CN109023501B - Preparation method of nano porous silicon single concave lens - Google Patents
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Abstract
The invention discloses a preparation method of a nano porous silicon single concave lens, which is characterized in that a thin platinum sheet which is conventionally used as an electrode is made into a hollow sphere, a spherical crown cut from the hollow sphere is made into a cathode, the convex surface of the spherical crown-shaped thin platinum sheet is opposite to a silicon wafer, a circular flat thin platinum sheet is used as an anode, a silicon wafer is placed between the spherical crown-shaped thin platinum sheet and the flat thin platinum sheet, and the silicon wafer divides corrosive liquid into two independent parts; firstly, a constant current source is adopted to carry out electric polishing on a silicon wafer, so that a concave spherical surface is formed on one surface of the silicon wafer close to a spherical crown-shaped thin platinum sheet electrode, and a plane is maintained on one surface close to a flat thin platinum sheet electrode; and then replacing the spherical crown-shaped thin platinum sheet electrode with a circular flat plate-type thin platinum sheet electrode, and carrying out electrochemical corrosion on the silicon wafer to form the nano porous silicon single concave lens. The method can obtain the nano porous silicon single concave lens, can be widely applied to micro-optical electromechanical systems, and makes a great contribution to the field of micro-optical electromechanical systems.
Description
Technical Field
The invention relates to the field of semiconductor technology and optical engineering, in particular to a preparation method of a nano porous silicon single concave lens.
Background
In 1956, Uhlir found the existence of porous silicon when the silicon wafer was subjected to electrochemical polishing treatment in HF solution; in 1990, Canham discovered that porous silicon emits visible light at room temperature, which opens up a new era for the research of porous silicon, namely, the research stage of luminescent porous silicon at room temperature; the luminescence of porous silicon at room temperature shows the wide application prospect of silicon in the aspects of optoelectronics, optical devices, display technology and the like. Particularly, in 1996, the first realization of a silicon-based optoelectronic integrated prototype device by Hirschman is a milestone for the application and research of porous silicon.
The porous silicon film is a spongy porous material with a large specific surface area. The material has the advantages of low cost, good biocompatibility and complete compatibility with the existing integrated circuit process. Although porous silicon has attracted much attention as a high-quality sensor material since the 90 s in the 20 th century, the use of porous silicon materials for optical devices has been rare and is especially rare in the field of optical, mechanical and electrical integration research.
Micro-Electro-Mechanical systems (MEMS) are also called Micro-electromechanical systems, microsystems, micromachines, and the like. The micro-sensor micro-actuator is a high-tech device which integrates a micro-sensor, a micro-actuator, a micro-mechanical structure, a micro-power supply, a micro-energy source, a signal processing and control circuit, a high-performance electronic integrated device, an interface and communication into a whole, and has the size of several millimeters or less.
In recent years, with the rapid development of microelectronic technology, the sizes of electronic devices, MEMS accelerometers, MEMS microphones, micro motors, micro pumps, micro vibrators, MEMS optical sensors, MEMS pressure sensors, MEMS gyroscopes, MEMS humidity sensors, and MEMS gas sensors have become smaller and smaller. The micro-optical-mechanical-electrical system integration research is rapidly developing, silicon-based micro-optical, mechanical, electrical and integration technologies are highly regarded, micro-optical elements such as lenses, prisms and reflectors are important components of the micro-optical-mechanical-electrical system, and can convert, transmit and process micro-optical paths to achieve the purposes of light emission, light collection, light polarization, light interference and light scattering, but the research on the micro-optical elements such as micro-lenses, prisms and reflectors prepared by using porous silicon materials is still few.
There is a literature on a method for preparing an oxidized porous silicon optical waveguide prism by using polymethyl methacrylate (PMMA) to mask silicon and using a selective electrochemical etching process, so as to respectively prepare a converging lens and a diverging lens based on porous silicon. Such a waveguide prism can significantly converge and diverge the polarized light beam traveling in the waveguide. However, the method has complex process and low controllability, and is difficult to realize micro-opto-electro-mechanical system integration.
Disclosure of Invention
The invention aims to provide a preparation method of a nano porous silicon single concave lens in order to realize the integration of silicon-based micro-optical, mechanical and electrical systems.
In order to achieve the purpose, the invention adopts the technical scheme that: a preparation method of a nanometer porous silicon single concave lens is characterized in that a thin platinum sheet which is conventionally used as an electrode is made into a hollow sphere, a spherical crown cut from the hollow sphere is made into a cathode, the convex surface of the spherical crown faces a silicon wafer, a circular flat thin platinum sheet is used as an anode, a silicon wafer is placed between the cathode of the spherical crown thin platinum sheet and the anode of the flat thin platinum sheet, the central axis of the silicon wafer, the central axis of the anode of the flat thin platinum sheet, the center of the circle of the spherical crown thin platinum sheet coincide with the central axis of the spherical crown thin platinum sheet, the distances from the silicon wafer to the anode and the cathode are equal, and the silicon wafer divides corrosive liquid into two independent parts; firstly, a constant current source is adopted to carry out electric polishing on a silicon wafer, so that a concave spherical surface is formed on one surface of the silicon wafer close to a cathode of the spherical crown thin platinum sheet, and a plane is kept on one surface of the silicon wafer close to an anode of the flat thin platinum sheet; and then replacing the spherical crown-shaped thin platinum sheet with a circular flat plate-type thin platinum sheet, and carrying out electrochemical corrosion on the silicon wafer to form the porous silicon single concave lens.
The principle of the invention is as follows: the preparation of the nanometer porous silicon single concave lens is divided into 2 processes, firstly, the silicon wafer is electropolished by using a large constant current corrosion current which is larger than the conventional electropolishing current of the silicon wafer, on one hand, the surface of the silicon wafer is electropolished under the condition of normal large constant current corrosion current density, as the large constant corrosion current is used, one surface is a spherical crown-shaped thin platinum sheet cathode, and the other surface is a round flat thin platinum sheet anode, the central axis of the two electrodes is taken as the center, the farther away from the central axis, the smaller the corrosion current density is, the slower the polishing speed of the silicon wafer is, so that the central axis of the silicon wafer is taken as the center, the farther away from the central axis, the shallower the polishing is, and the concave spherical surface is formed on the silicon wafer and the surface facing the spherical crown thin platinum sheet electrode, and; after the electropolishing is finished, carrying out electrochemical corrosion on the silicon wafer by using a small constant corrosion current which is smaller than the conventional electropolishing current of the silicon wafer to form a porous silicon film until the whole silicon wafer is completely formed into a single concave lens formed by porous silicon materials.
The curvature radius of the outer concave surface of the concave lens can be changed by changing the radius R of the hollow sphere of the thin platinum sheet, the height H of the spherical cap, the distance L between the plane of the spherical cap cathode and the flat plate anode and the electropolishing condition.
Preferably, the spherical cap height H = 0.01-0.5R of the spherical cap-shaped thin platinum sheet used as the cathode.
Preferably, the distance L = 0.02-10R between the plane of the bottom of the spherical-crown-shaped thin platinum sheet cathode and the flat-plate thin platinum sheet anode.
The invention has the beneficial effects that: the method can obtain the nano porous silicon single concave lens, can be widely applied to micro-optical electromechanical systems, and makes a great contribution to the field of micro-optical electromechanical systems.
Drawings
FIG. 1 is a schematic view of an electrolytic etching cell according to the present invention
The device comprises a corrosion tank 1, a silicon wafer 2, a spherical crown-shaped thin platinum sheet 3, a flat thin platinum sheet 4, a sealing support 5 and a sealing support.
Detailed Description
The present invention will be further described with reference to the following examples. The present invention is not limited to the above-described embodiments, and any modifications and variations may be made by those skilled in the art without departing from the scope of the present invention. Therefore, the following embodiments may be modified or changed in a similar manner without departing from the scope of the invention.
Example one
The preparation method of the nano porous silicon single concave lens specifically comprises the following steps:
1. selecting the silicon wafer type as P100A single-side polished silicon wafer 2 having a resistivity of 0.01 Ω · cm and a thickness of 500 μm, a thin platinum sheet (thickness of 200 μm) ball (radius of 2 cm) 3 having a length of the bottom face = the diameter of the silicon wafer as a cathode, and a circular flat thin platinum sheet 4 (thickness of 200 μm) as an anode; ensuring that the center axes of the silicon wafer 2, the flat thin platinum sheet 4 and the spherical thin platinum sheet 3 coincide with the center axis of the spherical thin platinum sheet 3, completely immersing the silicon wafer 2, the flat thin platinum sheet 4 and the spherical thin platinum sheet 3 in electrolytic corrosion liquid for electrochemical corrosion, wherein the polished surface of the silicon wafer 2 faces the convex surface of the spherical thin platinum sheet 3, and the electrolytic corrosion liquid is hydrofluoric acid: the absolute ethyl alcohol and the deionized water are prepared according to the volume ratio of 1:1: 2;
2. and (3) connecting a circuit: the method is characterized in that a corrosion liquid is placed in a corrosion tank 1, a silicon wafer 2 is placed in the middle of the corrosion tank 1 through a sealing support 5, the corrosion liquid in the corrosion tank 1 is divided into two independent parts by the silicon wafer 2, spherical crown-shaped thin platinum sheets 3 are symmetrically arranged at two ends of the corrosion tank 1 and serve as cathodes and flat thin platinum sheets 4 as anodes, the convex surfaces of the spherical crown-shaped thin platinum sheets 3 face the silicon wafer 2, the distance between the center of a circular surface projected at the bottom of each spherical crown-shaped thin platinum sheet 3 and the center of each flat thin platinum sheet 4 is 0.25cm, and the silicon wafer 2, the flat thin platinum sheets 4 and the spherical crown-shaped thin platinum sheets 3 (the corrosion diameter of the silicon wafer 2 is equal to the diameter of the circular surface projected at the bottom of each spherical crown-shaped thin platinum sheet 3 and is 2 cm) are soaked in the corrosion liquid. A constant current source is arranged outside the corrosion tank 1 and is generated by a TekVisaAFG3101 arbitrary waveform generator, the positive pole and the negative pole of the constant current source are respectively connected with the two electrodes of the round flat thin platinum sheet 4 and the spherical crown thin platinum sheet 3 through leads, and when the device works, the positive pole and the negative pole of the current source form a current loop through a corrosion liquid;
3. forming a concave surface on one surface and a planar silicon body on the other surface on the polished surface of the silicon wafer: the average polishing current of the constant current source is 120mA/cm2The electropolishing time is 20Min, so that the silicon wafer is polished into a concave surface on one surface, and the silicon body which is not corroded on the other surface and keeps a plane is not corroded;
4. corroding the porous silicon on the surface of the silicon wafer for 30 minutes by using a 2% sodium hydroxide solution (prepared by sodium hydroxide and deionized water in a mass ratio of 1: 49) to form a single-side concave lens silicon body with one side polished into a concave surface and the other side as a plane;
5. forming a porous silicon single-sided concave lens: changing the spherical thin platinum sheet 3 into a flat round thin platinum sheet (with the thickness of 200 μm), changing the corrosion current, corroding the silicon wafer to form a porous silicon film, and performing two tests, wherein the variation in the two tests is the corrosion current density which is 50mA/cm2And 40mA/cm2Forming porous silicon on the single-sided concave lens silicon body until the etching is finished to obtain a single-sided concave lens made of a porous silicon film material;
6. for convenience in studying the problem, we chose two sets of experiments whose experimental parameters and corresponding data are as follows:
| weaving machine Number (C) | Polishing Current (mA- cm2） | Polishing time (min) | Corrosion current (mA- cm2） | Time of etching (min) | Porous Degree of rotation | Center and edge of porous silicon concave lens Thickness (μm) |
| ⑴ | 120 | 20 | 50 | 150 | 60% | ~330、425 |
| ⑵ | 120 | 20 | 40 | 187 | 55% | ~325、420 |
7. According to the relevant documents and the combination of the experimental conditions, the porosity of the single-sided concave lens formed by the two formed porous silicon films is about 60% and 55%, the thickness of the center and the edge of the single-sided concave lens is about 330 μm and 425 μm, and the thickness of the edge of the single-sided concave lens is about 325 μm and 420 μm;
8. after the preparation of the nano porous silicon single-sided concave lens is finished, quickly putting the porous silicon single-sided concave lens sample into high-purity deionized water for cleaning for 10 minutes to replace electrochemical corrosion liquid (hydrofluoric acid and water) and other reaction products in the porous silicon single-sided concave lens; then, soaking the porous silicon single-sided concave lens in a mixed solution of hydrogen peroxide and deionized water (the volume ratio is 2:100) for post-treatment for 6 hours;
9. after the post-treatment is finished, washing with deionized water, and finally drying in the air;
10. and (5) obtaining a finished product after the product is qualified through inspection.
Example two
The preparation method of the nano porous silicon single concave lens specifically comprises the following steps:
1. selecting the silicon wafer type as P100A single-side polished silicon wafer 2 having a resistivity of 0.01 Ω · cm and a thickness of 500 μm, a thin platinum sheet (thickness of 200 μm) ball (radius of 2 cm) 3 having a length of the bottom face = the diameter of the silicon wafer as a cathode, and a circular flat thin platinum sheet 4 (thickness of 200 μm) as an anode; ensuring that the center axes of the silicon wafer 2, the flat thin platinum sheet 4 and the spherical thin platinum sheet 3 coincide with the center axis of the spherical thin platinum sheet 3, completely immersing the silicon wafer 2, the flat thin platinum sheet 4 and the spherical thin platinum sheet 3 in electrolytic corrosion liquid for electrochemical corrosion, wherein the polished surface of the silicon wafer 2 faces the convex surface of the spherical thin platinum sheet 3, and the electrolytic corrosion liquid is hydrofluoric acid: the absolute ethyl alcohol and the deionized water are prepared according to the volume ratio of 1:1: 2;
2. and (3) connecting a circuit: the method is characterized in that a corrosion solution is placed in a corrosion tank 1, a silicon wafer 2 is placed in the middle of the corrosion tank 1 through a sealing support 5, the corrosion solution in the corrosion tank 1 is divided into two independent parts by the silicon wafer 2, spherical crown-shaped thin platinum sheets 3 are symmetrically arranged at two ends of the corrosion tank 1 and serve as cathodes and a flat thin platinum sheet 4 as anodes, the convex surfaces of the spherical crown-shaped thin platinum sheets 3 face the silicon wafer 2, the distance between the center of a circular surface projected at the bottom of each spherical crown-shaped thin platinum sheet 3 and the center of the flat thin platinum sheet 4 is 0.25cm, and the silicon wafer 2, the flat thin platinum sheet 4 and the spherical crown-shaped thin platinum sheet 3 (the corrosion diameter of the silicon wafer 2 is equal to the diameter of the circular surface projected at the bottom of the spherical crown-shaped thin platinum sheet 3 and both are 2 cm) are soaked in the corrosion solution. A constant current source is arranged outside the corrosion tank 1 and is generated by a TekVisaAFG3101 arbitrary waveform generator, the positive pole and the negative pole of the constant current source are respectively connected with the two electrodes of the round flat thin platinum sheet 4 and the spherical crown thin platinum sheet 3 through leads, and when the device works, the positive pole and the negative pole of the current source form a current loop through a corrosion liquid;
3. forming a concave surface on one surface and a planar silicon body on the other surface on the polished surface of the silicon wafer: the average polishing current of the constant current source is 100mA/cm2The electropolishing time is 25Min, so that the silicon wafer is polished into a concave surface on one surface, and the silicon body which is not corroded on the other surface and keeps a plane is not corroded;
4. corroding the porous silicon on the surface of the silicon wafer for 30 minutes by using a 2% sodium hydroxide solution (prepared by sodium hydroxide and deionized water in a mass ratio of 1: 49) to form a single-side concave lens silicon body with one side polished into a concave surface and the other side as a plane;
5. forming a porous silicon single-sided concave lens: changing the spherical thin platinum sheet 3 into a flat round thin platinum sheet (with the thickness of 200 μm), changing the corrosion current, corroding the silicon wafer to form a porous silicon film, and performing two tests, wherein the variation in the two tests is the corrosion current density which is 50mA/cm2And 40mA/cm2Forming porous silicon on the single-sided concave lens silicon body until the etching is finished to obtain a single concave lens made of a porous silicon film material;
6. for convenience in studying the problem, we chose two sets of experiments whose experimental parameters and corresponding data are as follows:
| numbering | Polishing Current (mA- cm2） | Polishing time (min) | Corrosion current (mA- cm2） | Time of etching (min) | Porous Degree of rotation | Center thickness of porous silicon concave lens Degree (mum) |
| ⑴ | 100 | 25 | 50 | 150 | 58% | ~325、420 |
| ⑵ | 100 | 25 | 40 | 185 | 53% | ~320、415 |
7. According to the relevant documents and combining the experimental conditions, the porosity of the single-sided concave lens formed by the two formed porous silicon thin films is respectively about 58 and 53 percent, and the central thickness of the single-sided concave lens is respectively about 325 and 420 μm and 320 and 415 μm;
8. after the preparation of the nano porous silicon single-sided concave lens is finished, quickly putting the porous silicon single-sided concave lens sample into high-purity deionized water for cleaning for 10 minutes to replace electrochemical corrosion liquid (hydrofluoric acid and water) and other reaction products in the porous silicon concave lens; then, soaking the porous silicon single-sided concave lens in a mixed solution of hydrogen peroxide and deionized water (the volume ratio is 2:100) for post-treatment for 6 hours;
9. after the post-treatment is finished, washing with deionized water, and finally drying in the air;
10. and (5) obtaining a finished product after the product is qualified through inspection.
Claims (3)
1. A preparation method of a nano porous silicon single concave lens is characterized in that a thin platinum sheet which is conventionally used as an electrode is made into a hollow sphere, a spherical crown cut from the hollow sphere is made into a cathode, the spherical crown height H of the spherical crown-shaped thin platinum sheet used as the cathode is = 0.01-0.5R, wherein R is the radius of the hollow sphere where the spherical crown electrode is located; the convex surface of the spherical crown-shaped thin platinum sheet is opposite to the silicon wafer, wherein the length of the bottom surface of the spherical crown is equal to the diameter of the silicon wafer, the circular flat thin platinum sheet is used as an anode, the distance L between the plane of the bottom of the spherical crown-shaped thin platinum sheet cathode and the flat thin platinum sheet anode is = 0.02-10R, and R is the radius of a hollow sphere where the spherical crown electrode is located; and a silicon chip is placed between the spherical crown-shaped thin platinum sheet and the flat plate thin platinum sheet through a sealing support, the central axis of the silicon chip, the central axis of the flat plate thin platinum sheet, the circle center of the spherical crown-shaped thin platinum sheet coincide with the central axis of the spherical crown, the distances from the silicon chip to the anode and the cathode are equal, the silicon chip, the flat plate thin platinum sheet and the spherical crown-shaped thin platinum sheet are all immersed in electrolytic corrosion liquid, the silicon chip divides the corrosion liquid into two independent parts, and the electrolytic corrosion liquid is hydrofluoric acid: the absolute ethyl alcohol and the deionized water are prepared according to the volume ratio of 1:1: 2; firstly, electropolishing a silicon wafer by adopting a large constant-current corrosion current of a constant-current source, so that a concave spherical surface is formed on one surface of the silicon wafer close to a spherical crown-shaped thin platinum sheet electrode, and a plane is maintained on one surface close to a flat thin platinum sheet electrode; then, using a sodium hydroxide solution to corrode the porous silicon on the surface of the silicon wafer to form a concave lens siliceous body with one polished surface forming a concave surface shape and one un-corroded surface maintaining a plane; and then replacing the spherical-crown-shaped thin platinum sheet electrode with a circular flat-plate thin platinum sheet electrode, and carrying out electrochemical corrosion on the silicon wafer by using a small constant corrosion current which is smaller than the conventional polishing current of the silicon wafer to form the nano porous silicon single concave lens.
2. The method for preparing a nanoporous silicon single concave lens as claimed in claim 1, wherein the electropolishing is carried out by electropolishing a silicon wafer using a large constant current corrosion current, and on the one hand, under a normal condition of a large constant current corrosion current density larger than a conventional polishing current of the silicon wafer, since one surface used is a spherical crown-shaped electrode and the other surface used is a circular flat electrode, the farther away from the central axis, the smaller the corrosion current density, the slower the polishing speed of the silicon wafer, and thereby a concave spherical surface is formed on the surface of the silicon wafer close to the spherical crown-shaped thin platinum sheet, centered on the central axis of the silicon wafer, and the shallower the polishing is the farther away from the central axis.
3. The method for preparing a nano-porous silicon single concave lens according to claim 1 or 2, wherein the specific process of the electrochemical corrosion is to change the spherical-crown-shaped thin platinum sheet into a circular parallel thin platinum sheet after the electropolishing is completed, and to perform the electrochemical corrosion on the silicon wafer by using a small constant corrosion current smaller than the conventional polishing current of the silicon wafer to form a porous silicon thin film until the whole silicon wafer is completely formed into the single concave lens made of the porous silicon material.
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