CN115181949B - Gold and silver composite nanoparticle film for refractive index sensing and preparation method thereof - Google Patents
Gold and silver composite nanoparticle film for refractive index sensing and preparation method thereof Download PDFInfo
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- CN115181949B CN115181949B CN202210801528.3A CN202210801528A CN115181949B CN 115181949 B CN115181949 B CN 115181949B CN 202210801528 A CN202210801528 A CN 202210801528A CN 115181949 B CN115181949 B CN 115181949B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/142—Thermal or thermo-mechanical treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention discloses a gold and silver composite nano particle film for refractive index sensing and a preparation method thereof, wherein the method comprises the following steps: s1, cleaning a substrate: cleaning and drying a transparent substrate for later use; s2, depositing a silver nano film: preparing a silver nano film with uniform thickness on a transparent substrate by magnetron sputtering; s3, preparing silver nano particles: annealing the prepared silver nano film to form silver nano particles; s4, preparing a gold nano film: and (3) covering a gold nano film on the silver nano particles by magnetron sputtering to finish the preparation of the gold and silver composite nano particle film. The gold-silver composite nanoparticle film prepared by the invention comprises a transparent substrate, silver nanoparticles arranged on the substrate and a gold nano film covered on the silver nanoparticles. The preparation method is simple and can be used for large-area preparation. According to the invention, the gold nano film is covered on the silver nano particles, so that the oxidation of the silver nano material can be effectively prevented, and the stability is improved.
Description
Technical Field
The invention relates to the technical field of preparation of nano materials, in particular to a gold and silver composite nano particle film for refractive index sensing and a preparation method thereof.
Background
Nanomaterial and nanotechnology are widely recognized as one of the most important new materials and technology fields in the twentieth century. The nano material has quantum effect and small-size effect and surface effect, and is the leading field of physical, chemical and material research. The preparation method of the nano material is mature, and along with the development of nano technology, the nano material can be widely applied to the fields of chemical catalysis, information sensing, medical biology, new energy and other fields.
The surface plasmon effect of metal nanoparticles is that the surface electron cloud of the nanoparticles is excited by an electric field in an incident electromagnetic wave (or incident light) to generate interaction, so as to form surface plasmons. Such surface plasmons may generate electric fields with higher amplitudes than the incident electromagnetic wave 10 3 -10 7 The local electric field intensity is multiplied to form a local field enhancement effect. The noble metal nano-particle local surface plasmon resonance has obvious electromagnetic field enhancement, and the formants are very sensitive to the change of the refractive index of the surrounding environment, and the intensity and the position of the formants can be correspondingly changed by adjusting the material, the shape and the size of the nano-particle, so that the light can be controlled on the nano scale. The noble metal nano particles are commonly used in the field of high-sensitivity sensing, are very sensitive to the change of the refractive index of surrounding media, and can effectively improve the refractive index sensing sensitivity; however, there is a problem in that the nanoparticles are easily oxidized, thereby decreasing the sensitivity of the refractive index sensor.
Disclosure of Invention
The invention aims at: the preparation method of the gold-silver composite nanoparticle film for refractive index sensing can prevent silver nanoparticles from being oxidized and can enhance the sensitivity of refractive index sensing.
In order to further improve the sensitivity of refractive index sensing, the invention provides a preparation method of a gold-silver composite nano-particle film for refractive index sensing, which solves the problems; the invention is realized by the following specific technical scheme:
the preparation method of the gold-silver composite nanoparticle film for refractive index sensing is characterized by comprising the following steps of:
s1, cleaning a substrate: cleaning and drying a transparent substrate for later use;
s2, depositing a silver nano film: preparing a silver nano film with uniform thickness on the transparent substrate by magnetron sputtering;
s3, preparing silver nano particles: annealing the prepared silver nano film to form silver nano particles;
s4, preparing a gold nano film: and covering a layer of gold nano film on the silver nano particles by magnetron sputtering to finish the preparation of the gold and silver composite nano particle film.
The film material prepared by the process can prevent the oxidation of the silver nanoparticle material, and the film material with high sensitivity for refractive index sensing is obtained.
Further, a preparation method of the gold-silver composite nanoparticle film for refractive index sensing comprises the following steps: step S1, cleaning a substrate: and cleaning the transparent substrate by using a detergent, acetone and ethanol in sequence, taking no water mark and no impurity on the surface as standards, and then drying for later use.
Further, a preparation method of the gold-silver composite nanoparticle film for refractive index sensing comprises the following steps: the transparent substrate in the step S1 is selected from one of glass, quartz or transparent heat-resistant inorganic nonmetallic materials.
Further, a preparation method of the gold-silver composite nanoparticle film for refractive index sensing comprises the following steps: step S2, depositing a silver nano film: preparing a silver nano film with uniform thickness on the transparent substrate by magnetron sputtering; wherein: the magnetron sputtering process conditions are as follows: the sputtering current is 15-25mA, the ionization sputtering is carried out under the argon atmosphere, and the sputtering time is 40-60 seconds; the thickness of the silver nano film is 6-10nm.
Further, a preparation method of the gold-silver composite nanoparticle film for refractive index sensing comprises the following steps: step S3, preparing silver nano particles: annealing the prepared silver nano film in vacuum or inert gas environment by utilizing a thermal annealing technology to change the silver nano film into silver nano particles; wherein the annealing temperature is 300-450 ℃ and the annealing time is 30-120 minutes.
Further, a preparation method of the gold-silver composite nanoparticle film for refractive index sensing comprises the following steps: the particle size of the silver nano particles in the step S3 is 10-80nm.
Further, a preparation method of the gold-silver composite nanoparticle film for refractive index sensing comprises the following steps: step S4, preparing a gold nano film: covering a gold nano film on the silver nano particles by magnetron sputtering to finish the preparation of the gold-silver composite nano particle film;
wherein: the magnetron sputtering process conditions in this step are: the sputtering current is 10-20mA, the ionization sputtering is carried out in the argon atmosphere, and the sputtering time is 15-30 seconds; the thickness of the gold nano film is 1-3nm.
The composite nano particle film has two metal materials, changes the thickness of the gold and silver nano film and improves the surface refractive index sensitivity.
The gold and silver composite nanoparticle film for refractive index sensing is characterized by being prepared by the preparation method.
Further, a gold and silver composite nanoparticle film for refractive index sensing: the gold-silver composite nanoparticle film comprises a transparent substrate, silver nanoparticles arranged on the transparent substrate and a gold nanoparticle film covered on the silver nanoparticles.
The invention belongs to the field of nano material preparation, and relates to a preparation method of a gold-silver composite nano particle film for refractive index sensing, which consists of a transparent substrate, silver nano particles and a gold nano film; the preparation method comprises the following steps: firstly, uniformly depositing a layer of silver nano film with the thickness of 6-10nm on a glass or quartz or other transparent heat-resistant inorganic nonmetallic substrate by utilizing a magnetron sputtering coating method, and integrally placing the deposited silver nano film and a substrate material in an annealing furnace for annealing so that the silver nano film becomes silver nano particles on the substrate; performing magnetron sputtering coating for the second time on the basis to prepare a layer of uniform gold nano film which is covered on the silver nano particles, wherein the thickness of the gold nano film is 1-3nm; finally, the refractive index sensing chip film with high sensitivity and stability is formed.
The invention has the beneficial effects that:
(1) The invention provides a preparation method of a gold-silver composite nano-particle film for refractive index sensing, which mainly comprises 3 parts. And uniformly and sequentially covering two metal nano materials on the transparent substrate, wherein one metal nano material is silver nano particles, and the other metal nano material is a continuous gold nano film covered on the silver nano particles, so that the gold-silver composite nano particle film is formed. The gold nano-film is covered, so that the sensitivity of the whole film material to the medium refractive index sensing can be enhanced, and the chemical stability of the silver nano-particles can be protected.
(2) The preparation method of the invention has simple process and can be used for large-area preparation. Because the chemical property of silver is unstable and is easy to oxidize, the gold nano film is covered on the silver nano particles, so that the oxidation of the silver nano material can be effectively prevented, and the stability is improved.
(3) The nanoparticle film obtained by the preparation method has the function of improving the refractive index sensing sensitivity, and can be applied to a plurality of nano fields, such as the fields of biosensing, smart grids and the like.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the description of the embodiments will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic side view of a substrate material with a silver nano-film deposited after magnetron sputtering according to example 1;
FIG. 2 is a schematic diagram showing a side view of the annealed silver nano-film according to example 1;
FIG. 3 is a schematic structural diagram of a gold-silver composite nanoparticle film formed after sputtering a gold-nanoparticle film;
FIG. 4 is a chart of the extinction tube spectrum (refractive index sensing schematic) measured by an ultraviolet-visible-near infrared spectrometer.
The marks in the figure: 1 transparent substrate, 2 silver nano film, 3 gold nano film and 21 silver nano particle.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the invention. The following description of at least one exemplary embodiment is merely exemplary in nature and is in no way intended to limit the invention, its application, or uses. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
A preparation method of a gold-silver composite nanoparticle film for refractive index sensing comprises the following specific steps:
s1, cleaning a substrate: cleaning the glass substrate 1 sequentially with a detergent, acetone and ethanol, taking no water mark and no impurity on the surface as standards, and then drying for later use;
s2, depositing a silver nano film: preparing a silver nano film 2 by using a magnetron sputtering method, wherein the sputtering current is 20mA, and performing ionization sputtering under an argon atmosphere for 50s; a silver nano film 2 with the thickness of 10nm is obtained on the surface of a transparent glass substrate 1, and the silver nano film 2 is continuously covered on the surface of a glass substrate 1 material, as shown in figure 1;
s3, preparing silver nano particles: annealing the silver nano film 2 by adopting a thermal annealing technology, integrally placing the prepared silver nano film 2 and the transparent glass substrate 1 in an annealing furnace, and vacuumizing to 10 -1 Pa or below, then heating to 350 ℃ and preserving heat for half an hour, and after natural cooling, converting the silver nano-film 2 into silver nano-particle material 21, as shown in fig. 2; the size of the silver nano-particles 21 is controlled by the thickness of the silver nano-film 2 and the annealing process;
s4, preparing a gold nano film: and (3) performing magnetron sputtering on the surface of the whole material again by utilizing magnetron sputtering, wherein the sputtering current is 10mA, performing ionization sputtering under an argon atmosphere for 20s, preparing a gold nano film 3 with the thickness of 2nm on the surface of the material attached with the silver nano particles 21, and finally completing the preparation of the gold-silver composite nano particle film.
As shown in fig. 3, a gold-silver composite nanoparticle film for refractive index sensing, which includes a glass substrate 1 and silver nanoparticles 21 deposited on the glass substrate 1 and a gold-nanoparticle film 3 coated on the silver nanoparticles 21, is manufactured as described above.
The gold-silver composite nanoparticle film prepared in the above embodiment 1 is used as a core material of a refractive index sensing chip, in operation, a fluid medium is on the surface of the gold-silver composite nanoparticle film (as shown in fig. 4), in a specific medium environment, the gold-silver composite nanoparticle film of the invention shows an extinction spectrum, the extinction spectrum has a distinct characteristic absorption peak, which is a surface plasmon resonance peak, in different medium environments, a plurality of extinction spectrums are measured, the spectrums are not coincident, but change according to the change of refractive index, when the refractive index of the medium increases, the resonance characteristic peak moves towards the direction of long wavelength (as shown in fig. 4, the graph of an extinction tube measured by an ultraviolet-visible-near infrared spectrometer), and finally the refractive index of the medium flowing through the surface of the nanomaterial is detected according to the wavelength movement range corresponding to the resonance peak, and the sensitivity of the gold-silver composite nanoparticle film for refractive index sensing prepared in the invention reaches 580nm/RIU.
The above-described preferred embodiments of the present invention are only for illustrating the present invention, and are not to be construed as limiting the present invention. Obvious changes and modifications of the invention, which are introduced by the technical solution of the present invention, are still within the scope of the present invention.
Claims (7)
1. The application of the gold and silver composite nano particle film is characterized in that the preparation method of the gold and silver composite nano particle film comprises the following steps:
s1, cleaning a substrate: cleaning and drying the transparent substrate (1) for later use;
s2, depositing a silver nano film: preparing a layer of silver nano film (2) with uniform thickness on the transparent substrate (1) through magnetron sputtering;
s3, preparing silver nano particles: annealing the prepared silver nano film (2) to form silver nano particles (21);
s4, preparing a gold nano film: covering a layer of gold nano-film (3) on the silver nano-particles (21) by magnetron sputtering to finish the preparation of the gold-silver composite nano-particle film;
the gold and silver composite nano particle film is applied to refractive index sensing.
2. The use of a gold and silver composite nanoparticle film according to claim 1, wherein the step S1 of cleaning the substrate: and (3) cleaning the transparent substrate (1) sequentially by using a detergent, acetone and ethanol, taking no water mark on the surface as a standard, and drying for later use.
3. The use of a gold and silver composite nanoparticle film according to claim 1, wherein the transparent substrate (1) in step S1 is selected from one of transparent glass, transparent quartz or other transparent heat-resistant inorganic nonmetallic materials.
4. The use of a gold and silver composite nanoparticle film according to claim 1, wherein in step S2, a silver nano film is deposited: preparing a layer of silver nano film (2) with uniform thickness on the transparent substrate (1) through magnetron sputtering; wherein: the magnetron sputtering process conditions are as follows: the sputtering current is 15-25mA, the ionization sputtering is carried out under the argon atmosphere, and the sputtering time is 40-60 seconds; the thickness of the silver nano film (2) is 6-10nm.
5. The use of a gold and silver composite nanoparticle film according to claim 1, wherein in step S3, silver nanoparticles are prepared: annealing the prepared silver nano film (2) by utilizing a thermal annealing technology under a vacuum or inert gas environment to form silver nano particles (21) by the silver nano film (2); wherein: the annealing temperature is 300-450 ℃, and the annealing time is 30-120 minutes.
6. Use of a gold and silver composite nanoparticle film according to claim 1 or 5, characterized in that the particle size of the silver nanoparticles (21) in step S3 is 10-80nm.
7. The use of a gold and silver composite nanoparticle film according to claim 1, wherein the preparation of the gold and silver composite nanoparticle film in step S4: covering a gold nano film (3) on the silver nano particles (21) by magnetron sputtering to finish the preparation of the gold-silver composite nano particle film; wherein: the magnetron sputtering process conditions in this step are: the sputtering current is 10-20mA, the ionization sputtering is carried out in the argon atmosphere, and the sputtering time is 15-30 seconds; the thickness of the gold nano film (3) is 1-3nm.
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