CN100485525C - Manufacturing process of MEMS impression template based on wet etching - Google Patents
Manufacturing process of MEMS impression template based on wet etching Download PDFInfo
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- CN100485525C CN100485525C CNB2005100430706A CN200510043070A CN100485525C CN 100485525 C CN100485525 C CN 100485525C CN B2005100430706 A CNB2005100430706 A CN B2005100430706A CN 200510043070 A CN200510043070 A CN 200510043070A CN 100485525 C CN100485525 C CN 100485525C
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Abstract
The invention discloses a product design for using glass wet method to etch the coining etch mold, which comprises: cleaning the base material, depositing coupling agent, coating etch glue, exposing, purging, doing second solid, etching, extracting the glue and so on to obtain the coining mold. The method adopts single layer negative photoresist as etching mask, it adopts silane coupling agent to enhance the adherence between the etching mask and the surface of the glass, it uses depositing mode to coat the coupling agent to reduce the drilling rate, and it adopts HCI as etching liquid agent to improve the etching surface quality. The method is suit for preparing MEMS.
Description
Technical field
The invention belongs to microelectromechanical systems (MEMS) manufacturing field, relate to a kind of based on wet etching MEMS impression block manufacturing process, this process using individual layer negative photoresist is as etching mask, be applicable to making, also can be applied to the etching of microchannel in the microfluidic analysis chip and the making of the middle optical element of Micro-Opto-Electro-Mechanical Systems (MOEMS) based on impression block in the imprint lithography MEMS layering manufacturing process.
Background technology
Imprint lithography has been proved to be a kind of can carry out the technology that the nanometer feature sizes structure is made, owing to its high precision, low cost and be applicable to that the advantage of batch process becomes the strong rival of photoetching technique of future generation (NGL), and obtained certain application.The making of impression block is one of its gordian technique in the imprint lithography process, in the normal temperature imprint lithography, because the requirement that exposure and multilayer impression align needs to adopt transparent template.Usually, the making of impression block is to adopt direct electronic beam writing technology to etch figure on quartz glass, the advantage of this method is the figure that can etch less than the 100nm characteristic dimension, is applicable to the making of integrated circuit (IC) impression block, and its shortcoming is that efficient is low, cost is high.The MEMS pattern character size is at micron order, and IC manufacturing size is bigger relatively, when adopting electron-beam direct writing technology to make the impression block of so big figure, makes technology not have rationality owing to cost is too high.Because MEMS is lower with respect to the IC accuracy requirement, uses and make impression block based on the technology of glass wet etching and can reach and reduce cost the purpose of raising the efficiency.
In the glass wet etching, the making of etching mask is the critical process of decision etching quality and etching cost.Traditional etching mask is photoresist+Cr/Au metal level, its technical maturity, but the layer metal deposition time is long, cost is high, and " pin hole " etching defect appears easily.The silicon chip of using plasma enhanced chemical vapor deposition (PECVD) polysilicon membrane or employing and glass bonding is made etching mask and can be lost deeply, but these methods since technology too complexity cause cost too high.Adopt photoresist that double-deck Cr/Au metal level adds one deck 20 μ m as etching mask, can eliminate the etching surface defective, but technology is more complicated.Have the low advantage of the simple cost of technology with single-layer lithography glue as mask, but must solve the short and high problem of undercutting rate of anti-etching time,, satisfy the needs of impression with etching depth and the sidewall steepness that needing to obtain.In addition, consider to be easy to the demoulding in the impression, need take measures to improve the glass etching surface quality.
Summary of the invention
The objective of the invention is to solve a series of problem in order to simplify technology, to reduce cost, raise the efficiency and bring in the above-mentioned impression block making, a kind of manufacture method that is applicable to the impression block that MEMS makes is proposed, this method is simple, cheap, efficient, controlled, can provide useful graph outline for imprint step subsequently simultaneously.Adopt this method can make the little impression block of pattern character size to 100 μ m.
To achieve these goals, the invention provides following technical solution:
A kind of based on wet etching MEMS impression block manufacturing process, it is characterized in that this technology may further comprise the steps:
1) base material cleaning step, base material is the glass of microslide material, at first cleans glass with acetone, and then uses distilled water flushing, the glass after the flushing is inserted and is soaked 10min in the concentrated sulphuric acid; Use distilled water flushing after pulling out again, under 100 ℃ of conditions, dry 10min, remove dirt on glass;
2) evaporation coupling agent and post-processing step are under 80 ℃ the condition in temperature with the glass after cleaning, evaporation 30min, and then under 120 ℃ of conditions, baking 40min; At the coupling agent thin layer that obtains even compact on glass;
3) be coated with shop photoresist step, the mode of employing spin coating is carried out the shop that is coated with of photoresist, and photoresist layer thickness is 60 μ m, and its photoresist contains the following weight ratio raw material: epoxy acrylate 40～60%, one tripropylene glycol diacrylate 9～15% that contracts, tristane diacrylate methyl ester 20～45%, the basic phenyl ketone 3% of 1-hydroxyl, organic alkane coupling agent KH-570,0.5～1%, organic pure defoamer 0.5～1%, organic alkane levelling agent 1%, the summation of raw material is 100%;
4) step of exposure as exposed mask, is placed the transparent antiseize membrane of perfluoroethylene-propylene with the sensitive film of high-resolution laser film setter output between photoresist and exposed mask, expose with exposure machine then;
5) development step is developed as developer solution with absolute ethyl alcohol, and development time is 15s;
6) regelate step, the back of developing is the ultraviolet high-pressure mercury lamps irradiation 2min of 500W with power, makes the photoresist full solidification;
7) etch step, etching are to carry out under the ultrasonic agitation environment, and etching temperature is 25 ℃, and the composition of etching agent is: HF:NH
4F:HCL=0.5mol/L:0.75mol/L:0.5mol/L, etch rate are 0.5 μ m/min; Remove hydrochloric acid in the composition of etching agent, its etch rate is 0.4 μ m/min, and the composition of the etching agent of this moment is HF:NH
4F:=0.5mol/L:0.75mol/L;
8) technology of removing photoresist is inserted glass in the supersonic wave cleaning machine, and is heated to 100 ℃, removes the individual layer negative photoresist, promptly obtains impression block.
The present invention adopts the individual layer negative photoresist as etching mask, adopt silane coupling agent to strengthen the adhesive force of etching mask and glass surface, mode by evaporation is coated with shop coupling agent reduction undercutting rate, adopt the adjuvant of HCL as etching liquid, improve the etching surface quality, then eliminated the surface imperfection of etching by thickening bondline technology.
Description of drawings
Fig. 1 is a process principle figure of the present invention, describes technological process of the present invention.
Fig. 2 is a undercutting rate synoptic diagram, in order to definition undercutting rate and the reason of formation of undercutting is described and the present invention in the method that solves.
(Fig. 3 a) contrasts picture with the etching figure cross section profile of optimizing back (Fig. 3 b), has described coupling agent and has been coated with the effect of spreading process optimization Fig. 3 spreads process optimization for coupling agent of the present invention is coated with before.
(as the etching of etching liquid adjuvant comparison diagram as a result, photo is not to take at 175 times microscopically to Fig. 4 to Fig. 4 a) with HCL, has described the effect that adds behind the HCL in order not add HCL in the etching liquid according to the present invention.
The etching defect photo that Fig. 5 a produces when not adopting thick adhesive process, Fig. 5 b is for adopting the intact etching figure photo that obtains behind the thick adhesive process of the present invention, and above-mentioned photo is to take at 175 times microscopically, has described the effect that adopts thick adhesive process.
The MEMS impression block that Fig. 6 makes for the technology that adopts among the present invention.
The embodiment that provides below in conjunction with accompanying drawing and inventor describes in further detail the present invention.
Embodiment
Fig. 1 is an overall craft process flow diagram of the present invention, may further comprise the steps:
The glass cleaning (Fig. 1 a) is: at first clean glass with acetone, and then use distilled water flushing, insert and soak 10min in the concentrated sulphuric acid by the glass after the flushing; Use distilled water flushing after the taking-up again, under 100 ℃ of conditions, dry 10min, remove dirt on glass; Clean completely and can significantly reduce because glass surface pollutes the etching defect that brings.
That cleans that the back adopts that the mode of evaporation carries out silane coupling agent is coated with shop (Fig. 1 b), employed coupling agent model is KH-570, using coupling agent is in order to improve the adhesion of photoresist and glass, the technology of evaporation coupling agent is: temperature is 80 ℃, the evaporation time is 30min, carry out aftertreatment behind the evaporation, post-processing approach is to toast 40min under 120 ℃ of conditions.
Next carry out gluing, exposure, development (Fig. 1 c-e).In order to realize low cost, the applicant has developed a kind of negative photoresist as etching mask, the weight ratio prescription of this photoresist is: epoxy acrylate 40%, one tripropylene glycol diacrylate 9% that contracts, tristane diacrylate methyl ester 45%, the basic phenyl ketone 3% of 1-hydroxyl, organic alkane coupling agent KH-570,1%, organic pure defoamer 1%, organic alkane levelling agent 1%.
Certainly, the weight ratio prescription of above-mentioned negative photoresist can also be, epoxy acrylate 60%, one tripropylene glycol diacrylate 15% that contracts, tristane diacrylate methyl ester 20%, the basic phenyl ketone 3% of 1-hydroxyl, organic alkane coupling agent KH-570,0.5%, organic pure defoamer 0.5%, organic alkane levelling agent 1%.
Test of many times through the applicant proves that as long as in the scope of above-mentioned prescription, prepared negative photoresist can both meet the demands.
Adopt thickening bondline technology, bondline thickness is 60 μ m; , at first designing in CorelDRAW11 software as exposed mask with the sensitive film of high-resolution laser film setter output, is that the high-resolution laser film setter of 5500dpi prints on the transparent film as exposed mask with resolution then; Adopt single-layer lithography glue as etching mask; Used litho machine model is a SB-401B double-side type exposure machine, and the time shutter is 3s; Develop as developer solution with absolute ethyl alcohol, development time is 15s.
Carry out regelate after the development, its method is to be the ultraviolet high-pressure mercury lamps irradiation 2min of 500W with power, makes the photoresist full solidification, with the anti-etching power of further enhancing glue-line; (Fig. 1 f).
Then carry out etching (Fig. 1 g), etching is to carry out under the ultrasonic agitation environment, and etching temperature is 25 ℃, and the composition of etching agent is: HF:NH
4F:HCL=0.5mol/L:0.75mol/L:0.5mol/L, etch rate are 0.5 μ m/min; Remove hydrochloric acid in the composition of etching agent, its etch rate is 0.4 μ m/min, and the composition of the etching agent of this moment is HF:NH
4F:=0.5mol/L:0.75mol/L.
At last, glass is inserted in the supersonic wave cleaning machine, and be heated to 100 ℃ and remove photoresist (Fig. 1 h), promptly obtain impression block.
Technology of the present invention when adopting single-layer lithography glue as etching mask, must solve owing to undercutting causes the not good problem of etching graph outline, thereby makes the needs of steps such as subsequent etching in the template adaptation imprint lithography process of making.Among the present invention, by preferred coupling agent and optimize the evaporation coupling agent and the evaporation aftertreatment technology, make etching side direction undercutting rate be reduced to 0.6, obtain comparatively desirable etching graph outline.Dotted line is represented the etching profile of ideal situation lower-glass (1) among Fig. 2, at this moment, the angle of inclination in etching cross section is only caused by the isotropic essence of glass wet etching, the angle on slope is 45 °, and solid outline then is the etching result under the situation that has undercutting, among the figure, W is the width at groove top after the desirable etching, W ' is for existing under the undercutting situation width at groove top after the etching, and d is an etching depth, W
0Be the original width of etching mask (2), the undercutting rate is defined as
Adopt W
0Be the etching mask of 200 μ m when carrying out etching, use coupling agent to carry out surface treatment before, photoresist is peeled off behind the 5min in etching liquid fully.After adopting silane coupling agent KH-570 that glass surface is handled, same lines anti-etching time in etching liquid is brought up to 25min, and adhesive property obviously improves, but the undercutting rate is still up to 7.0.Since the HF etching liquid can very fast destruction glass surface coupling agent layer and glass is corroded, that is to say that coupling agent is the corrosion of ability HF acid not, therefore etching liquid can corrode coupling agent layer in etching process, from the infiltration at the interface of glass surface and etching mask, form undercutting.The coupling agent coating is thick more, and is then big more with the etching liquid contact area, easy more the erosion.So that need to optimize coupling agent is coated with shop technology, to obtain even compact and thin as far as possible coupling agent thin layer.The applicant adopts following three kinds of coupling agents to be coated with the shop mode in experimentation and compares experiment:
Mode 1: directly brush coupling agent at glass surface;
Mode 2: coupling agent is diluted to 2% alcoholic solution, brushes at glass surface;
Mode 3: be evaporation under 80 ℃ the condition in heating-up temperature, make the coupling agent volatilization, form skim at glass surface, the evaporation time is 2h.
Aforesaid way all carries out aftertreatment after being coated with the shop, and aftertreatment is to toast 40min under 120 ℃ condition.Lines with 200 μ m experimentize, and the anti-etching time of result is as follows: mode 1 is 25min, and mode 2 is 50min, and mode 3 is 90min.
Analyze its reason and be mode 3 with respect to preceding dual mode, the coupling agent of evaporation is thinner more even.So the applicant is in the mode of selecting evaporation and carried out further optimization experiment.In the experiment, considering evaporation temperature and evaporation time two factors, is that target is optimized to prolong anti-etching time.Experiment is found, anti-etching time increases along with the prolongation of evaporation time, opposite tendency then appears behind certain hour, this behavior explains is as follows: the evaporation time is too short, and then coupling agent layer is even inadequately, only can increase the thickness of coupling agent layer but after obtaining uniform coupling agent thin layer, increase the evaporation time again, make the easier erosion of suffering etching liquid in its etching process, so anti-etching time is carved with a peak value when certain evaporation, the evaporation time is oversize or too short anti-etching time is shortened.Peak of curve during 80 ℃ of evaporations reaches 125min apparently higher than the two other peak of curve, and 80 ℃ of coupling agent thin layers that more help obtaining even compact are described.So evaporation coupling agent technology is optimized at last among the present invention: temperature is 80 ℃, and the evaporation time is 30min, carries out aftertreatment behind the evaporation, and post-processing approach is to toast 40min under 120 ℃ of conditions.Fig. 3 a is the etching figure cross section profile before the coupling agent evaporation process is optimized, and Fig. 3 b is the comparison diagram after optimizing, and optimizes back undercutting rate and is reduced to 0.6, and the etching graphics shape is comparatively desirable, can satisfy the needs that impression block is made.
Among the present invention,, as the etching liquid adjuvant, improved the etching surface quality with HCl in order to satisfy the requirement of the easy demoulding of imprint process.When not adding HCl in the etching liquid, etching surface is too coarse, is difficult to satisfy the requirement of imprint process to the impression block surface quality.This is because in etching process, the indissoluble electrodeposition substance that the reaction of part composition and etching liquid generates in the glass plays etching mask at glass surface to the glass below it, thereby forms the uneven of etching surface, and the etching surface quality is descended.In order to address this is that, in etching liquid, add the HCL of 0.5mol/L, by the CaF of reaction with indissoluble
2And MgF
2Change the CaCL that is separately converted to Yi Rong
2And MgCL
2, avoid the etching mask effect of etching product, the etching surface roughness is obviously reduced.Fig. 4 a and Fig. 4 b are that the etching result who adds the HCl front and back contrasts photo, and as can be seen, the etching surface quality is significantly improved behind the adding hydrochloric acid, and the etching edge contour is also more clear simultaneously.
Among the present invention, adopt thickening bondline technology, bondline thickness is 60 μ m, has eliminated the etching defect of glass surface.Owing to exist micro-bubble inevitably in the photoresist, when glue-line was too thin, the existence of minute bubbles just destroyed etching mask easily, and at this moment, etching liquid will be penetrated into glass surface and corrode glass, finally produces etching defect.After bondline thickness increased, the micro-bubble of stochastic distribution was difficult to destroy etching mask, thereby eliminated the etching defect that bubble brings.In addition, when glass surface has dust granule to pollute, if bondline thickness less than particle diameter, etching liquid will infiltrate the etching glass surface along the position at particulate place in the etching process, thereby forms etching defect.This problem can be solved by the clean level that improves the etching environment, pollutes but thickening bondline can cover bigger surface particle, reduces the requirement to the process environments condition, thereby reduces cost.Fig. 5 a and Fig. 5 b adopt the etching result before and after the thick adhesive process to contrast photo, adopt thick adhesive process after, eliminated the defective of surface etch.
The different size that Fig. 6 makes for the technology that adopts among the present invention, the impression block example of different graphic height, the height of Fig. 6 a middle gear is about 10 μ m, and the gear height among Fig. 6 b is about 15 μ m, and the height of Fig. 6 c middle gear is about 20 μ m.The middle circle bore dia of Fig. 6 a middle gear is 100 μ m, and as can be seen from the figure, etching result is intact, illustrates that it is the ability of the impression block of 100 μ m that technology of the present invention possesses the pattern character size of making.
Claims (3)
1. one kind based on wet etching MEMS impression block manufacturing process, it is characterized in that this technology may further comprise the steps:
1) base material cleaning step, base material is the glass of microslide material, at first cleans glass with acetone, and then uses distilled water flushing, the glass after the flushing is inserted and is soaked 10min in the concentrated sulphuric acid; Use distilled water flushing after the taking-up again, under 100 ℃ of conditions, dry 10min then, remove dirt on glass;
2) evaporation coupling agent and evaporation post-processing step are under 80 ℃ the condition in temperature with the glass after cleaning, evaporation 30min, and under 120 ℃ of conditions, baking 40min is at the coupling agent thin layer that obtains even compact on glass then;
3) be coated with shop photoresist step, with single-layer lithography glue as etching mask, the mode of employing spin coating is carried out the shop that is coated with of photoresist, photoresist layer thickness is 60 μ m, its photoresist contains the following weight ratio raw material: epoxy acrylate 40～60%, one tripropylene glycol diacrylate 9～15% that contracts, tristane diacrylate methyl ester 20～45%, the basic phenyl ketone 3% of 1-hydroxyl, organic alkane coupling agent KH-570,0.5～1%, organic pure defoamer 0.5～1%, organic alkane levelling agent 1%, the summation of raw material are 100%;
4) step of exposure as exposed mask, is placed the transparent antiseize membrane of perfluoroethylene-propylene with the sensitive film of high-resolution laser film setter output between photoresist and exposed mask, expose with exposure machine then;
5) development step is developed as developer solution with absolute ethyl alcohol, and development time is 15s;
6) regelate step, the back of developing is the ultraviolet high-pressure mercury lamps irradiation 2min of 500W with power, makes the photoresist full solidification;
7) etch step, etching are to carry out under the ultrasonic agitation environment, and the composition of etching agent is: HF:NH
4F:HCL=0.5mol/L:0.75mol/L:0.5mol/L; Etching temperature is 25 ℃; Etch rate is 0.5 μ m/min;
8) technology of removing photoresist is inserted glass in the supersonic wave cleaning machine, and is heated to 100 ℃, removes the individual layer negative photoresist, promptly obtains impression block.
2. the method for claim 1 is characterized in that, described base material is various inorganic glass materials.
3. the method for claim 1 is characterized in that, in etch step, removes hydrochloric acid in the composition of etching agent, and its etch rate is 0.4 μ m/min; The composition of the etching agent of this moment is HF:NH
4F:=0.5mol/L:0.75mol/L.
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| US8623231B2 (en) * | 2008-06-11 | 2014-01-07 | Taiwan Semiconductor Manufacturing Company, Ltd. | Method for etching an ultra thin film |
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| WO2018053800A1 (en) * | 2016-09-23 | 2018-03-29 | 中国科学院深圳先进技术研究院 | Integrated micro-molding method for photomask |
| TWI766947B (en) * | 2017-02-16 | 2022-06-11 | 美商康寧公司 | Methods of making a glass article with a structured surface |
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| US11186518B2 (en) * | 2017-02-16 | 2021-11-30 | Corning Incorporated | Methods of making a glass article with a structured surface |
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| CN110083015A (en) * | 2019-04-08 | 2019-08-02 | 深圳市华星光电技术有限公司 | Improve the method for light resistance adhesive force |
| CN111977611B (en) * | 2020-08-31 | 2022-06-14 | 大连理工大学 | Manufacturing method of micro-nano cross-scale polymer spray needle |
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