CN1295508C - Low temperature binding method for glass microflow control chip - Google Patents
Low temperature binding method for glass microflow control chip Download PDFInfo
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- CN1295508C CN1295508C CNB2005100238947A CN200510023894A CN1295508C CN 1295508 C CN1295508 C CN 1295508C CN B2005100238947 A CNB2005100238947 A CN B2005100238947A CN 200510023894 A CN200510023894 A CN 200510023894A CN 1295508 C CN1295508 C CN 1295508C
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- bonding
- deionized water
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- vacuum
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Abstract
The present invention relates to a low temperature bonding method for microflow control glass chips, which specifically comprises the steps: (1) cleaning the surface of a substrate after corresponding figures are etched and a liquid storage tank is drilled; (2) bonding the substrate in advance by the method that after the cleaned substrate and a cover sheet are flushed by deionized water, the bonding faces of the substrate and the cover sheet are directly stuck in the deionized water, then are conveyed to a culture container, is put into a vacuum drying box with the drying temperature of 90 DEG C to 110 DEG C, are implemented with vacuum pumping so that the vacuum degree is 60 Pa to 90 Pa, and thus, the substrate is bonded in advance after the vacuum state is kept for two hours; (3) annealing after the is bonded in advance so as to improve bond strength by the method that the pressure of 0.2MPa to 0.4MPa is applied to the pre-bonded substrate, the temperature in the vacuum drying box is simultaneously set to 180 DEG C to 210 DEG C, the vacuum is pumped until the vacuum degree is from 60 Pa to 90 Pa, the power supply is cut off after keeping for 6 hours, the substrate is naturally cooled to room temperature. The bonding process is completed under a non-purification condition so that the pre-bonded substrate can be bonded and annealed at high temperature by applying certain pressure to the vacuum drying box.
Description
Technical field
The present invention relates to a kind of low-temperature bonding method for making of glass micro-fluidic chips, belong to the Micrometer-Nanometer Processing Technology field.
Background technology
Micro-total analysis system (Micro Total Analysis Systems, μ TAS) is the new research direction of the multidisciplinary intersection that grows up in the analytical chemistry field nineties in last century, it is with microelectromechanical systems (microelectromechanical systems, MEMS) be the basis, with life science is main research object, design and process the various microchannel networks of suitable biochemical analysis on the substrate of different materials, the chip that is used for this purpose often is called micro-fluidic chip.The material of making micro-fluidic chip is a lot, comprises polymkeric substance such as silicon, quartz, simple glass and PDMS, SU-8, and glass (comprising quartz and simple glass) is because its good optical characteristics is used more in the research of micro-fluidic chip.For the making of glass micro-fluidic chips, relate to many MEMS processing and making process and method, comprise steps such as photoetching, corrosion and bonding.As the final step of chip manufacturing, the quality of bonding effect has directly determined the success or failure of chip manufacturing.
Traditional bonding method, as thermal bonding, anode linkage etc., the whole process need of bonding is finished in the decontamination chamber, surface treatment before the chip bonding can be finished at the Clean room of lower grade, processes such as pre-bonding of chip and chip annealing bonding then need the purification condition of requirements at the higher level, and the annealing of bonding needs at high temperature just can finish.The annealing of high temperature, the expansion coefficient of slice, thin piece should be consistent about just requiring, otherwise at high temperature owing to non-homogeneous expansion, and cause the bonding failure.Development in recent years the low temperature or the room temperature bonding techniques of a lot of glass, as [1] H.Y.Wang such as Wang, R.S.Foote, S.C.Jacobson, J.H.Schneibe, J.M.Ramsey, Low temperature bonding for microfabrication ofchemical analysis devices, Sensors and Actuators B 45 (1997) 199-207. utilize sodium silicate to do bonding coat, low-temperature bonding under realizing 100 ℃, Nakanishi etc. [2] H.Nakanishi, T.Nishimoto, R.Nakamura, A.Yotsumoto, T.Yoshida, S.Shoji, Studies on SiO2-SiO2 bonding with hydrofluoric acid.Room temperature and low stressbonding technique for MEMS, Sensors and Actuators A 79 2000 237-244. utilize HF acid, realized room temperature lower-glass bonding, but the needed bonding conditions of these methods is all strict, need carry out at Clean room.The former sodium silicate is made the bonding coat bonding and has been changed the inner-walls of duct pattern, and the pipeline latch up phenomenon easily takes place, and latter's bonding needs strict HF acid concentration and pressure, and HF acid has strong corrosive attack to glass, and perviousness is strong.SUSS company has succeeded in developing a kind of low-temperature bonding instrument recently, can realize the bonding of multiple material, as Si-Si, and Si-SiO
2And SiO
2-SiO
2Deng bonding.But bonding process necessarily requires to finish in super-clean environment, and the preprocessing process that bonding surface need be special, as million cleanings, and infrared oven dry etc., these all need special device, the instrument costliness, common laboratory can't be born.
Summary of the invention
The object of the invention is to solve above-mentioned bonding method weak point, has proposed a kind of simple, the glass-chip low-temperature bonding method that can finish in common laboratory.This bonding is permanent bonding, and bond strength satisfies requirement of experiment fully, and this bonding method is bonded to the power height, can reach more than 95%.
For realizing that the technology that purpose of the present invention need solve is, 1, finish the preprocessing process such as strictness cleaning of substrate surface, better activate bonding surface, increase the surface-OH; 2, finish the pre-bonding process of chip in the laboratory of non-purification condition; 3, finish annealing process in the laboratory of non-purification condition, improve bond strength, realize the permanent bonding of substrate.
The low-temperature bonding method of glass micro chip provided by the invention is to use acetone, ethanol, Piranha washing lotion (H at first respectively
2SO
4: H
2O
2), RCA1, RCA2, the affine liquid of ammoniacal liquor hots plate, the substrate bonding surface is finished in immersion etc. strictness cleans, after in deionized water, fitting then, directly transfer to and realize the pre-bonding of substrate in the vacuum drying chamber; Behind the pre-bonding, in vacuum drying chamber, finish the bond anneal process adding certain pressure on the substrate, thereby improve bond strength.
Specifically, it is a kind of simple that this method provides, and is fit to the glass-chip low-temperature bonding technology of common lab.Be characterised in that specifically whole bonding process relates to following steps:
1 substrate bonding surface is strict to be cleaned, and increases surperficial compatibility by the affine liquid of ammoniacal liquor;
2 do not need to carry out the substrate oven dry, directly in deionized water cleaned substrate are fit together, to avoid the influence of dust granule para-linkage in the air.Transfer to then in the vacuum drying chamber, carry out pre-bonding;
After 3 pre-bondings are good, give the substrate plus-pressure, rising vacuum drying chamber temperature is carried out the chip annealing process, improves bond strength.
The concrete composition of described Piranha washing lotion is H
2SO
4/ H
2O
2Volume ratio be 4: 1, hotted plate 8-15 minute, after the cooling, use the deionized water rinse substrate;
Described RCA1 cleans, and purpose is to remove the insoluble organism on bonding face surface, and concrete proportioning is volume ratio NH
3H
2O: H
2O
2: H
2O=1: 1: 5; Be heated to boiling, continue heating 3-7 minute; Pour out the RCA1 washing lotion, wash down with deionized water again;
Described RCA2 cleaning fluid cleans, and purpose is to remove bonding surface ion and heavy metal atom dirt, and proportioning is HCl: H
2O
2: H
2O=1: 1: 5, be heated to the continuation heating of boiling back and pour out after 3-7 minute, use washed with de-ionized water;
Described ammoniacal liquor is affine, and liquid cleaning purpose is to increase surface-OH, improves the bonding compatibility, and concrete proportioning is NH
3H
2O: H
2O
2: H
2O=6: 3: 1, be heated to boiling, be incubated 20-40 minute, pour out affine liquid after the cooling.
Vacuum tightness is 60-90Pa during pre-bonding, finishes pre-bonding under the condition in following 2 hours for 90-110 ℃, and pre-bonding after annealing condition is that vacuum tightness is 60-90Pa, apply 0.2-0.4Mpa pressure 180-210 ℃ down annealing finished the chip low-temperature bonding in 6 hours.
The present invention has the following advantages and effect:
[1] bonding process can be finished in the common laboratory of non-purification condition, after the strict cleaning of chip, increases bonding surface-OH by the affine solution of ammoniacal liquor, improves to show compatibility, improves to be bonded to power in advance;
[2] need not oven dry and handle, be placed in the surface plate after directly in deionized water, substrate being fitted, in vacuum drying chamber, finish the pre-bonding of chip under the vacuum state;
[3] behind the pre-bonding of substrate, need not in high temperature sintering furnace, control the intensification cooling rate of temperature in the stove to finish high annealing by strictness, only need to exert pressure to substrate, in 200 ℃ vacuum drying chamber, finish chip annealing then under the vacuum state, realize the substrate bonding process, make chip;
[4] the whole low-temperature bonding process of substrate can be finished at Routine Test Lab, and the para-linkage environmental requirement is low, need not special bonding instrument, the bonding cost is low, and the chip that bonding is good is used for biological sample analysis, under high electric field, current stabilization, chip bonding intensity satisfies requirement of experiment fully.
Description of drawings
Fig. 1 is the pre-bonding front surface of chip provided by the invention cleaning process figure:
A) acetone ethanol ultrasonic cleaning
B) the Piranha washing lotion is hotted plate
C) RCA1 (NH
3H
2O: H
2O
2: H
2O=1: 1: 5) cleans
D) RCA2 (concentrated hydrochloric acid: H
2O
2: H
2O=1: 1: 5) cleans
E) the affine solution of ammoniacal liquor is hotted plate, is soaked
Fig. 2 be the pre-bonding of chip provided by the invention well after, in chip surface pressurization, and in vacuum drying chamber, anneal; Wherein: 1 surperficial compression aspect; 2 cover plates; 3 substrates; The 4 chips quartzy cushion block that pressurizes; The microchannel that corrodes on 5 substrates
Embodiment
Pass through specific embodiment: Capillary Electrophoresis microchip low-temperature bonding method, further set forth quartz provided by the present invention or glass-chip low-temperature bonding method.The present invention includes three parts:
1, the strict pretreating process that cleans of substrate bonding surface
2, the pre-bonding of substrate
3, the substrate process annealing realizes bonding
The flatness of substrate bonding surface, cleanliness and affine degree directly determine the success ratio height of bonding.The substrate bonding surface is carried out strictness clean, increase surperficial compatibility, to improve the success ratio of the pre-bonding of chip by suitable mode.
Embodiment 1 substrate carries out following concrete surface clean process after eroding away respective graphical and finishing the perforation processing of liquid storage tank:
1) at first uses deionized water rinse substrate 5min, use each ultrasonic cleaning 5min of acetone and ethanol then respectively, prepare the substrate 5min of bonding after the ultrasonic cleaning again with deionized water rinsing;
2) substrate is put into Piranha washing lotion (volume ratio H
2SO
4: H
2O
2=4: 1), hot plate 10min, pour out the Piranha washing lotion after the cooling, with deionized water rinse substrate 5min;
3) clean with a liquid RCA1, remove the insoluble organism in bonding face surface.No. one the concrete proportioning of liquid is volume ratio NH
3H
2O: H
2O
2: H
2O=1: 1: 5, heat a liquid RCA1 up to boiling, RCA1 is poured out, then deionized water rinsing 5min after continuing heating 5min in the boiling back;
4) clean with No. two liquid RCA2, remove bonding face surface ion and some heavy metal atom dirts etc.No. two the concrete proportioning of liquid is volume ratio HCl: H
2O
2: H
2O=1: 1: 5, heating was up to boiling, and RCA2 is poured out, then deionized water rinsing 5min after continuing heating 5min in the boiling back;
5) utilize the affine solution of ammoniacal liquor to hot plate substrate, improve the bonding surface compatibility to increase surface-OH.The concrete proportioning of the affine solution of ammoniacal liquor is volume ratio NH
3H
2O: H
2O: H
2O
2=6: 3: 1, the affine solution of heating ammoniacal liquor was up to boiling, and insulation heating 30min after the cooling, pours out affine liquid;
6) the pre-bonding of substrate.Behind deionized water rinse substrate and cover plate 10min, directly in deionized water, the bonding face of substrate and cover plate is fit together, transfer in the double dish, be placed in the vacuum drying chamber then.The vacuum drying chamber temperature is set at 100 ℃, vacuumizes to make vacuum tightness reach 70Pa and keep vacuum 2h to finish the pre-bonding of substrate;
7) the pre-bonding after annealing of substrate improves bond strength.On the good substrate of pre-bonding, add a mass to apply 0.2MPa pressure to substrate, the temperature of vacuum drying chamber is set at 180 ℃, vacuumize make vacuum tightness reach 80Pa and keep 6h after powered-down, naturally cool to room temperature, finish annealing process, the low-temperature bonding process is finished.This moment, bond strength increased, can't separate chip, and chip is permanent bonding.
Embodiment 2
Step 2 time of hotting plate is 15 minutes among the embodiment 1, bonding post-flush 7 minutes; Heating is 7 minutes in the step 3,4, and pouring out respectively and washing down the time after RCA1 and the RCA2 washing lotion is 5 minutes.
The pre-bonding vacuum tightness of low temperature is 90Pa, 110 ℃ of bonding temperatures, and the time still is 2 hours, and the vacuum tightness during pre-bonding after annealing is 65Pa, and pressure is 0.4MPa, and temperature is 210 ℃.All the other are with embodiment 1.
Claims (3)
1. the low-temperature bonding method of a glass micro-fluidic chips is characterized in that may further comprise the steps:
(1) substrate carries out surface clean after eroding away respective graphical and finishing the liquid storage tank perforation processing, uses the affine liquid surface clean of acetone, ethanol, Piranha washing lotion, RCA1, RCA2 and ammoniacal liquor successively, needs to wash out cleaning fluid with deionized water after each the cleaning;
(2) the pre-bonding of substrate, substrate after step (1) cleaned and cover plate with deionized water rinsing after, directly in deionized water, the bonding face of substrate and cover plate is fit together, transfer in the double dish, be placed in the vacuum drying chamber then, baking temperature is 90-110 ℃, vacuumizes to make vacuum tightness reach 60-90Pa and keep vacuum 2h to finish the pre-bonding of substrate;
(3) the pre-bonding after annealing of substrate improves bond strength, applies the pressure of 0.2-0.4MPa on the good substrate of pre-bonding, temperature with vacuum drying chamber is set at 180-210 ℃ simultaneously, vacuumizing vacuum tightness is powered-down behind the 60-90Pa maintenance 6h, naturally cools to room temperature, finishes annealing process.
2. by the low-temperature bonding method of the described glass micro-fluidic chips of claim 1, it is characterized in that the substrate surface cleaning step is successively:
(1) at first uses deionized water rinse substrate 5min, use each ultrasonic cleaning 5min of acetone and ethanol then respectively, prepare the substrate 5min of bonding after the ultrasonic cleaning again with deionized water rinsing;
(2) substrate is put into H
2SO
4: H
2O
2Volume ratio is 4: 1 a Piranha washing lotion, hots plate 8-15min, pours out the Piranha washing lotion after the cooling, with deionized water rinse substrate 5min;
(3) clean with the RCA1 cleaning fluid, remove the insoluble organism in bonding face surface; Concrete proportioning is volume ratio NH
3H
2O: H
2O
2: H
2O=1: 1: 5, RCA1 was up to boiling in heating, and the RCA1 cleaning fluid is poured out, then deionized water rinsing 5min after continuing heating 3-7min in the boiling back;
(4) clean with the RCA2 cleaning fluid, remove bonding face surface ion and some heavy metal atom dirts; Concrete proportioning is volume ratio HCl: H
2O
2: H
2O=1: 1: 5, heating was up to boiling, and the RCA2 cleaning fluid is poured out, then deionized water rinsing 5min after continuing heating 3-7min in the boiling back;
(5) utilize the affine solution of ammoniacal liquor to hot plate substrate, improve the bonding surface compatibility to increase surface-OH; The affine liquid of ammoniacal liquor consist of NH
3H
2O: H
2O: H
2O
2Volume ratio is 6: 3: 1, and heating is until boiling, and insulation heating 30min after the cooling, pours out the affine liquid of ammoniacal liquor.
3. by the low-temperature bonding method of the described glass micro-fluidic chips of claim 1, it is characterized in that applying of pressure is to realize by add a mass on the substrate of pre-bonding.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100238947A CN1295508C (en) | 2005-02-06 | 2005-02-06 | Low temperature binding method for glass microflow control chip |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100238947A CN1295508C (en) | 2005-02-06 | 2005-02-06 | Low temperature binding method for glass microflow control chip |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1648662A CN1648662A (en) | 2005-08-03 |
| CN1295508C true CN1295508C (en) | 2007-01-17 |
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ID=34875976
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2005100238947A Expired - Fee Related CN1295508C (en) | 2005-02-06 | 2005-02-06 | Low temperature binding method for glass microflow control chip |
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| CN100444347C (en) * | 2006-05-31 | 2008-12-17 | 中国科学院半导体研究所 | Cleaning and drying apparatus for bonding |
| CN101786799B (en) * | 2010-01-11 | 2012-07-25 | 北京航空航天大学 | Bonding method of diatom shell or kieselguhr and glass |
| CN103183310B (en) * | 2011-12-27 | 2015-08-19 | 中国科学院理化技术研究所 | A kind of method of low-temperature bonding of micro-fluidic chip |
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| CN114405562B (en) * | 2021-12-06 | 2023-04-18 | 北京保利微芯科技有限公司 | Microfluidic chip bonding device and control method thereof |
| CN114920468B (en) * | 2022-06-01 | 2023-12-05 | 北方夜视技术股份有限公司 | Borosilicate glass hydrophilic bonding method |
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