CN115582537B - Preparation method and application of large-size uniform nano noble metal film - Google Patents

Preparation method and application of large-size uniform nano noble metal film Download PDF

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CN115582537B
CN115582537B CN202211220661.6A CN202211220661A CN115582537B CN 115582537 B CN115582537 B CN 115582537B CN 202211220661 A CN202211220661 A CN 202211220661A CN 115582537 B CN115582537 B CN 115582537B
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CN115582537A (en
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邢廷洋
吴立军
叶豪
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Wenzhou Medical University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05Metallic powder characterised by the size or surface area of the particles
    • B22F1/054Nanosized particles
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/55Specular reflectivity
    • G01N21/552Attenuated total reflection
    • G01N21/553Attenuated total reflection and using surface plasmons
    • G01N21/554Attenuated total reflection and using surface plasmons detecting the surface plasmon resonance of nanostructured metals, e.g. localised surface plasmon resonance
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/65Raman scattering
    • G01N21/658Raman scattering enhancement Raman, e.g. surface plasmons
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30Hydrogen technology
    • Y02E60/50Fuel cells

Abstract

The invention provides a preparation method and application of a large-size uniform nano noble metal film, and belongs to the technical field of spectrum sensing. The invention provides a preparation method and application of a large-size uniform nano noble metal film, wherein the diffusion size of nano noble metal particle liquid drops is limited by using a super-hydrophobic coating, then the stability of nano particles in a colloid solution is regulated and controlled, and the large-size uniform nano noble metal film is prepared by balancing the action of the gravity of the nano particles and the integral retreating force of the liquid drops. Compared with the traditional preparation method of the nano noble metal film, the experimental process is simple and feasible, the success rate is high, the film size is large, the application range is wide, and the method has wide application prospect in the field of spectrum sensing based on the film technology.

Description

Preparation method and application of large-size uniform nano noble metal film
Technical Field
The invention relates to the technical field of spectrum sensing, in particular to a preparation method and application of a large-size uniform nano noble metal film.
Background
The abundant conduction electrons on the surface of the noble metal nano structure generate a localized surface plasmon resonance effect (hereinafter referred to as LSPR: localized Surface Plasmon Resonance) against a positive charge background under the irradiation of laser with a certain frequency. According to theoretical and experimental studies, noble metal nanoparticles are close to each other, and a local electric field between the particles is greatly enhanced due to the coupling effect of the LSPR. This phenomenon determines that if noble metal nanoparticles are unevenly distributed on a spectrum sensing substrate, quantitative determination of analyte concentration will cause problems, which hampers the application of spectrum sensing technology (surface enhanced fluorescence, surface enhanced raman scattering) in the field of quantitative detection.
Methods of preparing nano noble metal thin films generally include photolithography, high humidity evaporation, and three-phase self-assembly. The photolithography method can prepare a uniform monolayer precious metal nanoparticle assembly according to the requirements, and is characterized in that the prepared film has good uniformity, but the method has high cost and cannot be applied to the field of film preparation in a large area. The high humidity evaporation method is to reduce the evaporation rate of noble metal nano particles through a constant temperature and humidity environment, regulate the retractive force of the surface of liquid drops and obtain a uniform single-layer nano noble metal film. The high humidity evaporation method is only applied to self-assembly of gold nanorod films, and is mainly characterized by simple operation, but narrow application range, and the preparation time of the film often needs days due to the reduction of evaporation speed. The three-phase self-assembly method can obtain a single-layer film, but the method is complex and time-consuming to operate, requires a smart preparation process, is easy to break, and is difficult to be suitable for noble metal nano-particles with larger sizes. Therefore, there is a need for a preparation method of nano noble metal thin films, which is simple to operate, has high success rate, and can be prepared in a large and uniform size.
Disclosure of Invention
In view of the above, the present invention aims to provide a method for preparing a large-size uniform nano noble metal film and an application thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the preparation method of the large-size uniform nano noble metal film is characterized by comprising the following steps of:
providing a substrate, coating a super-hydrophobic material on the substrate, and drying to obtain a super-hydrophobic coating;
preparing round holes on the super-hydrophobic coating according to the required size;
preparing a nano noble metal colloid solution, regulating and controlling the stability of nano particles in the colloid solution, and obtaining the colloid solution in a critical state;
and (3) dripping a critical colloidal solution into the round hole, standing and drying.
Preferably, the substrate is a non-hydrophobic carrier; the coating mode comprises soaking and spraying.
Preferably, the superhydrophobic material is a fluorosilicone polymer.
Preferably, the method for preparing the round hole is to remove the super-hydrophobic layer in the range of the round hole by using laser engraving or physical damage; the diameter of the round hole is 1 mm-2 mm.
Preferably, the noble metal colloid solution is gold nanocube colloid solution, gold nanostar colloid solution or gold-silver alloy colloid solution.
Preferably, the method for controlling the stability of the nanoparticles in the colloidal solution comprises the following steps: centrifuging, adding halogen ion salt, and adding one or more of thiol-containing functional group molecules.
Preferably, the molar concentration of the nano particles in the colloidal solution in the critical state is 0.07nM to 0.2nM.
Preferably, the drop amount of the colloidal solution in the critical state is 2-5 mu L; the standing is that standing is carried out for 1-2 h at room temperature.
The invention also provides a nano noble metal film prepared by the preparation method of the large-size uniform nano noble metal film.
The invention also provides application of the nano noble metal film in the aspect of spectrum sensing technology.
The beneficial technical effects are as follows: the invention provides a preparation method and application of a large-size uniform nano noble metal film, wherein the diffusion size of nano noble metal particle liquid drops is limited by using a super-hydrophobic coating, then the stability of the nano particles in a colloid solution is regulated, and the large-size uniform nano noble metal film is prepared by balancing the gravity of the nano particles and the action of the whole back-off of the liquid drops. Compared with the traditional preparation method of the nano noble metal film, the experimental process is simple and feasible, the success rate is high, the film size is large, the application range is wide, and the method has wide application prospect in the field of spectrum sensing based on the film technology.
Drawings
FIG. 1 is a flow chart of the preparation of a large-sized nano noble metal thin film;
FIG. 2 is an SEM image of a gold nanocube film obtained in example 1;
FIG. 3 is an SEM image of a gold nano-star film obtained in example 2;
FIG. 4 is an SEM image of an AuNS@Ag film obtained in example 3;
FIG. 5 is an SEM image of a noble metal thin film obtained in comparative example 1;
FIG. 6 is an SEM image of a noble metal thin film obtained in comparative example 2.
Detailed Description
The invention provides a preparation method of a large-size uniform nano noble metal film, which is characterized by comprising the following steps:
providing a substrate, coating a super-hydrophobic material on the substrate, and drying to obtain a super-hydrophobic coating;
preparing round holes on the super-hydrophobic coating according to the required size;
preparing a nano noble metal colloid solution, regulating and controlling the stability of nano particles in the colloid solution, and obtaining the colloid solution in a critical state;
and (3) dripping a critical colloidal solution into the round hole, standing and drying.
In the invention, the preparation flow of the large-size nano noble metal film is shown in figure 1.
The invention provides a substrate, which is coated with a super-hydrophobic material and dried to obtain a super-hydrophobic coating.
In the present invention, the substrate is preferably a non-hydrophobic film carrier; the non-hydrophobic carrier is preferably a silicon wafer or a glass slide, and the size is preferably (2-5) mm 2 ×(2~5)mm 2 The method comprises the steps of carrying out a first treatment on the surface of the The non-hydrophobic carrier is further cleaned and dried before being coated, the cleaning is ultrasonic cleaning by sequentially using detergent, ethanol and ultrapure water, the drying is preferably carried out at 35-45 ℃ and the baking is carried out for 0.5-1.5 h; the coating mode preferably comprises soaking and spraying; the spraying is preferably spraying by using a spray pen or a spray gun; the drying is preferably carried out by baking for 1-3 hours at the temperature of 35-45 ℃ on a heating table; the thickness of the superhydrophobic layer is preferably 1 μm to 1mm.
In the present invention, the superhydrophobic material is preferably a fluorosilicone polymer; the superhydrophobic material is preferably a liquid; the fluorosilicone polymer is preferably XN-204A, XN-204B and XN-206C reagent of Shenzhen high Material technology Co.
According to the invention, round holes are prepared on the superhydrophobic coating according to the required size.
In the invention, the method for preparing the round hole is preferably to remove the super-hydrophobic layer in the range of the round hole by using laser engraving or physical damage; the diameter of the round hole is preferably 1 mm-2 mm. The diffusion of colloidal solution dripped into the round hole can be limited by only damaging the super-hydrophobic coating within the range of the round hole without damaging the substrate sheet, and the balance of the gravity and the retractive force of the nano particles is controlled based on the regulation and control action of the super-hydrophobic coating on the contact angle, so that the large-size and uniform nano noble metal film is obtained.
The invention prepares nano noble metal colloid solution, regulates and controls the stability of nano particles in the colloid solution, and obtains the colloid solution in a critical state.
In the invention, the noble metal colloid solution is preferably gold nanocube colloid solution, gold nanostar colloid solution or gold-silver alloy nanoparticle colloid solution; the invention is applicable to noble metal nano particles with different sizes, shapes and types, and has higher universality.
In the invention, the preparation method of the gold nanocube colloid solution comprises the following steps:
preparing gold nanoclusters by reducing chloroauric acid with sodium borohydride by using cetyltrimethylammonium bromide (CTAB) as a surfactant;
and taking the gold nanoclusters as seeds, adding CTAB again, and controlling the crystal face growth rate of the nanoparticles by Br ions to obtain a gold nanocube colloid solution.
In the invention, the preparation method of the gold nanostar colloidal solution comprises the following steps:
using CTAB as a surfactant, and reducing chloroauric acid by using sodium borohydride to prepare gold nanoclusters;
gold nanoclusters are used as seeds, L-reduced glutathione is used as a growth template, cetyl Trimethyl Ammonium Chloride (CTAC) is added, and ascorbic acid is used for reducing chloroauric acid, so that a gold nano star colloidal solution is prepared.
In the invention, the preparation method of the gold-silver alloy nanoparticle solution comprises the following steps:
using CTAB as a surfactant, and reducing chloroauric acid by using sodium borohydride to prepare gold nanoclusters;
centrifuging the gold nanosatellite solution, re-suspending with ultrapure water, sequentially adding CTAC solution and AgNO 3 Heating the solution and Ascorbic Acid (AA) solution in water bath to obtain the nanometer AuNS@Ag colloid solution.
In the present invention, the molar concentration of the nanoparticles in the noble metal colloid solution is 3.5pM to 0.01nM.
In the invention, the method for regulating the stability of the nano particles in the colloid solution comprises the following steps: centrifuging, adding halogen ion salt, and adding one or more of thiol-containing functional group molecules. The centrifugation may be a plurality of centrifugation; the halogen ion salt is one or more than one of NaCl, naBr, naI, KCl, KBr, KI; the thiol-containing functional group molecule is one or two of cysteine and glutathione; the molar concentration of the nano particles in the colloidal solution in the critical state is 0.07 nM-0.2 nM. The invention ensures that the nano particles in the colloid solution are in a critical state of stability by regulating and controlling, so that the nano particles in the colloid can balance the drop retreating force and the gravity. Meanwhile, the molar concentration of the nano particles in the colloid is adjusted according to the concentration of the nano particles in the colloid, so that the uniform coverage of round holes of a substrate can be met.
The invention is to drop critical colloidal solution into the round hole, and to stand and dry.
In the invention, the drop amount of the colloidal solution in the critical state is 2-5 mu L; the standing is that standing is carried out for 1-2 h at room temperature.
The invention also provides a nano noble metal film prepared by the preparation method of the large-size uniform nano noble metal film.
In the invention, the continuous size of the nano noble metal film prepared by the preparation method of the large-size uniform nano noble metal film reaches 3.14mm 2 Compared with other modes, the inventionThe nano noble metal film prepared by the method has better continuity and no obvious break.
The invention also provides application of the nano noble metal film in the aspect of spectrum sensing technology.
In the invention, the nano particles on the nano noble metal film are uniformly distributed and have larger size, so that the nano noble metal film can be applied to the preparation of a spectrum sensor, the accuracy of the spectrum sensing technology in the aspect of quantitative detection is improved, and the application of the spectrum sensing technology (such as a surface enhanced Raman scattering technology) in the field of quantitative detection is promoted.
For a better understanding of the present invention, the following examples are further illustrated, but are not limited to the following examples.
Example 1
A preparation method of a large-size uniform nano noble metal film comprises the following steps:
1) Cutting size of 3mm 2 ×3mm 2 Sequentially performing ultrasonic treatment on the single-sided polished silicon wafer by using a detergent, ethanol and ultrapure water, and drying at 45 ℃ for 0.5h;
filling XN-204A into a spray pen, coating the spray pen on the dried silicon wafer, and baking the silicon wafer on a heating table at 35 ℃ for 3 hours to obtain the silicon wafer coated with the superhydrophobic layer, wherein the thickness of the superhydrophobic layer is 1mm;
2) Preparing a round hole with the diameter of 1mm on the silicon wafer coated with the super-hydrophobic coating by using a laser engraving machine, wherein the laser engraving machine only damages the super-hydrophobic coating within the range of the round hole and does not damage the substrate silicon wafer;
3) Preparing a nano noble metal colloid solution:
taking 0.25mL of 10mM chloroauric acid solution, adding 7.5mL of 0.1M CTAB solution, uniformly mixing, adding 0.8mL of 10mM sodium borohydride solution which is newly prepared, stirring for 2min, and diluting 10 times with the 10mM CTAB solution in a 28 ℃ water bath for 3h to obtain a gold nanocluster solution;
taking 1.6mL of CTAB solution with the molar concentration of 0.1M, adding 8mL of ultrapure water, adding 0.95mL of AA solution with the molar concentration of 0.1M and 5 mu L of gold nanocluster solution again, uniformly mixing, and reacting at room temperature for 10min to prepare CTAB coated gold nanocube colloid solution with the side length of 50nM and the molar concentration of 0.01nM.
4) Preparing a colloidal solution in a critical state:
placing 1mL of gold nanocubes solution into a 1.5mL centrifuge tube, adding 0.1mL of 1M NaBr solution, uniformly mixing, reacting for 3h at room temperature, centrifuging at 6780rpm for 150s, removing supernatant, repeating the operations of centrifuging and removing supernatant for 2 times, and then carrying out ultrasonic resuspension on the residual precipitate in the centrifuge tube to 50 mu L by using ultrapure water to obtain a critical colloidal solution, wherein the molar concentration of the gold nanocubes in the critical colloidal solution is 0.2nM;
5) And (3) sucking 3 mu L of colloidal solution in a critical state by using a pipetting gun, dripping the colloidal solution into a round hole of the super-hydrophobic film, and standing for 1.5h at room temperature to obtain the large-size and uniform gold nanocube film.
The gold nanocube thin film obtained in example 1 was scanned by SEM, and the SEM results are shown in fig. 2.
Example 2
A preparation method of a large-size uniform nano noble metal film comprises the following steps:
1) Cutting size of 2mm 2 ×2mm 2 Sequentially performing ultrasonic treatment on the single-sided polished silicon wafer by using a detergent, ethanol and ultrapure water, and drying at 35 ℃ for 1.5 hours;
filling XN-204B into a spray pen, coating the spray pen on the dried silicon wafer, and baking the silicon wafer on a heating table at 45 ℃ for 1h to obtain the silicon wafer coated with the superhydrophobic layer, wherein the thickness of the superhydrophobic layer is 1 mu m;
2) Preparing a round hole with the diameter of 1mm on the silicon wafer coated with the superhydrophobic coating by using pointed tweezers, wherein the pointed tweezers only damage the superhydrophobic coating within the range of the round hole, and do not damage the substrate silicon wafer;
3) Preparing a nano noble metal colloid solution:
adding 0.25mL of 10mM chloroauric acid solution into 7.5mL of 0.1M CTAB solution, adding 0.8mL of 10mM sodium borohydride solution, uniformly mixing, stirring for 2min, reacting for 3h at room temperature, and diluting 100 times with 10mM CTAB solution to obtain gold nanocluster solution;
8mL of ultrapure water was taken, and 1.6mL of a 0.1M CTAC solution, 0.2mL of a 10mM chloroauric acid solution, 0.95mL of a 0.1M AA solution, 10. Mu.L of 2mM L-GSH, and 10. Mu.L of a seed solution were sequentially added. Preparing gold nano star colloidal solution with the gold nano star particle size of about 100nm and the molar concentration of 3.5 pM;
4) Preparing a colloidal solution in a critical state:
placing 1mL of gold nanostar colloidal solution into a 1.5mL centrifuge tube, adding 100 mu L of 1M NaCl solution, stirring uniformly, standing for 3h, centrifuging at 5000rpm for 5min, removing supernatant, and ultrasonically resuspending the rest precipitate in the centrifuge tube to 50 mu L with ultrapure water to obtain colloidal solution in a critical state; the molar concentration of gold nanostar in the colloidal solution in the critical state obtained was 0.07nM.
5) And (3) sucking 2 mu L of colloidal solution in a critical state by using a pipetting gun, dripping the colloidal solution into a round hole of the super-hydrophobic film, and standing for 1h at room temperature to obtain the gold nano-star film with large size and uniformity.
The gold nanostar film obtained in example 2 was scanned by SEM, and the SEM results are shown in fig. 3.
Example 3
A preparation method of a large-size uniform nano noble metal film comprises the following steps:
1) Cutting size is 5mm 2 ×5mm 2 Sequentially performing ultrasonic treatment on the single-sided polished silicon wafer by using a detergent, ethanol and ultrapure water, and drying at 40 ℃ for 1h;
filling XN-206C into a spray pen, coating the spray pen on the dried silicon wafer, and baking the silicon wafer on a heating table at 40 ℃ for 2 hours to obtain the silicon wafer coated with the superhydrophobic layer; the thickness of the resulting superhydrophobic layer was 500 μm.
2) A round hole with the diameter of 2mm is prepared on the silicon wafer coated with the super-hydrophobic layer by using a laser engraving machine, and the laser engraving machine only damages the super-hydrophobic coating within the range of the round hole and does not damage the substrate silicon wafer.
3) Preparing a nano noble metal colloid solution:
the gold nanostar solution was prepared according to the method in example 2;
taking 1mL of the prepared gold nanostar solution, centrifuging at 5000rpm for 300s, removing the supernatant, repeating the centrifugation and the supernatant removal, using ultrapure water to resuspend to 0.8mL, sequentially adding 0.4mL of a 0.1M CTAC solution, 10 mu L of a 10mM AgNO3 solution and 5 mu L of a 0.1M AA solution, uniformly mixing, and heating in a water bath at 65 ℃ for 3h to prepare the nano AuNS@Ag colloid solution with the particle size of 100nm and the molar concentration of 5.0 pM.
4) Preparing a colloidal solution in a critical state:
placing the AuNS@Ag colloidal solution into a 1.5mL centrifuge tube, adding 10 mu L of 2mM GSH solution, stirring uniformly, standing at room temperature for 2h, centrifuging at 5000rpm for 5min, removing supernatant, and carrying out ultrasonic resuspension on the residual precipitate in the centrifuge tube to 50 mu L by using ultrapure water to obtain a critical state colloidal solution, wherein the molar concentration of the AuNS@Ag in the critical state colloidal solution is 0.1nM.
5) And (3) sucking 5 mu L of colloidal solution in a critical state by using a pipetting gun, dripping the colloidal solution into a round hole of the super-hydrophobic film, and standing for 2 hours at room temperature to obtain the large-size and uniform AuNS@Ag film.
The AuNS@Ag film obtained in example 3 was scanned by SEM, and the SEM results are shown in FIG. 4.
Comparative example 1
This comparative example differs from example 1 in that the superhydrophobic film in example 1 was replaced with a silicon oxide film formed by chemical vapor deposition, and the other operations are the same as in example 1.
As shown in fig. 5, it can be seen from fig. 5 that the thin noble metal film obtained in comparative example 1 was scanned by SEM, and the thin noble metal film could not be uniformly formed due to the fact that the thin noble metal film could not balance the receding force and gravity of the liquid droplets, so that the nano noble metal colloid solution was deposited around to generate a coffee ring effect.
Comparative example 2
This comparative example differs from example 1 in that the nanoparticles in the noble metal colloid solution are not controlled to be in a critical state of stability, and the other operations are the same as in example 1.
The noble metal thin film obtained in comparative example 2 was scanned by SEM, and as shown in fig. 6, it can be seen from fig. 6 that the noble metal thin film cannot be formed in a large-sized, uniform nano-scale in comparative example 2.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.

Claims (5)

1. The preparation method of the large-size uniform nano noble metal film is characterized by comprising the following steps of:
providing a substrate, coating a super-hydrophobic material on the substrate, and drying to obtain a super-hydrophobic coating;
preparing round holes on the super-hydrophobic coating according to the required size; the method for preparing the round hole is to remove the super-hydrophobic layer in the range of the round hole by using laser engraving or physical damage; the diameter of the round hole is 1 mm-2 mm;
preparing a nano noble metal colloid solution, regulating and controlling the stability of nano particles in the colloid solution, and obtaining the colloid solution in a critical state; the regulating method for regulating the stability of the nano particles in the colloidal solution comprises the following steps: centrifuging, adding halogen ion salt, and adding one or more molecules containing thiol functional groups; the molar concentration of the nano particles in the colloidal solution in the critical state is 0.07 nM-0.2 nM;
and (3) dripping a critical colloidal solution into the round hole, standing and drying.
2. The method for preparing a large-sized, uniform nano noble metal thin film according to claim 1, wherein the substrate is a non-hydrophobic carrier; the coating mode comprises soaking and spraying.
3. The method for preparing a large-sized uniform nano noble metal thin film according to claim 1, wherein the super-hydrophobic material is a fluorosilicone polymer.
4. The method for preparing a large-sized and uniform nano noble metal thin film according to claim 1, wherein the noble metal colloid solution is a gold nanocube colloid solution, a gold nanostar colloid solution or a colloid solution of a nano gold-silver alloy.
5. The method for preparing a large-size uniform nano noble metal film according to claim 1, wherein the drop amount of the colloidal solution in the critical state is 2-5 μl; and standing for 1-2 h at room temperature.
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