CN101024482A - Method for constituting 3-D structure - Google Patents
Method for constituting 3-D structure Download PDFInfo
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- CN101024482A CN101024482A CN 200710055454 CN200710055454A CN101024482A CN 101024482 A CN101024482 A CN 101024482A CN 200710055454 CN200710055454 CN 200710055454 CN 200710055454 A CN200710055454 A CN 200710055454A CN 101024482 A CN101024482 A CN 101024482A
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Abstract
The invention relates to a method to construct 3D microstructure. It includes the following steps: using photoengraving method to construct 2D microstructure surface, extruding polymer performed polymer or ultraviolet glue precursor into the slot on 2D microstructure surface and taking heat or light polymerization to gain target material; constructing polymer or ultraviolet exposal glue array structure, washing sacrificed material at one time to gain the 3D microstructure. The invention has potential application value in the fields of shape, size, thickness, material, photon crystal, catalyst carrier, etc.
Description
Technical field
The present invention relates to a kind of method of constituting 3-D structure, specifically provide a kind of with the sacrificial structure material exceed pallet, progressively the method for multi-layer three-dimension micro structure array is constructed in layering.The shape of the micro structure array between different layers, size, thickness, material can be identical, also can be different.
Background technology
Three-dimensional microstructures (characteristic size from the hundreds of micron to the hundreds of nanometer) all has important scientific meaning and using value in fields such as microelectronics, material science, supermolecule science, cell biologies, specifically, three-dimensional microstructures can be applicable to photonic propulsion device, sensor, microfluidic device, micro electromechanical system, photonic crystal, the three-dimensional concrete aspect such as waveguide, super prism, microreactor and catalyst carrier that connects.Use just because of three-dimensional microstructures has so widely, it has attracted numerous Science and Technology workers' interest.
The existing construction method of three-dimensional microstructures is broadly divided into three major types: the first kind is the method for directly constructing (Directfabrication), specifically be divided into laser direct-writing (Direct Laser Writing) and holographic etching (Holographic lithography) again, it all is laser regional exposure on the multi-photon material photoresist of spin coating to focus on, utilize the exposure area to develop then with unexposed area deliquescent different wash-outs in solvent, construct the three-dimensional microstructures of multi-photon material photoresist, it is reported that the limit of resolution that this method can reach now is about 200nm.Second class is the method for (" Top-down ") from top to bottom, specifically comprise electron beam lithography (Electronicbeam lithography (EBL)), inductively coupled plasma etching (Inductively coupled plasma (ICP) etching) and soft etching (Soft-lithography) etc., be generally utilize existing moulding two dimension micro-structural to construct technology such as photoetching, electron beam lithography is constructed the retaining layer, constructs the three-dimensional microstructures of semi-conducting material in conjunction with the selectivity of the non-selective and wet etching that utilizes dry etching.Second class is the method for (" Bottom-up ") from bottom to top, specifically comprise electrostatic induction crystallisation (Electrostatically inducedcrystallization), gravity sedimentation (Gravity sedimentation), electricity hydraulics deposition (Electro-hydrodynamic deposition), colloid oriented growth (Colloidal epitaxy), material resources restriction (Physical confinement) and convection current self assembly methods such as (Convective self-assembly), specifically utilize colloid micro ball as construction material, under the external force booster action, make microballoon be assembled into three-dimensional structure with specific form crystal lattice.
Though above-mentioned preceding two class methods can be constructed out the high three-dimensional microstructures of structure arbitrary resolution, that its equipment requires is high, construct the cost height, consuming time, material is restricted.Colloid micro ball method cost is lower, but repeated reliability bad, the most serious be the three-dimensional microstructures that can not construct labyrinth.Also there is self deficiency based on above-mentioned each class methods, the proposition of new method and use and just seem particularly necessary.
Summary of the invention
The method that the purpose of this invention is to provide a kind of new constituting 3-D structure.
The present invention constructs two-dimentional micro-structure surface (as the sacrificial structure material) with methods such as photoetching, adopt stamping technique that polymer performed polymer or ultraviolet glue precursor are clamp-oned in the groove of the two-dimentional micro-structure surface for preparing previously, by original position heat or photopolymerization target material; On preceding one deck basis, construct fine structure material surface (equally as the sacrificial structure material) then once more, and progressively the polymer or the uv-exposure glue array structure of multilayer are constructed in layering, finally once wash away expendable material, promptly obtain the three-dimensional microstructures of target material.
The array microstructure of the regular three-dimensional microstructures different layers that the method is constructed can be difformity, different size, different-thickness, unlike material.It provides a kind of new approach for constructing of micro-structural and has expanded micro-structural and constructed applicable scope.
The method of the invention can be widely used in preparing all regulatable three-dimensional microstructures device of layers of material, shape, thickness, size.It all has potential using value at photonic propulsion device, sensor, microfluidic device, micro electromechanical system, photonic crystal, the three-dimensional aspects such as waveguide, super prism, microreactor and catalyst carrier that connect.
The method of the described constituting 3-D structure of this patent comprises the steps:
A) utilize the ultraviolet photolithographic technology, dry up step, in substrate, construct photoresist template with micron or submicrometer structure through spin coating photoresist, heating anneal, uv-exposure, development in substrate;
B) utilize method for stamping that level and smooth on-chip polymer performed polymer or uv-exposure glue precursor coating are squeezed in the gap of photoresist template;
C) level and smooth substrate is peeled off, thereby in substrate, formed photoresist and polymer performed polymer or the photoresist structure alternate with uv-exposure glue precursor;
D) leave standstill 2～24 hours after, polymerization or curing make the micron or the submicrometer structure substrate;
E) with 0～360 ° of above-mentioned substrate rotation, repeating step a～d constructs follow-up layers of material, size, shape micron or submicrometer structure identical or inequality;
F) utilize organic solvent to select to wash away photoresist, can in substrate, obtain polymer or uv-exposure glue pattern that multilayer has micron or submicrometer structure, thereby obtain three-dimensional microstructures.
The related substrate of step a comprises monocrystalline silicon, glass, ito glass, quartz, mica sheet, polymer (as polymethyl methacrylate (PMMA), polystyrene (PS), Merlon (PC), polyethylene (PE), polyvinyl chloride (PVC), polypropylene (PP) etc.) or the metallic substrates with smooth flat in the said method, or the above-mentioned substrate of modifying through the unimolecule self-assembling method, substrate is used after cleaning.
Photoetching is the method for preparing micro-structural of extensive use, utilize electromagnetic wave radiation inducing materials molecular structure generation chemical changes such as ultraviolet or X ray to produce sub-image, and the part-structure that is stopped by template is constant, method with etching becomes concavo-convex structure with sub-image then, has promptly obtained the micro-structural of identical with template (eurymeric photoresist) or opposite (negative photoresist).For photoetching, spin-coating film is a photoresist, it is characterized by uv-exposure region clustering body marriage chain and disconnects, and the link of cross at random of become easily dissolving (eurymeric photoresist) or uv-exposure zone main chain is more tight, and increase from chain tenesmus thing, polymeric solubility reduces (negative photoresist)
The photoresist of using among the present invention is the BP-212 type ultraviolet eurymeric photoresist that Beijing Inst. of Chemical Reagent produces, viscosity (25 ℃): (37 ± 2) * 10
-3PaS.Used litho machine is the G-25 type mask exposure machine that the prosperous southern photoproduction in Chengdu is produced, be applicable to the uv-exposure etching of hundred nanometers to the photoresist of several micron thickness, resolving accuracy can reach 1 micron, the thickness of our photoresist layer all is controlled at about 2 μ m among the present invention, photoresist spin coating condition is: 800～5000 commentaries on classics/S, rotation 10～90S.
Related uv-exposure glue comprises all kinds of eurymeric photoresist and the negative photoresists that micro-structural is constructed that are used in the said method, as BP-212 series ultraviolet eurymeric photoresist, BP-213 series ultraviolet eurymeric photoresist, BP-215 series ultraviolet eurymeric photoresist, BP-218 series ultraviolet eurymeric photoresist and BN-302 series ultraviolet negative photoresist, BN-303 series ultraviolet negative photoresist, BN-308 series ultraviolet negative photoresist, the BN-310 series ultraviolet negative photoresist of Beijing Inst. of Chemical Reagent's development.
Related polymer performed polymer coating comprises that reset conditions such as dimethyl silicone polymer (PDMS), acrylic acid double cyclopentenyl ester, phthalic acid two rare third fat (DAP), epoxy resin are the liquid of thickness in the said method, and it can polymerizing curable through heating or ultraviolet lighting processing.
We use AFM (Nanosope IIIa, Digital Instrument Co., Santa Babara, CA) and light microscope (Olympus Reflected Fluorescence System BX51, Japan) all-the-way tracking utilize the described method of this patent to make each process of micro-structural, by AFM and light microscope tracing observation to different sample various process, we find with this method is to realize the good method of three-dimensional microstructures, has good repeatability and stability.
We have constructed out different regular patterns with different polymer performed polymers in substrates such as quartz, glass, ito glass, monocrystalline silicon, metal, polymer.Substrate needed before using through preliminary treatment, (O-Plasma system 100, PVATepla Germany) handle 1～30min with the oxygen plasma system to be specially Inorganic Non-metallic Materials and polymeric material, make cleaning surfaces and hydrophilic, be convenient to the spin-coating film of photoresist.Metal material cleans 1～30min with chloroform, acetone, methyl alcohol, high purity water excusing from death successively, makes fully cleaning of surface.
Photo mask board is used acetone, high purity water ultrasonic cleaning 1～10min successively before use, and high pure nitrogen dries up.
The spin coating photoresist (condition of step a) is: 800～5000 commentaries on classics/S, and rotation 10～90S, spin coating finishes sample at 60～90 ℃ of following quenching 20min～5h.
Conditions of exposure (step a): the G-25 type mask exposure machine that we use the prosperous southern photoproduction in Chengdu to produce, control exposure electric current 2～5A, time for exposure 20～200s.
(step a): the sample that finishes of exposure develops in developer solution and puts into distilled water behind 1～20s and clean residual developer solution development conditions.
Moulding process (step b and c): on level and smooth substrate (glass, level and smooth polymer flake or plastic sheeting), coat one layer of polymeric performed polymer or uv-exposure glue precursor, tip upside down on after smoothening on the photoresist template, under 10～20bar pressure, keep 5～60min, polymer performed polymer or uv-exposure glue are coated with in the gap that precursor coating is squeezed into photoresist, thereby form polymer performed polymer or uv-exposure glue precursor pattern with the photoresist structure complementation.
Polymerization is that substrate with polymer performed polymer and the alternate structure of photoresist is at 60～200 ℃ of following polymerization 2～20h, or with the substrate of uv-exposure glue precursor and the alternate structure of the photoresist 3～30min that exposes under 100～1000W exposure power.
Utilizing organic solvent to select wash-out is that the sample of having constructed sandwich construction is put into ethanol or acetone, soaks 1～15min, and the photoresist in micron or the submicrometer structure photoresist template is washed away fully, obtains the Three-dimension Target micro-structural at last under substrate.
The method on constituting 3-D structure recited above surface, the template of photoetching for the second time or impression employed template for the first time can be different size, difformity, and can rotate arbitrarily angled (0～360 °), polymer performed polymer that each layer is used or uv-exposure glue material also can be inequality.
The characteristics of the method for the invention are that layers of material, shape, thickness, the size of the three-dimensional microstructures for preparing is all adjustable, and this fabrication techniques three-dimensional microstructures also has size little (photolithography limitation 100～200nm), cost is low, technology is simple, good reproducibility, efficient height, area are big, be suitable for advantages such as multiple polymers material in addition.This method all has potential using value at aspects such as nano science, material science, electronic technology, photoelectric device and optics, biochip and microfluidic devices.Can be widely used in the various all regulatable three-dimensional microstructures of layer material, shape, thickness, size of preparation.
Description of drawings
Fig. 1: the schematic diagram of constituting 3-D structure method of the present invention;
Fig. 2 (a): the microphotograph of the PDMS three-dimensional microstructures of on quartz substrate, constructing;
Fig. 2 (b): the three-dimensional little atomic force 3-D view of the PDMS that on quartz substrate, constructs;
Fig. 3 (a): the microphotograph of the uv-exposure glue three-dimensional microstructures of on quartz substrate, constructing;
Fig. 3 (b): the atomic force 3-D view of the uv-exposure glue three-dimensional microstructures of on quartz substrate, constructing;
Fig. 4 (a): the microphotograph of the uv-exposure glue three-dimensional microstructures of on monocrystal silicon substrate, constructing;
Fig. 4 (b): the microphotograph of the uv-exposure glue three-dimensional microstructures of in the ito glass substrate, constructing;
Fig. 5 (a): angle is the microphotograph of 90 ° three-dimensional microstructures between the different layers of constructing;
Fig. 5 (b): angle is the microphotograph of 45 ° three-dimensional microstructures between the different layers of constructing;
Fig. 6 (a): the microphotograph of the three-dimensional microstructures of the different layers same size of constructing;
Fig. 6 (b): the microphotograph of the three-dimensional microstructures of the different layers different size of constructing;
Fig. 7 (a): the microphotograph of the three-dimensional microstructures that the different layers of constructing is identical shaped;
Fig. 7 (b): the microphotograph of the difform three-dimensional microstructures of constructing of different layers;
Fig. 8: the microphotograph of the three-dimensional microstructures of the different layers different materials of constructing;
Fig. 9 (a): be the fluorescence microscope photo behind the evaporation quinacridone on the three-dimensional microstructures of different materials at upper strata and bottom;
Fig. 9 (b): be the sepectrophotofluorometer spectrum behind the evaporation quinacridone on the three-dimensional microstructures of different materials at upper strata and bottom;
Figure 10 (a): be the fluorescence microscope photo behind the evaporation pyrazoles anthracene on the three-dimensional microstructures of different materials at upper strata and bottom;
Figure 10 (b): be the sepectrophotofluorometer spectrum behind the evaporation pyrazoles anthracene on the three-dimensional microstructures of different materials at upper strata and bottom;
As shown in Figure 1,2 for the substrate of photoetching (impression), can be monocrystalline silicon, glass, ito glass, quartz, mica sheet, polymer (as polymethyl methacrylate (PMMA), polystyrene (PS), Merlon (PC), polyethylene (PE), polyvinyl chloride (PVC), polypropylene (PP) etc.) or metallic substrates in this invention with smooth flat, or the above-mentioned substrate of modifying through the unimolecule self-assembling method.1 for having the photoresist through the uv-exposure development of micro-structural; 4 for being used to be coated with the substrate of polymer performed polymer or uv-exposure glue precursor, and it is peeled off and can throw away after impression finishes only as the support of carrier polymer performed polymer or uv-exposure glue, can select smooth glass for use, also can select other substrate for use; 3 is polymer performed polymer or ultraviolet glue precursor coating; 5 for clamp-oning polymer performed polymer or the uv-exposure glue in the photoresist template micro-structural groove; 6 is the second layer photoresist structure of constructing on preceding one deck architecture basics; 7 for clamp-oning photoresist micro-structural 6 grooves interior polymer performed polymer or uv-exposure glue behind the impression for the second time.
The present invention utilizes technology such as above-mentioned ultraviolet photolithographic to have in spin coating in the substrate 2 of photoresist and constructs photoresist micro-structural 1 (Fig. 1 steps A), be stamped in (Fig. 1 step B) on the polymer performed polymer or uv-exposure gel coating 3 that is spun on the smooth substrate 4 as template again, 10～20bar keep-ups pressure, 5～60min, thereby polymer performed polymer coating 3 is clamp-oned in photoresist 1 groove therebetween, then smooth substrate 4 is peeled off, thereby in substrate 2, form polymer performed polymer or uv-exposure glue 3 structures alternate, and smooth substrate can be abandoned (Fig. 1 step C) after peeling off as expendable material with photoresist 1.After leaving standstill 2～24 hours, under the condition of illumination or heating, impel polymer performed polymer or 3 polymerizations of uv-exposure glue or be cured as polymer or uv-exposure plastic structure 5 (Fig. 1 step D), the second layer photoresist structure 6 that on preceding one deck architecture basics, continues to construct (Fig. 1 step e); Impress once more polymer performed polymer or uv-exposure glue 7 are clamp-oned (Fig. 1 step F) in the micro-structural groove; Under the condition of illumination or heating, impel polymer performed polymer or uv-exposure glue precursor polymeric or curing (Fig. 1 step G) once more; Utilize the photoresist structure that dissolves away of solvent selectivity again according to deliquescent difference, can in substrate 2, obtain three-dimensional microstructures (Fig. 1 step H).
As shown in Figure 2, be the PDMS three-dimensional microstructures of on quartz substrate, constructing, micro-structural cycles 13 μ m, band 8 μ m, groove 5 μ m;
Shown in Figure 3, be the uv-exposure glue three-dimensional microstructures of on quartz substrate, constructing, micro-structural cycles 13 μ m, band 8 μ m, groove 5 μ m;
Shown in Figure 4, at uv-exposure glue three-dimensional microstructures of constructing on the monocrystal silicon substrate and the uv-exposure glue three-dimensional microstructures in the ito glass substrate, constructed, micro-structural cycles 13 μ m, band 8 μ m, groove 5 μ m;
Shown in Figure 5, for constructing the three-dimensional microstructures of angle between different layers, two interlayer direction differences, but physical dimension is identical, micro-structural cycles 13 μ m, and band 8 μ m, groove 5 μ m, two interlayer angles are respectively 90 °, 45 °;
Shown in Figure 6, construct the three-dimensional microstructures of different layers different size, be respectively upper strata and bottom and be cycles 20 μ m, band 10 μ m, the three-dimensional microstructures of groove 10 μ m, with the upper strata be cycles 20 μ m, band 10 μ m, groove 10 μ m, bottom are cycles 50 μ m, band 25 μ m, the three-dimensional microstructures of groove 25 μ m; The upper strata is vertical mutually with the bottom direction.
Shown in Figure 7, construct the difform three-dimensional microstructures of different layers.Be respectively upper strata and bottom and be cycles 20 μ m, band 10 μ m, the ribbon structure of groove 10 μ m and upper strata are cycles 20 μ m, band 10 μ m, the ribbon structure of groove 10 μ m, bottom are cycles 50 μ m, band 25 μ m, the rectangular configuration of groove 25 μ m; The upper strata is vertical mutually with the bottom direction.
Shown in Figure 8, the three-dimensional microstructures of the different layers different materials of constructing.The upper strata is a uv-exposure glue, and bottom is PDMS, and is two-layer measure-alike, but direction is vertical mutually micro-structural cycles 13 μ m, band 8 μ m, groove 5 μ m is set;
Shown in Figure 9, material regulation and control fluorescence molecule form and character are orange on uv-exposure glue behind evaporation quinacridone on the three-dimensional microstructures of upper strata and bottom different materials, are green on the PDMS;
Shown in Figure 10, material regulation and control fluorescence molecule form and character behind evaporation pyrazoles anthracene on the three-dimensional microstructures of upper strata and bottom different materials are green on uv-exposure glue, be blue on the PDMS.
The specific embodiment
Further illustrate the inventive method and application below by embodiment, rather than will limit the present invention with these embodiment.The present invention has adopted quartz, glass, several substrates of silicon chip respectively, makes the structure motherboard with the method for photoetching, does packing material with PDMS, uv-exposure glue then, has constructed the surface of micro-structural.
Embodiment 1:
Select for use quartz as base material, before using,, make cleaning surfaces and hydrophilic, be convenient to the spin-coating film of photoresist through oxygen plasma system handles 5min.The condition of spin coating photoresist is: 1500 commentaries on classics/S, and rotation 15S, 30min quenches sample after spin coating finishes under 80 ℃ of conditions.Under the mask exposure machine, control exposure electric current 3.5A then, exposure 40s, the development 3s in developer solution (BP-212 ultraviolet eurymeric photoresist developing liquid) that finishes exposes, put into distilled water and clean residual developer solution, dry up with nitrogen, promptly get the photoresist template, micro-structural cycles 13 μ m, groove 8 μ m, band 5 μ m.
This template is stamped on the smooth glass substrate that scribbles the PDMS performed polymer, keep 15bar pressure 10min, thereby the PDMS performed polymer is clamp-oned in the groove between photoresist, then with the smooth glass substrate desquamation, after leaving standstill 2 hours, 68 ℃ of following heating impelled performed polymer to be polymerized to PDMS in 6 hours, continue photoetching and construct second layer photoresist structure on preceding one deck architecture basics, physical dimension is identical with ground floor, impresses once more the PDMS performed polymer is clamp-oned in the photoresist micro-structural groove; Heat down at 68 ℃ once more and impel the performed polymer polymerization; Dissolve away photoresist structure with acetone at last, nitrogen dries up, and promptly obtains PDMS three-dimensional microstructures (see Fig. 2, the angle between two-layer photoresist template is 90 °).
Embodiment 2:
Select for use quartz as base material, before using,, make cleaning surfaces and hydrophilic, be convenient to the spin-coating film of photoresist through oxygen plasma system handles 5min.The condition of spin coating photoresist is: ground floor: 1500 commentaries on classics/S, and rotation 15S, spin coating finishes sample at 80 ℃ of following quenching 30min.Under the mask exposure machine, control exposure electric current 3.5A then, exposure 40s, the 3s that develops in developer solution that finishes that exposes puts into distilled water and cleans residual developer solution, dries up with nitrogen, promptly gets the photoresist template, micro-structural cycles 13 μ m, groove 8 μ m, band 5 μ m.
This template is stamped in scribbles uv-exposure glue precursor (P/N6031 NORLAND OPTICALADHENSIVE, Norland products, Inc.Cranbury, NJ, P/N6031 type light-sensitive emulsion, northern part of the country Products Co., Ltd, New Jersey) on the smooth glass substrate, keeps 10bar pressure 8min, uv-exposure glue precursor is clamp-oned in the groove between photoresist, then with the smooth glass substrate desquamation, after leaving standstill 2 hours, (300 ± 50W) exposure 5min impel precursor cures to uviol lamp, continue photoetching and construct second layer photoresist structure (physical dimension is identical on preceding one deck architecture basics, 1.2 microns of ground floor thickness, 1.0 microns of second layer thickness, structural thickness is regulated and control by the rotating speed of regulation and control spin coating photoresist, and second layer spin coating condition is 1 800 commentaries on classics/S, rotation 15S, two interlayers are 90 degree); Impress once more uv-exposure glue precursor is clamp-oned in the photoresist micro-structural groove, repeat above-mentioned steps, the 5min that exposes once more impels precursor cures; Dissolve away photoresist structure with acetone at last, nitrogen dries up, and promptly obtains uv-exposure glue three-dimensional microstructures (see figure 3).
Embodiment 3:
Select for use monocrystalline silicon and ito glass as base material respectively, before using,, make cleaning surfaces and hydrophilic, be convenient to the spin-coating film of photoresist through oxygen plasma system handles 5min.The condition of spin coating photoresist is: 1500 commentaries on classics/S, rotation 15S revolves figure and finishes sample at 80 ℃ of following quenching 30min.Under the mask exposure machine, control exposure electric current 3.5A then, exposure 40s, the 3s that develops in developer solution that finishes that exposes puts into distilled water and cleans residual developer solution, dries up with nitrogen, promptly gets the photoresist template, micro-structural cycles 13 μ m, groove 8 μ m, band 5 μ m.
This template is stamped on the smooth glass substrate that scribbles uv-exposure glue precursor, keep 10bar pressure 8min, uv-exposure glue precursor is clamp-oned in the groove between photoresist, then with the smooth glass substrate desquamation, after leaving standstill 2 hours, (300 ± 50W) exposure 5min impel precursor cures to uviol lamp, continue photoetching and construct second layer photoresist structure (physical dimension is identical, and two interlayers are 90 degree) on preceding one deck architecture basics; Impress once more uv-exposure glue precursor is clamp-oned in the photoresist micro-structural groove, repeat above-mentioned steps, the 5min that exposes once more impels precursor cures; Dissolve away photoresist structure with acetone at last, nitrogen dries up, and promptly obtains uv-exposure glue three-dimensional microstructures (see figure 4).
Embodiment 4:
Select for use quartz as base material, before using,, make cleaning surfaces and hydrophilic, be convenient to the spin-coating film of photoresist through oxygen plasma system handles 5min.The condition of spin coating photoresist is: 1500 commentaries on classics/S, rotation 15S revolves figure and finishes sample at 80 ℃ of following quenching 30min.Under the mask exposure machine, control exposure electric current 3.5A then, exposure 40s, the 3s that develops in developer solution that finishes exposes, put into distilled water and clean residual developer solution, dry up, promptly get photoresist template (micro-structural cycles 13 μ m with nitrogen, groove 15 μ m, band 10 μ m).
This template is stamped on the smooth glass substrate that scribbles the PDMS performed polymer, keep 15bar pressure 10min, the PDMS performed polymer is clamp-oned in the groove between photoresist, then with the smooth glass substrate desquamation, after leaving standstill 2 hours, heating impels performed polymer to be polymerized to PDMS under 68 ℃, selects quadrature 90 degree and 45 degree to intersect the continuation photoetching on preceding one deck architecture basics respectively and constructs second layer photoresist structure (physical dimension is identical); Impress once more the PDMS performed polymer is clamp-oned in the photoresist micro-structural groove, repeat above-mentioned steps, heat down in 68 ℃ once more and impel the performed polymer polymerization; Dissolve away photoresist structure with acetone at last, nitrogen dries up, and promptly obtains PDMS three-dimensional microstructures (see figure 5).
Embodiment 5:
Select for use quartz as base material, before using,, make cleaning surfaces and hydrophilic, be convenient to the spin-coating film of photoresist through oxygen plasma system handles 5min.The condition of spin coating photoresist is: 1500 commentaries on classics/S, rotation 15S revolves figure and finishes sample at 80 ℃ of following quenching 30min.Under the mask exposure machine, control exposure electric current 3.5A then, exposure 40s, the exposure 3s that develops in developer solution that finishes puts into distilled water and cleans residual developer solution, dries up with nitrogen, (sample is cycles 20 μ m promptly to get the photoresist template, band 10 μ m, the micro-structural of groove 10 μ m, another sample is cycles 50 μ m, band 25 μ m, the micro-structural of groove 25 μ m).
This template is stamped on the smooth glass substrate that scribbles uv-exposure glue precursor, keep 10bar pressure 8min, uv-exposure glue precursor is clamp-oned in the groove between photoresist, then with the smooth glass substrate desquamation, after leaving standstill 2 hours, (300 ± 50W) exposure 5min impel precursor cures to uviol lamp, on preceding one deck architecture basics, continue photoetching and construct second layer photoresist structure (two interlayers are 90 degree), be cycles 20 μ m, band 10 μ m, the micro-structural of groove 10 μ m impresses once more uv-exposure glue precursor is clamp-oned in the photoresist micro-structural groove, repeat above-mentioned steps, the 5min that exposes once more impels precursor cures; Dissolve away photoresist structure with acetone at last, nitrogen dries up, and promptly obtains uv-exposure glue three-dimensional microstructures (see figure 6).
Embodiment 6:
Select for use quartz as base material, before using,, make cleaning surfaces and hydrophilic, be convenient to the spin-coating film of photoresist through oxygen plasma system handles 5min.The condition of spin coating photoresist is: 1500 commentaries on classics/S, rotation 15S revolves figure and finishes sample at 80 ℃ of following quenching 30min.Under the mask exposure machine, control exposure electric current 3.5A then, exposure 40s, the 3s that develops in developer solution that finishes that exposes puts into distilled water and cleans residual developer solution, dry up with nitrogen, (sample is cycles 20 μ m, band 10 μ m, the linear micro-structural of groove 10 μ m promptly to get the photoresist template, another sample is cycles 50 μ m, band 25 μ m, groove 25 μ m, the rectangle micro-structural of length 250 μ m).
This template is stamped on the smooth glass substrate that scribbles uv-exposure glue precursor, keep 10bar pressure 8min, uv-exposure glue precursor is clamp-oned in the groove between photoresist, then with the smooth glass substrate desquamation, after leaving standstill 0.5 hour, (300 ± 50W) exposure 5min impel precursor cures to uviol lamp, on preceding one deck architecture basics, continue photoetching and construct second layer photoresist structure (two interlayers are 90 degree), be cycles 20 μ m, band 10 μ m, the linear micro-structural of groove 10 μ m impresses once more uv-exposure glue precursor is clamp-oned in the photoresist micro-structural groove; The 5min that exposes once more impels precursor cures; Dissolve away photoresist structure with acetone at last, nitrogen dries up, and promptly obtains uv-exposure glue three-dimensional microstructures (see figure 7).
Embodiment 7:
Select for use monocrystalline silicon as base material, before using,, make cleaning surfaces and hydrophilic, be convenient to the spin-coating film of photoresist through oxygen plasma system handles 5min.The condition of spin coating photoresist is: 1500 commentaries on classics/S, rotation 15S revolves figure and finishes sample at 80 ℃ of following quenching 30min.Under the mask exposure machine, control exposure electric current 3.5A then, exposure 40s, the 3s that develops in developer solution that finishes exposes, put into distilled water and clean residual developer solution, dry up, promptly get photoresist template (micro-structural cycles 13 μ m with nitrogen, groove 8 μ m, band 5 μ m).
This template is stamped on the smooth glass substrate that scribbles the PDMS performed polymer, keep 15bar pressure 10min, the PDMS performed polymer is clamp-oned in the groove between photoresist, then with the smooth glass substrate desquamation, after leaving standstill 2 hours, heating impels performed polymer to be polymerized to PDMS under 68 ℃, continues photoetching and construct second layer photoresist structure (physical dimension is identical, and two interlayers are 90 degree) on preceding one deck architecture basics; Impress once more uv-exposure glue precursor is clamp-oned in the photoresist micro-structural groove; Exposure 5min impels precursor cures under uviol lamp; Dissolve away photoresist structure with acetone at last, nitrogen dries up, and promptly obtains PDMS/ uv-exposure glue three-dimensional microstructures (see figure 8).
Embodiment 8:
The different three-dimensional microstructures of layers of material of this patent preparation, thereon evaporation with a kind of light emitting molecule after, can utilize the different induced fluorescence molecules of substrate layers of material structure to have different coherent conditions, thereby on three dimension scale, only promptly can realize the constructing of three-dimensional microstructures of different fluorescence radiation colors with a kind of dye molecule by evaporation.
Be the structural formula of the quinacridone that is applied in the present embodiment below, select this luminophor for use, just be used for this patent is described, rather than to the restriction of this patent.
N，N’-di(n-butyl)quinacridone(DBQa)
Above-mentioned material can be by the method for bibliographical information synthetic (Kaiqi Ye, Jia Wang, Hui Sun, Yu Liu, Zhongcheng Mu, Fei Li, Shimei Jiang, Jingying Zhang, Hongxing Zhang, Yue Wang, andChi-Ming Che, J.Phys.Chem.B 2005,109,8008-8116; Trofimenko, S.), sample is purified through vacuum sublimation before the evaporation.
The three-dimensional microstructures of constructing with said method (1. .I:PDMS/II: uv-exposure glue (embodiment 7); 2. .I:PDMS/II:PDMS (embodiment 1); 3. .I: uv-exposure glue/II: uv-exposure glue (embodiment 2), on (I: represent the 1st layer, II: represent the 2nd layer), with the method evaporation 10nm quinacridone (DBQA) of vacuum evaporation.Promptly can be observed under the fluorescence microscope by 1. planting structure for, the bottom green, top layer is orange; 2. plant structure, bottom green, top layer green for; 3. plant structure for, bottom is orange, and top layer is orange; From fluorogram, can observe the result who conforms to fluorescence micrograph: 4. be 1. to plant the fluorogram of structure, therefrom we can see the green fluorescence peak (left side) that the DBQA on the I:PDMS sends, and can see II again: the fluorescent orange peak (right side) that the DBQA on the uv-exposure glue sends; 5. be 2. to plant the fluorogram of structure, therefrom we can only see the green fluorescence peak that the DBQA on the PDMS sends; 6. be 3. to plant the fluorogram of structure, therefrom we can only see the fluorescent orange peak that the DBQA on the uv-exposure glue sends, as shown in Figure 9.
Embodiment 9:
Be the structural formula of the pyrazoles anthracene molecule that is applied in the present embodiment below, select this luminophor for use, just be used for this patent is described, rather than to the restriction of this patent.
3-(9-anthrye)pyrazole(ANP)
Above-mentioned material can be by the method for bibliographical information synthetic (Calabrese J.C.and Thopson, J.S.Inorg.Chem.1987,26,1507-1514; Trofimenko, S.; Calabrese J.C.; Kochi, J.K.; Wolowiec, S.; Hulsberggen, F.B.and Reedijk, J.Inorg.Chem.1987,26,1507-1514), sample is purified through vacuum sublimation before the evaporation.
The three-dimensional microstructures of constructing with said method (1. .I:PDMS/II: uv-exposure glue (embodiment 7); 2. .I:PDMS/II:PDMS (embodiment 1); 3. .I: uv-exposure glue/II: (I: represent ground floor uv-exposure glue (embodiment 2)), II: represent the 2nd layer) on, can observe under method evaporation 10nm pyrazoles anthracene (ANP) fluorescence microscope with vacuum evaporation for and 1. plant structure, bottom blueness, top layer green; 2. plant structure, bottom blueness, top layer blueness for; 3. plant structure, bottom green, top layer green for; From fluorogram, can observe the result who conforms to fluorescence micrograph: 4. be 1. to plant the fluorogram of structure, therefrom we can see the blue-fluorescence peak (left side) that the ANP on the I:PDMS sends, and can see II again: the green fluorescence peak (right side) that the ANP on the uv-exposure glue sends; 5. be 2. to plant the fluorogram of structure, therefrom we can only see the blue-fluorescence peak that the ANP on the PDMS sends; 6. be 3. to plant the fluorogram of structure, therefrom we can only see the green fluorescence peak that the ANP on the uv-exposure glue sends, as shown in figure 10.
Claims (9)
1, a kind of method of constituting 3-D structure comprises the steps:
A) utilize the ultraviolet photolithographic technology, dry up step, in substrate, construct photoresist template with micron or submicrometer structure through spin coating photoresist, heating anneal, uv-exposure, development in substrate;
B) utilize method for stamping that level and smooth on-chip polymer performed polymer or uv-exposure glue precursor coating are squeezed in the gap of photoresist template;
C) level and smooth substrate is peeled off, thereby in substrate, formed photoresist and polymer performed polymer or the photoresist structure alternate with uv-exposure glue precursor;
D) leave standstill 2～24 hours after, polymerization or curing make the micron or the submicrometer structure substrate;
E) with 0～360 ° of above-mentioned substrate rotation, repeating step a～d constructs follow-up layers of material, size, shape micron or submicrometer structure identical or inequality;
F) utilize organic solvent to select to wash away photoresist, can in substrate, obtain polymer or uv-exposure glue pattern that multilayer has micron or submicrometer structure, thereby obtain three-dimensional microstructures.
2, the method for constituting 3-D structure as claimed in claim 1 is characterized in that: the condition of spin coating photoresist is 800～5000 commentaries on classics/S, rotation 10～90S, and spin coating finishes sample at 60～90 ℃ of following quenching 20min～5h; Conditions of exposure is control exposure electric current 2～5A, time for exposure 20～200s; Development is the sample that exposure finishes to be developed put into distilled water behind 1～20s and clean residual developer solution in developer solution.
3, the method for constituting 3-D structure as claimed in claim 1, it is characterized in that: impression is to coat one layer of polymeric performed polymer or uv-exposure glue precursor on level and smooth substrate, tip upside down on after smoothening on the photoresist template with micron or submicrometer structure, under 10～20bar pressure, keep 5～60min, polymer performed polymer or uv-exposure glue are coated with in the gap that precursor coating is squeezed into photoresist, thereby form polymer performed polymer or uv-exposure glue precursor pattern with the photoresist structure complementation.
4, the method for constituting 3-D structure as claimed in claim 1, it is characterized in that: substrate is monocrystalline silicon, glass, ito glass, quartz, mica sheet, polymethyl methacrylate, polystyrene, Merlon, polyethylene, polyvinyl chloride, polypropylene or the metal with smooth flat, or the above-mentioned substrate of modifying through the unimolecule self-assembling method.
5, the method for constituting 3-D structure as claimed in claim 4, it is characterized in that: substrate is the process preliminary treatment before using, Inorganic Non-metallic Materials or polymeric material make cleaning surfaces and hydrophilic with oxygen plasma system handles 1～30min, are convenient to the spin-coating film of photoresist; Metal material cleans 1～30min with chloroform, acetone, methyl alcohol, high purity water excusing from death successively, makes fully cleaning of surface.
6, the method for constituting 3-D structure as claimed in claim 1 is characterized in that: polymer performed polymer coating is dimethyl silicone polymer, acrylic acid double cyclopentenyl ester, phthalic acid two rare third fat or epoxy resin.
7, the method for constituting 3-D structure as claimed in claim 1, it is characterized in that: polymerization is that substrate with polymer performed polymer and the alternate structure of photoresist is at 60～200 ℃ of following polymerization 2～20h, or with the substrate of uv-exposure glue precursor and the alternate structure of the photoresist 3～30min that exposes under 100～1000W exposure power.
8, the method for constituting 3-D structure as claimed in claim 1, it is characterized in that: utilizing organic solvent to select wash-out is that the sample of having constructed sandwich construction is put into ethanol or acetone, soak 1～15min, photoresist in micron or the submicrometer structure photoresist template is washed away fully, under substrate, obtain the Three-dimension Target micro-structural at last.
9, the constructed application of three-dimensional microstructures aspect photonic propulsion device, sensor, microfluidic device, micro electromechanical system, photonic crystal, three-dimensional connection waveguide, super prism, microreactor and catalyst carrier of any one method of claim 1-8.
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