CN108226123B - Method for preparing surface enhanced Raman scattering substrate by femtosecond laser - Google Patents
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Abstract
The invention relates to the technical field of nano material processing, in particular to a method for preparing a surface enhanced Raman scattering substrate by femtosecond laser, which comprises the steps of preparing a film forming solution → preparing an Ag/PVP film → etching the film by femtosecond laser → developing to obtain the surface enhanced Raman scattering substrate.
Description
Technical Field
The invention relates to the technical field of nano material processing, in particular to a method for preparing a surface enhanced Raman scattering substrate by femtosecond laser.
Background
In recent years, there is an increasing amount of literature on the study of Surface Enhanced Raman Scattering (SERS) effects, and an important feature of SERS technology is that it has an active substrate, i.e., an analyte molecule is adsorbed onto the surface of the substrate to exhibit a strong raman enhancing effect. Therefore, the carrier adsorbed by the molecule is very critical, and the research on the novel and efficient active substrate is always a hotspot in the research on the SERS field. The continued discovery of new active substrates expands the range of applications of SERS technology. An excellent active substrate should have the following characteristics: the preparation cost is low, the preparation process is simple, the used reagent is green and pollution-free, the use and the storage are convenient, and the strong enhancement capability and the excellent stability and the reproducibility are realized. Therefore, the preparation of active substrates with the above-mentioned excellent properties has been a goal pursued by SERS researchers.
SERS is a surface effect, and the preparation of a substrate determines the application prospect of SERS. In the study of surface enhanced raman spectroscopy, an important phenomenon was found, namely the "hot spot" phenomenon. The preparation of the high-activity SERS substrate with multiple hot spots and controllable distribution is a difficult problem to be overcome in the technical field. Noble metal colloids are the most widely used and most convenient active substrate to prepare, and are mainly concentrated on the preparation of noble metal particles, roughened electrodes, films and the like at present. Although the classical preparation of gold and silver colloid is relatively simple, the morphology and aggregation degree of the aggregate are not controllable after the substrate is added with an analyte, and the SERS reproducibility is poor. The preparation method of the rough and super-modified electrode is simple and rapid, but the controllability is not strong, the order and the uniformity of an active substrate cannot be ensured, the surface appearance of the substrate is disordered, the influence factors are many, and the reproducibility is poor.
Moreover, as the most commonly used micro-nano structure of silver, the silver is easily oxidized in the air, so that the chemical stability of the silver is poor, and the long-term use of the silver is severely restricted. Thus, various attempts have been made to improve the chemical stability of silver substrates, while avoiding significant negative effects on their raman enhancing effect. To achieve this, the most common method at present is to cover the silver substrate with a stable protective layer, and the common cover layer is made of carbon film materials such as titanium dioxide, silicon dioxide, aluminum oxide, and graphene, however, this method has the most important problem that the preparation process is complex, complicated, and time-consuming to form a stable, ultra-thin, and non-porous protective layer, and in addition, such preparation process requires special treatment of the substrate in advance, and the preparation process also requires strict control of the reaction conditions, and the reaction time is long.
Therefore, there is a need to find a simple and feasible method for preparing a silver substrate with improved stability and without significant influence on the raman enhancement capability of silver.
Disclosure of Invention
In view of the above, there is a need to provide a method for preparing a surface enhanced raman scattering substrate by using a femtosecond laser.
In order to achieve the purpose, the invention adopts the following technical scheme:
the method for preparing the surface enhanced Raman scattering substrate by the femtosecond laser comprises the following steps:
step 1) preparation of film forming liquid: preparing an aqueous solution containing polyvinylpyrrolidone and silver nitrate;
step 2) film preparation: spin-coating the film-forming liquid drop on a film-forming substrate, and drying to obtain a film;
step 3) etching: the film is placed on a three-dimensional nanometer displacement table, femtosecond pulse laser direct writing is adopted, and a large-area silver nanometer structure can be etched by scanning on the film;
step 4) developing: and placing the etched film in ethanol for soaking for a period of time, taking out, placing in hot water for soaking for a period of time, taking out, and drying to obtain the silver micro-nano structure substrate.
Further, in the deposition solution: the molar concentration range of the polyvinylpyrrolidone is 0.18-0.22 mol/L; the molar concentration range of the silver nitrate is 0.1-0.2 mol/L.
In the invention, the PVP content is too low, and the film forming property is not good; the PVP content is too high, so that silver nanoparticle clusters become large, and the Raman enhancement becomes poor;
the concentration of silver nitrate is too low, the content of silver is low, so that reduced silver nanoparticles are reduced, the space between the formed silver nanoparticles is enlarged, and the silver is not favorable for being used as a Raman enhancement substrate; conversely, if the concentration is too high, the silver content is too high, resulting in large clusters of reduced silver nanoparticles and poor uniformity and poor raman enhancement.
Preferably, in the deposition solution: the molar concentration of the polyvinylpyrrolidone is 0.19 mol/L; the molar concentration of the silver nitrate is 0.2 mol/L.
Further, in the film forming solution in the step 1), the molar concentration ratio of PVP to silver nitrate is 1: 1-2: 1.
Preferably, the molar concentration ratio of PVP to silver nitrate in the deposition solution is 1: 1.
Further, the laser power in the step 3) is 10-40 mw; the scanning distance is 0.2-0.8 um.
In the invention, the laser power influences the structure of silver to a certain extent, the structure of the silver nanoparticles is in a state of good Raman enhancement, the silver nanoparticles can be formed at the power of 30-40, the scanning interval is different according to the power, the size of a light spot can be changed, and the interval is determined according to the size of the line width of a single line engraved by different powers; such as: the 10mw spacing is 0.3um, the 20mw spacing is 0.5um, etc., and the scanning spacing is selected in the approximate range of 0.2-0.8 um.
Preferably, the laser power is 30-40 mw, and the scanning distance is 0.5-0.8 um.
More preferably, the laser power is 30mw, and the scanning distance is 0.7 um.
Further, in the step 3), the wavelength of the femtosecond pulse laser is 790-810 nm, and the pulse width is 130 femtoseconds (femtosecond: fs), the pulse repetition frequency was 76MHz, and the film was processed with an objective lens having a 100-fold aperture of 1.4.
Preferably, the femtosecond pulse laser has a wavelength of 800nm, a pulse width of 130 femtoseconds, and a pulse repetition frequency of 76MHz, and processes the film by using an objective lens with a 100-fold-value aperture of 1.4.
Further, the spin coating process in the step 2) comprises the following steps: rotating the spin coater at a rotating speed of 500-700 rpm for 8-10 seconds, and then rotating at 1400-1600 rpm for 25-35 seconds to perform spin coating;
the drying process comprises the following steps: naturally airing, and then drying for 9-11 minutes at 95-105 ℃ by using an oven to obtain the film.
Preferably, the spin coating process is: rotating the spin coater at 500 rpm for 9 seconds, and then rotating the spin coater at 1500 rpm for 30 seconds to spin;
the drying process comprises the following steps: air-drying, and then drying for 10 minutes at 100 ℃ by using an oven to obtain the film.
Further, the stirring in the steps 1) to 3) is ultrasonic stirring, and the stirring time is 0.5 hour.
Further, the etched film in the step 4) is placed in ethanol to be soaked for 0.5-2 hours, then taken out, placed in deionized water, dried in an oven at 80-95 ℃ for 0.2-1 hour, taken out, and dried by nitrogen to obtain the silver micro-nano structure substrate.
Preferably, the etched film is placed in an ethanol solution to be soaked for 2 hours, then taken out, placed in deionized water, dried in an oven at 90 ℃ for 0.5 hour, taken out again, and dried by using nitrogen to obtain the silver micro-nano structure substrate.
The invention has the beneficial effects that:
the invention uses femtosecond laser to etch a film formed by polyvinylpyrrolidone (PVP for short) and Ag salt solution to prepare the silver micro-nano structure material which is used as a Raman enhancement substrate. And etching the film under the condition of femtosecond pulse laser to reduce Ag + into silver and form a nano structure. The invention utilizes a three-dimensional nanometer displacement platform to etch silver nanometer particles with required area, and finally develops the structure by using ethanol and deionized water. The invention has the advantages of simple manufacture, low substrate cost, convenient use and storage, strong enhancing capability, good stability and reproducibility, and is an excellent novel SERS substrate material.
Drawings
FIG. 1 is a schematic diagram of an apparatus structure for a femtosecond laser etching process;
FIG. 2 shows PVP and AgNO3SEM images of substrates at a molar ratio of 2: 1; the corresponding scanning speeds in the figure are all 4 um/s; the femtosecond laser power corresponding to graphs a, b, c and d is respectively 10mw, 20mw, 30mw and 40 mw; graph a shows a grating structure with a period of 125nm, graph b shows a grating structure with a period of 65nm, graph c shows a structure from a silver nano-grating to a silver nano-particle in a transition state, and graph d shows a structure state of the silver nano-particle;
FIG. 3 shows PVP and AgNO3A schematic diagram of the effect of the substrate surface enhanced Raman scattering test with a molar concentration ratio of 1: 1; the corresponding scanning speed in the upper graph is 4um/s, and the femtosecond laser power corresponding to the graphs e, f and g is 3mw, 15mw and 25mw respectively; FIG. E, F, G is an enlarged schematic view of the sequence from silver nanowires to silver nanograsters to silver nanoparticles with an average size of 36nm, and the distance between the particles can be as small as 1nm, thus creating many "hot spots" in the sequence from e, f, and g, respectively", the concentration of p-toluene thiophenol can be detected to reach 10 by the silver nano particle substrate-13mol/L, which is a concentration value never reached in the prior art, and the prior art of the laser direct writing technology can only reach the interval of 20nm, which seriously limits the requirement of silver nanoparticles as a Raman enhancement substrate;
FIG. 4 is a graph showing Raman enhancement signals of p-toluenesulfonyl phenols in each of the graphs E, F, G, each at a concentration of 10-13mol/L, the reinforcing effect of the silver nanoparticles is better, and the larger the laser power is, the better the corresponding signal reinforcing effect is in a certain power range;
FIG. 5 shows that in the structural form of Ag nanoparticles shown in FIG. G, SERS effect enhancement signals of p-toluenesulphonol at different positions of the substrate are good in uniformity.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention clearer, the technical solutions of the present invention will be further clearly and completely described below with reference to the embodiments of the present invention. It should be noted that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The following describes in detail the application of the femtosecond laser to prepare the surface enhanced raman scattering substrate according to the present invention with reference to the accompanying drawings and examples.
As shown in FIG. 1, the laser passes through an optical switch (optical gate), controls the polarization state and power of light through an attenuation sheet and a lambda/2 or lambda/4 glass slide, and is collimated and expanded through two confocal lenses. The laser light is transmitted through the dichroic mirror, is not reflected, and is focused on the sample surface through an oil immersion objective lens (100 ×, NA ═ 1.4). The natural light scattered from the surface of the sample is reflected by the dichroic mirror, and a real-time monitoring signal is collected by the CCD. The sample is fixed on a three-dimensional nanometer displacement table, and the movement of the sample is controlled by a computer. In the experiment, the laser beam is fixed, and the nano displacement table is controlled by Labview programming, so that the sample can be accurately moved at a high speed and with high exposure time.
The specific implementation process comprises the following steps:
(1) preparing a film forming solution:
preparation of solution E1: adding 0.125 g of polyvinylpyrrolidone into 3 ml of deionized water, and carrying out ultrasonic stirring for half an hour to obtain a solution A1; adding 0.1 g of silver nitrate into 3 ml of deionized water, and ultrasonically stirring for half an hour to obtain a solution C1; solution A1 was then added to solution C1 and stirred ultrasonically for half an hour to give solution E1. The molar ratio of PVP to silver nitrate in solution E1 was 2: 1. The average molecular weight of the pvc in this experiment was 58000. The experiment can not generate chemical reaction at normal temperature.
Solution E2: adding 0.125 g of polyvinylpyrrolidone into 3 ml of deionized water, and carrying out ultrasonic stirring for half an hour to obtain a solution A2; adding 0.2 g of silver nitrate into 3 ml of deionized water, and ultrasonically stirring for half an hour to obtain a solution C2; solution A2 was then added to solution C2 and stirred ultrasonically for half an hour to give solution E2. The molar ratio of PVP to silver nitrate in solution E2 was 1: 1.
(2) film production
And respectively dripping the solutions E1 and E2 on a glass slide substrate for uniformly coating, spin-coating by a spin coater at the rotation speed of 500 rpm for 9 seconds, then at the rotation speed of 1500 rpm for 30 seconds, finishing spin-coating, naturally drying, and baking in an oven at 100 ℃ for 10 minutes to obtain the film.
(3) Femtosecond laser etching
The film is placed on a three-dimensional nanometer displacement table, the displacement table is controlled by a computer to move, femtosecond pulse laser direct writing is carried out, a large-area silver nanometer structure can be etched by scanning on the film, and the schematic diagram of processing equipment is shown in figure 1;
the wavelength of the femtosecond pulse laser in the etching process is 800nm, the pulse width is 130 femtoseconds, the pulse repetition frequency is 76MHz, and an objective lens with the aperture of 100 times of the value of 1.4 is used for processing the film.
(4) Development
And (3) soaking the etched film in an ethanol solution for 1 hour, taking out, putting the film into deionized water, drying the film in a 90 ℃ oven for half an hour, taking out, and drying the film by using nitrogen to obtain the microstructure substrate.
(5) Substrate surface enhanced Raman Scattering test
Prepared at a concentration of 10-13The substrates prepared by the method are respectively soaked in a p-toluene thiophenol solution for two hours, taken out and naturally dried, and then a Raman spectrometer is used for testing the signals of the p-toluene thiophenol.
The wavelength of laser used by the Raman spectrometer is 633nm, the magnification factor is 50 times, and the aperture is 0.75, and the objective is irradiated on the silver nanoparticles adsorbed with the p-toluene thiophenol molecules to obtain Raman enhancement signals of the adsorbed molecules. The characteristic peak position of the Raman signal of the p-toluenesulphonol is 1076cm-1And 1593cm-1Two places.
In the femtosecond laser etching process, the power of the laser can control the form of the silver nano structure. Three different structures can be obtained by different powers, which are respectively: the structure comprises a continuous silver wire, a silver grating structure with the period less than one tenth of the wavelength and a silver nanoparticle structure with the diameter of 30-50 nm, and fig. 2 shows a morphology chart of the silver grating structure and the nanoparticle structure. Generally, silver nanowires are more studied, but the silver nanowires are only limited to study on the conductivity of the silver nanowires, the invention further obtains a silver nano grating structure with a period less than one tenth of the wavelength and a silver nano particle structure, which are different structural characteristics generated along with the increase of power, for the silver nano particles, a higher enhancement factor is obtained as a substrate for raman enhancement, in order to obtain denser silver nano particles, the spacing between the silver nano particles is smaller, the raman enhancement effect is better, a solution with a higher Ag concentration can be selected, namely, the molar concentration ratio of PVP to silver nitrate is 1:1 (the concentration of silver nitrate is 0.2mol/L, the concentration of PVP is 0.2mol/L), and the SEM is shown in fig. 3. And according to the size difference of the laser facula when different power, set up the interval of scanning, make every line scanned connect exactly, can obtain the silver nanoparticle of large area, the size of silver nanoparticle is even, and compactness is good, and the "hot spot" is more.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (7)
1. A method for preparing a surface enhanced Raman scattering substrate by femtosecond laser is characterized by comprising the following steps:
step 1) preparation of film forming liquid: preparing an aqueous solution containing polyvinylpyrrolidone and silver nitrate;
step 2) film preparation: spin-coating the film-forming liquid drop on a film-forming substrate, and drying to obtain a film;
step 3) etching: the film is placed on a three-dimensional nanometer displacement table, femtosecond pulse laser direct writing is adopted, and a large-area silver nanometer structure can be etched by scanning on the film;
step 4) developing: placing the etched film in ethanol for soaking for a period of time, taking out, placing in hot water for soaking for a period of time, taking out, and drying to obtain a silver micro-nano structure substrate;
the laser power in the step 3) is 10-40 mw; the scanning interval is 0.2-0.8 um; the femtosecond pulse laser has the wavelength of 790-810 nm, the pulse width of 130 femtoseconds, the pulse repetition frequency of 76MHz, and an objective lens with the aperture of 1.4 times of 100 is used for processing the film.
2. The femtosecond laser method for preparing a surface-enhanced raman scattering substrate according to claim 1, wherein in the deposition solution: the molar concentration range of the polyvinylpyrrolidone is 0.18-0.22 mol/L; the molar concentration range of the silver nitrate is 0.1-0.2 mol/L.
3. The method for preparing the surface-enhanced Raman scattering substrate by the femtosecond laser according to claim 2, wherein the molar concentration ratio of PVP to silver nitrate in the deposition solution in the step 1) is 1: 1-2: 1.
4. The method for preparing the surface-enhanced Raman scattering substrate according to claim 1, wherein the laser power is 30-40 mw, and the scanning distance is 0.5-0.8 um.
5. The method for preparing the surface-enhanced Raman scattering substrate by using the femtosecond laser according to claim 1, wherein the spin coating process in the step 2) is as follows: rotating the spin coater at a rotating speed of 500-700 rpm for 8-10 seconds, and then rotating at 1400-1600 rpm for 25-35 seconds to spin;
the drying process comprises the following steps: naturally airing, and then drying for 9-11 minutes at 95-105 ℃ by using an oven to obtain the film.
6. The method for preparing the surface-enhanced Raman scattering substrate by the femtosecond laser according to claim 1, wherein stirring is required in the film forming liquid preparation process in the step 1), and the stirring is ultrasonic stirring and is performed for 0.5 hour.
7. The method for preparing the surface-enhanced Raman scattering substrate by the femtosecond laser according to claim 1, wherein the etched film in the step 4) is soaked in ethanol for 0.5 to 2 hours, then taken out, put into deionized water, dried in an oven at 80 to 95 ℃ for 0.2 to 1 hour, taken out again, and dried by nitrogen to obtain the silver micro-nano structure substrate.
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| CN111560122B (en) * | 2020-04-14 | 2022-11-22 | 华南师范大学 | Method for enhancing PVP photosensitivity and crosslinking method |
| WO2022260539A1 (en) * | 2021-06-08 | 2022-12-15 | Auckland Uniservices Ltd | Substrates, methods of patterning thin films, and their use |
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