CN114672858B - Nano gold film for enhancing Raman scattering activity and preparation method thereof - Google Patents
Nano gold film for enhancing Raman scattering activity and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a nano gold film for enhancing Raman scattering activity and a preparation method thereof, wherein the nano gold film for enhancing Raman scattering activity comprises a conductive substrate and a three-dimensional multilayer gold nanoparticle film stacked on the conductive substrate; the thickness of the three-dimensional multilayer gold nanoparticle film is 0.1-2 mu m, the gold nanoparticles are of a spheroid polyhedral structure, and the particle size of the gold nanoparticles is 150-400nm. According to the nano gold film for enhancing the Raman scattering activity and the preparation method thereof, after the gold seed crystal is attached to the conductive substrate, the gold seed crystal is used as a nucleation point, and the three-dimensional multi-layer gold nanoparticle film is formed on the conductive substrate through cultivation by an electrodeposition method, wherein the gold nanoparticle film is formed by mutually stacking and assembling gold nanoparticles with large particle size, has a single structure and a plurality of surface-enhanced Raman scattering (SERS) hot spots, and is beneficial to guaranteeing the uniformity and high detection sensitivity of SERS signals.
Description
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to a nano gold film for enhancing Raman scattering activity and a preparation method thereof.
Background
The Surface Enhanced Raman Scattering (SERS) spectrum detection technology has wide application prospects in the fields of analytical chemistry, environmental pollutant monitoring, drug monitoring, food safety detection and the like. Due to the resonance property of the surface plasmon, the stability of chemical property and the like, the gold nano unit assembled structure has wide application in SERS spectrum.
Recently, some beneficial attempts and efforts have been made to obtain gold nano-unit assembled structures with surface plasmon resonance properties, such as the article entitled "Instant interfacial self-assembly for homogeneous nanoparticle monolayer enabled conformal 'lift-on' thin film technology", sci.adv.2021,7, eabk2852 ("conformal lifting thin film technology for preparing uniform nanoparticle monolayers based on transient interfacial self-assembly", "Science Advances", volume 7 article No. eabk2852 of 2021). The single-layer gold nanoparticle film mentioned in the article is a film assembled by single-layer gold nanoparticles covered on a substrate, and the preparation method comprises the steps of obtaining the single-layer film assembled by gold nanoparticles by a liquid level self-assembly method, and then directly transferring the single-layer film to the surface of the substrate to obtain a product. Although the film has better uniformity, the film and the preparation method thereof have the defects that: firstly, gold nanoparticles in the film are only single-layer, so that the SERS activity is restricted, and the uniformity of the gold nanoparticles is easily damaged by water waiting solution to be detected, so that the uniformity of SERS signals is seriously influenced; secondly, the preparation method cannot obtain a film product with higher SERS activity and the uniformity of SERS signals of the film product is not damaged by water waiting for the detection solution.
The invention discloses a gold nanoparticle assembled film and a preparation method thereof and application thereof (the patent with the publication number of CN 106967978B) published in 2017, 7 and 21. The thin film is a thin film with the thickness of 200nm-2 mu m, which is formed by mutually adhering multiple layers of gold nanoparticles, wherein the particle size of the gold nanoparticles is 30-120nm, and gaps or gaps are formed among the gold nanoparticles, and are less than or equal to 10 nm; sputtering a gold film on the surface of a conductive substrate to obtain the conductive substrate with the gold film on the surface, taking a graphite sheet as an anode, placing the conductive substrate with the gold film on the surface as a cathode in a gold electrolyte, and electrodepositing under constant current to obtain a target product. However, in actual production, it was found that it was difficult to prepare the target product by electrodeposition when a gold film having the same thickness range was sputtered on the surface of the conductive substrate by a sputtering apparatus; the preparation method is highly dependent on sputtering instruments and experimental conditions, and the repeatability of the preparation method is poor, so that the application and popularization of the preparation method are severely restricted. In addition, the size of the gold nanoparticles has a remarkable effect on the surface plasmon resonance (LSPR) absorption peak, and the LSPR absorption peak can be adjusted from the ultraviolet range to the near infrared or even the mid-infrared range by adjusting the size. Therefore, a new method is developed to prepare a film assembled by gold nanoparticles with larger size, and the LSPR absorption peak of the gold film is controlled, so that the method is applied to SERS detection with different excitation wavelengths, and has important significance.
Disclosure of Invention
Based on the technical problems, the invention provides a nano gold film for enhancing Raman scattering activity and a preparation method thereof, wherein after gold seed crystals are attached to a conductive substrate, the gold seed crystals are utilized as nucleation points, a three-dimensional multilayer gold nanoparticle film is formed on the conductive substrate through cultivation by an electrodeposition method, and the gold nanoparticle film is formed by mutually stacking and assembling gold nanoparticles with large particle size, has a single structure and a plurality of SERS hot spots, and is beneficial to ensuring the uniformity and high detection sensitivity of SERS signals.
The invention provides a nano gold film for enhancing Raman scattering activity, which comprises a conductive substrate and a three-dimensional multilayer gold nanoparticle film stacked on the conductive substrate;
the thickness of the three-dimensional multilayer gold nanoparticle film is 0.1-2 mu m, gold nanoparticles are of a nearly spherical polyhedral structure, and the particle size of the gold nanoparticles is 150-400nm.
Preferably, the three-dimensional multilayer gold nanoparticle film is provided with a plurality of nanovoids among gold nanoparticles, and the number of the nanovoids with the size of less than or equal to 10nm is not less than 80% based on the total number of all the nanovoids.
Preferably, the number of layers of the three-dimensional multilayer gold nanoparticle film is 2-6.
Preferably, the conductive substrate is a silicon wafer substrate, an indium tin oxide substrate or a fluorine-doped tin dioxide conductive glass substrate.
The invention provides a preparation method of the nano gold film for enhancing Raman scattering activity, which comprises the following steps: and after attaching gold seed crystals to the conductive substrate, performing electrodeposition in a gold electrolyte containing a dispersing agent by taking the conductive substrate attached with the gold seed crystals as a negative electrode, and culturing to form a three-dimensional multilayer gold nanoparticle film on the conductive substrate by taking the gold seed crystals as nucleation points.
Preferably, the "attaching gold seed to conductive substrate" has the steps of: uniformly coating a gold seed crystal solution on a conductive substrate, and drying, namely attaching the gold seed crystal on the conductive substrate to obtain the conductive substrate attached with the gold seed crystal;
preferably, the Jin Zijing solution is obtained by dissolving gold ion salt and a dispersing agent in water and then reducing the gold ion salt and the dispersing agent by a reducing agent under an acidic condition, wherein the gold ion salt is preferably gold chloride, the dispersing agent is preferably polyvinylpyrrolidone, the reducing agent is preferably sodium borohydride, and the particle size of Jin Zijing is preferably 3-50nm;
preferably, the coating method is spin coating, and the spin coating rotating speed is preferably 100-300r/min;
preferably, the conductive substrate is a silicon wafer substrate, an indium tin oxide substrate or a fluorine-doped tin dioxide conductive glass substrate.
Preferably, the gold electrolyte comprises a gold ion salt, a dispersant and an acid reagent;
preferably, the gold ion salt is gold chloride, the dispersing agent is polyvinylpyrrolidone, and the acid reagent is hydrochloric acid;
preferably, the mass ratio of the gold ion salt, the dispersing agent and the acid agent is 2-10:100-300:3-9.
Preferably, the electrodeposition parameters include: the current density is 10-30 mu A/cm 2 The electrodeposition time is 0.5-6h.
According to the invention, the electrolyte comprising gold ion salt, dispersing agent and acid reagent is selected, so that the deposition efficiency of gold particles can be enhanced, the gold particles are relatively uniform in size, and the gold nano-film which has a smoother surface and is stacked into a multilayer structure can be obtained; the former has more nano-voids with a size less than or equal to 10nm compared with the electrolyte only comprising gold ion salt and acid reagent, thereby obtaining higher SERS activity.
The invention also provides an application of the nano gold film for enhancing the Raman scattering activity, which comprises the following steps: and carrying out Raman detection on the object to be detected by taking the nano gold film as a Raman detection substrate.
Preferably, the use of the nano gold film for enhancing raman scattering activity comprises: and carrying out Raman detection on rhodamine 6G under the condition that the excitation wavelength is 532nm by taking the nano gold film as a Raman detection substrate.
Compared with the prior art, the invention has the beneficial effects that:
(1) The nano gold film comprises a conductive substrate and a three-dimensional multilayer gold nanoparticle film stacked on the conductive substrate, wherein gold nanoparticles are of a large-size approximately spherical polyhedral structure, and have a very high specific surface area after being stacked and assembled together to obtain the nano gold film, so that the SERS activity is greatly improved; gold nanoparticles are distributed in a staggered manner, nano gaps are formed between adjacent gold nanoparticles, and the gaps are connected with each other to form a network of gaps, so that the gold nanoparticles are favorable for becoming hot spots for inducing SERS; when gold nanoparticles with a nearly spherical polyhedral structure are stacked, compared with spherical gold nanoparticles, the gold nanoparticles have surface contact, and the gold nanoparticles are only in point contact, so that the gold nanoparticles have higher stacking density, and the number ratio of the size of the nano voids which is less than or equal to 10nm is higher than that of the gold nanoparticles which are used as the total number of all nano voids, and the gold nanoparticles have higher SERS activity; the whole structure of the nano gold film is uniform, so that the nano gold film has high SERS activity, stability and uniformity; the gold nanoparticles are mutually stacked to form a multi-layer structure, so that the SERS activity of the gold nanoparticles can be improved multiple times, and the phenomenon that the uniformity of SERS signals of the gold nanoparticles is damaged due to the fact that water is waiting for dissolution of a measuring solution can be avoided.
(2) By taking the nano gold film as an SERS active substrate and carrying out repeated and multi-batch tests on rhodamine 6G under different concentrations, the concentration of the rhodamine 6G as a measured object is as low as 10 -11 The detection can still be effectively detected in mol/L, and the consistency and repeatability of the detection are very good for multiple points and any point on the product.
(3) According to the preparation method of the gold nanoparticle film, a layer of gold seed crystal is uniformly covered on the surface of the conductive substrate, and the gold nanoparticle film is formed by growing Jin Zijing serving as a nucleation point on the conductive substrate through electrodeposition.
Drawings
FIG. 1 is a scanning electron microscope image of a nano-gold film according to example 1 of the present invention;
FIG. 2 is a cross-sectional Scanning Electron Microscope (SEM) image of a nano-gold film according to example 1 of the present invention;
FIG. 3 is a scanning electron microscope image of the nanogold film according to examples 2 to 6;
FIG. 4 is a scanning electron microscope image of the nanogold film according to comparative example 1;
FIG. 5 is a scanning electron microscope image of the nanogold film according to comparative example 2;
fig. 6 is a raman detection result spectrum of rhodamine 6G by the nano-gold film described in example 1.
Detailed Description
The present invention will be described in detail by way of specific examples, which should be clearly set forth for the purpose of illustration and are not to be construed as limiting the scope of the present invention.
Example 1
The embodiment provides a nano gold film for enhancing Raman scattering activity, which is prepared by the following method:
(1) Adding 3mg of gold chloride tetrahydrate and 0.3g of polyvinylpyrrolidone (K29-32) into 20mL of deionized water successively to form a mixed solution, then adding 200 mu L of hydrochloric acid with the concentration of 30g/L into the mixed solution, then adding 1g/L of sodium borohydride solution into the mixed solution dropwise until the mixed solution turns into dark reddish brown, preparing a gold seed solution, keeping the size of Jin Zijing particles in the range of 3-50nm, sealing and standing for 24 hours, and using;
(2) An ITO conductive glass with the thickness of 1.5mm, the area of 1cm multiplied by 3cm, the resistance of less than 6Ω and the transmittance of more than or equal to 84 percent is taken as a conductive substrate, the ITO conductive glass is cleaned by ethanol and deionized water in sequence, 100 mu L of the Jin Zijing solution is uniformly spin-coated on the ITO conductive glass at the rotation speed of 200r/min by adopting a spin coating method, and the ITO conductive glass with a layer of gold seed crystal attached to the surface is prepared after the ITO conductive glass is put into an oven at 80 ℃ for drying;
(3) Sequentially adding 3mg of gold chloride tetrahydrate, 0.15g of polyvinylpyrrolidone (K29-32) and 200 mu L of hydrochloric acid with the concentration of 30g/L into 15mL of deionized water, and uniformly stirring to form a mixed solution, thus obtaining gold electrolyte;
(4) Taking ITO conductive glass with a layer of gold seed crystal attached to the surface as a cathode, taking a rectangular graphite sheet as an anode, placing the cathode in the gold electrolyte, and obtaining the gold-doped ITO conductive glass with the gold seed crystal attached to the surface at the current density of25μA/cm 2 Electrodepositing for 6 hours under the constant current condition, and growing gold nano-particles on the ITO conductive glass by taking gold seed crystals as nucleation points to obtain the nano-gold film;
(5) The nano gold film is washed three times by deionized water, soaked in water for 30min to wash polyvinylpyrrolidone on the surface of the product, and the obtained product is dried at 60 ℃ and then subjected to scanning electron microscopy, the results are shown in fig. 1 and 2, fig. 1 is a scanning electron microscopy image of the nano gold film of example 1, and fig. 2 is a cross-sectional scanning electron microscopy image of the nano gold film of example 1.
Referring to fig. 1 and 2, the nano gold film is a three-dimensional multilayer gold nanoparticle film, the thickness of the gold nanoparticle film is 0.8 μm, the gold nanoparticles are of a nearly spherical polyhedral structure, the particle size range is 150-400nm, the gold nanoparticle film has a plurality of nano voids among the gold nanoparticles, and the number of layers of the gold nanoparticle film is 5.
The nano gold film is used as a Raman detection substrate, and a confocal laser Raman spectrometer is used for detecting the nano gold film containing 2X 10 - 9 mol/L and 1X 10 -11 The mol/L rhodamine 6G to-be-detected objects are respectively characterized, wherein the wavelength of excitation light of a laser Raman spectrometer is 532nm, the power is 0.1-2mW, the integration time is 1-120s, the detection result is shown in FIG. 6, and FIG. 6 is a Raman detection result map of the nano gold film to the rhodamine 6G, which is described in the embodiment 1.
Referring to FIG. 6, the nano-gold film of example 1 has very high SERS activity as a SERS substrate, and a detection concentration as low as 1×10 -11 The mol/L rhodamine 6G still can obtain SERS spectra, and the characteristic peak is more obvious.
Example 2
This example provides a nano-gold film with enhanced Raman scattering activity, which is prepared in the same manner as in example 1, except that in step (4), the current density is 25. Mu.A/cm 2 Electrodepositing for 5s under constant current condition.
Example 3
This example provides a nano-gold film with enhanced raman scattering activity, which is prepared in the same manner as in example 1, except thatIn the step (4), the current density was 25. Mu.A/cm 2 Electrodeposition for 120s under constant current conditions.
Example 4
This example provides a nano-gold film with enhanced Raman scattering activity, which is prepared in the same manner as in example 1, except that in step (4), the current density is 25. Mu.A/cm 2 Electrodepositing 180s under constant current condition.
Example 5
This example provides a nano-gold film with enhanced Raman scattering activity, which is prepared in the same manner as in example 1, except that in step (4), the current density is 25. Mu.A/cm 2 Electrodeposition was performed for 900s under constant current conditions.
The nano gold film described in example 5 was used as a SERS substrate, and a high concentration of rhodamine 6G was detected to obtain SERS spectra.
Example 6
This example provides a nano-gold film with enhanced Raman scattering activity, which is prepared in the same manner as in example 1, except that in step (4), the current density is 25. Mu.A/cm 2 Electrodeposition was performed for 1800s (0.5 h) under constant current conditions.
The products obtained in examples 2-6 were subjected to scanning electron microscopy, and the results are shown in FIG. 3, and FIG. 3 (a-e) are scanning electron microscopy images of the nanogold films described in examples 2-6, respectively.
Referring to fig. 3, as the time of electrodeposition increases, gold nanoparticles in the nano-gold thin film become larger and larger until three-dimensional multi-layered gold nanoparticle film is formed by stacking, and have high SERS activity.
Comparative example 1
The comparative example provides a nano gold film for enhancing Raman scattering activity, which is prepared by the following method:
(1) An ITO conductive glass with the thickness of 1.5mm, the resistance of less than 6 omega and the transmittance of more than or equal to 84 percent is used as a conductive substrate, ethanol and deionized water are sequentially used for cleaning the ITO conductive glass, a sputtering instrument is used for sputtering the ITO conductive glass to form a gold film with the thickness of 10nm, and the ITO conductive glass with a layer of gold film attached to the surface is prepared;
(2) Sequentially adding 3mg of gold chloride tetrahydrate, 0.15g of polyvinylpyrrolidone (K29-32) and 200 mu L of hydrochloric acid with the concentration of 30g/L into 15mL of deionized water, and uniformly stirring to form a mixed solution, thus obtaining gold electrolyte;
(3) Taking ITO conductive glass with a gold film attached to the surface as a cathode, taking a rectangular graphite sheet as an anode, placing the cathode in the gold electrolyte, and obtaining the anode with the current density of 25 mu A/cm 2 Electrodepositing for 6 hours under the constant current condition to obtain the nano gold film;
(4) The nano gold film is washed three times by deionized water, soaked in water for 30min, and the obtained product is dried at 60 ℃ and then subjected to scanning electron microscope detection, the result is shown in fig. 4, and fig. 4 is a scanning electron microscope image of the nano gold film of comparative example 1.
Referring to fig. 4, it can be seen that the nano gold film obtained in this comparative example produced a dense gold film, which had no significant gaps, which lacked hot spots, and had very low SERS activity.
It is known that the comparative example method is highly dependent on sputtering instruments and experimental conditions, and the repeatability of the preparation method is poor, so that the application and popularization of the comparative example method are severely restricted.
Comparative example 2
The comparative example provides a nano gold film for enhancing Raman scattering activity, which is prepared by the following method:
(1) Taking ITO conductive glass with the thickness of 1.5mm, the resistance of less than 6Ω and the transmittance of more than or equal to 84% as a conductive substrate, and cleaning the ITO conductive glass by ethanol and deionized water in sequence;
(2) Sequentially adding 3mg of gold chloride tetrahydrate, 0.15g of polyvinylpyrrolidone (K29-32) and 200 mu L of hydrochloric acid with the concentration of 30g/L into 15mL of deionized water, and uniformly stirring to form a mixed solution, thus obtaining gold electrolyte;
(3) Taking the cleaned ITO conductive glass as a cathode and a rectangular graphite sheet as an anode, placing the cathode in the gold electrolyte, and controlling the current density to be 25 mu A/cm 2 Electrodepositing for 6h under the constant current condition to obtain the nano-meterA gold film;
(4) The nano gold film is washed three times by deionized water, soaked in water for 30min, and the obtained product is dried at 60 ℃ and then subjected to scanning electron microscope detection, the result is shown in fig. 5, and fig. 5 is a scanning electron microscope image of the nano gold film in comparative example 2.
Referring to fig. 5, it can be seen that the gold nano-synapses in the gold nano-film obtained in the comparative example have a large curvature area, but are dispersed throughout the film in small amounts, and cannot form uniform hot spots in a large area.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (3)
1. The nano gold film for enhancing the Raman scattering activity is characterized by comprising a conductive substrate and a three-dimensional multilayer gold nanoparticle film stacked on the conductive substrate;
the thickness of the three-dimensional multilayer gold nanoparticle film is 0.1-2 mu m, gold nanoparticles are of a nearly spherical polyhedral structure, and the particle size of the gold nanoparticles is 150-400nm;
the three-dimensional multilayer gold nanoparticle film is provided with a plurality of nanovoids among gold nanoparticles; taking the total number of all nano voids as a reference, the number of the nano voids with the size less than or equal to 10nm is not less than 80 percent;
the number of layers of the three-dimensional multilayer gold nanoparticle film is 2-6;
the preparation method of the nano gold film comprises the following steps: uniformly coating a gold seed crystal solution on a conductive substrate, drying, and attaching the gold seed crystal on the conductive substrate to obtain the conductive substrate attached with the gold seed crystal, wherein the Jin Zijing solution is obtained by dissolving gold chloride and polyvinylpyrrolidone in water and then reducing the gold seed crystal with the particle size of 3-50nm under an acidic condition, the coating method is spin coating method, the spin coating rotating speed is 100-300r/min, and the conductive substrate is siliconA sheet substrate, an indium tin oxide substrate, or a fluorine-doped tin dioxide conductive glass substrate; taking the conductive substrate attached with the gold seed crystal as a negative electrode, and performing electrodeposition in gold electrolyte of gold chloride, polyvinylpyrrolidone and hydrochloric acid in a mass ratio of 2-10:100-300:3-9, wherein the electrodeposition parameters comprise: the current density is 10-30 mu A/cm 2 And (3) electrodepositing for 6 hours, and culturing on the conductive substrate by taking gold seed crystals as nucleation points to form the three-dimensional multilayer gold nanoparticle film.
2. Use of the nanogold film for enhancing raman scattering activity according to claim 1, comprising: and taking the nano gold film as an enhanced Raman detection substrate to carry out Raman detection on the object to be detected.
3. Use of a nanogold film for enhancing raman scattering activity according to claim 2, comprising: and carrying out Raman detection on rhodamine 6G under the condition that the excitation wavelength is 532nm by taking the nano gold film as a Raman detection substrate.
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| 金纳米颗粒阵列基底的化学置换制备及其表面增强拉曼散射特性研究;李玉;黄小平;王影;侯宇蒙;陈涛;张培锋;黄秋莹;赵青;光谱学与光谱分析;37(012);3725-3729 * |
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