the advantages of low cost, simple operation, adjustable process, good repeatability, stability and reliability.
The large-area nano-film structure is prepared by adopting an in-situ reduction self-assembly method, and the size, the inter-particle distance and the close packing degree of the nano-particles on the nano-film structure can be regulated and controlled by controlling the self-assembly time. The method is simple, safe and convenient to operate, and experimental parameters are easy to control. The macro size of the prepared large-area nano film structure is about 4cm2The close packing degree is high; the distance between the particles is about 20nm, and the overall appearance is uniform.
By controlling the soaking time of the glass slide after dripping the ascorbic acid and sodium citrate mixed solution, the gold ions can be reduced in situ and self-assembled into a large-area nano structure, and the purposes of improving the close packing degree, the particle spacing, the particle size and the like of the large-area nano structure film are achieved.
The gold chlorate ions are reduced in situ, and meanwhile, the large-area nano gold structure film is self-assembled. The nanostructure film substrate has good SERS performance, and SERS signals of 53 sample points are randomly tested on the substrate (based on Raman shift peaks such as 1621.9 cm)-1) Is less than 10%.
Drawings
Fig. 1 is a flowchart of a method for preparing a surface enhanced raman substrate with a large-area nanomembrane structure according to an embodiment of the present invention.
FIG. 2 is a UV-Vis spectrum (UV-Vis) of the surface enhanced Raman substrate with a large-area nano-film structure provided by the embodiment of the invention
Fig. 3 is a Scanning Electron Micrograph (SEM) of a surface enhanced raman substrate of a large area nanomembrane structure provided by an embodiment of the present invention.
FIG. 4 is a surface enhanced Raman substrate pair 10 with a large-area nanomembrane structure according to an embodiment of the present invention-5The test effect graph of (1) Crystal Violet (CV).
Fig. 5 is a TEM image of the nanogold seed synthesized in the example of the invention.
Fig. 6 is a schematic diagram of a method for preparing a surface enhanced raman substrate with a large-area nanomembrane structure according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The surface enhanced Raman substrate with the large-area nano-film structure provided by the embodiment of the invention is a SERS substrate with a surface enhanced Raman scattering activity, and is a nano-film structure.
As shown in fig. 1, the method for preparing a surface enhanced raman substrate with a large-area nanomembrane structure provided by the embodiment of the present invention includes the following steps:
s101: adopting a polylysine modified glass slide as an initial substrate, soaking and activating the glass slide in a certain volume of nano-gold seed solution, and then placing the glass slide in a chloroauric acid solution with a certain concentration;
s102: and dropwise adding a mixed solution of ascorbic acid and sodium citrate with a certain concentration ratio, so that chloroauric acid radical ions are continuously reduced to form nanogold on the polylysine modified glass slide and adsorbed on the glass slide to form a nanomembrane structure with a certain surface roughness.
The invention is further described with reference to specific examples.
Example 1
1) Cutting the common polylysine modified carrier into 2 × 2cm pieces with a glass knife2The left and right small blocks are reserved.
2) 0.025mM chloroauric acid (HAuCl) in 10mL4) To the solution was added 100. mu.L of a 1% sodium citrate solution and stirred well, followed by rapid addition of 500. mu.L of 10mM sodium borohydride (NaBH) in an ice bath4) Reacting the solution for 30min, adding the small polylysine-modified slide glass, and soaking in a refrigerator at 6 deg.C overnight to promote the amino group (-NH) on the surface of the polylysine-modified slide glass2) Activation and hydrophilic properties of (a).
3) The soaked slide glass was rinsed with pure water and immersed in 10mL of 10-4M in chloroauric acid. Simultaneously, 10mL of the mixed solution of ascorbic acid and sodium citrate is dropwise added by a micro-injection pump, the dropping speed of the micro-injection pump is 20mL/h, and the concentrations of the ascorbic acid and the sodium citrate are 0.05 percent and 0.025 percent respectively. Standing for 30min after the dropwise addition is completed to obtain a large-area nano-film structure (as shown in figure 3A), taking out the slide covered with the large-area nano-structure, washing with ultrapure water, blow-drying with nitrogen, and hermetically storing.
4) Placing the glass slide plated with the large-area nano structure at 10-5Soaking the crystal violet solution of M in the solution for 15min, taking out, washing with ultrapure water, drying with nitrogen, performing a test by integrating 5s under a laser Raman spectrometer with the wavelength of 532nm, and randomly selecting 53 points from the substrate to obtain a Surface Enhanced Raman Spectrum (SERS) and a statistical analysis result thereof, as shown in FIG. 4.
Example 2
1)Cutting the common polylysine modified carrier into 2 × 2cm pieces with a glass knife2The left and right small blocks are reserved.
2) 0.025mM chloroauric acid (HAuCl) in 10mL4) To the solution was added 100. mu.L of a 1% sodium citrate solution and stirred well, followed by rapid addition of 500. mu.L of 10mM sodium borohydride (NaBH) in an ice bath4) Reacting the solution for 30min, adding the small polylysine-modified slide glass, and soaking in a refrigerator at 6 deg.C overnight to promote the amino group (-NH) on the surface of the polylysine-modified slide glass2) Activation and hydrophilic properties of (a).
3) The soaked slide glass was rinsed with pure water and immersed in 10mL of 10-4M in chloroauric acid. Simultaneously, 10mL of the mixed solution of ascorbic acid and sodium citrate is dropwise added by a micro-injection pump, the dropping speed of the micro-injection pump is 20mL/h, and the concentrations of the ascorbic acid and the sodium citrate are 0.05 percent and 0.025 percent respectively. Standing for 2h after the dropwise addition is completed to obtain a large-area nano-film structure (as shown in figure 3B), taking out the slide covered with the large-area nano-structure, washing with ultrapure water, blow-drying with nitrogen, and hermetically storing.
4) Placing the glass slide plated with the large-area nano structure at 10-5And soaking the crystal violet solution of M in the crystal violet solution for 15min, taking out, washing with ultrapure water, drying with nitrogen, integrating for 5s under a laser Raman spectrometer with the wavelength of 532nm for testing, and randomly selecting 10 points on the substrate to obtain a Surface Enhanced Raman Spectrum (SERS) of the substrate.
Example 3
1) Cutting the common polylysine modified carrier into 2 × 2cm pieces with a glass knife2The left and right small blocks are reserved.
2) 0.025mM chloroauric acid (HAuCl) in 10mL4) To the solution was added 100. mu.L of a 1% sodium citrate solution and stirred well, followed by rapid addition of 500. mu.L of 10mM sodium borohydride (NaBH) in an ice bath4) Reacting the solution for 30min, adding the small polylysine-modified slide glass, and soaking in a refrigerator at 6 deg.C overnight to promote the amino group (-NH) on the surface of the polylysine-modified slide glass2) Activation and hydrophilic properties of (a).
3) The soaked slide glass was rinsed with pure water and immersed in 10mL of 10-4M in chloroauric acid. Simultaneously, 10mL of the mixed solution of ascorbic acid and sodium citrate is dropwise added by a micro-injection pump, the dropping speed of the micro-injection pump is 20mL/h, and the concentrations of the ascorbic acid and the sodium citrate are 0.01 percent and 0.025 percent respectively. Standing for 2h after the dropwise addition is completed to obtain a large-area nano-film structure, taking out the slide covered with the large-area nano-structure, washing with ultrapure water, drying with nitrogen, and hermetically storing.
4) Placing the glass slide plated with the large-area nano structure at 10-5And soaking the crystal violet solution of M in the solution for 15min, taking out, washing with ultrapure water, drying with nitrogen, integrating for 5s under a laser Raman spectrometer with the wavelength of 532nm for testing, and randomly selecting 10 points from the substrate to obtain a Surface Enhanced Raman Spectrum (SERS).
Example 4
1) Cutting the common polylysine modified carrier into 2 × 2cm pieces with a glass knife2The left and right small blocks are reserved.
2) 0.025mM chloroauric acid (HAuCl) in 10mL4) To the solution was added 100. mu.L of a 1% sodium citrate solution and stirred well, followed by rapid addition of 500. mu.L of 10mM sodium borohydride (NaBH) in an ice bath4) Reacting the solution for 30min, adding the small polylysine-modified slide glass, and soaking in a refrigerator at 6 deg.C overnight to promote the amino group (-NH) on the surface of the polylysine-modified slide glass2) Activation and hydrophilic properties of (a).
3) The soaked slide glass was rinsed with pure water and immersed in 10mL of 10-4M in chloroauric acid. Simultaneously, 10mL of the mixed solution of ascorbic acid and sodium citrate is dropwise added by a micro-injection pump, the dropping speed of the micro-injection pump is 20mL/h, and the concentrations of the ascorbic acid and the sodium citrate are 0.05 percent and 0.05 percent respectively. Standing for 2h after the dropwise addition is completed to obtain a large-area nano-film structure, taking out the slide covered with the large-area nano-structure, washing with ultrapure water, drying with nitrogen, and hermetically storing.
4) Placing the glass slide plated with the large-area nano structure into 10-5Immersing in crystal violet solution of MTaking out after soaking for 15min, washing with ultrapure water, drying with nitrogen, integrating for 5s under a laser Raman spectrometer with the wavelength of 532nm for testing, and randomly selecting 10 points on the substrate to obtain a Surface Enhanced Raman Spectrum (SERS).
Example 5
1) Cutting the common polylysine modified carrier into 2 × 2cm pieces with a glass knife2Soaking the small pieces in pure water for 2 hr to promote polylysine to modify the surface amino groups (-NH)2) Activation and hydrophilic properties of (a).
2) The soaked slide is taken out and immersed into 10mL of glass with the concentration of 10-4M in chloroauric acid. Simultaneously, 10mL of the mixed solution of ascorbic acid and sodium citrate is dropwise added by a micro-injection pump, the dropping speed of the micro-injection pump is 20mL/h, and the concentrations of the ascorbic acid and the sodium citrate are 0.05 percent and 0.025 percent respectively. Standing for 24h after the dropwise addition is completed to obtain a large-area nano-film structure, taking out the slide covered with the large-area nano-structure, washing with ultrapure water, drying with nitrogen, and hermetically storing.
4) Placing the glass slide plated with the large-area nano structure at 10-5And soaking the crystal violet solution of M in the solution for 15min, taking out, washing with ultrapure water, drying with nitrogen, integrating for 5s under a laser Raman spectrometer with the wavelength of 532nm for testing, and randomly selecting 10 points from the substrate to obtain a Surface Enhanced Raman Spectrum (SERS).
Example 6
1) Cutting the common polylysine modified carrier into 2 × 2cm pieces with a glass knife2Soaking the small pieces in pure water for 2 hr to promote polylysine to modify the surface amino groups (-NH)2) Activation and hydrophilic properties of (a).
2) The soaked slide was removed and immersed in 10mL of 10-4M in chloroauric acid. Simultaneously, 10mL of the mixed solution of ascorbic acid and sodium citrate is dropwise added by a micro-injection pump, the dropping speed of the micro-injection pump is 20mL/h, and the concentrations of the ascorbic acid and the sodium citrate are 0.05 percent and 0.025 percent respectively. Standing for 10h after the dropwise addition is finished to obtain a large-area nano-film structure, taking out the nano-film structure, and covering a large surfaceAnd (4) accumulating the nano-structured slide, washing with ultrapure water, drying with nitrogen, and hermetically storing.
4) Placing the glass slide plated with the large-area nano structure at 10-5And soaking the crystal violet solution of M in the solution for 15min, taking out, washing with ultrapure water, drying with nitrogen, integrating for 5s under a laser Raman spectrometer with the wavelength of 532nm for testing, and randomly selecting 10 points from the substrate to obtain a Surface Enhanced Raman Spectrum (SERS).
The curves in fig. 2 respectively show the ultraviolet-visible absorption spectrum of the nanomembrane after 30min of in-situ reduction self-assembly in example 1 and the nanomembrane after 2h of in-situ reduction self-assembly in example 2, and the absorption spectrum of the glass.
FIG. 3A is the SEM topography of the nano-film after 30min of in-situ reduction self-assembly in example 1, and it can be seen that the nano-film is completely covered and the nano-particles are highly densely packed. And 3B is an SEM topography of the nano film after in-situ reduction self-assembly for 2h, and can be seen that the nano particle close packing degree of the in-situ reduction self-assembly is further enhanced, and the particle size is obviously increased.
FIG. 4 is a graph of SERS spectra of the nanofilm of example 1 and a statistical analysis of its Raman-shifted peaks. FIG. 5 is a transmission electron micrograph of gold seeds of examples 1 to 4.
Fig. 6 is a schematic diagram of a method for preparing a surface enhanced raman substrate with a large-area nanomembrane structure according to an embodiment of the present invention.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.

Claims (2)

1. A preparation method of a surface enhanced Raman substrate with a large-area nano-film structure is characterized by comprising the following steps: adopting a polylysine modified glass slide as an initial substrate, soaking and activating the glass slide in a gold seed solution, and then placing the glass slide in a chloroauric acid solution with a certain concentration; dropwise adding a mixed solution of ascorbic acid and sodium citrate with a certain concentration ratio, so that chloroauric acid radical ions are continuously reduced to form nanogold on a polylysine modified glass slide and adsorbed on the glass slide to form a nanomembrane structure with a certain surface roughness;
the preparation method of the surface enhanced Raman substrate with the large-area nano-film structure comprises the following specific steps:
1) cutting polylysine modified carrier pieces into 2 x 2cm pieces with a glass knife2The small blocks are reserved;
2) adding 100 mu L of 1% mass volume percentage concentration (w/v) sodium citrate solution into 10mL of 0.025mM chloroauric acid solution, stirring uniformly, then quickly adding 500 mu L of 10mM ice bath sodium borohydride solution, reacting for 30min, adding the small polylysine modified slide glass, soaking in a refrigerator at 6 ℃ overnight to promote the surface amino group-NH of the polylysine modified slide glass2Activation and hydrophilic properties of (a);
3) the soaked slide glass was rinsed with pure water and immersed in 10mL of 10-4Simultaneously dropwise adding 10mL of a mixed solution of ascorbic acid and sodium citrate into the M chloroauric acid solution by using a micro-injection pump, wherein the dropping speed of the micro-injection pump is 20mL/h, the concentrations of the ascorbic acid and the sodium citrate are respectively 0.05 percent and 0.025 percent, and the concentrations are mass volume percentage concentrations and w/v; after the dropwise addition is finished, standing the solution for a certain time to finish the in-situ reduction self-assembly process of the nano gold particles, namely obtaining a large-area nano membrane structure, taking out the slide covered with the large-area nano gold structure, washing the slide with ultrapure water, drying the slide with nitrogen, and hermetically storing the slide for later use;
4) placing the glass slide plated with the large-area nano structure at 10-5Soaking the crystal violet solution of M in the crystal violet solution for 15min, taking out, washing with ultrapure water, drying with nitrogen, and testing by integrating for 5s under a laser Raman spectrometer with the wavelength of 532nm to obtain a surface enhanced Raman spectrum;
the preparation method of the surface enhanced Raman substrate with the large-area nano-film structure has the advantages of low cost, simple operation, adjustable technological process, good repeatability, stability and reliability.
2. The method for preparing the surface-enhanced Raman substrate with the large-area nano-film structure according to claim 1, and the surface-enhanced Raman substrate with the large-area nano-film structure.
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