CN101887851A - Method of double side alignment photoetching and magnetic field auxiliary electrochemical corrosion of silicon-based three-dimensional structure - Google Patents
Method of double side alignment photoetching and magnetic field auxiliary electrochemical corrosion of silicon-based three-dimensional structure Download PDFInfo
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- CN101887851A CN101887851A CN 201010186679 CN201010186679A CN101887851A CN 101887851 A CN101887851 A CN 101887851A CN 201010186679 CN201010186679 CN 201010186679 CN 201010186679 A CN201010186679 A CN 201010186679A CN 101887851 A CN101887851 A CN 101887851A
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Abstract
The invention relates to a method of double side alignment photoetching and magnetic field auxiliary electrochemical corrosion of a silicon-based three-dimensional structure, comprising the following steps of double side alignment photoetching a silicon wafer, pre-corroding sunk holes, preparing a corrosion solution, preparing before electrochemical corrosion, implementing electrochemical corrosion and post-processing, wherein in the process of pre-corroding the sunk holes, the double side alignment photoetching silicon wafer is put into a KOH solution with the molar concentration of 5-8, is in pre-corroding for 5-10m under the temperature of 80-100 DEG C, and double sides of the silicon wafer are corroded with the pre-corrosion sunk holes with the depth of 3-6 microns according to the technological requirements. The invention has the advantages of strong practicability, simple process, easy operability and the like and can enable currents in the process of electrochemical corrosion to be limited in a double side alignment graph opening region particularly after the silicon wafer is treated by double side alignment photoetching and the pre-corrosion sunk hole with a certain depth is pre-corroded to inhibit and eliminate the generation of the edge effect, thereby increasing the steep performance of a three-dimensional periodic structure.
Description
Technical field
The present invention relates to material science and electrochemical field, particularly relate to a kind of method of double-sided alignment photoetching and magnetic field auxiliary electrochemical corrosion of silicon-based three-dimensional structure.
Background technology
The electrochemical corrosion technology is the emerging silicon-based three-dimensional structure process technology that grew up in recent years, and electrochemistry deep etch silicon microstructure exhausts based on the hole.Since electrochemical corrosion course and hole be distributed with confidential relation, by space charge region (SCR) pattern, electrochemical etching depends on the generation in hole and on every side the distribution at the tip consumingly.Because for the bigger figure of spacing, owing to there is bigger interval between figure and the figure, in these zones, because these sizes at interval are often big than the distance between figure internal holes and the hole, the positive contact corrosion liquid of graph area, spread to the front at the silicon chip back side in the hole, electron hole velocity magnitude and direction are constantly changing, be not all vertically to pass in diffusion process from graphical window, but ceaselessly scatter on all directions, so the space depletion layer often can not cover these zones, be that these regional charge carriers can not be depleted, the hole that is entered by the back side can be diffused into the zone between the figure in this case, does not exhaust the hole and arrives SiO
2Insulation masking layer place can not pass and make the Electric Field Distribution inequality in the place's accumulation of insulation mask, the sudden change of Electric Field Distribution can cause the hole to be injected from the sidewall border of structure, around being distributed in that etching liquid and figure have a common boundary, do not exhaust the hole between figure and finally leak into figure opening part and corrosive liquid generation electrochemical reaction, produce edge effect, sidewall is corroded, causes sidewall not steep.So electrochemical corrosion is difficult to obtain the steep three-dimensional periodic structure of big spacing of 20-300 μ m.
Summary of the invention
Technical problem to be solved by this invention is: the method that a kind of double-sided alignment photoetching and magnetic field auxiliary electrochemical corrosion of silicon-based three-dimensional structure is provided, the figure open area that makes electric current be limited in the double-sided alignment photoetching and behind the pre-etching hole, form, suppress and eliminate the generation of edge effect, thereby increase the steep property of three-dimensional periodic structure.This method can realize that spacing is the steep three-dimensional periodic structures such as big spacing periodicity borehole structure, lobe formation and platform shape structure of 20-300 μ m.
The present invention solves its technical problem and adopts following technical scheme:
The method of the double-sided alignment photoetching and magnetic field auxiliary electrochemical corrosion of silicon-based three-dimensional structure provided by the invention, it may further comprise the steps:
(1) double-sided alignment photoetching silicon chip: utilize mask aligner and pattern mask that silicon chip is carried out the double-sided alignment photoetching, mask graph is transferred on silicon chip two-sided;
(2) pre-etching hole: it is 5～8 KOH solution that the silicon chip of double-sided alignment photoetching is put into molar concentration, 80-100 ℃ following pre-etching 5-10 minute; According to technological requirement, in the two-sided pre-etching hole that erodes away the 3-6 micrometer depth of silicon chip;
(3) configuration corrosive liquid: HF, DMF and water are mixed, the volume ratio of forming the three is (2.5～3.5): (14～18): 1 corrosive liquid is as the negative pole corrosive liquid, wherein, HF is the hydrofluoric acid of volumetric concentration 40%, and DMF is the dimethyl formamide of volumetric concentration 99.5%; With the pure NH of the analysis of volumetric concentration 96%
4The HF of F, volumetric concentration 40% and water mix, and the volume ratio of forming the three is that 3: 6: 10 hydrofluoric acid buffered etch liquid is as anodal corrosive liquid;
(4) preparation before the electrochemical corrosion:
The double flute etching apparatus is placed in the fume hood, again the corrosive liquid that configures is added respectively in the etching tank of both sides, connect two pairs of electrodes;
Magnetic field configuration:, simultaneously vertical with direction of an electric field with vertical 100 crystal orientation of magnetic direction; This magnetic direction is decided to be the x axle.
With photoetching good and through pre-etching hole silicon chip pack in the described etching tank;
(5) enforcement of electrochemical corrosion: according to technological requirement, under the synergy in corrosive liquid, 0.01～0.08A electric current and magnetic field to photoetching good and through pre-etching hole silicon chip carry out electrochemical corrosion;
(6) reprocessing: after electrochemical corrosion finishes silicon chip taken off with deionized water and rinse well, dry then;
Through above-mentioned steps, obtain product with silicon-based.
In the above-mentioned steps:
The shape of described mask graph can be circular, square, square, prismatic or antiparallelogram array.
The present invention can dispose the negative pole corrosive liquid by following method: with the mixing of HF, DMF and water, the volume ratio of forming the three is 3: 16: 1 a corrosive liquid.
Described magnetic field can be the magnetic field of 10～100mT intensity, and its preferred value is 72mT.
Described technological requirement is meant: adopt the direct current of 0.01～0.08A, its preferred value is 0.04A.Etching time is 100～300 minutes, and its preferred value is 120 minutes.Corrosion depth is 30～100 microns, and its preferred value is 68 microns.The corrosion spacing is 20～300 microns, and its preferred value is 300 microns.
The present invention compares with the method for traditional silicon-based three-dimensional structure electrochemical corrosion and mainly contains following advantage:
One. technology is simple: avoided having reduced technology difficulty at silicon chip back side plating conductive metal layer, be of value to the compatibility of body silicon process technology and IC technology.
They are two years old. practical: having solved spacing well is the etching problem of big spacing periodically round bowl structure, lobe formation and the platform shape structure of 20～300 μ m, and etching depth can reach 30～100 microns dark.
They are three years old. and behind the pre-etching hole of silicon chip through double-sided alignment photoetching and pre-etching certain depth, the electric current when making electrochemical corrosion is limited in double-sided alignment figure open area, suppresses and eliminate the generation of edge effect, thereby increases the steep property of three-dimensional periodic structure.
They are four years old. workable:
Because the existence in magnetic field can stop bifurcation structure thereby can suppress transverse current, so just can well control to electrochemical corrosion course by the distribution in control hole.
Based on the design principle of Hall effect, vertical (100) crystal orientation (this direction is decided to be the x axle) of magnetic direction is simultaneously vertical with direction of an electric field.The litho pattern spacing is 20-300 μ m, difformity array such as that mask graph is respectively is circular, square, square, prismatic or antiparallelogram.Double flute electrochemical corrosion device is placed vertical magnetic field, and magnitude of field intensity is provided by electromagnet, and the magnetic flux density with tesla's instrumentation electromagnet comes controlling magnetic field intensity size by regulating magnet coil electricity electric current.
Embodiment
The invention provides a kind of method of silicon-based three-dimensional structure double-sided alignment photoetching and magnetic field auxiliary electrochemical corrosion, this method is a kind of method of improving the steep property of the big spacing figure of electrochemical corrosion silicon-based three-dimensional structure, is a kind of method that is different from the silicon-based three-dimensional structure electrochemical corrosion of prior art.Specifically: adopt double flute corrosion device (claiming container again), make the silicon chip of two-sided oxidation by lithography two-sided figure by double-sided alignment, after the photoetching sample being placed on molar concentration is 80-100 ℃ of heating pre-etching 5-10min in the 5-8M KOH solution, erode away the pre-etching hole that the degree of depth is the 3-6 micron silicon chip two-sided, purpose is that all the other are local by insulation SiO at the figure back side and the positive unique window that passes through of electric current that forms
2Film insulation, thus make electric current only enter and flow out from graph area, and pass through at non-graph area no current.Then the silicon chip of pre-etching is packed in the hole of groove of this container; Container is made by the polytetrafluoroethylmaterial material of acid-fast alkali-proof.Between sealing ring and the holddown groove entire container is divided into two parts fully, graphite electrode is respectively placed in both sides, and two graphite electrodes connect the positive pole and the negative pole of direct-flow voltage regulation source respectively, fix two etching tanks with screw-driving, in order to avoid leakage.The negative pole corrosive liquid is made up of the volumetric concentration 40%HF of different proportionings and the hybrid corrosion liquid of volumetric concentration 99.5%DMF and water, and the volume ratio of forming the three is (2.5～3.5): (14～18): 1 corrosive liquid; Anodal corrosive liquid is that the HF of the pure NH4F of the analysis of volumetric concentration 96%, volumetric concentration 40% and water are mixed, and the volume ratio of forming the three is 3: 6: 10 a hydrofluoric acid buffered etch liquid.Two ends add adjustable corrosion current, and electric current passes silicon chip through solution.Like this, becoming the anode of electrochemical reaction over against the silicon chip of negative electrode, carry out anodic oxidation reactions, also is the electrochemical corrosion reaction.Simultaneously, add magnetic field in the vertical current direction.Externally-applied magnetic field has further suppressed the deflection of electric current.
The invention will be further described below in conjunction with specific embodiment, but do not limit the present invention.
To form graphical window behind double-sided alignment photoetching and pre-etching hole packs in the etching tank for the sample of circular, square, square, prismatic or antiparallelogram array, corrosion current is 0.01-0.08A, final corrosion is intact lobe formation, this method need not added any compensation block on mask, the corrosion process controllability is good; Figure is not limited by lattice and etching time, can process the micro-structural of arbitrary shape; Need not the crystal orientation during figure transfer and aim at, simplified operating procedure.
Embodiment 1:
Utilize square array mask double-sided alignment to be lithographically the SiO that contains of square array
2N type Si (100) sample of masking layer is packed into after 10 minutes through pre-etching in the etching tank, the square window length of side is 300 μ m, spacing also is 300 μ m, vertical magnetic field intensity 63mT, corrosion current 0.04A, etching time 150min, figure top is intact square, and whole figure corner angle are clearly demarcated, and salient angle is intact, be the truncated rectangular pyramids shape, corrosion depth is about 71um.
Embodiment 2:
Utilize square array mask double-sided alignment to be lithographically the SiO that contains of square array
2N type Si (100) sample of masking layer is packed into after 5 minutes through pre-etching in the etching tank, the square window length of side is 100 μ m, spacing also is 100 μ m, vertical magnetic field intensity 63mT, corrosion current 0.05A, etching time 100min, figure top is intact square, and whole figure corner angle are clearly demarcated, and salient angle is intact, be the truncated rectangular pyramids shape, corrosion depth is about 53um.
Embodiment 3:
Etching condition is a 63mT vertical magnetic field intensity, and etching time is 190min, corrosion current 0.04A, and other conditions increase etching time with embodiment 1, and table surface height increases.
Embodiment 4:
Utilize circular array mask double-sided alignment to be lithographically the SiO that contains of circular array
2N type Si (100) sample of masking layer is packed into after 10 minutes through pre-etching in the etching tank, round diameter is 100 μ m, spacing is 300 μ m, vertical magnetic field intensity 72mT, corrosion current 0.04A, etching time 190min, figure top is intact circle, whole figure corner angle are clearly demarcated, and salient angle is intact, are the class circle and lean on the shape corrosion depth and be about 90um.
Embodiment 5:
Utilize circular array mask double-sided alignment to be lithographically the SiO that contains of circular array
2N type Si (100) sample of masking layer is packed into after 6 minutes through pre-etching in the etching tank, and round diameter is 50 μ m, and spacing is 100 μ m, vertical magnetic field intensity is to 72mT, and corrosion current is 0.04A, etching time 190min, corrosion depth is darker, and the steep property of sidewall is better.From experimental phenomena, general trend is the increase along with magnetic field intensity, be increased to 72mT from 0mT, the steep property of corrosion back sidewall silicon takes an evident turn for the better, externally-applied magnetic field can effectively improve the steep property of sidewall after showing double-sided alignment photoetching pre-etching, illustrate that double-sided alignment photoetching pre-etching can play the effect of restriction energization area, vertical magnetic field can produce horizontal corrosion rate in sidewall bottom, make sidewall bottom corrosion rate trend towards top part corrosion speed.
Embodiment 6:
Utilize square array mask double-sided alignment to be lithographically the SiO that contains of square array
2P type Si (100) sample of masking layer is packed into after 5 minutes through pre-etching in the etching tank, the square window length of side is 300 μ m, spacing also is 300 μ m, vertical magnetic field intensity 72mT, corrosion current 0.04A, etching time 120min, figure top is intact square, and whole figure corner angle are clearly demarcated, and salient angle is intact, be the truncated rectangular pyramids shape, corrosion depth is about 68um.
Embodiment 7:
Utilize prismatic array mask double-sided alignment to be lithographically the SiO that contains of prismatic array
2P type Si (100) sample of masking layer is packed into after 10 minutes through pre-etching in the etching tank, the prismatic window length of side is 100 μ m, spacing also is 300 μ m, vertical magnetic field intensity 72mT, corrosion current 0.04A, etching time 180min, figure top is intact prismatic, and whole figure corner angle are clearly demarcated, and salient angle is intact, be prismatic platform shape, corrosion depth is about 77um.
Embodiment 8:
Utilize square array mask double-sided alignment to be lithographically the SiO that contains of square array
2P type Si (111) sample of masking layer and N type epitaxial loayer is packed into after 5 minutes through pre-etching in the etching tank, the square window length of side is 300 μ m, spacing also is 300 μ m, vertical magnetic field intensity 72mT, corrosion current 0.02A, etching time 300min, figure top is intact square, and whole figure corner angle are clearly demarcated, and salient angle is intact, be the truncated rectangular pyramids shape, corrosion depth is about 64um.
Embodiment 9:
Utilize circular array mask double-sided alignment to be lithographically the SiO that contains of circular array
2P type Si (111) sample of masking layer and N type epitaxial loayer is packed into after 10 minutes through pre-etching in the etching tank, round diameter is 100 μ m, spacing is 300 μ m, vertical magnetic field intensity 72mT, corrosion current 0.02A, etching time 180min, figure top is intact circle, and whole figure corner angle are clearly demarcated, and salient angle is intact, be closely cylindric, corrosion depth is about 43um.
The present invention adopts following method will obtain product with silicon-based and utilizes scanning electron microscopy work surface and cross-section morphology observation and analysis, to check the quality of this product, this method is: will obtain product with silicon-based surface and section keep flat respectively with the vertical sample stage that is placed on scanning electron microscopy on, put into afterwards on the specimen holder of scanning electron microscopy, vacuumize and observe.
Claims (7)
1. the method for the double-sided alignment photoetching and magnetic field auxiliary electrochemical corrosion of a silicon-based three-dimensional structure is characterized in that the step of this method comprises:
(1) double-sided alignment photoetching silicon chip: utilize mask aligner and pattern mask that silicon chip is carried out the double-sided alignment photoetching, mask graph is transferred on silicon chip two-sided;
(2) pre-etching hole: it is 5～8 KOH solution that the silicon chip of double-sided alignment photoetching is put into molar concentration, 80-100 ℃ following pre-etching 5-10 minute; According to technological requirement, in the two-sided pre-etching hole that erodes away the 3-6 micrometer depth of silicon chip;
(3) configuration corrosive liquid: HF, DMF and water are mixed, the volume ratio of forming the three is (2.5～3.5): (14～18): 1 corrosive liquid is as the negative pole corrosive liquid, wherein, HF is the hydrofluoric acid of volumetric concentration 40%, and DMF is the dimethyl formamide of volumetric concentration 99.5%; With the pure NH of the analysis of volumetric concentration 96%
4The HF of F, volumetric concentration 40% and water mix, and the volume ratio of forming the three is that 3: 6: 10 hydrofluoric acid buffered etch liquid is as anodal corrosive liquid;
(4) preparation before the electrochemical corrosion:
The double flute etching apparatus is placed in the fume hood, again the corrosive liquid that configures is added respectively in the etching tank of both sides, connect two pairs of electrodes;
Magnetic field configuration:, simultaneously vertical with direction of an electric field with vertical 100 crystal orientation of magnetic direction; This magnetic direction is decided to be the x axle.
Photoetching is good and in the silicon chip in pre-etching hole is packed described etching tank into;
(5) enforcement of electrochemical corrosion: according to technological requirement, silicon chip good to photoetching and through the pre-etching hole carries out electrochemical corrosion under the synergy in corrosive liquid, 0.01～0.08A electric current and magnetic field;
(6) reprocessing: after electrochemical corrosion finishes silicon chip taken off with deionized water and rinse well, dry then;
Through above-mentioned steps, obtain product with silicon-based.
2. method according to claim 1 is characterized in that being shaped as of mask graph is circular, square, square, prismatic or antiparallelogram array.
3. method according to claim 1, it is characterized in that by following method configuration negative pole corrosive liquid: with the mixing of HF, DMF and water, the volume ratio of forming the three is 3: 16: 1 a corrosive liquid.
4. method according to claim 1 is characterized in that described magnetic field is the magnetic field of 10～100mT intensity.
5. method according to claim 4 is characterized in that described magnetic field is the magnetic field of 72mT intensity.
6. root is dug the described method of claim 1, it is characterized in that described technological requirement is meant: adopt the direct current of 0.01～0.08A, etching time is 100～300 minutes, and corrosion depth is 30～100 microns, and the corrosion spacing is 20～300 microns.
7. method according to claim 6 is characterized in that described technological requirement is meant: adopt the direct current of 0.04A, etching time is 120 minutes, and corrosion depth is 68 microns, and the corrosion spacing is 300 microns.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109860039A (en) * | 2018-12-21 | 2019-06-07 | 苏州矩阵光电有限公司 | A kind of device and method of magnetic field auxiliary chemical etching |
| CN110071198A (en) * | 2019-04-17 | 2019-07-30 | 深圳市华星光电半导体显示技术有限公司 | A kind of light-emitting component and preparation method thereof, array substrate |
| CN113031129A (en) * | 2021-03-04 | 2021-06-25 | 中国科学院光电技术研究所 | Method for preparing double-sided random micro-lens array by combining photoetching and wet etching |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101350380A (en) * | 2008-09-01 | 2009-01-21 | 上海联孚新能源科技有限公司 | Method for preparing monocrystalline silicon solar battery pile fabrics in magnetic field |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101350380A (en) * | 2008-09-01 | 2009-01-21 | 上海联孚新能源科技有限公司 | Method for preparing monocrystalline silicon solar battery pile fabrics in magnetic field |
Non-Patent Citations (1)
| Title |
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| 《Applied Physics Letter》 19961118 Takashi Nakagawa, Hideki Koyama, Nobuyoshi Koshida Control of structure and optical anisotropy in porous Si by magnetic-field assisted anodization 3206-3208 1-7 第69卷, 第21期 2 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109860039A (en) * | 2018-12-21 | 2019-06-07 | 苏州矩阵光电有限公司 | A kind of device and method of magnetic field auxiliary chemical etching |
| CN110071198A (en) * | 2019-04-17 | 2019-07-30 | 深圳市华星光电半导体显示技术有限公司 | A kind of light-emitting component and preparation method thereof, array substrate |
| CN113031129A (en) * | 2021-03-04 | 2021-06-25 | 中国科学院光电技术研究所 | Method for preparing double-sided random micro-lens array by combining photoetching and wet etching |
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