CN102627255B - Micro-nano integrated processing technology based implantable three-dimensional anti-drag micro-channel and preparation method thereof - Google Patents
Micro-nano integrated processing technology based implantable three-dimensional anti-drag micro-channel and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a micro-nano integrated processing technology based implantable three-dimensional anti-drag micro-channel and a preparation method thereof. The preparation method comprises the steps of: directly preparing a high density and high aspect ratio nano forest structure on each surface of a silicon-based micron dimension groove by utilizing DRIE (Deep Reactive Ion Etching) without mask optimization; then transferring the silicon-based micron dimension groove and the nano forest structure on the surface thereof to PDMS (Polydimethylsiloxane) by utilizing a casting mould method; then carrying out a surface physicochemical treatment on the PDMS by utilizing a DRIE post-treatment technology to reduce a surface energy, thereby realizing the PDMS three-dimensional anti-drag micro-channel with super-hydrophobic properties. The micro-nano integrated processing technology based implantable three-dimensional anti-drag micro-channel, disclosed by the invention, can improve surface to volume ratio extremely, reduce the surface energy, thereby enabling the surface of the micro-channel to have the super-hydrophobic properties, realize an excellent anti-drag effect, and further improve steady super-hydrophobic properties of the surface, thereby extremely improving the anti-drag effect thereof; and the micro-nano integrated processing technology based implantable three-dimensional anti-drag micro-channel, disclosed by the invention, has the advantages of simple technology, low cost and easy industrialization.
Description
Technical field
The present invention relates to micro-processing technology field, particularly a kind of implantable three-dimensional anti-drag micro-channel based on the integrated process technology of micro-nano and preparation method.
Background technology
MEMS (Microelectro mechanical system, MEMS) since last century, the eighties occurred, as a multi-field cross discipline that is emerging, new and high technology, be described as the new technology revolution that the new century leads microelectronic industry to develop, be subject to domestic and international extensive concern.Wherein, biomedical MEMS (Bio-medical MEMS) is as one of most important branch of MEMS, be subject to the close attention of scientific research institution and industrial circle, wherein the most noticeable is that micro-total analysis system (micro total analysi ssystems, i.e. μ TAS) also claims chip lab (Lab-on-a-chip).It sample preparation, biochemical reaction and result is detected three steps to be integrated on single device, and can perform the complete microsystem of particular analysis function, can be divided into chip type and the large class of non-chip type two.The real chip type micro-total analysis system of its development priority at present, comprise micro-array chip (Microarray Chip) and micro-fluidic chip (Microfluidic chip) two classes, there is sample detection threshold value low, highly sensitive, analysis speed is fast, advantage with low cost, realizes industrialization abroad, and the enterprise producing biochip is thousands of.
The decline core of analysis system of said chip is on substrate, use micro-processing technology to prepare groove structure, based on analytical chemistry and analytical biochemistry, realizes the real-time detection of biological sample, treatment and analysis.Its groove structure characteristic size arrives hundreds of micron tens usually, different from the groove of macro-scale, due to the impact of dimensional effect, when fluid flows in the groove structure of micro-nano magnitude, its viscosity resistance becomes very huge, make liquid flow abnormal difficult, according to Poiseuille's law, the biquadratic of pressure reduction needed for passage and size is inversely proportional to, this means that the driving of microfluid needs very large external motivating force and corresponding drive unit (usually needing the effect ability smooth outflow by external motivating force), for example Micropump, micro-valve and micro-energy etc., this brings a series of shortcoming, as complex structure, the stability of a system is low, power consumption is high, be difficult to realize microminaturization.Therefore, the fluid channel realizing having a drag-reduction effect is one of micro-total analysis system research field key scientific problems urgently to be resolved hurrily.
And due to the particularity of biomedical sector demand, implantable anti-drag micro-channel more becomes the most important thing of micro-total analysis system research, wherein modal material is dimethyl silicone polymer (i.e. Polydimethylsiloxane, is abbreviated as PDMS).It is a kind of the macromolecule organic silicon compound, and be otherwise known as organosilicon, has cost low, nontoxic, nonflammable, bio-compatibility is good, and the feature such as light transmission is excellent, therefore in technical field of micro and nano fabrication, particularly the direction such as micro-fluidic, biomedical micro-system is widely used.Although namely PDMS material itself has hydrophobicity (contact angle is about 105 °-120 °), under micro-scale, due to the remarkable enhancing of laminar flow effect, surface force and capillary effect etc., its viscosity resistance is very large.
Past, a lot of technology was developed in order to realize having the body structure surface of drag-reduction effect during the decade, comprised polymer drag reducing agent, the technology such as drag-reducing coating, biomimetic features copy, the two size granule modifications of micro-nano.Polymer drag reducing agent and drag-reducing coating [example: Choi K S, Appl Sci Res, 1989,46:209-216] be the class be most widely used, its process is simple, but this injection polymer drag reducing agent or coating drag-reducing coating form the method at drag reduction interface, and drag reducer waste is serious, service life wretched insufficiency.
Biomimetic features copies, and [example: Bechert D W, AIAA Shear Flow Control Conference, 1985] repeats out by the natural surface texture with drag-reduction effect by micro-processing technology, but its drag reduction efficiency is lower.Recent study personnel propose a kind of drag reduction runner design [example: Lu Si based on the two size granule finishing of micro-nano, Chinese science: G collects, 2010,40:916-924], can realize efficient drag-reduction effect, but realize the two size granule structure of above-mentioned micro-nano and usually need multistep complicated technology, cost is high, what is more important is difficult to realize drag reduction structures on the sidewall and end face of groove, namely cannot realize real three-dimensional anti-drag micro-channel.
Summary of the invention
In order to overcome the deficiency of prior art structure, the invention provides the implantable three-dimensional anti-drag micro-channel based on the integrated process technology of micro-nano and preparation method.
The object of the invention is to propose a kind of implantable three-dimensional anti-drag micro-channel based on the integrated process technology of micro-nano and preparation method, utilize and optimize deep reaction ion etching (DRIE) technique without mask, directly realize high density high-aspect-ratio nanoforest structure in each surface preparation of micro-meter scale groove, then molding method is utilized to transfer on PDMS by the nanoforest structure on micro-meter scale groove and surface thereof, recycling DRIE aftertreatment technology carries out Surface Physical Chemistry process to PDMS, reduce surface energy, thus the three-dimensional anti-drag micro-channel of the PDMS realizing having superhydrophobic characteristic, this preparation method's technique is simple, cost is low, drag reduction efficiency is high, what is more important has implantable.
For achieving the above object, the invention provides a kind of implantable three-dimensional anti-drag micro-channel structure based on the integrated process technology of micro-nano, this structure comprises: PDMS substrate, PDMS cover plate, micron trenches, nanometer sieve aperture array.
The thickness of PDMS substrate and PDMS cover plate is 50 μm-1000 μm;
PDMS cover plate is bonded on PDMS substrate;
Micron trenches is made on PDMS substrate, forms closed cavity by PDMS substrate and PDMS cover plate, and cross section is del or inverted trapezoidal or semicircle, and its characteristic size is 10 μm-1000 μm;
Nanometer sieve aperture array is made in micron trenches surface, the sieve aperture of to be diameter be 10nm-1000nm, degree of depth 10nm-5000nm, spacing 10nm-1000nm.
Present invention also offers a kind of implantable three-dimensional anti-drag micro-channel preparation method based on the integrated process technology of micro-nano, the method comprises:
Step 1: by corroding in conjunction with photoetching and chemistry or physics, silicon-based substrate makes micron trenches mould, and cross section is that triangle is trapezoidal or semicircle;
Step 2: utilize and optimize deep reaction ion etching technique without mask, directly make high density high-aspect-ratio nanoforest on silica-based micron trenches mould and smooth silicon chip surface;
Step 3: utilize PDMS mold technique, modulation process parameter, with silica-based micron trenches mould and nanoforest for template, realizes the PDMS cover plate with nanometer sieve aperture array, PDMS substrate and micron trenches;
Step 4: utilize DRIE aftertreatment technology, regulation and control parameter, carries out physical chemistry process to PDMS cover plate and PDMS substrate, wherein PDMS substrate comprises micron trenches, reduce its surface energy, improve its stable ultra-hydrophobic characteristic;
Step 5: exerted pressure by high temperature bonding or normal temperature physics, by PDMS substrate and PDMS cover plate bonding, is formed and closes fluid channel.
In such scheme, optimize deep reaction ion etching technique without mask described in step 2, comprise the following steps: adopt plasma etching or non-plasma etching to carry out roughening process to silicon chip surface; Control described DRIE technological parameter, directly prepare high density high-aspect-ratio nanoforest structure.
The technological parameter that described DRIE prepares nanoforest comprises: coil power is 800W-900W; Pressure is 20mTorr-30mTorr; Etching gas SF
6flow is 20sccm-45sccm, passivation gas C
4f
8flow is 30sccm-50sccm (SF
6and C
4f
8gas flow ratio is 1: 1-1: 2); Platen power is 6W-12W; Etching/passivation time ratio is 10s: 10s-4s: 4s; Etching/passivation cycle 60-200 time.
In such scheme, described in step 3, technological parameter comprises: temperature is 50-100 DEG C, and the time is 30 minutes-2 hours.
In such scheme, the aftertreatment technology of DRIE described in step 4 parameter comprises: coil power is 800W-900W; Pressure is 20mTorr-30mTorr; Etching gas SF
6flow is 0sccm, passivation gas C
4f
8flow is 30sccm-50sccm; Platen power is 6W-12W; Etching/passivation time ratio is 0s: 10s-0s: 4s; Etching/passivation cycle 1-40 time.
Beneficial effect of the present invention:
1, the implantable three-dimensional anti-drag micro-channel structure based on the integrated process technology of micro-nano of the present invention's proposition, DRIE technique is optimized without mask owing to adopting, on the basis not destroying original micron scale structures, all can growing high density high-aspect-ratio nanoscale silicon tip array on each surface of micron trenches, realize nanoforest and cover 100% of micron trenches; And adopt molded technology by above-mentioned micro-nano compound structure Graphic transitions to PDMS surface, thus real three-dimensional anti-drag micro-channel can be realized.
2, the implantable three-dimensional anti-drag micro-channel structure based on the integrated process technology of micro-nano of the present invention's proposition, owing to achieving high density nanoscale sieve aperture array in micron trenches each surface preparation, therefore its area-volume ratio can greatly be improved, thus make fluid channel surface have superhydrophobic characteristic, realize the effect of excellent anti-drag.
3, the implantable three-dimensional anti-drag micro-channel preparation method based on the integrated process technology of micro-nano of the present invention's proposition, utilizes and optimizes DRIE technique and PDMS molded technology without mask, only need two-step process, PDMS micro-nano compound structure can be realized, technique is simple, with low cost, is easy to industrialization.
4, the implantable three-dimensional anti-drag micro-channel preparation method based on the integrated process technology of micro-nano of the present invention's proposition, plasma technique is utilized to process PDMS cover plate and micron trenches, its roughness can be increased from physics angle of taking on a new look, and chemically modification angle deposit fluoro-based polymers reduces its surface energy, thus improve its stable ultra-hydrophobic characteristic further, thus greatly improve its drag-reduction effect.
Accompanying drawing explanation
When considered in conjunction with the accompanying drawings, by referring to detailed description below, more completely can understand the present invention better and easily learn wherein many adjoint advantages, but accompanying drawing described herein is used to provide a further understanding of the present invention, form a part of the present invention, schematic description and description of the present invention, for explaining the present invention, does not form inappropriate limitation of the present invention, wherein:
Fig. 1 (a) is one of the implantable three-dimensional anti-drag micro-channel structure based on the integrated process technology of micro-nano of the present invention schematic diagram;
Fig. 1 (b) is two schematic diagrames of the implantable three-dimensional anti-drag micro-channel structure based on the integrated process technology of micro-nano of the present invention;
Fig. 1 (c) is three schematic diagrames of the implantable three-dimensional anti-drag micro-channel structure based on the integrated process technology of micro-nano of the present invention;
Fig. 2 is the implantable three-dimensional anti-drag micro-channel preparation method process chart based on the integrated process technology of micro-nano of the present invention;
Fig. 3 is the micron trenches stereoscan photograph of the implantable three-dimensional anti-drag micro-channel based on the integrated process technology of micro-nano of the present invention;
Fig. 4 is the PDMS cover plate stereoscan photograph at the implantable three-dimensional anti-drag micro-channel top based on the integrated process technology of micro-nano of the present invention;
Fig. 5 is the implantable three-dimensional anti-drag micro-channel contact angle test result figure based on the integrated process technology of micro-nano of the present invention.
Below in conjunction with drawings and Examples, the present invention is further described.
Detailed description of the invention
Obviously, the many modifications and variations that those skilled in the art do based on aim of the present invention belong to protection scope of the present invention.
For enabling above-mentioned purpose of the present invention, feature and advantage become apparent more, are described in further detail the embodiment of the present invention below in conjunction with the drawings and specific embodiments.
The concrete steps of a kind of implantable three-dimensional anti-drag micro-channel structure based on the integrated process technology of micro-nano provided by the invention and preparation method thereof are set forth below in conjunction with accompanying drawing 1 to Fig. 5.
With reference to Fig. 1, Fig. 1 (a) to Fig. 1 (c) for of the present invention based on the implantable three-dimensional anti-drag micro-channel structure schematic diagram of the integrated process technology of micro-nano, its cross section is respectively: Fig. 1 (a) del structure, Fig. 1 (b) inverted trapezoidal structure, Fig. 1 (c) semicircular structure.Its structure comprises: PDMS substrate 1, PDMS cover plate 2, micron trenches 3, nanometer sieve aperture array 4.
Reference Fig. 2, Fig. 2 are the implantable three-dimensional anti-drag micro-channel preparation method process chart based on the integrated process technology of micro-nano of the present invention.Then the preparation process of structure shown in Fig. 1 (a) to Fig. 1 (c) is as follows:
Step 110: by corroding in conjunction with photoetching and chemistry or physics, silicon-based substrate makes micron trenches mould, and cross section is that triangle is trapezoidal or semicircle, and its characteristic size is 1 μm-1000 μm;
Step 120: utilize and optimize deep reaction ion etching technique without mask, directly on silica-based micron trenches mould and smooth silicon chip surface, make high density high-aspect-ratio nanoforest structure, be diameter be 50nm-1000nm, the silicon cone of height 100nm-5000nm, spacing 100nm-1000nm;
Step 130: utilize PDMS mold technique, modulation process parameter: temperature is 50-100 DEG C, time is 30 minutes-2 hours, with silica-based micron trenches mould and nanoforest for template, realize PDMS cover plate 2 and the PDMS substrate 1 with nanometer sieve aperture array 4, wherein PDMS substrate 1 comprises micron trenches 3;
Step 140: utilize DRIE aftertreatment technology, regulation and control parameter, carries out physical chemistry process to PDMS cover plate 2 and PDMS substrate 1, wherein PDMS substrate 1 comprises micron trenches 3, reduce its surface energy, improve its stable ultra-hydrophobic characteristic;
Step 150: exerted pressure by high temperature bonding or normal temperature physics, by PDMS substrate 1 and PDMS cover plate 2 bonding, is formed and closes fluid channel.
With reference to the micron trenches stereoscan photograph that Fig. 3, Fig. 3 are the implantable three-dimensional anti-drag micro-channel based on the integrated process technology of micro-nano of the present invention, its cross section is del, and base material is PDMS.Cross section described in above-mentioned steps 130 is del or inverted trapezoidal or semicircle, and its groove depth is 1 μm-500 μm, and groove width is 1 μm-1000 μm.
With reference to the PDMS cover plate stereoscan photograph that Fig. 4, Fig. 4 are the implantable three-dimensional anti-drag micro-channel top based on the integrated process technology of micro-nano of the present invention.The array of nanometer sieve aperture described in above-mentioned steps 130, diameter is 10nm-1000nm, degree of depth 10nm-5000nm, spacing 10nm-1000nm.
Reference Fig. 5, Fig. 5 are the implantable three-dimensional anti-drag micro-channel contact angle test result figure based on the integrated process technology of micro-nano of the present invention, and its contact angle is greater than 170 °, have excellent super-hydrophobic property of reduction drag.
As mentioned above, embodiments of the invention are explained, but as long as do not depart from inventive point of the present invention in fact and effect can have a lot of distortion, this will be readily apparent to persons skilled in the art.Therefore, such variation is also all included within protection scope of the present invention.
Claims (1)
1. the implantable three-dimensional anti-drag micro-channel preparation method based on the integrated process technology of micro-nano, it is characterized in that: utilize and optimize deep reaction ion etching DRIE technique without mask, directly realize high density high-aspect-ratio nanoforest structure in each surface preparation of micro-meter scale groove, then molding method is utilized to transfer on PDMS by the nanoforest structure on micro-meter scale groove and surface thereof, recycling DRIE aftertreatment technology carries out Surface Physical Chemistry process to PDMS, reduce surface energy, thus the three-dimensional anti-drag micro-channel of the PDMS realizing having superhydrophobic characteristic;
Comprise step as follows:
Step 1: by corroding in conjunction with photoetching and chemistry or physics, silicon-based substrate makes micron trenches mould, and cross section is that triangle is trapezoidal or semicircle;
Step 2: utilize and optimize deep reaction ion etching technique without mask, directly make high density high-aspect-ratio nanoforest on silica-based micron trenches mould and smooth silicon chip surface;
Step 3: utilize PDMS mold technique, modulation process parameter, with silica-based micron trenches mould and nanoforest for template, realizes the PDMS cover plate with nanometer sieve aperture array, PDMS substrate and micron trenches;
Step 4: utilize DRIE aftertreatment technology, regulation and control parameter, carries out physical chemistry process to PDMS cover plate and PDMS substrate, wherein PDMS substrate comprises micron trenches, reduce its surface energy, improve its stable ultra-hydrophobic characteristic;
Step 5: exerted pressure by high temperature bonding or normal temperature physics, by PDMS substrate and PDMS cover plate bonding, is formed and closes fluid channel;
Optimize deep reaction ion etching technique without mask described in step 2, comprise the following steps: adopt plasma etching or non-plasma etching to carry out roughening process to silicon chip surface; Control described DRIE technological parameter, directly prepare high density high-aspect-ratio nanoforest structure;
The technological parameter that described DRIE prepares nanoforest comprises: coil power is 800W-900W; Pressure is 20mTorr-30mTorr; Etching gas SF
6flow is 20sccm-45sccm, passivation gas C
4f
8flow is 30sccm-50sccm; SF
6and C
4f
8gas flow ratio is 1:1-1:2; Platen power is 6W-12W; Etching/passivation time is than being 10s:10s-4s:4s; Etching/passivation cycle 60-200 time;
Described in step 3, technological parameter comprises: temperature is 50-100 DEG C, and the time is 30 minutes-2 hours;
The aftertreatment technology of DRIE described in step 4 parameter comprises: coil power is 800W-900W; Pressure is 20mTorr-30mTorr; Etching gas SF
6flow is 0sccm, passivation gas C
4f
8flow is 30sccm-50sccm; Platen power is 6W-12W; Etching/passivation time is than being 0s:10s-0s:4s; Etching/passivation cycle 1-40 time.
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| CN104326433B (en) * | 2014-10-31 | 2016-05-18 | 中国科学院光电技术研究所 | A kind ofly receive runner preparation method based on template-mediated be full of cracks effect |
| CN105772120A (en) * | 2016-03-07 | 2016-07-20 | 北京同方生物芯片技术有限公司 | Batched bonding packaging method for polymeric biochips and positioning device |
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