CN115535959A - Wet etching auxiliary femtosecond laser processing method for monocrystalline silicon microstructure array - Google Patents
Wet etching auxiliary femtosecond laser processing method for monocrystalline silicon microstructure array Download PDFInfo
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- CN115535959A CN115535959A CN202211473482.3A CN202211473482A CN115535959A CN 115535959 A CN115535959 A CN 115535959A CN 202211473482 A CN202211473482 A CN 202211473482A CN 115535959 A CN115535959 A CN 115535959A
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00015—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems
- B81C1/00214—Processes for the simultaneaous manufacturing of a network or an array of similar microstructural devices
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- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K26/00—Working by laser beam, e.g. welding, cutting or boring
- B23K26/36—Removing material
- B23K26/362—Laser etching
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00436—Shaping materials, i.e. techniques for structuring the substrate or the layers on the substrate
- B81C1/00444—Surface micromachining, i.e. structuring layers on the substrate
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- B81C1/00436—Shaping materials, i.e. techniques for structuring the substrate or the layers on the substrate
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Abstract
The invention belongs to the field of processing of a microstructure array, and particularly provides a method for processing a monocrystalline silicon microstructure array by using a wet etching auxiliary femtosecond laser, wherein after the crystal of the monocrystalline silicon is determined, the femtosecond laser is adopted to process along the direction parallel to or/and perpendicular to the crystal direction, and the microstructure array is formed on the surface of the monocrystalline silicon; and carrying out wet etching on the processed monocrystalline silicon in anisotropic etching liquid. The femtosecond laser is used for directly processing along the crystal direction of the monocrystalline silicon, and then wet etching is carried out on the monocrystalline silicon, so that a mask is not needed, and the processing efficiency is greatly improved. Meanwhile, the method can obtain inverted pyramid arrays, V-shaped groove arrays and regular pyramid array structures with complete profiles, good structural consistency and high surface quality, can effectively improve the optical performance of the material, and has important application in micro solar cells and micro optical systems.
Description
Technical Field
The invention belongs to the field of processing of microstructure arrays, and particularly relates to a method for processing a microstructure array along a monocrystalline silicon crystal direction by using a femtosecond laser assisted with wet etching.
Background
The monocrystalline silicon is a non-metallic crystal material, and has the advantages of good heat conductivity, excellent mechanical strength, high refractive index and infrared transmittance, and excellent physical properties. Different types of microstructures such as inverted pyramid structures, micro-nano structures, groove array structures, three-dimensional suspension structures and the like are processed on the surface of a monocrystalline silicon material, so that the monocrystalline silicon material has different properties and functions, and the microstructure is widely applied to micro solar cells, micro optical systems and other commercialized products.
At present, the processing methods of single crystal silicon materials are various, the mechanical processing can realize the large-size and high-precision preparation of the materials, but the processing efficiency is low, and the processing of an array structure with a complex section outline is difficult to complete; the wet etching process is simple and high in efficiency, but most of the wet etching process needs a mask plate in the processing process, and the working procedure is complex.
The femtosecond laser wet etching technology integrates the advantages of femtosecond laser direct writing micro machining and wet etching, such as simple process, high precision and the like, and is applied to the machining of micropores with high aspect ratio, microlens arrays and arrays with complex structures. When the femtosecond laser is combined with the wet etching technology to process materials, firstly, the femtosecond laser is adopted to ablate the materials to change the structure (lattice change, surface modification, micropore generation and the like) of the materials, a mask is not required to be prepared, and then the wet etching technology is adopted to remove the materials in a laser processing area (modified area), so that a microstructure with a certain shape and size is formed. The wet etching technology is to use an etchant which chemically reacts with a material to be processed to enable the material to generate a soluble substance in the processing process, so that the material is removed to obtain a corresponding microstructure.
In the wet etching process after the femtosecond laser processing of the monocrystalline silicon, the processes are mainly divided into isotropic etching and anisotropic etching according to different corrosive liquids. By virtue of the advantages of greenness, no toxicity, simple preparation and the like, the KOH solution is often used for anisotropic wet etching of monocrystalline silicon. Processing a micropore structure on the surface of monocrystalline silicon by using femtosecond laser, and performing wet etching on the micropore structure to obtain an etched pit with an inverted pyramid profile, wherein the side wall of the etched pit is in a <111> crystal orientation, and the included angle between the etched pit and the horizontal direction (the <100> crystal orientation) is 54.74 degrees; the structures such as parallel grooves, crossed grooves and the like are processed on the surface of the monocrystalline silicon by femtosecond laser, and then wet etching is carried out on the structures, so that the structures such as V-shaped grooves, regular pyramids and the like can be obtained.
Single crystal silicon is a crystalline material in which the arrangement direction (i.e., crystal orientation) of crystal column groups is fixed. During the KOH solution wet etch, material is removed along the crystal orientation. In the existing femtosecond laser wet etching processing technology, the influence of the monocrystalline silicon crystal orientation on the etching result is not considered yet. If micro-holes, groove arrays and the like are processed on the surface of the monocrystalline silicon in any direction (non-parallel or vertical to a certain crystal direction) by using femtosecond laser, and then wet etching is carried out on the monocrystalline silicon, due to the fact that etching rates of different crystal directions are different, the profiles of the obtained inverted pyramid pit arrays, V-shaped groove arrays, regular pyramid arrays and the like are incomplete and asymmetrical, the arrangement among structures is not regular, and the application of the microstructured monocrystalline silicon in the fields of micro-solar cells, micro-optical systems and the like is limited.
Disclosure of Invention
In order to solve the technical problems in the prior art, the invention provides a processing method of a monocrystalline silicon surface microstructure array.
In order to achieve the purpose, the invention is realized by the following technical scheme:
in a first aspect, an embodiment of the present invention provides a method for processing a single crystal silicon microstructure array by using a femtosecond laser assisted by wet etching, including:
after the crystal of the single crystal silicon is determined, processing the single crystal silicon along the direction parallel to or/and vertical to the crystal direction by using femtosecond laser to form a microstructure array on the surface of the single crystal silicon;
and carrying out wet etching on the processed monocrystalline silicon in anisotropic etching liquid.
As a further technical scheme, the microstructure array is a micropore array, a square lattice array or a groove array;
as a further technical scheme, the diameter of the micropores is in the micrometer scale.
As a further technical scheme, the distance between the micropores in the X and Y directions is in the micron order and is equal to the diameter of the micropores.
As a further technical scheme, the mass fraction of the anisotropic etching liquid is 20-40%.
As a further technical scheme, the etching temperature is 20-80 ℃.
As a further technical scheme, the etching time is 1 min-12 h.
As a further technical solution, single crystal silicon is processed in deionized water using a femtosecond laser.
As a further technical scheme, the specific method for processing the monocrystalline silicon by using the femtosecond laser in the deionized water comprises the following steps: fixing monocrystalline silicon at the bottom of a water tank, and placing the water tank above a sample table; deionized water is filled in the water tank, the front end of the objective lens is positioned below the deionized water, and the femtosecond laser acts on the surface of the single crystal silicon through the deionized water.
As a further technical scheme, the monocrystalline silicon is processed by femtosecond laser in air water.
As a further technical solution, a specific method of processing in air by using a femtosecond laser is as follows: the femtosecond laser directly focuses on the surface of the monocrystalline silicon after passing through the objective lens, the monocrystalline silicon is placed above the sample stage, and the nano motion platform controls the sample stage to move in the X and Y directions.
The beneficial effects of the above-mentioned embodiment of the present invention are as follows:
1. the invention provides a novel processing method of a microstructure array, which utilizes femtosecond laser to directly process along the crystal direction of monocrystalline silicon and then carry out wet etching on the monocrystalline silicon, does not need a mask and greatly improves the processing efficiency. Meanwhile, the method can obtain inverted pyramid arrays, V-shaped groove arrays and regular pyramid array structures with complete outlines, good structural consistency and high surface quality, can effectively improve the optical performance of materials, and has important application in micro solar cells and micro optical systems.
2. The invention prepares a series of micro-structure arrays on the monocrystalline silicon surface, can further improve the surface characteristics (hydrophilic and hydrophobic properties and the like) of the material, thereby leading the monocrystalline silicon solar cell to have self-cleaning function or improving the preparation efficiency of textured monocrystalline silicon, and has important application in the optical field.
3. The invention adopts femtosecond laser to directly write the monocrystalline silicon and then carry out wet etching, has simple process and can quickly prepare the microstructure array with complete outline and good structural consistency. The method can be used for preparing the monocrystalline silicon die, and further improves the processing efficiency in the die pressing process.
4. According to the invention, the monocrystalline silicon is processed by using the femtosecond laser in the deionized water and then is subjected to wet etching, so that the silicon dioxide content of a laser processing area can be further reduced, and the etching rate in the wet etching process is improved.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
FIG. 1 is a schematic diagram of a wet etching process after a femtosecond laser processes a micro-pore array structure along a single crystal silicon crystal direction;
FIG. 2 is a schematic diagram of an array of etched pits in an inverted pyramid profile;
FIG. 3 is a schematic view of the primary and secondary alignment surfaces of single crystal silicon;
FIG. 4 is a schematic diagram of a wet etching process after a femtosecond laser processes a groove array structure along a monocrystalline silicon crystal direction;
FIG. 5 is a schematic view of a V-groove array;
FIG. 6 is a schematic diagram of wet etching after femtosecond laser processes a lattice array structure along the crystal direction of single crystal silicon;
FIG. 7 is a schematic view of a positive pyramid array;
FIG. 8 is a schematic diagram of a femtosecond laser processing monocrystalline silicon in a deionized water environment;
in the figure: 1 femtosecond laser, 2 objective lenses, 3 monocrystalline silicon, 4 sample stages, 5 ablation holes, 6 non-ablation areas, 7 clamping frames, 8 water tanks, 9 KOH solution and 10 deionized water.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention. As used herein, the singular forms "a", "an", and/or "the" are intended to include the plural forms as well, unless the invention expressly state otherwise, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof;
it should be noted that, in this embodiment, besides KOH solution, ethylenediamine pyrocatechol (EDP) and tetramethylammonium hydroxide (TMAH) can also be used as etching solution for anisotropic wet etching of single crystal silicon. The three etching solutions can be used for preparing an inverted pyramid structure on the surface of (100) crystal face monocrystalline silicon, wherein a method of wet etching by using ethylenediamine pyrocatechol (EDP) and tetramethylammonium hydroxide (TMAH) after the monocrystalline silicon is processed by femtosecond laser along the crystal direction is also in the protection scope of the patent. This example is described by taking a KOH solution as an example only.
Further, in the above-mentioned case,
as described in the background art, in the existing femtosecond laser wet etching processing technology, the influence of the crystal orientation of the monocrystalline silicon on the etching result has not been considered. If micro-holes, groove arrays and the like are processed on the surface of the monocrystalline silicon in any direction (non-parallel or vertical to a certain crystal direction) by femtosecond laser, and then wet etching is carried out on the monocrystalline silicon, because the etching rates of different crystal directions are inconsistent, the profiles of the obtained inverted pyramid pit arrays, V-shaped groove arrays, positive pyramid arrays and the like are incomplete and asymmetric, and the structures are arranged irregularly, so that the application of the microstructured monocrystalline silicon in the fields of micro solar cells, micro optical systems and the like can be limited.
Example 1
In a typical embodiment of the present invention, after a certain crystal of the single crystal silicon 3 is determined, the processing method of the single crystal silicon surface microstructure array provided by the present invention adopts the femtosecond laser 1 to process along the direction parallel or/and perpendicular to the crystal direction, and the structured single crystal silicon 3 is wet-etched in the KOH solution 9, so as to obtain the microstructure array with complete contour and orderly arrangement, which comprises the following specific steps:
firstly, a femtosecond laser micro-machining system is utilized to machine monocrystalline silicon, femtosecond laser 1 passes through an objective lens 2 and then is focused on the surface of the monocrystalline silicon 3, the monocrystalline silicon 3 is placed above a sample table 4, and a nano-motion platform controls the sample table 4 to move in the X direction and the Y direction. The femtosecond laser 1 is adjusted to a punching mode, and after the crystal orientation of the single crystal silicon 3 is determined, a series of micro holes are processed in a direction parallel to the crystal orientation, and then the series of micro holes are processed continuously in a direction perpendicular to the crystal orientation, thereby obtaining a micro hole array, as shown in fig. 1. Next, the processed single crystal silicon 3 is clamped by a polytetrafluoroethylene clamping frame 7, and is placed in a KOH solution 9 for etching, so as to obtain an etched pit array with an inverted pyramid outline, as shown in fig. 2, the ablation holes 5 and the non-ablation regions 6 in fig. 2 form a pit array together.
The crystal orientation refers to the arrangement direction of the crystal group, and in order to determine the crystal orientation of the wafer, the silicon wafer generally has a plurality of positioning surfaces, as shown in fig. 3, the largest plane is called as a main positioning surface and is used for determining the crystal orientation of the crystal-related device; the other smaller planes are called sub-planes and are used to identify the crystal orientation and conductivity type of the material.
The silicon material used in this example was P-type single-side polished (100) plane single crystal silicon of CZ growth mode, with a resistivity of 1-10 Ω · m and a thickness of 500 ± 10 μm. Wherein the direction of the main positioning plane of the (100) crystal plane single crystal silicon is defined as<110>And (4) crystal orientation. In a direction parallel to the main locating plane during machining (<110>Crystal orientation) the monocrystalline silicon is cut (using a diamond cutting head) to 10 x 0.5 mm 3 The side edges of the single crystal silicon small blocks are parallel or vertical<110>And (4) crystal orientation. Thus, the femtosecond laser processing described in this embodiment will be along the crystal direction<110>And (4) processing the crystal orientation.
In the embodiment, the pulse width of a laser in the femtosecond laser micro-machining system is 35 fs, the wavelength is 800 nm, and the maximum repetition frequency is 1 KHz. The processed monocrystalline silicon 3 is placed on the processing system, and a micropore array structure is processed on the surface of the monocrystalline silicon 3 by using the femtosecond laser 1. The diameter of the micropores is micrometer magnitude, and the distance between the micropores in the X direction and the Y direction is also micrometer magnitude and the micropores are consistent.
The KOH solution 9 in this embodiment is used for anisotropic wet etching of single crystal silicon, and has a greater selectivity to the crystal orientation of single crystal silicon 3, and the etching rate ratio among the <110> crystal orientation, <100> crystal orientation, and <111> crystal orientation is 200. Therefore, in the etching process, the etching rate of the <100> crystal direction is high, and the material removal rate is high; the etching rate of the <111> crystal orientation is slow, and the material removal rate is slow. Meanwhile, the angle between the (100) plane and the (111) plane is 54.74 °. After a certain etching time, the <100> crystal orientation material is etched and removed, and an etched pit with an inverted pyramid profile having a (111) crystal plane on the sidewall is obtained, and the included angle between the sidewall of the inverted pyramid structure and the upper surface is 54.74 °, as shown in fig. 2.
Furthermore, the mass fraction of the KOH solution 9 in the embodiment is 20-40%, the etching temperature is 20-80 ℃, and the etching time is 1 min-12 h.
Example 2
In the present embodiment, a femtosecond laser is used to machine a groove array structure on the surface of the single crystal silicon 3 along a direction parallel to the crystal direction, as shown in fig. 4, the width and the pitch of the grooves are both in the micrometer range. The processed monocrystalline silicon 3 is put into a KOH solution 9 for wet etching, so as to obtain a V-shaped groove array structure, as shown in fig. 5. The preparation method and the equipment of the V-shaped groove array structure are the same as those of embodiment 1, and are not repeated herein.
Example 3
In the present embodiment, a femtosecond laser is used to process a lattice array structure on the surface of the single crystal silicon 3 along the directions parallel and perpendicular to the crystal direction, as shown in fig. 6, the width and the spacing of the trenches are both in the micrometer scale, and the spacing of the trenches in the X and Y directions is kept consistent. The processed single crystal silicon 3 is put into a KOH solution 9 for wet etching, so that an array structure with a positive pyramid profile can be obtained, as shown in fig. 7. The method and apparatus for preparing the positive pyramid profile array structure are the same as those in embodiment 1, and are not described herein again.
Example 4
In this embodiment, a method of processing single crystal silicon by femtosecond laser in deionized water and then performing wet etching is provided, as shown in fig. 8, the single crystal silicon is fixed at the bottom of a water tank 8, and the water tank 8 is placed above a sample stage 4. Deionized water 10 is filled in the water tank 8, the front end of the objective lens 2 is positioned below the deionized water, and the femtosecond laser 1 acts on the surface of the monocrystalline silicon 3 through the deionized water. Compared with the processing in the air, the content of oxygen element in the deionized water 10 is less, and the generated oxide (silicon dioxide) is easily carried away by the deionized water, so that the silicon dioxide content of the processing area on the surface of the monocrystalline silicon 3 is lower. Because the reaction rate of silicon dioxide with KOH solution is relatively slow (about 1/180 of the reaction rate of silicon with KOH solution), single crystal silicon 3 processed in deionized water 10 has a faster etch rate due to the lower silicon dioxide content. The method is identical to example 1 except that the femtosecond laser processing environment is different from the method (the method processing environment is deionized water, and the method processing method is air).
Unless otherwise specified, references to "processing along a crystal direction" in this patent refer to processing along a <110> crystal direction parallel or perpendicular to single crystal silicon.
Unless otherwise specified, all references to "femtosecond laser processing" in this patent refer to processing in an air environment. The single crystal silicon in examples 1, 2 and 3 was femtosecond laser processed in air and the single crystal silicon in example 4 was femtosecond laser processed in deionized water, but the structures of examples 1 to 3 could be processed by the method of example 4.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. 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 (10)
1. A wet etching auxiliary femtosecond laser processing method of a monocrystalline silicon microstructure array is characterized by comprising the following steps:
after the crystal of the single crystal silicon is determined, processing the single crystal silicon along the direction parallel to or/and vertical to the crystal direction by using femtosecond laser to form a microstructure array on the surface of the single crystal silicon;
and carrying out wet etching on the processed monocrystalline silicon in anisotropic etching liquid.
2. The method for processing a single-crystal silicon microstructure array by wet etching with the assistance of femtosecond laser according to claim 1, wherein the single-crystal silicon is processed by the femtosecond laser in air or deionized water.
3. The method for processing the single crystal silicon microstructure array by wet etching assisted femtosecond laser according to claim 2, wherein the specific method for processing in air by the femtosecond laser is as follows: the femtosecond laser directly focuses on the surface of the monocrystalline silicon after passing through the objective lens, the monocrystalline silicon is placed above the sample stage, and the nano motion platform controls the sample stage to move in the X and Y directions.
4. The method for processing a monocrystalline silicon microstructure array by wet etching assisted femtosecond laser according to claim 2, wherein the specific method for processing monocrystalline silicon by femtosecond laser in deionized water is as follows: fixing monocrystalline silicon at the bottom of a water tank, and placing the water tank above a sample table; deionized water is filled in the water tank, the front end of the objective lens is positioned below the deionized water, and the femtosecond laser acts on the surface of the single crystal silicon through the deionized water.
5. The wet etching assisted femtosecond laser processing method of the single crystal silicon microstructure array as claimed in claim 1, wherein the mass fraction of the anisotropic etching liquid is 20% -40%.
6. The wet etching assisted femtosecond laser processing method for the single crystal silicon microstructure array as claimed in claim 5, wherein the etching temperature is 20 ℃ -80 ℃.
7. The wet etching assisted femtosecond laser processing method of the single crystal silicon microstructure array as claimed in claim 5, wherein the etching time is 1 min-12 h.
8. The method for processing the monocrystalline silicon microstructure array by using the femtosecond laser assisted by wet etching as recited in claim 1, wherein the microstructure array is a micro-hole array, a square lattice array or a groove array.
9. The method of claim 8, wherein the micro-holes have a diameter of the order of micrometers.
10. The method of claim 9, wherein the micro holes are spaced in the X and Y directions at a distance on the order of microns equal to the diameter of the micro holes.
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