CN110629262B - Preparation method of surface plasmon metamaterial - Google Patents
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- CN110629262B CN110629262B CN201910767482.6A CN201910767482A CN110629262B CN 110629262 B CN110629262 B CN 110629262B CN 201910767482 A CN201910767482 A CN 201910767482A CN 110629262 B CN110629262 B CN 110629262B
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Abstract
The invention provides a preparation method of a surface plasmon metamaterial, and belongs to the technical field of nanophotonics and nano processing. The invention adopts electroplating technology, realizes the control of the thickness of the intermediate medium layer in the metal-medium-metal by controlling the thickness of the spin-coating photoresist, and different medium layer thicknesses can be used as an optical cavity and coupled with surface plasmons, thereby realizing different optical responses; meanwhile, the optical absorption is enhanced by using the ohmic loss of metal, and the near-perfect optical absorption (the absorption rate is close to 100%) and high-quality factor optical cavity can be realized by combining the electromagnetic energy confinement effect of the surface plasmon.
Description
Technical Field
The invention relates to the technical field of nanophotonics and nano processing, in particular to a preparation method of a surface plasmon metamaterial.
Background
Surface plasmons are mainly based on the interaction process of electromagnetic radiation and conduction electrons in metal interfaces or metal structures of sub-wavelength size, and this interaction will lead to optical near-field enhancement and optical nonlinear effects of sub-wavelength size. The subwavelength structures are arranged into an array according to a certain rule, and the array can have special electromagnetic properties which are not possessed by natural materials, namely surface plasmon meta-materials. The special electromagnetic properties of the metamaterial mainly depend on the shape, size, direction, arrangement mode and the like of the subwavelength unit structure. With the continuous development of micro and nano processing technology, people can manufacture metal nano structures with various geometric shapes by utilizing the technologies of deep ultraviolet lithography, electron beam exposure, focused ion beam etching, nano imprinting and the like. For example, the prepared nano grating, nano hole and metal-dielectric layer-metal multilayer structure can effectively excite surface plasmon and realize the regulation and control of parameters such as frequency, polarization, phase and the like of electromagnetic waves. The metal-dielectric layer-metal multilayer structure is one of the most widely applied surface plasmon metamaterial structures at present, bound surface plasmons can be supported by the metal-dielectric layer-metal multilayer structure on interfaces of different materials, and when the distance between adjacent interfaces is close to the mechanical range or is smaller than the attenuation length of the plasmons excited by the interfaces, a coupling effect can be generated between the surface plasmons on the different interfaces. In a multilayer structure of metal-dielectric layer-metal or dielectric-metal layer-dielectric and the like, surface plasmons generated by the metal layer can form an oscillation mode in the dielectric layers on the two sides. Similar to an optical cavity, the structure can efficiently localize the optical field energy in the dielectric layer, so that the structure has huge application prospects in the aspects of optical absorbers and optical biochemical detection.
Although the optical microcavity structure of the multilayer structure shows a plurality of excellent performances, the optical microcavity structure also provides a great challenge for the current micro-nano processing method, and a simple, convenient, standard, systematic and mature processing technology is still lacked. The prior art method is expensive, low in yield, incapable of realizing large-area processing, few in types of machinable structures and the like. Therefore, the development of a flexible, highly controllable and stable metal-dielectric layer-metal or dielectric-metal layer-dielectric optical microcavity structure processing method is of great significance for the design and processing of novel nano-optical cavity structures and the realization of nano-optics application.
Disclosure of Invention
The invention aims to provide a method for processing a cavity coupling resonance surface plasmon polariton metamaterial, aiming at the application requirements and the defects of the prior art.
In order to achieve the purpose of the invention, the technical scheme adopted by the invention comprises the following steps:
a preparation method of a surface plasmon metamaterial comprises the following steps:
(1) preparing a substrate material;
(2) a physical vapor deposition or chemical vapor deposition conductive film with the thickness range of 5-20 nanometers is used as an electroplating seed layer on the substrate;
(3) and (3) photoetching a pattern: spin-coating photoresist, and preparing an air dielectric layer pattern through exposure and development;
(4) electroplating by adopting a square wave pulse method, wherein the voltage is 1-100V, the duty ratio is 10% -90%, and the current is 0.001-1A, and filling the photoetching pattern; continuing electroplating, namely electroplating by adopting a square wave pulse method, wherein the voltage is 1-100V, the duty ratio is 10% -90%, the current is 0.001-1A, and transversely growing a metal film by taking the filled photoetching pattern as a seed layer to form a large-area metal film, wherein the thickness of the metal film is 100 nanometers to 10 micrometers;
(5) soaking in a solution capable of dissolving the photoresist to remove the residual photoresist; and forming the cavity coupling resonance surface plasmon polariton metamaterial of a metal-air dielectric layer-metal structure.
In the above steps, the substrate material in step (1) may be a transparent material such as glass, quartz, etc.
In the above steps, the conductive film in step (2) may be indium tin oxide or a metal film, wherein if gold, silver or copper is used, a titanium or chromium film is required to be added as an adhesion layer.
In the above steps, the lithography method in step (3) is electron beam exposure or deep ultraviolet lithography, the lithography pattern may be a symmetric structure such as a circle, a square, a cross, or the like, or an asymmetric structure such as an ellipse, a triangle, or the like, and the critical dimension of the lithography pattern is between 100 nm and 1 μm.
In the step (3), the thickness of the photoresist is 10 nanometers to 1 micrometer.
The invention has the following technical advantages:
(1) the electroplating process is adopted, the process method is simple, stable and cheap, and large-area processing can be realized;
(2) the thickness of the intermediate dielectric layer is controlled by controlling the thickness of the spin-on photoresist, and different optical responses can be realized by different thicknesses of the dielectric layers;
(3) the metal-air dielectric layer-metal multilayer structure design utilizes ohmic loss of metal to enhance optical absorption, and is combined with the electromagnetic energy confinement effect of surface plasmon to realize optical near-perfect absorption (the absorption rate is close to 100%) and high-quality factor optical cavity, so that the metal-air dielectric layer-metal multilayer structure has huge application potential in the aspects of optical devices and biochemical sensing.
(4) The dielectric layer designed by the invention is an open air dielectric layer, and different substances can be filled inwards, so that the invention can be applied to biochemical sensing.
Drawings
FIG. 1 is a schematic flow chart of a method for preparing a surface plasmon metamaterial, wherein 1 is a metal thin film, 2 is a substrate, 3 is photoresist, 4 is an electroplated gold film, and 5 is an air dielectric layer;
FIG. 2 is an electron micrograph of the surface plasmon metamaterial prepared in example 1 at different plating times, wherein (a) shows a plating time of 10 minutes and (b) shows a plating time of 15 minutes;
FIG. 3 is an optical microscope photograph of a surface plasmon metamaterial prepared in the present invention;
FIG. 4 is an electron micrograph of a surface plasmon metamaterial prepared according to the present invention.
Detailed Description
The invention is described in detail below with reference to the figures and examples.
Example 1:
(1) the substrate material adopts glass;
(2) the method for depositing the metal film on the glass substrate by using the electron beam evaporation coating comprises the following steps: 3 nanometer titanium and 5 nanometer gold;
(3) forming a pattern on the metal film by lithography using electron beam lithography, specifically: firstly, coating photoresist PMMA with the thickness of 120 nanometers in a spinning mode, and preparing a preset pattern through exposure and development;
(4) electroplating and filling the photoetching pattern: electroplating by adopting a square wave pulse method, wherein the voltage is 10V, the duty ratio is 20%, the current is 0.001A, and the time is 10 minutes;
(5) electroplating to grow a gold film: electroplating by adopting a square wave pulse method, wherein the voltage is 10V, the duty ratio is 80%, the current is 0.01A, and the time is 5 minutes;
(6) soaking the substrate in an acetone solution to remove the residual photoresist; and forming the cavity coupling resonance surface plasmon polariton metamaterial of a metal-air dielectric layer-metal structure.
Example 2:
(1) the substrate material adopts glass;
(2) the method for depositing the metal film on the glass substrate by using the electron beam evaporation coating comprises the following steps: 3 nanometer chromium and 5 nanometer silver;
(3) forming a pattern on the metal film by lithography using electron beam lithography, specifically: firstly, coating photoresist PMMA with the thickness of 120 nanometers in a spinning mode, and preparing a preset pattern through exposure and development;
(4) electroplating and filling the photoetching pattern: electroplating by adopting a square wave pulse method, wherein the voltage is 20V, the duty ratio is 50%, the current is 0.001A, and the time is 5 minutes;
(5) electroplating to grow a gold film: electroplating by adopting a square wave pulse method, wherein the voltage is 20V, the duty ratio is 50%, the current is 0.001A, and the time is 10 minutes;
(6) soaking the substrate in an acetone solution to remove the residual photoresist; and forming the cavity coupling resonance surface plasmon polariton metamaterial of a metal-air dielectric layer-metal structure.
Example 3:
(1) the substrate material adopts glass;
(2) depositing an indium tin oxide film on a glass substrate by using an evaporation coating, wherein the thickness of the indium tin oxide film is between 5 and 20 nanometers;
(3) photoetching by using an ultraviolet photoetching machine to form patterning, specifically: spin-coating 150 nm ultraviolet photoresist, and preparing a predetermined pattern by exposure and development;
(4) electroplating and filling the photoetching pattern: electroplating by adopting a square wave pulse method, wherein the voltage is 10V, the duty ratio is 20%, the current is 0.01A, and the time is 15 minutes;
(5) electroplating to grow a gold film: the voltage is 80V, the duty ratio is 20%, the current is 0.01A, and the time is 45 minutes;
(6) soaking the substrate in acetone solution to remove the residual photoresist; and forming the cavity coupling resonance surface plasmon polariton metamaterial of a metal-air dielectric layer-metal structure.
Although the present invention has been described with reference to the preferred embodiments, it is not intended to be limited thereto. Those skilled in the art can make numerous possible variations and modifications to the present invention, or modify equivalent embodiments, using the methods and techniques disclosed above, without departing from the scope of the present invention. Therefore, any simple modification, equivalent change and modification made to the above embodiments according to the technical essence of the present invention are still within the scope of the protection of the technical solution of the present invention, unless the contents of the technical solution of the present invention are departed.
Claims (5)
1. A preparation method of a surface plasmon metamaterial comprises the following steps:
(1) performing physical vapor deposition or chemical vapor deposition on the substrate material to obtain a conductive film with a thickness of 5-20 nm as a plating seed layer;
(2) spin-coating a photoresist, and preparing an air dielectric layer pattern through exposure and development, wherein the air dielectric layer pattern is circular, square, cross-shaped, oval or triangular, the key size of the air dielectric layer pattern is 100 nanometers to 1 micrometer, and the thickness of the photoresist is 10 nanometers to 1 micrometer;
(3) electroplating by adopting a square wave pulse method, wherein the voltage is 1-100V, the duty ratio is 10% -90%, and the current is 0.001-1A, and filling the photoetching pattern; continuing electroplating, similarly adopting a square wave pulse method to electroplate, wherein the voltage is 1-100V, the duty ratio is 10% -90%, the current is 0.001-1A, and transversely growing a metal film by taking the filled photoetching pattern as a seed layer to form a large-area metal film with the thickness of 100 nanometers-10 micrometers;
(4) soaking in a solution capable of dissolving the photoresist to remove the residual photoresist; and forming the cavity coupling resonance surface plasmon polariton metamaterial of a metal-air dielectric layer-metal structure.
2. The method for preparing a surface plasmon metamaterial according to claim 1, wherein the substrate material of step (1) is glass or quartz.
3. The method for preparing a surface plasmon metamaterial according to claim 1, wherein the conductive film in step (1) is indium tin oxide or a metal film.
4. The method for preparing a surface plasmon metamaterial according to claim 3, wherein the metal thin film is gold, silver or copper, and a titanium or chromium thin film is added as an adhesive layer.
5. The method for preparing a surface plasmon metamaterial according to claim 1, wherein the photolithography method in the step (2) is an electron beam exposure or deep ultraviolet lithography technique.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0594937A (en) * | 1991-10-01 | 1993-04-16 | Sumitomo Electric Ind Ltd | Formation method of fine structure body |
| CN101360849A (en) * | 2005-11-18 | 2009-02-04 | 莱里斯奥鲁斯技术公司 | Method for forming multi-layer structure |
| CN104495742A (en) * | 2014-12-15 | 2015-04-08 | 北京大学 | Process for processing surface plasmon polariton coupled nano array based on scallop effect |
| CN109095435A (en) * | 2018-08-02 | 2018-12-28 | 北京大学 | A kind of three-dimensional all-metal micro-cavity structure surface phasmon array-processing method |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0594937A (en) * | 1991-10-01 | 1993-04-16 | Sumitomo Electric Ind Ltd | Formation method of fine structure body |
| CN101360849A (en) * | 2005-11-18 | 2009-02-04 | 莱里斯奥鲁斯技术公司 | Method for forming multi-layer structure |
| CN104495742A (en) * | 2014-12-15 | 2015-04-08 | 北京大学 | Process for processing surface plasmon polariton coupled nano array based on scallop effect |
| CN109095435A (en) * | 2018-08-02 | 2018-12-28 | 北京大学 | A kind of three-dimensional all-metal micro-cavity structure surface phasmon array-processing method |
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