CN114114474A - Damage-resistant wide-angle antireflection composite micro-nano structure and preparation method thereof - Google Patents
Damage-resistant wide-angle antireflection composite micro-nano structure and preparation method thereof Download PDFInfo
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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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/40—Oxides
- C23C16/403—Oxides of aluminium, magnesium or beryllium
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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
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
- C23C16/45525—Atomic layer deposition [ALD]
- C23C16/45527—Atomic layer deposition [ALD] characterized by the ALD cycle, e.g. different flows or temperatures during half-reactions, unusual pulsing sequence, use of precursor mixtures or auxiliary reactants or activations
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- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/06—Silicon
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- C30B33/02—Heat treatment
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Abstract
A damage-resistant wide-angle antireflection composite micro-nano structure and a preparation method thereof belong to the technical field of optics, and are constructed in any optical spectrum section for overcoming a high aspect ratio, the structure is composed of a microstructure unit array, the period of the microstructure unit meets the condition of subwavelength, and each microstructure unit comprises a bionic moth-eye micro-nano structure prepared on the surface of an optical material substrate and a composite protective film layer grown on the surface of the moth-eye structure in a common manner; the bionic moth eye micro-nano structure is a round table, a cone or a cylinder, the composite protective layer is made of a high-transmittance material, and the bionic moth eye micro-nano structure is wrapped in the composite protective layer; compared with a single moth eye structure, the anti-environmental damage performance of the anti-reflection composite micro-nano structure is reduced under the condition that the transmittance is ensured at normal incidence and wide angles, so that the effects of reducing the depth-to-width ratio and the full duty ratio are achieved, the micro-nano composite structure is compactly arranged on the surface of the substrate, and a certain anti-damage effect is achieved.
Description
Technical Field
The invention relates to a damage-resistant wide-angle antireflection composite micro-nano structure and a preparation method thereof, belonging to the technical field of optics.
Background
In the application of optical devices, great demands are placed on wide-spectrum wide-angle antireflection, but the window surfaces are in contact with the outside indirectly or indirectly and cannot be influenced by various environmental forces, and moth-eye micro-nano structure devices need to have stable mechanical properties in the actual use process. Linhe, university of Changchun's university and the like, in research on anti-reflection optical super-surface of moth eye in visible light, near infrared and intermediate infrared composite wave band2O3The protective film layer is proved to have Al with a certain thickness by a method of film coating pencil test2O3On the basis of hardly influencing antireflection performance, the protective film layer can effectively increase the damage-resistant hardness of the moth-eye structure and improve the environmental adaptability of the moth-eye structure device.
The existing bionic moth-eye technology needs to modulate the duty ratio of a material in a space, so that the material has the characteristic of discrete discontinuity in the form of the space. The bionic moth-eye micro-nano structure has certain aspect ratio characteristics, which have high requirements on the form and process precision of materials, but the high aspect ratio unit structure has certain problems in environmental damage resistance, and the larger the aspect ratio is, the sparsity of the moth-eye structure arranged on the surface of the substrate and the reduction of the damage resistance can be caused. Therefore, improving the damage resistance of the surface is one of the important problems to be solved by the long-term development of the bionic moth-eye micro-nano device.
With the continuous progress of the technology, a plurality of new micro-nano processing technologies appear. The atomic layer deposition technology is one of the technologies, and is a continuous self-terminating special chemical vapor deposition film technology, and a vapor phase precursor is introduced into a reaction chamber in a pulse mode and generates a chemical adsorption reaction on the surface of a substrate, so that the atomic layer deposition technology has self-limiting growth, good three-dimensional conformality and uniform growth of a film, and the thickness of the film can be accurately controlled. The atomic layer deposition technology has wide application prospect in the fields of microelectronics, photoelectrons, micro-electro-mechanical systems, displays, biology, corrosion resistance, sealing coatings and the like, and provides a principle guarantee for the preparation of the composite micro-nano structure.
Disclosure of Invention
The invention provides a damage-resistant wide-angle antireflection composite micro-nano structure and a preparation method thereof, aiming at overcoming the problem of reduced environmental damage resistance caused by a moth-eye micro-nano structure with a high depth-to-width ratio, and the depth-to-width ratio can be reduced and the damage resistance can be improved on the premise of ensuring the high transmittance of the micro-nano structure.
The technical scheme for solving the technical problem is as follows:
a damage-resistant wide-angle antireflection composite micro-nano structure is constructed in any optical spectrum segment and is characterized by comprising a micro-structure unit array, wherein the period of the micro-structure unit array meets the condition of subwavelength, and each micro-structure unit comprises a bionic moth-eye micro-nano structure prepared on the surface of an optical material substrate and a composite protective film layer grown on the surface of the moth-eye structure in a common manner;
the bionic moth eye micro-nano structure is a round table, a cone or a cylinder, the composite protective layer is made of a high-transmittance material, and the bionic moth eye micro-nano structure is wrapped in the composite protective layer;
the diameter of the bottom end of the composite protective layer is required to meet the condition that D is D1+2dsin alpha, D is less than or equal to p, and the diameter of the top end of the structure also satisfies D1＝d2+2dsinα，D1P is less than or equal to p, and the structural height satisfies H1＝H2Wherein D is the diameter of the bottom end of the second protective layer, D1The top diameter of the second protective layer, d1The diameter of the bottom end of the bionic moth eye micro-nano structure, d2The diameter of the top end of the bionic moth eye micro-nano structure is H1Height of the bionic moth eye micro-nano structure, H2The distance between a composite protective layer at the top end of the bionic moth-eye micro-nano structure and a composite protective layer on the surface of the substrate is represented as p, the period of the moth-eye structure array is represented as d, the thickness of a film layer is represented as d, and alpha is the base angle of the moth-eye structure.
A preparation method of a damage-resistant wide-angle antireflection composite micro-nano structure is characterized by comprising the following steps:
step 1: preparing a graphic mask plate by a laser direct writing or nanosphere self-assembly technology;
the laser direct writing controls the whole direct writing working process through laser direct writing software, firstly, the design and the manufacture of a direct writing graph are carried out, after the laser direct writing control software reads a design drawing, a laser beam scanning path is automatically generated according to the information of the design drawing and the set filling interval, a moving platform finishes the movement in a two-dimensional plane, and the height adjustment is finished by combining the vertical movement; fixing a substrate on an objective table, controlling the objective table to move by a moving platform, monitoring by a visual imaging system consisting of a CCD camera and a lens, accurately positioning the center of a laser beam to the substrate, and focusing the laser beam by moving an axis up and down to obtain a converged laser beam; after positioning and focusing are finished, controlling the laser beam to perform scanning writing on the substrate through a double-vibrating-mirror scanning system according to a laser beam scanning path generated by control software, and finally detecting the forming quality of a laser beam writing graph through a visual imaging system;
the preparation process of the nanosphere self-assembly technology comprises the steps of taking an evaporation pan with a proper size, injecting deionized water with a proper height into the evaporation pan, simultaneously placing and adjusting a substrate with hydrophilicity, placing the substrate on a quartz plate with a certain thickness, and obliquely placing a glass plate which is also subjected to hydrophilicity treatment; after the liquid level is static, taking a trace amount of nanosphere mixed liquid, and slowly dripping the nanosphere mixed liquid on a glass inclined plate to ensure that liquid drops slide into water under the action of gravity; when more nanospheres slide into the liquid surface, the obvious motion track of the microsphere polymer with small area in a heart-shaped surrounding manner can be observed, and the dripping of the solution is stopped until the monomolecular film layer of the nanospheres is fully paved on the whole evaporating dish; at the moment, slowly adding a surfactant dropwise along the side wall of the vessel at a position far away from the substrate to compact the monomolecular layer and ensure that the nanospheres form a hexagonal close-packed structure;
step 2: transferring the mask plate pattern to a substrate material by a wet or dry etching technology to prepare a bionic moth eye structure; the wet etching process comprises the steps of firstly diffusing a reactant to the surface of an etched material, then reacting the reactant with the etched material, and diffusing a product after reaction to a solution after leaving the etching surface and discharging the product along with the solution; dry etching is carried out, wherein the duty ratio of a structure to be etched in a duty ratio structure is adjusted; selecting proper etching gas, and adjusting the gas proportion, the upper and lower radio frequency power, the pressure intensity and the etching temperature to be unchanged, wherein the longer the etching time is, the larger the etching depth is; after etching is finished, the redundant mask material can be placed in acetone for soaking and ultrasonic treatment, then alcohol and deionized water are sequentially used for ultrasonic cleaning, and high-purity nitrogen or argon is blown dry and can be removed;
and step 3: putting the sample wafer in the step 2 into a quartz tube type electric furnace, and performing thermal oxidation treatment by using oxygen in air in a hearth to eliminate lattice damage and tiny gaps generated when a moth eye structure grows; thermal oxidation to form SiO2Etching the sample wafer of the film by hydrofluoric acid to remove the redundant oxide layer film on the surface, wherein the aim of etching by hydrofluoric acid is to ensure that the side wall of the whole structure is smooth and has no damage;
and 4, step 4: uniformly growing a hard film layer on the surface of the prepared bionic moth eye structure by utilizing an atomic layer deposition technology to finish the preparation of the composite protective film layer; after the temperature of the atomic layer deposition equipment is raised, putting the sample wafer into a reaction chamber; in the process of depositing a composite protective layer by adopting an atomic layer deposition technology, the deposition of a protective film layer is completed by utilizing the reaction between two precursors, each cycle mainly comprises the steps that the first precursor enters a reaction chamber by means of steam pulse, the chemical adsorption reaction is carried out on the surface of an exposed substrate or a film, the steam and reaction byproducts of the first precursor which is not adsorbed by the surface are taken out of the reaction chamber by cleaning gas, the second precursor enters the reaction chamber by means of steam pulse and continues to carry out surface chemical reaction with the adsorbed surface of the first precursor, and the steam and reaction byproducts of the second precursor which are not adsorbed by the surface are taken out of the reaction chamber by the cleaning gas, so that one cycle is completed; the thickness of the film is controlled by the number of reaction cycles.
The invention has the beneficial effects that: compared with a single moth eye structure, the antireflection composite micro-nano structure achieves the effects of reducing the depth-to-width ratio and the full duty ratio under the condition that the transmittance is ensured at normal incidence and wide angles, so that the micro-nano composite structure is compactly arranged on the surface of the substrate, and a certain damage resistance effect is achieved. According to the preparation method of the damage-resistant wide-angle antireflection composite micro-nano structure, after a moth-eye structure grows on the surface of a silicon substrate, a thermal oxidation process is used for oxidizing micro damage appearing on the surface of the structure in the growing process, so that the side wall of each structure is undamaged, smooth and clean and has no sharp step or defect. The high-transmittance protective film layer is deposited by the film layer in an atomic layer deposition mode, so that the composite structure is prepared, and the damage resistance effect is achieved. The atomic layer deposition has good three-dimensional shape retention and film uniformity, and meanwhile, the thickness of the film layer can be accurately controlled.
Drawings
Fig. 1 is a structural schematic diagram of a graphene composite micro-nano fiber-based 2 μm wavelength converter with high conversion efficiency.
FIG. 2 is a schematic structural diagram of a 2 μm tunable fiber laser according to the present invention.
FIG. 3 is a spectrum diagram of a 2 μm semiconductor laser according to the present invention.
FIG. 4 is a 2 μm tunable fiber laser spectrum diagram according to the present invention.
Fig. 5 is a diagram of the full-optical wavelength conversion spectrum based on the four-wave mixing effect.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings.
As shown in fig. 1, the damage-resistant wide-angle antireflection composite micro-nano structure can be constructed in any optical spectrum, the structure is totally divided into two layers, i is a bionic moth-eye micro-nano structure prepared on the surface of an optical material substrate, and ii is a composite protective film layer commonly grown on the surface of the moth-eye structure. The unit period of the bionic moth eye micro-nano structure array unit prepared on the substrate still meets the sub-wavelength condition, namely the microstructure unit is a round table, a cone or a cylinder, the second layer of protective layer is made of a high-transmittance material, and the first layer of moth eye structure is wrapped in the second layer of protective layer. The diameter of the bottom end of the protective layer structure is required to satisfy the condition that D is D1+2dsin alpha, D is less than or equal to p, and the diameter of the top end of the structure also satisfies D1＝d2+2dsinα，D1P is less than or equal to p, and the structural height satisfies H1＝H2Wherein D is the diameter of the bottom end of the second protective layer, D1The top diameter of the second protective layer, d1The diameter of the bottom end of the moth eye structure, d2The diameter of the top of the moth eye structure, H1Height of the bionic moth eye micro-nano structure, H2The distance between a composite protective layer at the top end of the bionic moth-eye micro-nano structure and a composite protective layer on the surface of the substrate is represented as p, the period of the moth-eye structure array is represented as d, the thickness of a film layer is represented as d, and alpha is the base angle of the moth-eye structure.
On the basis of the basic structure, the wide-spectrum and wide-angle optical transmittance of the composite structure meets the design requirements through further structural parameter optimization.
The preparation method of the damage-resistant wide-angle antireflection composite micro-nano structure, which is disclosed by the invention, takes a silicon substrate as an example to be explained as follows:
step 1: preparing a graphic mask plate by a laser direct writing or nanosphere self-assembly technology;
the laser direct writing needs to control the whole direct writing working process through laser direct writing software, firstly, the design and the manufacture of a direct writing graph are carried out, and the direct writing graph is generally finished by adopting AutoCAD. After the laser direct-writing control software reads the design drawing, a laser beam scanning path is automatically generated according to the design drawing information and the set filling interval, the moving platform completes the movement in a two-dimensional plane, and the height adjustment is completed by combining the vertical movement. The base is fixed on the objective table, the objective table is controlled by the movable platform to move, and the monitoring is carried out by a visual imaging system consisting of a CCD camera and a lens, so that the center of a laser beam can be accurately positioned to the base, and the laser beam is focused by moving an axis up and down to obtain the best converged laser beam. After positioning and focusing are finished, controlling the laser beam to perform scanning writing on the substrate through a double-vibration mirror scanning system according to a laser beam scanning path generated by control software, and finally detecting the forming quality of a laser beam writing graph through a visual imaging system.
The preparation process of the self-assembled monomolecular film layer takes spin coating Polystyrene (PS) microspheres as an example, an evaporation dish with a proper size is taken, deionized water with a proper height is injected into the evaporation dish, a substrate with hydrophilicity is placed and adjusted at the same time, the substrate is placed on a quartz plate with a certain thickness, and a glass plate which is also subjected to hydrophilicity treatment is obliquely placed. After the liquid surface is static, taking a trace PS microsphere mixed solution, and slowly dripping the mixed solution on a glass inclined plate to ensure that the liquid drops slide into water under the action of gravity. When more PS microspheres slide into the liquid surface, an obvious motion track of a small-area microsphere polymer in a heart-shaped surrounding manner can be observed, and the dripping of the solution is stopped until the PS monomolecular film layer is fully paved on the whole evaporating dish. And at the moment, slowly adding SDS (sodium dodecyl sulfate) surfactant dropwise along the side wall of the vessel at a position far away from the substrate to push a monomolecular layer to ensure that the PS microspheres form a hexagonal close-packed structure.
Step 2: and transferring the mask plate pattern to the substrate material by a dry etching technology or a wet etching technology to prepare the bionic moth eye structure. The wet etching process comprises the steps of firstly diffusing a reactant to the surface of an etched material, then reacting the reactant with the etched material, and then diffusing a product after reaction to a solution after leaving the etching surface, and discharging the product along with the solution. The dry etching method firstly adjusts the duty ratio of the structure to be etched, and the etching gas is SF6And CHF3When the gas proportion, the upper and lower radio frequency power, the pressure intensity and the etching temperature are adjusted to be unchanged, the longer the etching time is, the larger the etching depth is. After the etching is finished, the redundant mask material can be placed in acetone for soaking and ultrasonic treatment, then alcohol and deionized water are sequentially used for ultrasonic cleaning, and high-purity nitrogen or argon is blown dry and can be removed.
And step 3: and (3) putting the sample wafer in the step (2) into a quartz tube type electric furnace, and performing thermal oxidation treatment by using oxygen in air in a hearth, wherein the step can eliminate lattice damage and micro gaps generated in the process of growing the moth-eye structure. Thermal oxidation to form SiO2And etching the film sample wafer by hydrofluoric acid to remove the redundant oxide film on the surface, wherein the aim of etching by hydrofluoric acid is to ensure that the side wall of the whole structure is smooth and has no damage.
And 4, step 4: and uniformly growing a hard film layer on the surface of the prepared bionic moth eye structure by utilizing an atomic layer deposition technology to finish the preparation of the composite structure. And after the temperature of the atomic layer deposition equipment is raised, putting the sample wafer into the reaction chamber. With Al2O3An atomic layer deposition process of a thin film is taken as an example, precursors selected by ALD are trimethyl aluminum (TMA) and deionized water (H2O), each cycle mainly comprises that TMA steam pulse enters a reaction chamber, chemical adsorption reaction occurs on the surface of an exposed substrate or film, excessive TMA steam and reaction byproducts which are not adsorbed by the surface of a cleaning gas bar are taken out of the reaction chamber, water steam pulse enters the reaction chamber and continues to perform surface chemical reaction with the adsorbed surface of the TMA, and the cleaning gas takes the excessive water steam and the reaction-completed byproducts out of the reaction chamber, so that one cycle is completed. Al (Al)2O3The thickness of the film is controlled by the number of reaction cycles.
Example 1:
the composite structures of the present invention will be further illustrated by the following experimental data:
as shown in fig. 1 and fig. 2, which are a cross-sectional view and a three-dimensional effect view of an anti-damage wide-angle antireflection composite micro-nano structure, the diameter of the top end of a truncated cone moth-eye structure is 100nm, the diameter of the bottom end is 800nm, the height is 1.5 μm, the period is 1 μm, and the thickness of a film layer is 100 nm. The silicon substrate is part of region I and the high transmittance protective film is part of region II, in this example, an alumina material is used.
As shown in fig. 3, which is a wavelength-transmittance graph of the composite moth-eye structure at normal incidence, the average transmittance was 96.82% or more, which is 8.25% higher than the transmittance of a single moth-eye structure.
As shown in fig. 4, which is a wavelength-average transmittance graph of a wide-angle composite structure, it can be obtained that the transmittance of the composite micro-nano structure is higher than 96% at 0 ° to 10 °, and the highest point can reach 98%. The highest transmittance is obtained at 35-40 DEG when the incident angle is increased, the average transmittance in the range of 3.5-4.9 μm is higher than 97%, and the higher transmittance is realized in the incident angle range. With further increase in the angle of incidence, the average transmittance decreases. A transmittance of about 94% in the range of 3.5 μm to 4.9 μm when the incident angle is increased to 45 ° or more. Therefore, the micro-nano composite structure can ensure good anti-reflection characteristic within the range of 0-45 degrees.
Therefore, the damage-resistant wide-angle composite structure has strong transmission performance in the mid-infrared region, wherein the average transmittance reaches 96.82% under the normal incidence condition, and the peak transmittance reaches 98.42%. The average transmittance is 96.8% in the angle range of 0-45 DEG, and the characteristic of wide-angle high transmittance is realized.
As shown in fig. 5, a method for preparing a damage-resistant wide-angle antireflection composite micro-nano structure includes the following steps:
step 1: respectively ultrasonically cleaning a monocrystalline silicon piece for 10min by using acetone, ethanol and deionized water, soaking the cleaned monocrystalline silicon piece in the piranha solution for 12h, ultrasonically oscillating by using the deionized water to clean and blow-dry the substrate, and finishing the surface hydrophilic treatment of the silicon-based material.
Step 2: 5 wt% SDS surfactant solution was prepared. Taking a proper amount of PS microspheres with the size of 1 mu m, adding absolute ethyl alcohol and deionized water into the PS microspheres, and carrying out low-frequency ultrasonic oscillation for 3 minutes to dilute the microsphere solution and make the microsphere solution have ductility. And (3) putting the monocrystalline silicon wafer processed in the step (1) into an evaporating dish, and spin-coating the prepared PS microspheres on the surface to form a self-assembled monomolecular film layer so as to finish the preparation of the self-assembled PS microsphere mask plate.
And step 3: and (3) finishing the preparation of the moth eye array by utilizing an inductively coupled plasma etching (ICP) technology. Firstly, the duty ratio of a structure to be etched duty ratio structure, namely the duty ratio of PS microspheres is adjusted, and O is utilized2The particle size of the PS microspheres can be effectively reduced by physically bombarding the colloidal particles through pressure. Ensuring the pressure at 1Pa, the upper and lower radio frequency powers at 300W and 50W, O2The gas flow of the gas is 50sccm, the shortening time is 40-60 s, and the PS microspheres with the diameter of about 800nm are obtained. ICP selects gas as SF respectively6And CHF3The corresponding gas ratio is 30:10, the ICP power is 300W, the RF power is 20W, the pressure is 0.5Pa, the etching temperature is 10 ℃, and the etching time is 400-600 s. And (3) placing the etched sample wafer in acetone for soaking and ultrasonic treatment for about 10min, then sequentially cleaning the sample wafer by using alcohol and deionized water, and blow-drying by using nitrogen, wherein in the ultrasonic treatment process, the ultrasonic frequency should be low-frequency ultrasonic treatment so as to avoid damaging the etched structure, and the aim is to remove the residual PS microspheres.
And 4, step 4: putting the sample wafer in the step 3 into a quartz tube type electric furnace, performing thermal oxidation treatment by using oxygen in air in a hearth, wherein the oxidation temperature is 1050 ℃, the oxidation time is 10min, the heating rate is 10 ℃/min,
and 5: putting the sample wafer subjected to thermal oxidation in the step 4 into hydrofluoric acid (HF) buffer solution for surface SiO2Etching the film, wherein the concentration of hydrofluoric acid is 40%, and the formula of buffer solution is HF: NH4F:H2O is 3:6:10, and the etching time is 2 s.
Step 6: depositing a surface alumina film on a monocrystalline silicon wafer by utilizing an Atomic Layer Deposition (ALD) system, wherein precursors selected by the ALD system are trimethyl aluminum (TMA) and deionized water (H)2O), deposition temperature 200 ℃. First, TMA is at N2The plasma was carried into the reaction chamber with a pulse of 0.02s and chemisorbed on the substrate Si. Then, with N2Purging and carrying away residual TMA, N in the chamber2The purge time was 5 s; second, H2O is in N2The carried lower pulse enters the reaction chamber and reacts with TMA adsorbed on the substrate to generate Al2O3And by-product CH4The time was 0.02 s. Likewise, CH4And excess water from N2The purge was carried out of the reaction chamber for 5 s. Al (Al)2O3The thickness of the film is controlled by the number of reaction cycles, which is 1000 cycles, Al2O3Is 100 nm.
Claims (2)
1. A damage-resistant wide-angle antireflection composite micro-nano structure is constructed in any optical spectrum segment and is characterized by comprising a micro-structure unit array, wherein the period of the micro-structure unit array meets the condition of subwavelength, and each micro-structure unit comprises a bionic moth-eye micro-nano structure prepared on the surface of an optical material substrate and a composite protective film layer grown on the surface of the moth-eye structure in a common manner;
the bionic moth eye micro-nano structure is a round table, a cone or a cylinder, the composite protective layer is made of a high-transmittance material, and the bionic moth eye micro-nano structure is wrapped in the composite protective layer;
the diameter of the bottom end of the composite protective layer is required to meet the condition that D is D1+2dsin alpha, D is less than or equal to p, and the diameter of the top end of the structure also satisfies D1＝d2+2dsinα，D1P is less than or equal to p, and the structural height satisfies H1＝H2Wherein D is the diameter of the bottom end of the second protective layer, D1The top diameter of the second protective layer, d1The diameter of the bottom end of the bionic moth eye micro-nano structure, d2The diameter of the top end of the bionic moth eye micro-nano structure is H1Height of the bionic moth eye micro-nano structure, H2The distance between a composite protective layer at the top end of the bionic moth-eye micro-nano structure and a composite protective layer on the surface of the substrate is represented as p, the period of the moth-eye structure array is represented as d, the thickness of a film layer is represented as d, and alpha is the base angle of the moth-eye structure.
2. A preparation method of a damage-resistant wide-angle antireflection composite micro-nano structure is characterized by comprising the following steps:
step 1: preparing a graphic mask plate by a laser direct writing or nanosphere self-assembly technology;
the laser direct writing controls the whole direct writing working process through laser direct writing software, firstly, the design and the manufacture of a direct writing graph are carried out, after the laser direct writing control software reads a design drawing, a laser beam scanning path is automatically generated according to the information of the design drawing and the set filling interval, a moving platform finishes the movement in a two-dimensional plane, and the height adjustment is finished by combining the vertical movement; fixing a substrate on an objective table, controlling the objective table to move by a moving platform, monitoring by a visual imaging system consisting of a CCD camera and a lens, accurately positioning the center of a laser beam to the substrate, and focusing the laser beam by moving an axis up and down to obtain a converged laser beam; after positioning and focusing are finished, controlling the laser beam to perform scanning writing on the substrate through a double-vibrating-mirror scanning system according to a laser beam scanning path generated by control software, and finally detecting the forming quality of a laser beam writing graph through a visual imaging system;
the preparation process of the nanosphere self-assembly technology comprises the steps of taking an evaporation pan with a proper size, injecting deionized water with a proper height into the evaporation pan, simultaneously placing and adjusting a substrate with hydrophilicity, placing the substrate on a quartz plate with a certain thickness, and obliquely placing a glass plate which is also subjected to hydrophilicity treatment; after the liquid level is static, taking a trace amount of nanosphere mixed liquid, and slowly dripping the nanosphere mixed liquid on a glass inclined plate to ensure that liquid drops slide into water under the action of gravity; when more nanospheres slide into the liquid surface, the obvious motion track of the microsphere polymer with small area in a heart-shaped surrounding manner can be observed, and the dripping of the solution is stopped until the monomolecular film layer of the nanospheres is fully paved on the whole evaporating dish; at the moment, slowly adding a surfactant dropwise along the side wall of the vessel at a position far away from the substrate to compact the monomolecular layer and ensure that the nanospheres form a hexagonal close-packed structure;
step 2: transferring the mask plate pattern to a substrate material by a wet or dry etching technology to prepare a bionic moth eye structure; the wet etching process comprises the steps of firstly diffusing a reactant to the surface of an etched material, then reacting the reactant with the etched material, and diffusing a product after reaction to a solution after leaving the etching surface and discharging the product along with the solution; dry etching is carried out, wherein the duty ratio of a structure to be etched in a duty ratio structure is adjusted; selecting proper etching gas, and adjusting the gas proportion, the upper and lower radio frequency power, the pressure intensity and the etching temperature to be unchanged, wherein the longer the etching time is, the larger the etching depth is; after etching is finished, the redundant mask material can be placed in acetone for soaking and ultrasonic treatment, then alcohol and deionized water are sequentially used for ultrasonic cleaning, and high-purity nitrogen or argon is blown dry and can be removed;
and step 3: putting the sample wafer in the step 2 into a quartz tube type electric furnace, and performing thermal oxidation treatment by using oxygen in air in a hearth to eliminate lattice damage and tiny gaps generated when a moth eye structure grows; thermal oxidation to form SiO2Etching the sample wafer of the film by hydrofluoric acid to remove the redundant oxide layer film on the surface, wherein the aim of etching by hydrofluoric acid is to ensure that the side wall of the whole structure is smooth and has no damage;
and 4, step 4: uniformly growing a hard film layer on the surface of the prepared bionic moth eye structure by utilizing an atomic layer deposition technology to finish the preparation of the composite protective film layer; after the temperature of the atomic layer deposition equipment is raised, putting the sample wafer into a reaction chamber; in the process of depositing a composite protective layer by adopting an atomic layer deposition technology, the deposition of a protective film layer is completed by utilizing the reaction between two precursors, each cycle mainly comprises the steps that the precursor 1 enters a reaction chamber by steam pulse, the chemical adsorption reaction is carried out on the surface of an exposed substrate or film, the cleaning gas takes the steam and reaction byproducts of the redundant precursor 1 which are not adsorbed by the surface out of the reaction chamber, the precursor 2 enters the reaction chamber by steam pulse and continues to carry out surface chemical reaction with the adsorbed surface of the precursor 1, and the cleaning gas takes the steam and reaction byproducts of the redundant precursor 2 out of the reaction chamber, so that one cycle is completed; the thickness of the film is controlled by the number of reaction cycles.
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