CN1195981C - Low vacunm bonding method of polydimethylsiloxane chip - Google Patents
Low vacunm bonding method of polydimethylsiloxane chip Download PDFInfo
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- CN1195981C CN1195981C CN 03130857 CN03130857A CN1195981C CN 1195981 C CN1195981 C CN 1195981C CN 03130857 CN03130857 CN 03130857 CN 03130857 A CN03130857 A CN 03130857A CN 1195981 C CN1195981 C CN 1195981C
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Abstract
The present invention relates to a low-vacuum bonding method of a polydimethyl siloxane chip. The method comprises the steps that a fresh polymerized silicon rubber sample is stripped to obtain a chip assembly; the chip assembly is placed in a vacuum chamber, and air is pumped to obtain vacuum; the vacuum chamber is repeatedly flushed by air to exhaust residue gases; the air is pumped again to form vacuum; the vacuum chamber is pressurized so that the oxygen in the vacuum chamber starts glowing; oxygen plasma bombardment is carried out on the surface of the chip assembly; the pressure in the vacuum chamber is balanced with the atmospheric pressure; the vacuum chamber is opened, and the chip assembly treated by the oxygen plasma is pasted. The polydimethyl siloxane chip has high bonding intensity, and verified by a pulling force experiment, the intensity of the polydimethyl siloxane chip can exceed the intensity of the PDMS main body. The present invention has the advantages of simple equipment, low requirement for vacuum degree, short air pumping and exhausting time and high efficiency.
Description
(1) technical field
The present invention relates to a kind of low vacuum bonding method, especially a kind of polydimethylsiloxanechip chip low vacuum bonding method.
(2) background technology
Micro-fluidic chip (microfluidic chip) has a wide range of applications at analytic system, biological medicine, chemistry and biochemical field.Traditional micro-fluidic chip has been continued to use the IC industrial technology, mainly is as material with silicon and glass; Thereby must be through making the series of process processes such as etching of mask, photoetching, microchannel, complex manufacturing technology, the cycle is long, efficient is lower, and its sidewall of the microfluidic channel that etches on this hard material is difficult to accomplish not only smooth but also steep.Yet with the high molecular polymer is the material micro-fluidic chip, can overcome above difficulty, thereby realizes low-costly and in high volume, high efficiency manufacture craft.This wherein is most widely used with dimethyl silicone polymer (PDMS) especially, because it has following advantage: 1) can realize by the method for model copy producing in batches; 2) it self very transparent, can be applicable to many pick-up units (UV, visible light absorb and fluorescence etc.); 3) cold polymerization (65 ℃); 4) nontoxic, biologically inert can be directly used in biological sample; 5) the reversible deformation of energy; 6) can be reversibly and self and other many material bondings, also can realize irreversible bonding by oxygen plasma treatment; 7) but the surface chemistry people for controlling; 8) good springiness, applicable to smooth, non-planar surfaces, and when it can not damage substrate and self during the demoulding from complex model, thereby can realize constructing of complete microfluidic channel.
A common micro-fluidic chip is formed to form the microfluidic channel of sealing by bonding by two or two above wafer assemblies.Bonding is a step crucial in the entire chip manufacture craft process, because have only the complete seal that realizes microfluidic channels in the chip by good bonding techniques, whole micro-fluid chip just has the value of use.PDMS chip bonding mode commonly used at present has: reversible keying and irreversible bonding two big classes.One of great advantage of reversible keying is reusable, but the intensity of bonding is lower, in use the phenomenon of leakage can occur.The bond strength of irreversible bonding is very big, can surpass the intensity of its body, thereby can realize the complete sealing of chip.Irreversible bonding method commonly used is with oxygen plasma treatment PDMS surface, promptly the chip assembly thin slice is placed the oxygen plasma generation device of high vacuum, bombard sheet surface with oxygen plasma, directly two plate sheets are fitted then, just can realize the bonding of irreversible degree, form complete micro-fluidic chip (referring to 1.David C.Duffy, J.Copper McDonald, Oliver J.A.Schueller, George M.Whitesides Anal.Chem1998,70:4974-4984; 2.J.Copper McDonald, David C.Duffy, Janelle R.Anderson, DanielT.Chiu, Hongkai Wu, Oliver J.A.Schueller, George M.Whitesides Electrophoresis2000,21:27-40; 3.Xiaomei Yu, Dacheng Zhang, Xiang Wang, Ting Li, Xiuhan Li MEMS2002 Workshop Digest 2002:741-744.)。Also have adopt the ultraviolet irradiation chip carry out irreversible bonding report (Meng Fei, Chen Hengwu, Fang Qun, etc., SCI, 2002,7:1264-1268).But this method need be shone the long time (general several hrs), and can not realize irreversible bonding soon after the irradiation, must place long time.
About the irreversible bonding techniques with oxygen plasma treatment PDMS chip, the system vacuum degree of all having relatively high expectations to remove the foreign gas in the vacuum chamber, guarantees that the purity of oxygen and the branch of control oxygen are pressed in the Pa order of magnitude at present.Therefore the integral body to equipment requires than higher, and common laboratory is difficult to realize.And the time of general oxygen plasma treatment is 40～60s, and it is higher that chip is heated up, and destroys the surface chemistry composition of chip easily, and the performance of some chips is impacted.
(3) summary of the invention
The present invention aims to provide simple, cheap, the irreversible bonding method of low vacuum of dimethyl silicone polymer (PDMS) chip efficiently of a kind of technology.
Said bonding method is:
1, with fresh the peeling off of silicon rubber sample after the polymerization, obtains the PDMS chip assembly;
2, the fresh PDMS chip assembly of peeling off is put into vacuum chamber, being evacuated down to vacuum tightness (base vacuum degree) is 13.3～39.9Pa;
3, wash vacuum chamber repeatedly at least 2 times with oxygen, the residual gas in the described vacuum chamber is discharged;
4, close Oxygen Flow, it is 13.3～39.9Pa that vacuum chamber is evacuated down to vacuum tightness (oxygen pressure);
5, add high pressure and make oxygen build-up of luminance in the vacuum chamber, the oxygen plasma bombardment is carried out on PDMS chip assembly surface;
6, bombardment finishes and promptly opens air release, to the vacuum interacvity air-filling until with the atmospheric pressure balance, open vacuum chamber, will be through on-the-spot applying of the good PDMS chip assembly of oxygen plasma treatment;
7, applying back insulation.
The voltage that the PDMS chip surface is carried out the oxygen plasma bombardment is preferably 1400～2000V, and bombardment time is preferably 5～40s.
Holding temperature after the PDMS chip is fitted is preferably 80～150 ℃, and temperature retention time is 1h at least preferably.
Bonding mechanism of the present invention is described as follows: before oxygen plasma treatment, the PDMS surface mainly is-Si (CH
3)
3Form exist; And after oxygen plasma treatment, its surface has produced a large amount of Si-OH keys.Therefore after handling the on-the-spot applying of back PDMS chip, handling, just can between two chips, produce a large amount of Si-O-Si keys, thereby realize the irreversible bonding of chip through the uniform temperature insulation.
Experiment showed, 1) adopt the good chip bonding intensity of bonding of the present invention very high, to measure through pulling experiment, it has surpassed the intensity of PDMS body.
2) instrument and equipment of the present invention's use is simple:
A. the vacuum tightness of this technical requirement is lower, 0.1～0.3Torr only, thus just can realize with the logical vacuum oil pump (final vacuum is about 0.1Pa) of a Daepori, simultaneously just owing to this, it requires also just very low to whole vacuum system, just can realize in a common annular seal space; If by the document of being given in the above-mentioned background technology (1.David C.Duffy, J.CopperMcDonald, Oliver J.A.Schueller, George M.Whitesides Anal.Chem 1998,70:4974-4984; 2.J.Copper McDonald, David C.Duffy, Janelle R.Anderson, Daniel T.Chiu, Hongkai Wu, Oliver J.A.Schueller, George M.Whitesides Electrophoresis2000,21:27-40; 3.Xiaomei Yu, Dacheng Zhang, Xiang Wang, Ting Li, Xiuhan Li MEMS2002 Workshop Digest 2002:741-744.) requirement, reach the Pa order of magnitude, then need expensive diffusion pump or molecular pump equal vacuum pump (referring to Xu Chenghai, etc., vacuum and low temperature technology and equipment, Beijing: metallurgical industry publishing house, 1995:21), and need complicated vacuum seal system, the cost of entire equipment will tenfold growth, so report uses in the document all is more valuable plasma production device.
B. adopt pure oxygen to wash vacuum chamber repeatedly and gas is extracted out, make the concentration of other residual gas in the vacuum chamber reduce significantly, just reached and adopted the same effect of high vacuum system by pump.
C. this technology pumpdown time, deflation time are all very short, have improved efficient on the one hand, also more help bonding on the other hand.Because not long with the time of keeping after air contacts,, just help bonding more so the short more PDMS surfactivity of deflation time is strong more through the PDMS surface active state after the oxygen plasma treatment.
In sum, the invention provides a kind of simple, cheap, bonding method of PDMS chip efficiently.In an embodiment with the present invention is further illustrated.
(4) description of drawings
Fig. 1 is PDMS chip profile scanning electron microscope (SEM) figure behind the bonding.
Fig. 2 is microchannel profile scanning electron microscope (SEM) figure of not bonding.
Fig. 3 is microchannel profile scanning electron microscope (SEM) figure behind the bonding.
(5) embodiment
Embodiment 1:
Pour silastic material into the chip mould, fresh peeling off after the polymerization obtains the PDMS chip assembly, puts it into vacuum chamber, and the base vacuum degree that vacuumizes up to the chamber is 26.6Pa; Wash repeatedly 3 times with oxygen, discharge residual gas, close Oxygen Flow, vacuumize (being oxygen pressure) again to 39.9Pa, the 1400V that adds high pressure (electric current is 220mA) makes oxygen build-up of luminance in the chamber, the PDMS chip surface is carried out the oxygen plasma bombardment, and the time is 40s; Open air release, in vacuum chamber, be inflated to and the atmospheric pressure balance, open vacuum chamber again, chip is fitted, be incubated 2h down, promptly realize irreversible bonding at 100 ℃.
After oxygen plasma treatment, the PDMS chip surface has very strong water wettability, and its contact angle approaches 0 °, but the variation gradually of prolongation water wettability in time almost returns to the state before being untreated behind about 30～60min.
Realize behind the irreversible bonding the section situation as shown in Figure 1.As can be seen from Figure 1, the PDMS chip assembly combination that bonding is good is very tight, do not have any small crack between two assemblies, even scanning electron microscope (SEM) can not be found sharp interface down.
The sealing situation of microfluidic channel is seen Fig. 2,3 before and after the bonding.
In Fig. 3, do not see in passage bonding side outer rim behind the bonding and do not arrive tangible bonded interface vestige, therefore, the method can obtain the good microfluidic channel of sealing.
Embodiment 2:
Pour silastic material into the chip mould, fresh peeling off after the polymerization obtains the PDMS chip assembly, puts it into vacuum chamber, and the base vacuum degree that vacuumizes up to the chamber is 19.95Pa; Wash repeatedly 2 times with oxygen, discharge residual gas, close Oxygen Flow, vacuumize (being oxygen pressure) again to 33.25Pa, the 2000V that adds high pressure (electric current is 380mA) makes oxygen build-up of luminance in the chamber, the PDMS chip surface is carried out the oxygen plasma bombardment, and the time is 5s; Open air release, in vacuum chamber, be inflated to and the atmospheric pressure balance, open vacuum chamber again, chip is fitted, be incubated 1.5h down, promptly realize irreversible bonding at 120 ℃.
After oxygen plasma treatment, the PDMS chip surface has very strong water wettability, and its contact angle approaches 0 °, but the variation gradually of prolongation water wettability in time almost returns to the state before being untreated behind about 30～60min.
Embodiment 3～10:
Its bonding method similar embodiment 1,2, its experiment condition is as shown in the table:
| Embodiment | Base vacuum degree/Pa | Oxygen pressure/Pa | Time/Sec | Voltage/V | Electric current/mA |
| 3 | 26.6 | 26.2 | 35 | 1400 | 220 |
| 4 | 39.9 | 13.1 | 40 | 1500 | 245 |
| 5 | 33.25 | 33.25 | 30 | 1500 | 245 |
| 6 | 39.9 | 19.95 | 25 | 1400 | 220 |
| 7 | 13.3 | 26.6 | 40 | 1400 | 220 |
| 8 | 26.6 | 39.9 | 5 | 2000 | 380 |
| 9 | 19.95 | 26.6 | 15 | 2000 | 380 |
| 10 | 39.9 | 39.9 | 30 | 1600 | 240 |
Experiment shows, the water wettability of the PDMS chip of crossing through oxygen plasma treatment all is greatly improved, and water droplet can spread out (contact angle is near 0 °) rapidly on the PDMS surface
Claims (5)
1, polydimethylsiloxanechip chip low vacuum bonding method is characterized in that the steps include:
1), with fresh the peeling off of silicon rubber sample after the polymerization, obtain the PDMS chip assembly;
2), the fresh PDMS chip assembly of peeling off is put into vacuum chamber, being evacuated down to the base vacuum degree is 13.3～39.9Pa;
3), wash vacuum chamber repeatedly at least 2 times, the residual gas in the described vacuum chamber is discharged with oxygen;
4), close Oxygen Flow, it is 13.3～39.9Pa that vacuum chamber is evacuated down to oxygen pressure;
5), adding high pressure makes the interior oxygen build-up of luminance of vacuum chamber, and the oxygen plasma bombardment is carried out on PDMS chip assembly surface;
6), bombardment finishes and opens air release immediately, to the vacuum interacvity air-filling until with the atmospheric pressure balance; Open vacuum chamber, will be through on-the-spot applying of the good PDMS chip assembly of oxygen plasma treatment;
7), applying back insulation.
2, polydimethylsiloxanechip chip low vacuum bonding method as claimed in claim 1, the voltage that it is characterized in that the PDMS chip surface is carried out oxygen plasma bombardment is 1400～2000V.
3, polydimethylsiloxanechip chip low vacuum bonding method as claimed in claim 1 or 2, the time that it is characterized in that the PDMS chip surface is carried out oxygen plasma bombardment is 5～40s.
4, polydimethylsiloxanechip chip low vacuum bonding method as claimed in claim 1 is characterized in that the holding temperature after the PDMS chip is fitted is 80～150 ℃.
5,, it is characterized in that the temperature retention time 1h at least after the PDMS chip is fitted as claim 1 or 4 described polydimethylsiloxanechip chip low vacuum bonding methods.
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| CN 03130857 CN1195981C (en) | 2003-05-15 | 2003-05-15 | Low vacunm bonding method of polydimethylsiloxane chip |
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102276862A (en) * | 2011-04-28 | 2011-12-14 | 西北工业大学 | Method for irreversibly bonding polymethyl methacrylate (PMMA) chip and polydimethylsiloxane (PDMS) chip |
| CN102701145A (en) * | 2012-05-04 | 2012-10-03 | 南京大学 | Method for irreversible bonding of high-quality polydimethylsiloxane (PDMS)-polyolefine plastics |
| CN102910578B (en) * | 2012-11-07 | 2015-11-18 | 中国科学院上海微系统与信息技术研究所 | A kind of method adopting hybrid plasma to realize silicon base chip and PDMS chip bonding |
| CN103964375B (en) * | 2013-02-01 | 2018-10-16 | 中芯国际集成电路制造(上海)有限公司 | Die bonding method |
| CN105333992B (en) * | 2014-06-27 | 2018-03-30 | 中芯国际集成电路制造(上海)有限公司 | A kind of method for measuring the vacuum in bonding chamber |
| CN104607256A (en) * | 2014-12-31 | 2015-05-13 | 北京同方生物芯片技术有限公司 | Plasma auxiliary thermo-compression bonding micro-fluidic chip and preparation method thereof |
| CN106959269B (en) * | 2017-03-29 | 2020-07-31 | 天津大学 | Simplified chip bonding strength measuring device and method |
| CN107014691B (en) * | 2017-04-01 | 2020-09-01 | 天津大学 | Device and method for measuring bonding strength of chip |
| CN108162368A (en) * | 2017-12-27 | 2018-06-15 | 北京百奥芯科技有限公司 | A kind of thermal bonding method of control plastic chip and the chip obtained |
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