CN109056049A - A kind of preparation method of nano-structure porous silicon biconcave lens - Google Patents
A kind of preparation method of nano-structure porous silicon biconcave lens Download PDFInfo
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- CN109056049A CN109056049A CN201810935379.3A CN201810935379A CN109056049A CN 109056049 A CN109056049 A CN 109056049A CN 201810935379 A CN201810935379 A CN 201810935379A CN 109056049 A CN109056049 A CN 109056049A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F3/00—Electrolytic etching or polishing
- C25F3/16—Polishing
- C25F3/30—Polishing of semiconducting materials
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Abstract
The invention discloses a kind of preparation methods of nano-structure porous silicon biconcave lens, this method is that the conventional platinized platinum as electrode is made into hollow ball and the two symmetrical spherical crowns intercepted from hollow ball are made into electrode, silicon wafer is placed between two spherical crown electrodes, and two convex surfaces of two spherical crown electrodes face silicon wafer, corrosive liquid is separated into two independent parts by silicon wafer;Electropolishing is first carried out to silicon wafer using constant-current source and two sides before and after silicon wafer is made to form same spill ball surface;It changes two symmetrical spherical crown electrodes into parallel plate type electrode again, electrochemical corrosion is carried out to silicon wafer two sides and forms porous biconcave lens.By means of the present invention, nano-structure porous silicon biconcave lens can be obtained, micro-opto-electromechanical system can be widely used in, has made great contribution for micro optoelectro mechanical system field.
Description
Technical field
The present invention relates to semiconductor technologies and optical engineering field, and in particular to a kind of system of nano-structure porous silicon biconcave lens
Preparation Method.
Background technique
1956, Uhlir carried out the presence that porous silicon is had found when electrochemical polishing treatment to silicon wafer in HF solution;
Nineteen ninety, Canham have found that porous silicon issues visible light at room temperature, this research for being found to be porous silicon opens the new century
Member, i.e. light-emitting porous silicon conceptual phase at room temperature;The Luminous display of porous silicon at room temperature silicon is in photoelectronics, optical device
And the application prospect that display technology etc. is wide.Especially 1996, Hirschman realized the integrated original of silicon based opto-electronics for the first time
Type device is a milestone of porous silicon application study.
Porous silicon film is a kind of spongiform porous material for having huge specific surface area.This material has cost simultaneously
Cheap, bio-compatibility it is good and can and existing integrated circuit technology it is completely compatible.Although porous silicon from the 1990s with
It is widely paid close attention to as a kind of good sensor material by people, but so far to using porous silica material to prepare optics device
Part is also less, especially rare in terms of optical, mechanical and electronic integration research.
MEMS (MEMS, Micro-Electro-Mechanical System), also referred to as mems
System, micro-system and micromechanics etc..Be collection microsensor, microactrator, micro mechanical structure, micro battery, micro- energy, signal processing and
Control circuit, high-performance electronic integrated device, interface and communication etc. are at several millimeters in the microdevice or system, size of one
To smaller high-tech device.
In recent years, with the fast development of microelectric technique, electronic device, mems accelerometer, MEMS microphone, micro- horse
It reaches, Micropump, micro-oscillator, MEMS optical sensor, MEMS pressure sensor, MEMS gyroscope, MEMS humidity sensor, MEMS gas
The size of body sensor is smaller and smaller.Micro-opto-electromechanical system Integrated research is fast-developing, and silicon substrate is micro- light, mechanical, electrical and integrated
Technology is just highly valued, and the micro optical elements such as lens, prism and reflecting mirror are the important composition portions of micro-opto-electromechanical system
Point, they can convert microoptical circuit, transmitted and be handled, to reach the transmitting of light, aggregation, polarization, interference and scattering
Purpose, but using porous silica material prepare the micro optical elements such as lenticule, prism and reflecting mirror study it is also seldom.
There is document to shelter using polymethyl methacrylate (Polymethylmethacrylate, abbreviation PMMA)
Silicon, the method for preparing oxidized porous silicon optical waveguide prism using the electrochemical corrosion course of selectivity are prepared respectively based on more
The convergence of hole silicon and divergent lens.This kind of waveguide prism can significantly converge and dissipate the light beam transmitted in waveguide.But
This method and process is complicated, and controllability is not strong, it is also difficult to realize that micro- opto-mechanical-electric system is integrated.
Summary of the invention
In order to realize that the micro- light, mechanical, electrical micro-system of silicon substrate is integrated, the object of the present invention is to provide a kind of nano-structure porous silicon concave-concaves
The preparation method of lens.
To achieve the above object, the technical solution adopted by the present invention: a kind of preparation method of nano-structure porous silicon biconcave lens,
It is characterized in that, this method is that the conventional platinized platinum as electrode is made into hollow ball and two intercepted from hollow ball
Identical symmetrical spherical crown is made into electrode, and two convex surfaces of two spherical crowns face silicon wafer, place between two spherical crown electrodes
Silicon wafer, two spherical crown electrode bottom surfaces with silicon wafer where plane it is parallel, silicon wafer central axis, spherical crown electrode the center of circle and spherical crown in
Mandrel line (three) is overlapped, and silicon wafer being equidistant from left and right two spherical crown electrodes, and corrosive liquid is separated into two solely by silicon wafer
Vertical part;Electropolishing is carried out to silicon wafer using constant-current source and two sides before and after silicon wafer is made to form same spill ball surface;Again will
Two symmetrical spherical crown electrodes change parallel plate electrode into, carry out electrochemical corrosion to silicon wafer two sides and form nano-structure porous silicon
Concavees lens.
The principle of the present invention is: 2 processes of the preparation of nano-structure porous silicon biconcave lens point, firstly, identical using size
Positive and negative big constant current corrosion current carries out electropolishing to silicon wafer, on the one hand, in the big constant current of (being greater than silicon wafer routine electropolishing electric current)
Under the conditions of corrosion electric current density, electropolishing is carried out simultaneously to former and later two surfaces of silicon wafer, due to using size identical
Positive and negative perseverance corrosion current and be spherical electrode, remoter from central axis centered on two spherical crown electrode centers axis, corrosion electricity
Current density is smaller, slower to the polishing velocity of silicon wafer, to be formed centered on silicon wafer central axis, polishing remoter from central axis
It is more shallow, due to applying identical polishing electric current on the forward and backward two sides of silicon wafer, cause to form same spill on the forward and backward two sides of silicon wafer
Ball surface.Secondly, being completed in electropolishing and then changing two spherical crown electrodes into parallel circular plate electrode, while using instead and (being less than
Silicon wafer routine electropolishing electric current) small positive and negative permanent corrosion current on the forward and backward two sides of silicon wafer carries out electrochemical corrosion simultaneously, it is formed
Porous silicon film, until entire silicon wafer is completely formed the concavees lens being made of porous silica material.
By change thin platinized platinum hollow ball radius R, spherical crown height H and two spherical crown bottoms where between plane away from
Radius of curvature from two outer surfaces that the size of L and electropolishing condition can change biconcave lens of the present invention.
Preferably as platinized platinum spherical crown height H=0.01 ~ 0.5R of spherical crown electrode.
Preferably, the distance between plane L=0.02 ~ 10R where two platinized platinum spherical crown electrode bases.
The beneficial effects of the present invention are: by means of the present invention, nano-structure porous silicon biconcave lens can be obtained, can answer extensively
For micro-opto-electromechanical system, great contribution is made for micro optoelectro mechanical system field.
Detailed description of the invention
Fig. 1 is the electrolytic etching slot structure schematic diagram involved in the present invention arrived
Wherein, 1, etching tank, 2, silicon wafer, 3, spherical thin platinized platinum, 4, sealed support.
Specific embodiment
The present invention is further illustrated combined with specific embodiments below.It is as described below, it is only preferable reality of the invention
Example is applied, is not limited the present invention, any those skilled in the art are possibly also with the present invention
Disclosed technology contents are changed to the equivalent embodiment changed on an equal basis.Therefore all contents without departing from the present invention program, according to
Simple modification or equivalent variations are made to following embodiment according to technical spirit of the invention, protection scope of the present invention should all be fallen in
It is interior.
Embodiment one
The preparation method of this nano-structure porous silicon biconcave lens of the invention, specifically comprises the following steps:
1, selecting silicon wafer type is P100, resistivity be 0.01 Ω .cm, the round silicon wafer with a thickness of 500 μm of twin polishings, two
A platinized platinum (with a thickness of 200 μm) ball (radius is 2cm) hat base length=silicon wafer diameter is as electrode;Silicon wafer and spherical thin platinum
Piece 3, which is fully immersed in electrolytic etching liquid, carries out electrochemical corrosion, and plane where silicon wafer and two spherical thin 3 bottoms of platinized platinum is flat
The center overlapping of axles of row and three, electrolytic etching liquid is by hydrofluoric acid: dehydrated alcohol and deionized water are matched with volume ratio for 1:1:2
System.
2, it connects circuit: being placed with corrosive liquid in etching tank 1, the centre in etching tank 1 is solid by sealed support 4
Determine silicon wafer 2, the corrosive liquid in etching tank 1 is separated into independent two parts by silicon wafer 2 and sealed support 4, two in etching tank 1
It holds and is symmetrical arranged 2 spherical thin platinized platinums 3 and does electrode, and the convex surface of two spherical thin platinized platinums 3 is all facing to silicon wafer 2, two
Distance L is 0.25cm, the corruption of silicon wafer 2 and spherical thin platinized platinum 3(silicon wafer 2 between planar central where spherical 3 bottom of thin platinized platinum
The circular flat diameter that erosion diameter and domed 3 bottom of thin platinized platinum are projected is equal, is 2 centimetres) all it is immersed in corrosion
In liquid, silicon wafer 2 is parallel with planes where two spherical thin 3 bottoms of platinized platinum and the center of silicon wafer central axis and spherical thin platinized platinum
Overlapping of axles.It is externally provided with constant-current source in etching tank 1, constant-current source is generated by TekVisa AFG3101 arbitrary waveform generator,
The positive and negative electrode of the constant-current source is connect by conducting wire with two spherical thin 3 electrodes of platinized platinum, and when work, the positive and negative anodes of current source lead to
Excessive erosion liquid forms current loop.
3, form concave shape silicon shape body in silicon wafer polishing both surfaces: constant-current source is positive and negative square-wave signal, and frequency is 10Hz, is put down
Polishing size of current is -120 and 120mA/cm2, the electropolishing time is 20Min, makes silicon wafer on front and back two sides while being polished to
Concave shape silicon shape body.
4, using 2% sodium hydroxide solution (press sodium hydroxide: deionized water is what 1:49 was prepared with mass ratio) silicon wafer table
The porous silicon in face corrodes 20 minutes, forms two sides concave shape silicon shape body.
5, porous silicon concavees lens are formed: two spherical crown electrodes are changed into plate circle platinum plate electrode (with a thickness of 200 μm), it is permanent
Stream source is positive and negative square-wave signal, and frequency is 10Hz, meanwhile, two groups of tests are carried out, and the variable quantity in two groups of tests is corrosion electricity
Current density, and corrosion electric current density is -50 and 50mA/cm2, -40 and 40mA/cm2, it is formed simultaneously on concave shape silicon shape body two sides
Porous silicon obtains the biconcave lens being made of porous silicon film material until etching.
6, for the convenience to study a question, we have selected two groups of experiments, and experiment parameter and corresponding data are as follows:
Number | Polish electric current (mA/cm2) | Polishing time (min) | Corrosion current (mA/cm2) | Etching time (min) | Vesicularity | Porous silicon concavees lens center, edge thickness (μm) |
⑴ | 120 | 20 | 50 | 150 | 60% | ~325、420 |
⑵ | 120 | 20 | 40 | 187 | 55% | ~320、415 |
7, according to pertinent literature and in conjunction with above-mentioned experiment condition, the two-sided concave for being formed by two porous silicon films composition is obtained
The vesicularity of lens respectively may be about 60%, 55%, the center of biconcave lens, edge thickness be respectively about 325,420 μm and 320,
415μm;
8, when nano-structure porous silicon biconcave lens preparation after, by porous silicon double concavees lens print be put into rapidly high-purity go from
It is cleaned 10 minutes in sub- water, generates the electrochemical corrosive liquid (hydrofluoric acid and water) in porous silicon double concavees lens and other reactions
Object cements out;Then, porous silicon concavees lens are immersed in the mixed liquor of hydrogen peroxide and deionized water (volume ratio 2:100)
In carry out post-processing 6 hours;
9, it after post-processing, is rinsed using deionized water, is finally dried in air;
It 10, is after the assay was approved finished product.
Embodiment two
The preparation method of this nano-structure porous silicon biconcave lens of the invention, specifically comprises the following steps:
1, selecting silicon wafer type is P100, resistivity be 0.01 Ω .cm, the round silicon wafer with a thickness of 500 μm of twin polishings, two
A platinized platinum (with a thickness of 200 μm) ball (radius is 2cm) hat base length L=silicon wafer diameter is as electrode;Silicon wafer and spherical thin platinum
Piece 3, which is fully immersed in electrolytic etching liquid, carries out electrochemical corrosion, planes where silicon wafer and two spherical platinized platinum bottoms it is parallel and
The center overlapping of axles of three, electrolytic etching liquid are by hydrofluoric acid: dehydrated alcohol and deionized water are that 1:1:2 is prepared with volume ratio
's.
2, it connects circuit: being placed with corrosive liquid in etching tank 1, the centre in etching tank 1 is solid by sealed support 4
Determine silicon wafer 2, the corrosive liquid in etching tank 1 is separated into independent two parts by silicon wafer 2 and sealed support 4, two in etching tank 1
It holds and is symmetrical arranged 2 spherical thin platinized platinums 3 and does electrode, and the convex surface of two spherical thin platinized platinums 3 is all facing to silicon wafer 2, two
Distance is 0.25cm, the corruption of silicon wafer 2 and spherical thin platinized platinum 3(silicon wafer 2 between planar central where spherical 3 bottom of thin platinized platinum
Circular flat diameter where losing diameter and domed 3 bottom of thin platinized platinum is equal, is 2 centimetres) all it is immersed in corrosive liquid,
Silicon wafer 2 is parallel with two spherical thin 3 bottoms of platinized platinum and the center overlapping of axles of silicon wafer central axis and spherical thin platinized platinum.In etching tank
1 is externally provided with constant-current source, and constant-current source is generated by TekVisa AFG3101 arbitrary waveform generator, the constant-current source it is positive and negative
Pole is connect by conducting wire with two spherical thin 3 electrodes of platinized platinum, and when work, the positive and negative anodes of current source form electric current by corrosive liquid
Circuit.
3, form concave shape silicon shape body in silicon wafer polishing both surfaces: constant-current source is positive and negative square-wave signal, and frequency is 10Hz, is put down
Polishing size of current is -100 and 100mA/cm2, the electropolishing time is 25Min, makes silicon wafer on front and back two sides while being polished to
Concave shape silicon shape body.
4, using 2% sodium hydroxide solution (press sodium hydroxide: deionized water is what 1:49 was prepared with mass ratio) silicon wafer
The porous silicon on surface corrodes 20 minutes, forms two sides concave shape silicon shape body.
5, porous silicon concavees lens are formed: changing two spherical electrodes into planar rondure platinum plate electrode, constant-current source be just,
Negative square-wave signal, frequency are 10Hz, meanwhile, two groups of tests are carried out, and the variable quantity in two groups of tests is corrosion electric current density, and
Corrosion electric current density is -50 and 50mA/cm2, -40 and 40mA/cm2, it is formed simultaneously porous silicon on concave shape silicon shape body two sides, directly
To etching, the double concave lens being made of porous silicon film material are obtained.
6, for the convenience to study a question, we have selected two groups of experiments, and experiment parameter and corresponding data are as follows:
Number | Polish electric current (mA/cm2) | Polishing time (min) | Corrosion current (mA/cm2) | Etching time (min) | Vesicularity | Porous silicon concavees lens center, edge thickness (μm) |
⑴ | 100 | 25 | 50 | 150 | 59% | ~315、410 |
⑵ | 100 | 25 | 40 | 185 | 54% | ~310、405 |
7, according to pertinent literature and in conjunction with above-mentioned experiment condition, the concavees lens for being formed by two porous silicon films composition are obtained
Vesicularity respectively may be about 59%, 54%, the center of biconcave lens, edge thickness are respectively about 315,410 μm and 310,405 μ
m;
8, after the preparation of nano-structure porous silicon double concave lens, porous silicon double concave lens print is put into rapidly high-purity
It is cleaned 10 minutes in deionized water, makes electrochemical corrosive liquid (hydrofluoric acid and water) in porous silicon double concave lens and other anti-
Product is answered to cement out;Then, by porous silicon double concave lens be immersed in hydrogen peroxide and deionized water (volume ratio 2:
100) post-processing 6 hours is carried out in mixed liquor;
9, it after post-processing, is rinsed using deionized water, is finally dried in air;
It 10, is after the assay was approved finished product.
Claims (5)
1. a kind of preparation method of nano-structure porous silicon biconcave lens, which is characterized in that this method is by the conventional platinum as electrode
Piece is made into hollow ball and the two symmetrical spherical crowns intercepted from hollow ball is made into electrode, two spherical crown electrodes it
Between place silicon wafer, and two convex surfaces of two spherical crown electrodes face silicon wafer, two spherical crown electrode bottom surfaces with it is flat where silicon wafer
Face is parallel, silicon wafer central axis, spherical crown electrode the center of circle be overlapped with the central axis of spherical crown electrode, silicon wafer is from left and right two balls
Hat electrode is equidistant, and corrosive liquid is separated into two independent parts by silicon wafer;Electric throwing is first carried out to silicon wafer using constant-current source
Light and so that two sides before and after silicon wafer is formed same spill ball surface;Change two symmetrical spherical crown electrodes into parallel board-like electricity again
Pole carries out electrochemical corrosion to silicon wafer two sides and forms porous biconcave lens.
2. the preparation method of nano-structure porous silicon biconcave lens according to claim 1, which is characterized in that above-mentioned electropolishing
Detailed process is: firstly, big constant current corrosion current that is identical positive and negative using size and being greater than silicon wafer routine polishing electric current is to silicon
Piece carries out electropolishing, on the one hand, under the conditions of normal big constant current corrosion electric current density, to former and later two surfaces of silicon wafer and meanwhile into
Row electropolishing, due to using the identical positive and negative permanent corrosion current of size and being spherical electrode, in two spherical crown electrodes
Remoter from central axis centered on mandrel, corrosion electric current density is smaller, slower to the polishing velocity of silicon wafer, to be formed with silicon wafer
Remoter from central axis centered on central axis, polishing is more shallow, since two sides applies identical polishing electric current before and after silicon wafer, causes
Two sides forms same spill ball surface before and after silicon wafer.
3. the preparation method of nano-structure porous silicon biconcave lens according to claim 1 or 2, which is characterized in that above-mentioned electrification
The detailed process for learning corrosion is to complete in electropolishing and then change two spherical crown electrodes into parallel circular plate electrode, change simultaneously
Be less than the identical permanent corrosion current of small and positive and negative size of the conventional polishing electric current of silicon wafer before and after silicon wafer both sides simultaneously into
Row electrochemical corrosion forms porous silicon film, until entire silicon wafer is completely formed the biconcave lens being made of porous silica material.
4. the preparation method of nano-structure porous silicon biconcave lens according to claim 3, which is characterized in that as spherical crown electrode
Platinized platinum spherical crown height H=0.01 ~ 0.5R, wherein R be spherical crown electrode where hollow ball radius.
5. the preparation method of nano-structure porous silicon biconcave lens according to claim 4, which is characterized in that two spherical crown electrodes
Plane where bottom is parallel and distance L=0.02 ~ 10R between the two, and wherein R is the hollow ball radius where spherical crown electrode.
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