CN113064227B - Preparation method of sinusoidal grating - Google Patents
Preparation method of sinusoidal grating Download PDFInfo
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- CN113064227B CN113064227B CN202110307016.7A CN202110307016A CN113064227B CN 113064227 B CN113064227 B CN 113064227B CN 202110307016 A CN202110307016 A CN 202110307016A CN 113064227 B CN113064227 B CN 113064227B
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/18—Diffraction gratings
- G02B5/1847—Manufacturing methods
- G02B5/1857—Manufacturing methods using exposure or etching means, e.g. holography, photolithography, exposure to electron or ion beams
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- G—PHYSICS
- G02—OPTICS
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Abstract
The invention discloses a preparation method of a sinusoidal grating, which comprises the following steps: depositing an adhesion film layer and a first noble metal film layer on the upper surface of the substrate in sequence; coating photoresist on the surface of the first noble metal film layer, and manufacturing a sinusoidal grating photoresist mask pattern by utilizing a photoetching technology; electroplating a second noble metal film layer on the surface which is not covered with the photoresist in the first noble metal film layer; removing the photoresist of the sinusoidal grating photoresist mask pattern; etching the adhesion film layer and the first noble metal film layer on the upper surface of the substrate to obtain a sinusoidal grating template; placing the sinusoidal grating template into etching liquid consisting of hydrofluoric acid and an oxidant, and carrying out metal catalytic etching to obtain a sinusoidal grating; and cleaning and drying the sinusoidal grating.
Description
Technical Field
The invention relates to the technical field of grating micro-nano processing, in particular to a preparation method of a sinusoidal grating.
Background
The sinusoidal grating has simple structure, has the characteristics of dispersion, beam splitting, phase matching, high-order diffraction elimination and the like, and can be used for spectrometers, color testers and the like. In recent years, the application range of sinusoidal grating microstructures has expanded from the field of spectroscopy to the fields of metrology science, optical communications, and the like.
In the prior art, two methods for manufacturing the sinusoidal grating are provided, namely a two-beam interference method and a focused ion beam sputter etching method. The double-beam interference method mainly uses two beams of coherent plane light waves which are symmetrical to the normal of a substrate and enter the surface of the substrate, interference fringes are recorded through photoresist on the substrate, and a sinusoidal grating is obtained after development, but the requirements on light paths and environments are extremely high. The focused ion beam sputter etching method performs structural processing by making ions focused by an electromagnetic lens and having certain energy incident on the surface of a material and interacting with the surface of a target, but has higher cost and lower efficiency, and the prepared sinusoidal grating has poorer surface shape.
Disclosure of Invention
In view of this, the invention provides a method for manufacturing a sinusoidal grating, in order to solve the problems that the sinusoidal grating prepared in the prior art has a poor surface shape, is difficult to manufacture, and has high cost.
In order to achieve the above object, the present invention provides a method for preparing a sinusoidal grating, comprising: depositing an adhesion film layer and a first noble metal film layer on the upper surface of the substrate in sequence; coating photoresist on the surface of the first noble metal film layer, and manufacturing a sinusoidal grating photoresist mask pattern by utilizing a photoetching technology; electroplating a second noble metal film layer on the surface which is not covered with the photoresist in the first noble metal film layer; removing the photoresist of the sine grating photoresist mask pattern; etching the adhesion film layer and the first noble metal film layer on the upper surface of the substrate to obtain a sinusoidal grating template; placing the sinusoidal grating template into etching liquid consisting of hydrofluoric acid and an oxidant, and carrying out metal catalytic etching to obtain a sinusoidal grating; the second noble metal film layer is used as a catalyst for metal catalytic etching; and cleaning and drying the prepared sinusoidal grating.
Optionally, the substrate comprises a silicon wafer, which may be monocrystalline silicon of P-type (100) crystal orientation, with a thickness greater than 1 mm.
Optionally, the adhesion film layer includes one of a titanium film or a chromium film, and the first noble metal film layer includes one of a gold film, a silver film, or a platinum film.
Optionally, the deposition method of the adhesion film layer and the first noble metal film layer comprises one of magnetron sputtering, ion beam sputtering or electron beam evaporation, and the thicknesses of the adhesion film layer and the first noble metal film layer are both less than 50 nm.
Optionally, the sinusoidal grating mask pattern comprises an array of lines on the micrometer scale or nanometer scale.
Optionally, the lithography technique comprises one of optical lithography or electron beam lithography.
Optionally, the first noble metal film layer is made of the same material as the second noble metal film layer, and the thickness of the second noble metal film layer is in the range of 15nm to 25 nm.
Optionally, etching the adhesion film layer and the first noble metal film layer on the upper surface of the substrate to obtain the sinusoidal grating template includes: and etching the adhesion film layer and the first noble metal film layer on the upper surface of the substrate by adopting inductively coupled plasma to obtain the sinusoidal grating template.
Optionally, the oxidant comprises one of hydrogen peroxide, potassium permanganate or silver nitrate.
Optionally, the concentration range of the hydrofluoric acid is between 1mol/L and 20mol/L, the concentration range of the hydrogen peroxide is between 0.1mol/L and 1mol/L, and the temperature range of the etching solution is between-10 ℃ and 30 ℃.
The invention firstly deposits an adhesion film layer and a first noble metal film layer on the surface of a substrate, then carries out photoetching to manufacture a sinusoidal grating photoresist mask pattern, electroplates a second noble metal film layer, removes the photoresist of the sinusoidal grating photoresist mask pattern, then etches the adhesion film layer and the first noble metal film layer, and finally uses a metal catalytic etching technology to etch the substrate to obtain the sinusoidal grating. The etching direction of the metal catalytic etching is vertical to the surface of the substrate and downward, the side wall of the manufactured grating is steep, the etching depth is not limited and can be determined by the reaction time; the metal catalytic etching is a wet etching method, the side wall of the grating is extremely smooth, and the roughness can reach 1nm RMS magnitude. Therefore, compared with the prior art, the beneficial technical effects of the invention are as follows: can manufacture large-area, high-precision and good-surface-shape sinusoidal grating.
Drawings
FIG. 1 is a flow chart of a sinusoidal grating fabrication method according to an embodiment of the present invention;
FIG. 2 is a cross-sectional view of a structure of an adhesion film layer and a first noble metal film layer deposited on an upper surface of a substrate according to an embodiment of the present invention;
FIG. 3 is a top view of a sinusoidal grating photoresist mask fabricated on the surface of a first noble metal layer according to an embodiment of the present invention;
FIG. 4 is a sectional view of the structure of a substrate after electroplating of a second noble metal film layer, according to an embodiment of the present invention;
FIG. 5 is a cross-sectional view of the structure of the substrate after removal of the photoresist according to an embodiment of the present invention;
FIG. 6 is a cross-sectional view of a sinusoidal grating template according to an embodiment of the present invention;
FIG. 7 is a cross-sectional view of a sinusoidal grating structure obtained after metal catalytic etching according to an embodiment of the present invention;
fig. 8 is a schematic diagram of a sinusoidal grating obtained after cleaning and drying according to an embodiment of the present invention.
[ legends of drawings ]
1-a substrate; 2-an adhesive film layer; 3-a first noble metal film layer; 4-photoresist; 5-second noble metal film layer
Detailed Description
In order that the objects, technical solutions and advantages of the present invention will become more apparent, the present invention will be further described in detail with reference to the accompanying drawings in conjunction with the following specific embodiments.
The invention provides a preparation method of a sinusoidal grating. Fig. 1 is a flowchart of a sinusoidal grating manufacturing method according to an embodiment of the present invention. FIG. 2 is a cross-sectional view of a structure of an adhesion film layer and a first noble metal film layer deposited on the upper surface of a substrate according to an embodiment of the present invention.
As shown in fig. 1, the preparation method includes operations S101 to S107.
In operation S101, an adhesion film layer 2 and a first noble metal film layer 3 are sequentially deposited on the upper surface of the substrate 1, as shown in fig. 2.
According to the embodiment of the present invention, for example, the substrate 1 may be P-type single crystal silicon of (100) crystal orientation, and may have a thickness of 2 mm.
According to an embodiment of the present invention, the adhesion film layer includes one of a titanium film or a chromium film, and the first noble metal film layer includes one of a gold film, a silver film, or a platinum film.
According to the embodiment of the present invention, the thickness of each of the adhesion film layer and the first noble metal film layer is less than 50 nm.
According to the embodiment of the invention, the adhesion film layer can be a titanium film, and the thickness of the titanium film can be 2 nm-3 nm, and can be selected from 2nm, 2.2nm, 2.4nm, 2.6nm and 3 nm.
According to the embodiment of the invention, the first noble metal film layer can be a gold film, and the thickness of the gold film can be 10nm to 15nm, and can be selected from 10nm, 11nm, 12nm, 13nm and 15 nm.
According to the embodiment of the invention, the titanium film and the gold film can be deposited by adopting a magnetron sputtering method, an ion beam sputtering method or an electron beam evaporation coating method.
FIG. 3 is a top view of a sinusoidal grating photoresist mask fabricated on the surface of a first noble metal layer according to an embodiment of the present invention.
In operation S102, a photoresist 4 is coated on the surface of the first noble metal film layer 3, and a sinusoidal grating photoresist mask pattern is formed by using a photolithography technique, as shown in fig. 3.
According to the embodiment of the invention, the sinusoidal grating mask pattern is a line array, the period can be 1-2 μm, and the line width can be 0.5-1 μm.
According to the embodiment of the invention, for example, the photoresist can be a positive photoresist, and the photoresist mask pattern is consistent with the target pattern due to the positive photoresist.
According to the embodiment of the present invention, the photoresist is coated by using a spin coating method, the coating thickness is in the range of 50nm to 100nm, and the coating thickness can be reduced or increased according to the actual process conditions, which is not particularly limited in the embodiment of the present invention. Wherein, the adjustment of the coating thickness can be realized by adjusting the rotating speed and the proportion of the solvent in the photoresist.
According to the embodiment of the invention, the gluing process comprises the following steps: coating photoresist on the surface, and baking the photoresist.
According to an embodiment of the invention, the lithography technique may be electron beam lithography, the electron beam voltage may be, for example, 100kV, the current may be, for example, 200pA, and the electron dose may be, for example, 1000 uC/cm2。
FIG. 4 is a cross-sectional view of the structure of the substrate after electroplating of the second noble metal film layer according to an embodiment of the present invention.
In operation S103, a second noble metal film layer 5 is electroplated on the surface of the first noble metal film layer 3 not covered with the photoresist 4, as shown in FIG. 4.
According to the embodiment of the present invention, the first noble metal film layer 3 and the second noble metal film layer 5 are made of the same material.
According to an embodiment of the present invention, the second noble metal film thickness 5 may be 15nm to 25nm, and may be selected from 15nm, 18nm, 20nm, 22nm, and 25 nm.
FIG. 5 is a cross-sectional view of the structure of the substrate after removal of the photoresist in accordance with an embodiment of the present invention.
In operation S104, the photoresist 4 of the sinusoidal grating photoresist mask pattern is removed, as shown in fig. 5.
According to the embodiment of the invention, the photoresist 4 of the sine grating photoresist mask pattern is removed by a wet photoresist removing method, the used solution is acetone, absolute ethyl alcohol and deionized water in sequence, and then N is used2And (5) drying.
Fig. 6 is a structural cross-sectional view of a sinusoidal grating template according to an embodiment of the present invention.
In operation S105, the adhesion film layer 2 and the first noble metal film 3 on the upper surface of the substrate 1 are etched to obtain a sinusoidal grating template, as shown in fig. 6.
According to the embodiment of the invention, etching the adhesion film layer 2 and the first noble metal film layer 3 on the upper surface of the substrate 1 to obtain the sinusoidal grating template comprises the following steps: and etching the adhesion film layer 2 and the first noble metal film layer 3 on the upper surface of the substrate 1 by adopting inductively coupled plasma to obtain the sinusoidal grating template.
According to the embodiment of the invention, the adhesion film layer 2 and the first noble metal film layer 3 on the upper surface of the substrate 1 are etched by using inductively coupled plasma, and the process gas used for etching can be argon gas and hydrogen bromide, wherein the flow rate of the argon gas can be 28sccm, the flow rate of the hydrogen bromide can be 80sccm, the working pressure can be 800Pa, and the power can be 300W.
Fig. 7 is a structural cross-sectional view of a sinusoidal grating obtained after metal catalytic etching according to an embodiment of the present invention.
In operation S106, the sinusoidal grating template is placed in an etching solution composed of hydrofluoric acid and an oxidant, and metal catalytic etching is performed to obtain a sinusoidal grating, as shown in fig. 7.
According to an embodiment of the invention, hydrofluoric acid is used to dissolve the adhesion film layer 2 of the sinusoidal grating template.
According to the embodiment of the invention, the etching solution is used for carrying out metal catalytic etching on the substrate 1 of the sinusoidal grating template, wherein the etching solution can be composed of hydrofluoric acid and an oxidizing agent.
According to the embodiment of the present invention, the first noble metal film layer 3 serves as a catalyst for metal-catalyzed etching.
According to the embodiment of the invention, the substrate 1 is subjected to metal catalytic etching by using the etching solution and the first noble metal film layer 3, so that the sinusoidal grating is obtained. Specifically, after the adhesion film layer 2 of the sinusoidal grating template is dissolved by hydrofluoric acid, the first noble metal layer 3 of the sinusoidal grating template is in direct contact with the substrate 1, and the first noble metal film layer 3 can be used as a catalyst for metal catalytic etching.
According to an embodiment of the present invention, the oxidizing agent comprises one of hydrogen peroxide, potassium permanganate, or silver nitrate.
According to the embodiment of the invention, the concentration range of the hydrofluoric acid is between 1mol/L and 20mol/L, and can be selected from 1mol/L, 5mol/L, 10mol/L, 15mol/L and 20 mol/L.
According to the embodiment of the invention, the oxidant can be hydrogen peroxide, and the concentration range of the hydrogen peroxide is 0.1 mol/L-1 mol/L, and can be selected from 0.1mol/L, 0.2mol/L, 0.5mol/L, 0.8mol/L and 1 mol/L.
According to the embodiment of the invention, the temperature of the etching solution ranges from-10 ℃ to 30 ℃, and can be selected from-10 ℃, 0 ℃, 10 ℃, 20 ℃ and 30 ℃.
Fig. 8 is a schematic diagram of a sinusoidal grating obtained after cleaning and drying according to an embodiment of the present invention.
In operation S107, the sinusoidal grating is cleaned and dried.
According to the embodiment of the invention, the prepared sinusoidal grating is washed by deionized water and isopropanol in sequence, then placed for natural drying, and the washed and dried sinusoidal grating is straightened, as shown in fig. 8.
According to the embodiment of the invention, the sinusoidal grating is prepared by depositing an adhesion film layer and a first noble metal film layer on the surface of a substrate, photoetching to prepare a sinusoidal grating photoresist mask pattern, electroplating a second noble metal film layer, removing photoresist of the sinusoidal grating photoresist mask pattern, etching the adhesion film layer and the first noble metal film layer, and finally etching the substrate by using a metal catalytic etching technology. The etching direction of the metal catalytic etching is vertical to the surface of the substrate and downward, the side wall of the manufactured grating is steep, the etching depth is not limited and can be determined by the reaction time; the metal catalytic etching is a wet etching method, and the side wall of the grating is extremely smooth and can reach 1nm RMS magnitude. Therefore, the sinusoidal grating preparation method provided by the invention can be used for preparing the sinusoidal grating with large area, high precision and good surface shape.
The above-mentioned embodiments, objects, technical solutions and advantages of the present invention are further described in detail, it should be understood that the above-mentioned embodiments are only examples of the present invention, and should not be construed as limiting the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. A preparation method of a sinusoidal grating is characterized by comprising the following steps:
depositing an adhesion film layer and a first noble metal film layer on the upper surface of the substrate in sequence;
coating photoresist on the surface of the first noble metal film layer, and manufacturing a sinusoidal grating photoresist mask pattern by utilizing a photoetching technology;
electroplating a second noble metal film layer on the surface which is not covered with the photoresist in the first noble metal film layer;
removing the photoresist of the sinusoidal grating photoresist mask pattern;
etching the adhesion film layer and the first noble metal film layer on the upper surface of the substrate to obtain a sinusoidal grating template;
placing the sinusoidal grating template into etching liquid consisting of hydrofluoric acid and an oxidant, and carrying out metal catalytic etching to obtain a sinusoidal grating; the hydrofluoric acid is used for dissolving the adhesion film layer, the etching liquid is used for carrying out metal catalytic etching on the substrate, and the second noble metal film layer is used as a catalyst for the metal catalytic etching;
cleaning and drying the sinusoidal grating;
wherein the thickness of the substrate is greater than 1 mm;
the thicknesses of the adhesion film layer and the first noble metal film layer are both less than 50 nm;
the thickness range of the second noble metal film layer is between 15nm and 25 nm;
the concentration range of the hydrofluoric acid is between 1mol/L and 20 mol/L;
the oxidant comprises one of hydrogen peroxide, potassium permanganate or silver nitrate, wherein the concentration range of the hydrogen peroxide is between 0.1mol/L and 1 mol/L;
the temperature range of the etching solution is-10 ℃ to 30 ℃.
2. The method of claim 1, wherein the substrate comprises a silicon wafer comprising P-type (100) crystal oriented single crystal silicon.
3. The method of manufacturing a sinusoidal grating according to claim 1, wherein said adhesion film layer comprises one of a titanium film or a chromium film, and said first noble metal film layer comprises one of a gold film, a silver film or a platinum film.
4. The method of claim 1, wherein the adhesion film layer and the first noble metal film layer are deposited by one of magnetron sputtering, ion beam sputtering or electron beam evaporation.
5. The method of claim 1, wherein the sinusoidal grating mask pattern comprises an array of micro-scale or nano-scale lines.
6. The method of claim 1, wherein the lithography technique comprises one of optical lithography or electron beam lithography.
7. The method of claim 1, wherein said first noble metal film layer is made of the same material as said second noble metal film layer.
8. The method for manufacturing a sinusoidal grating according to claim 1, wherein the etching the adhesion film layer and the first noble metal film layer on the upper surface of the substrate to obtain the sinusoidal grating template comprises:
and etching the adhesion film layer and the first noble metal film layer on the upper surface of the substrate by adopting inductive coupling plasma to obtain the sinusoidal grating template.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103149615A (en) * | 2013-03-14 | 2013-06-12 | 上海交通大学 | Preparation method of multilayer metal grating |
| CN108469644A (en) * | 2018-02-28 | 2018-08-31 | 中国科学院高能物理研究所 | grating and preparation method thereof |
| CN108680979A (en) * | 2018-06-21 | 2018-10-19 | 中国人民解放军63908部队 | Two-dimension grating resists Polarization-Sensitive SERS substrates and its processing method |
| CN108873133A (en) * | 2018-05-23 | 2018-11-23 | 中山大学 | A kind of one-dimensional double-level-metal grating and preparation method thereof |
| JP2021015023A (en) * | 2019-07-11 | 2021-02-12 | 株式会社ミツトヨ | Method of manufacturing scales |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103149615A (en) * | 2013-03-14 | 2013-06-12 | 上海交通大学 | Preparation method of multilayer metal grating |
| CN108469644A (en) * | 2018-02-28 | 2018-08-31 | 中国科学院高能物理研究所 | grating and preparation method thereof |
| CN108873133A (en) * | 2018-05-23 | 2018-11-23 | 中山大学 | A kind of one-dimensional double-level-metal grating and preparation method thereof |
| CN108680979A (en) * | 2018-06-21 | 2018-10-19 | 中国人民解放军63908部队 | Two-dimension grating resists Polarization-Sensitive SERS substrates and its processing method |
| JP2021015023A (en) * | 2019-07-11 | 2021-02-12 | 株式会社ミツトヨ | Method of manufacturing scales |
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