CN111175856B - Strawberry-shaped broadband anti-reflection micro-nano structure on germanium surface and preparation method thereof - Google Patents
Strawberry-shaped broadband anti-reflection micro-nano structure on germanium surface and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a strawberry-shaped broadband anti-reflection micro-nano structure on a germanium surface and a preparation method thereof, belonging to the technical field of infrared optical material processing and application. According to the invention, an array formed by periodically arranging micro-nano three-dimensional strawberry-shaped structure units in a close-packed hexagonal mode is directly processed on the germanium substrate, so that the anti-reflection of the whole transmission waveband of the germanium substrate can be realized, and the problems of environment adaptability and film quality of a multilayer film are solved; in addition, the anti-reflection of different spectral widths can be met by adjusting the size and the arrangement period of the three-dimensional strawberry-shaped structural units, and the requirement of rapid development of the infrared technology on the anti-reflection of a wide spectrum is met.
Description
Technical Field
The invention particularly relates to a strawberry-shaped micro-nano structure capable of realizing broadband anti-reflection by processing on a germanium surface and a preparation method thereof, belonging to the technical field of infrared optical material processing and application.
Background
Germanium single crystal is one of the preferred optical materials for infrared optical elements and windows as a high refractive index semiconductor material with excellent performance. The transmission waveband of the germanium single crystal can cover 1.8-25 mu m, and comprises two infrared windows of 3-5 mu m and 8-12 mu m of 3 atmospheric windows. However, the refractive index of the germanium single crystal is more than 4 in the wavelength band of 1.8-25 μm, the Fresnel reflection loss is serious, and the germanium single crystal must be subjected to anti-reflection treatment as an optical element.
The traditional method for reducing reflection and increasing transmission is to plate a plurality of layers of reflection increasing films on the surface of a substrate material, the existing technology of infrared reflection increasing films with two infrared windows of 3-5 microns and 8-12 microns is mature, but the method brings many limitations to the performance and the application range of the method due to the introduction of new film layer materials, such as the problems of limited alternative film materials in the nature, thermal stability, severe environment resistance, thermal expansion mismatch, adhesive force and the like. In addition, the anti-reflection wave bands in the prior art are mainly concentrated on two infrared windows of 3-5 microns and 8-12 microns, and few broad-band anti-reflection films cannot meet the use requirements of broad-band, dual-band and multi-band anti-reflection technologies, namely severe environments, due to the problems of film materials, processes, film layer quality and the like.
Various limiting problems of the antireflection film can be solved by directly preparing the antireflection micro-nano structure on the substrate, and it is reported that black germanium is prepared by taking germanium single crystal as the substrate, so that high-efficiency antireflection of 0.25-1.7 microns is realized, but the purpose is to increase absorption; and a cylindrical and round hole-shaped anti-reflection micro-nano structure is prepared on the germanium substrate, the anti-reflection wave band is mainly concentrated on 8-12 mu m of long wave, and the coverage wave band is narrower. The research on the anti-reflection micro-nano structure of the germanium substrate with the double wave bands, the three wave bands and other wide wave bands is not reported, and the special requirements of the infrared germanium optical element on the environment and the application range of the wide wave band, the high durability and the like cannot be met.
Disclosure of Invention
In order to solve the problems of insecure multilayer antireflection film and broadband antireflection of a germanium substrate, the invention provides a strawberry-shaped broadband antireflection micro-nano structure on the surface of germanium and a preparation method thereof.
The purpose of the invention is realized by the following technical scheme.
A strawberry-shaped broadband anti-reflection micro-nano structure on a germanium surface is formed by periodically arranging three-dimensional strawberry-shaped structure units with micro-nano sizes on the surface of a germanium substrate in a close-packed hexagonal mode, wherein the arrangement period is T;
the three-dimensional strawberry-shaped structural unit is a regular triangular frustum or a regular triangular prism, the cross section of the regular triangular frustum or the regular triangular prism is in the shape of an equilateral triangle with three corners all being rounded corners, and the height of the regular triangular frustum or the regular triangular prism is H (namely the vertical distance between two bottom surfaces in the regular triangular frustum or the regular triangular prism); the center of the equilateral triangle is taken as the center of a circle, and the central angle corresponding to the fillet is 15-30 degrees;
when the three-dimensional strawberry-shaped structure unit is a regular triangular frustum, the regular triangular frustum is in an inverted state on the germanium substrate, the bottom surface with a larger area is positioned on the surface of the germanium substrate, the bottom surface with a smaller area is positioned in the germanium substrate, and an included angle between the side edge of the regular triangular frustum and the bottom surface with the larger area is more than or equal to 60 degrees and less than 90 degrees;
wherein T is less than or equal to lambda0/ns，H＝λ0h/T is 0.5-0.9; in the formula, λ0Is the center wavelength of the target band, nsIs the refractive index of the germanium substrate, f is the fill factor, and h is the height of an equilateral triangle located on the surface of the germanium substrate (i.e., the distance from a rounded corner of the equilateral triangle to its corresponding side).
The preparation method of the strawberry-shaped broadband anti-reflection micro-nano structure on the surface of the germanium comprises the following steps:
(1) coating a layer of imprinting glue for nanoimprint on the surface of a germanium substrate;
wherein the thickness of the imprinting glue layer is preferably 100 nm-200 nm;
(2) imprinting an imprinting adhesive layer on the surface of a germanium substrate by using a template with a target pattern, placing the imprinting adhesive layer at a temperature which is 30-100 ℃ higher than the glass transition temperature of the imprinting adhesive and under a pressure of 3-14 MPa, preserving heat and pressure for 1-30 min, and transferring the target pattern to the imprinting adhesive layer;
the target pattern is consistent with the shape of a micro-nano structure etched on the germanium substrate; the template with the target pattern is made of SiC and Si3N4Or SiO2；
(3) Removing the imprinting adhesive layer outside the target pattern region on the germanium substrate by adopting reactive ion etching to expose the surface of the germanium substrate;
wherein, the etching parameters are as follows: etching gas O2The flow is 30-60 sccm, the etching power is 60-120W, the bias power is 30-80W, and the etching time is changed along with the thickness change of the imprinting glue layer until the germanium surface is exposed; relative to the imprinting glue layer with the thickness of 100 nm-200 nm, the etching time is 20 s-100 s;
(4) performing reactive ion etching on the residual imprinting adhesive layer according to the target pattern structure, and transferring the target pattern to the surface of the germanium substrate through etching;
wherein, the etching parameters are as follows: etching gas Cl2The flow rate is 20 sccm-60 sccm, and the etching gas BCl3The flow rate is 20sccm to 60sccm, and the inert gas Ar2The flow rate is 20 sccm-60 sccm, the etching power is 60W-150W, the bias power is 20W-50W, the etching pressure is 1 Pa-5 Pa, and the etching time is 10 s-300 s; wherein, with the increase of the etching depth on the surface of the germanium substrate, the Ar can be increased2The flow rate reduces the relative content of the etching gas so as to realize that the cross section area of the regular triangular frustum is reduced from large to small;
(5) and removing the residual imprinting adhesive layer to obtain a strawberry-shaped broadband anti-reflection micro-nano structure on the surface of the germanium substrate.
Further, soaking the deeply etched germanium substrate by using an acetone or sulfuric acid aqueous solution to remove the residual imprinting glue layer; wherein the mass fraction of the sulfuric acid aqueous solution is preferably not more than 20%.
Has the advantages that:
(1) the micro-nano structure is directly processed and recessed into the germanium substrate surface, the preparation process is simple, new film materials are avoided being introduced, and the problems of limited multilayer film materials and film quality of the traditional plated infrared antireflection film are solved;
(2) the micro-nano structure can realize the anti-reflection of the whole transmission waveband (1.8-25 mu m) of the germanium substrate, and can realize the anti-reflection of any spectral width in a transparent area of the germanium substrate by adjusting the size and the arrangement period of the three-dimensional strawberry-shaped structure units, thereby meeting the requirement of the rapid development of the infrared technology on the anti-reflection of wide spectrum.
Drawings
Fig. 1 is a surface Scanning Electron Microscope (SEM) image of a germanium single crystal having a strawberry-shaped broadband antireflection micro-nano structure on the surface prepared in example 1.
Fig. 2 is a schematic structural diagram of the three-dimensional strawberry-shaped structural unit.
Fig. 3 is a graph comparing the transmittance of the germanium single crystal with the strawberry-shaped broadband antireflection micro-nano structure on the surface prepared in example 1 with that of an untreated germanium single crystal.
Detailed Description
The invention is further illustrated by the following figures and detailed description, wherein the process is conventional unless otherwise specified, and the starting materials are commercially available from a public disclosure without further specification.
Example 1
Taking a wave band of 3-12 microns comprising two atmospheric windows of 3-5 microns and 8-12 microns as an example, processing a strawberry-shaped wide-band anti-reflection micro-nano structure on the surface of a germanium single crystal, wherein the micro-nano structure is formed by periodically arranging three-dimensional strawberry-shaped structural units with micro-nano sizes on the surface of the germanium single crystal in a close-packed hexagonal mode, the arrangement period T is 1.2 microns, and the filling factor f is 0.7; as can be seen from fig. 2, the three-dimensional strawberry-shaped structural unit is a regular triangular frustum, the cross section of the regular triangular frustum is in the shape of an equilateral triangle with three corners being fillets, the regular triangular frustum is in an inverted state on the germanium single crystal, the bottom surface with a larger area is located on the surface of the germanium single crystal, the bottom surface with a smaller area is located inside the germanium single crystal, an included angle between a lateral edge of the regular triangular frustum and the bottom surface with a larger area is 70 °, the height H of the regular triangular frustum is 1.2 μm, and the angles of the three fillets are 30 °;
the preparation method of the strawberry-shaped broadband antireflection micro-nano structure comprises the following steps:
(1) coating a nano imprinting glue (mr-NIL6000E, Suzhou crystal silicon technology) layer with the thickness of 200nm on the surface of the germanium single crystal in a whirl coating mode;
(2) imprinting a nano-imprinting adhesive layer on the surface of the germanium single crystal by using a SiC template with a target pattern (formed by arranging three-dimensional strawberry-shaped structural units and consistent with a micro-nano structure etched on the surface of the germanium single crystal), placing the nano-imprinting adhesive layer at 100 ℃ and 40bar, keeping the temperature and pressure for 100s, and transferring the target pattern to the nano-imprinting adhesive layer;
(3) removing the nanoimprint lithography glue layer outside the target pattern region on the germanium single crystal by adopting reactive ion etching to expose the surface of the germanium single crystal;
wherein, the etching parameters are as follows: etching gas O2The flow is 30sccm, the etching power is 100W, the bias power is 30W, and the etching time is 60 s;
(4) performing reactive ion etching on the residual nanoimprint lithography glue layer according to the target graph structure, and transferring the target graph to the surface of the germanium single crystal through etching;
wherein, the etching parameters are as follows: etching gas Cl2Flow rate of 30sccm, etching gas BCl3Flow rate of 30sccm, inert gas Ar2The flow is 20 sccm-60 sccm, the etching power is 100W, the bias power is 30W, the etching pressure is 3Pa, and the etching time is 22 s; in the etching process, the Ar is gradually increased along with the increase of the etching depth on the surface of the germanium substrate2Flow rate of etching gas (Cl)2、BCl3) The relative content of the germanium is gradually reduced, so that an inverted regular triangular frustum with a cross section area from large to small is etched on the germanium single crystal;
(5) and (3) soaking the etched germanium single crystal in the step (4) in a sulfuric acid aqueous solution with the mass fraction of 10%, removing the residual nanoimprint lithography glue layer, and obtaining the strawberry-shaped broadband antireflection micro-nano structure on the surface of the germanium single crystal.
The prepared germanium single crystal surface with the strawberry-shaped broadband antireflection micro-nano structure on the surface is subjected to shape characterization by a scanning electron microscope, and the result is shown in figure 1. As can be seen from the SEM photograph in fig. 1, a close-packed hexagonal strawberry-like micro-nano structure was obtained on the surface of the germanium single crystal, and the structure was consistent with the designed structure.
Transmittance characterization of the untreated germanium single crystal and the treated germanium single crystal with the strawberry-shaped broadband antireflection micro-nano structure on the surface was performed by using WGH-30/6 type dual-beam infrared spectrophotometer, and the results are shown in fig. 3 (the solid line represents the untreated germanium single crystal, and the dotted line represents the treated germanium single crystal with the strawberry-shaped broadband antireflection micro-nano structure on the surface). According to the test result, after the strawberry-shaped wide-waveband anti-reflection micro-nano structure is processed on the surface of the germanium single crystal, the transmittance of the germanium single crystal in a waveband of 3-12 microns is improved by about 13% on average, and the anti-reflection effect is obvious.
In summary, the above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. A strawberry-shaped broadband anti-reflection micro-nano structure on a germanium surface is characterized in that: the micro-nano structure is formed by periodically arranging micro-nano three-dimensional strawberry-shaped structure units on the surface of a germanium substrate in a close-packed hexagonal mode, and the arrangement period is T;
the three-dimensional strawberry-shaped structural unit is a regular triangular frustum or a regular triangular prism, the cross section of the three-dimensional strawberry-shaped structural unit is in the shape of an equilateral triangle with three corners all being rounded corners, the height of the equilateral triangle is H, the center of the equilateral triangle is taken as the center of a circle, and the central angle corresponding to the rounded corner is 15-30 degrees; when the three-dimensional strawberry-shaped structure unit is a regular triangular platform, the regular triangular platform is in an inverted state on the germanium substrate, the bottom surface with a larger area is positioned on the surface of the germanium substrate, the bottom surface with a smaller area is positioned in the germanium substrate, and an included angle between a side edge and the bottom surface with the larger area is more than or equal to 60 degrees and less than 90 degrees;
wherein when the three-dimensional strawberry-shaped structural unit is a regular triangular frustum or a regular triangular prism, T is less than or equal to lambda0/ns，H＝λ0h/T is 0.5-0.9; in the formula, λ0Is the center wavelength of the target band, nsIs the refractive index of the germanium substrate, f is the filling factor, h is the height of an equilateral triangle on the surface of the germanium substrate, i.e. h is the distance from a rounded corner of the equilateral triangle to the corresponding side.
2. A preparation method of the strawberry-shaped broadband anti-reflection micro-nano structure on the surface of the germanium according to claim 1 is characterized by comprising the following steps: the steps of the method are as follows,
(1) coating a layer of imprinting glue for nanoimprint on the surface of a germanium substrate;
(2) imprinting an imprinting adhesive layer on the surface of a germanium substrate by using a template with a target pattern, placing the imprinting adhesive layer at a temperature which is 30-100 ℃ higher than the glass transition temperature of the imprinting adhesive and under a pressure of 3-14 MPa, preserving heat and pressure for 1-30 min, and transferring the target pattern to the imprinting adhesive layer;
(3) removing the imprinting adhesive layer outside the target pattern region on the germanium substrate by adopting reactive ion etching to expose the surface of the germanium substrate;
(4) performing reactive ion etching on the residual imprinting adhesive layer according to the target pattern structure, and transferring the target pattern to the surface of the germanium substrate through etching;
(5) removing the residual imprinting adhesive layer, and obtaining a strawberry-shaped broadband anti-reflection micro-nano structure on the surface of the germanium substrate;
and the target pattern is consistent with the shape of the strawberry-shaped broadband antireflection micro-nano structure obtained on the surface of the germanium substrate.
3. The preparation method of the strawberry-shaped broadband anti-reflection micro-nano structure on the surface of the germanium according to claim 2, which is characterized by comprising the following steps: in the step (1), the thickness of the coated imprinting glue layer is 100 nm-200 nm.
4. The preparation method of the strawberry-shaped broadband anti-reflection micro-nano structure on the surface of the germanium according to claim 2, which is characterized by comprising the following steps: in the step (2), the template with the target pattern is made of SiC or Si3N4Or SiO2。
5. The preparation method of the strawberry-shaped broadband anti-reflection micro-nano structure on the surface of the germanium according to claim 2, which is characterized by comprising the following steps: in the step (3), the parameters of reactive ion etching: etching gas O2The flow rate is 30-60 sccm, the etching power is 60-120W, and the bias power is 30-80W.
6. The preparation method of the strawberry-shaped broadband anti-reflection micro-nano structure on the surface of the germanium according to claim 5, wherein the preparation method is characterized in that: when the thickness of the imprinting glue layer is 100 nm-200 nm, the etching time is 20 s-100 s.
7. The preparation method of the strawberry-shaped broadband anti-reflection micro-nano structure on the surface of the germanium according to claim 2, which is characterized by comprising the following steps: in the step (4), the parameters of reactive ion etching: etching gas Cl2The flow rate is 20 sccm-60 sccm, and the etching gas BCl3The flow rate is 20sccm to 60sccm, and the inert gas Ar2The flow rate is 20 sccm-60 sccm, the etching power is 60W-150W, the bias power is 20W-50W, the etching pressure is 1 Pa-5 Pa, and the etching time is 10 s-300 s.
8. The preparation method of the strawberry-shaped broadband anti-reflection micro-nano structure on the surface of the germanium according to claim 2, which is characterized by comprising the following steps: and soaking the deeply etched germanium substrate in acetone or sulfuric acid water solution to remove the residual imprinting glue layer.
9. The preparation method of the strawberry-shaped broadband anti-reflection micro-nano structure on the surface of the germanium according to claim 8, wherein the preparation method comprises the following steps: the mass fraction of the sulfuric acid aqueous solution is not more than 20%.
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