CN101837950A - Device and method for assembling nanostructure directly by using two-block copolymer - Google Patents
Device and method for assembling nanostructure directly by using two-block copolymer Download PDFInfo
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- CN101837950A CN101837950A CN 201010179564 CN201010179564A CN101837950A CN 101837950 A CN101837950 A CN 101837950A CN 201010179564 CN201010179564 CN 201010179564 CN 201010179564 A CN201010179564 A CN 201010179564A CN 101837950 A CN101837950 A CN 101837950A
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Abstract
The invention relates to a device and a method for assembling a nanostructure directly by using two-block copolymer. The whole device comprises a conductive template with a chemical surface pattern, the two-block copolymer PS-b-PMMA, a conductive substrate and a direct current electric field, wherein the two-block copolymer PS-b-PMMA is arranged between the conductive template and the substrate. Orientation and morphology of micro-phase separation of the two-block copolymer are regulated and controlled by combined action of the conductive template with the chemical surface pattern and the electric field, thus promoting the micro-phase separation of the two-block copolymer to be arranged controllably and orderly to a certain degree and assembling the nanostructure directly. The device and the method can realize the manufacturing of large-area Sub-10nm structures of long-range order and are especially suitable for the manufacturing of high-density nanometer pores in periodical array, nanometer columns and layered nanostructures and the like.
Description
Technical field
The present invention relates to belong to nanostructured and make the field, relate in particular to the apparatus and method that a kind of template and electric field are induced assembling nanostructure directly by using two-block copolymer.
Background technology
The nanostructured manufacturing is the basic and crucial of nanotechnology research and application, at present the manufacturing of nanostructured is mainly by two kinds of approach: a kind of is " (Top-down) from top to bottom " method (for example electron-beam direct writing, optical lithography, focused particle beam, etching, nano impression, soft lithographic etc.), and another kind is " (Bottom-up) from bottom to top " method (for example scan-probe micro-manufactured, dip in a nano-photoetching, biomolecule self assembly, template assist self assembly etc.).The block copolymer self assembly is a kind of nanostructured new method of constructing from bottom to top that developed recently gets up.Block copolymer (BlockCopolymers) be block copolymer again, by the homopolymerization segment that the different structure unit is formed, is incorporated into the copolymer of main chain by covalent bond.Different homopolymerization segments can be two or more, and every segment only contains a kind of construction unit, and the length of each segment does not have strict restriction.Because being connected by chemical bond by mutual exclusive segment on the thermodynamics, block copolymer forms, this design feature causes block copolymer not have the macroface separating behavior of blend, micron-scale phase separation can only take place, and forms colourful ordered phase form on meso-scale.These microcosmic ordered phase forms have good Modulatory character and relatively easy preparation method, composition, the chain length by changing block copolymer, apply the outfield or change preparation method etc. and can make block copolymer see pattern by Jie that self assembly produces various high-sequentials.The self-assembling technique of block copolymer has become a kind of very potential nanostructured manufacture method from bottom to top.
But also there is intrinsic defective in the block copolymer self-assembly process: if not further constraint, the self assembly domain structure does not have first-selected orientation and forms unordered " fingerprint " structure under the nature.And the topmost limitation of periodic nano-structure that is formed for different nanometer technologies application with block copolymer is: local self-assembled structures is very accurate, but realizes the nano-micro structure arrangement of long-range order in being difficult on a large scale.Therefore, how low-cost, and simple realize regulating and control that pattern is various, the degree of order is high, the self-assembled nanometer micro-structural of good stability according to people's will, form the nanostructured of large tracts of land, long-range order, for further expanding the application of block copolymer self assembly ordered nano-structure in nanometer technology, be a technical barrier that presses for solution.In addition, how methods such as top-down electron-beam direct writing, optical lithography, nano impression and etching and self-assembling method from bottom to top organically being combined the nanostructured for preparing large tracts of land, arbitrary shape complexity, also is hot issue and the advanced subject that presses for solution in the present nanometer manufacturing field.
Block copolymer self assembly at present mainly adopts single outfield (electric field, surface field, the mechanical field of force etc.) to regulate and control the block copolymer self-assembled nano structures, what impel block copolymer microcell orientations is the single shaft driving force, this causes self-assembled structures that As time goes on decay can take place, and can produce more defective.
In addition, the method of the direct assembling nanostructure of template-mediated block copolymer also has following limitation at present: the repeat usage of template is low, be difficult to realize to repeat the manufacturing with the uniformity nanostructured, can't realize the manufacturing of the low-cost and mass of nanostructured.
Although nano-imprint lithography be a kind of high rate/low cost production and and high accuracy nanostructured manufacture method, but at present it faces making, the chromatography precision of 1:1 impressing mould, the challenge such as service life, productivity ratio and defective of mould for it, and especially die deformation, adhesion (big force of impression causes) and filling are incomplete etc. is unusual stubborn problem.Limited the more extensive use of nanometer embossing.Therefore, press for the new nanostructured manufacture method of exploitation.
Summary of the invention
It is poor that purpose of the present invention solves present block copolymer self assembly manufacturing nanostructured production cost height (recycling rate of waterused of template is low), production efficiency low (the self assembly time is long), uniformity and repeatable manufacturing exactly, and the problem that is difficult to realize the manufacturing of large tracts of land, long-range order nanostructured, provide a kind of and have that production cost is low, technology simple, high conformity, be fit to mass and prepare the template of large tracts of land, long-range order nanostructured and the apparatus and method that electric field is induced assembling nanostructure directly by using two-block copolymer.
To achieve these goals, the present invention takes following technical solution:
A kind of template and electric field are induced the device of assembling nanostructure directly by using two-block copolymer, it comprises the substrate and the DC electric field of a conduction template with chemical surface figure, polystyrene-poly methyl methacrylate PS-b-PMMA di-block copolymer, conductionization, wherein di-block copolymer PS-b-PMMA places between conduction template and the substrate, the conduction template is connected with the anode of DC electric field, and substrate then is connected with the negative electrode of DC electric field.
Described substrate is made up of the conductive metal layer of laying on silicon substrate and the silicon substrate, and conductive metal layer is connected with the negative electrode of DC electric field.
Described conduction template is made up of conductive layer and mould with chemical surface figure of modification, and conductive layer is connected with anode, and the chemical surface figure has preference or wellability mutually to di-block copolymer PMMA, then is neutrality to the infiltration of PS phase.
A kind of template and electric field are induced the method for assembling nanostructure directly by using two-block copolymer, its " from top to bottom " and " from bottom to top " nanostructured manufacture method of combining that is a kind of, and its concrete steps are:
1) makes the conduction template;
2) to substrate pretreatment;
3) spin coating di-block copolymer PS-b-PMMA in substrate;
4) apply the direct assembling nanostructure of DC electric field and annealing in process;
5) remove the conduction template, the template of will conducting electricity is separated with di-block copolymer;
Crosslinking curing PS phase when 6) degree of depth UV exposure degraded PMMA is identical;
7) remove the PMMA phase;
8) PS phase figure is transferred to substrate.
In the described step 3), spin coating di-block copolymer PS-b-PMMA in substrate, its volume fraction
fBe 0.6-0.8, its thickness is 1-3 μ m.
In the described step 4), between conduction template and substrate, apply DC electric field 30～40V/ μ m perpendicular to substrate, its anode links to each other with the conduction template, negative electrode links to each other with substrate, and under 160 ℃～190 ℃, annealed 8-12 hour, di-block copolymer generation microphase-separated is directly assembled out the layered nano-structure perpendicular to substrate; Nanostructured
xWith
yDirection character depends on the graphic feature on the template,
zGrowth to character shape is controlled by extra electric field and di-block copolymer primary coat thickness.
In the described step 6), adopt the DUV exposure, dosage is 25J/cm
2, the time for exposure is 2-5 minute, thereby in degraded PMMA crosslinking curing PS phase when identical.
In the described step 7), remove the PMMA phase time and use glacial acetic acid to soak 2-4 hour, thereby the PMMA phase after decomposing is removed in dissolving.
Method of inducing polystyrene-poly methyl methacrylate (PS-b-PMMA) assembling nanostructure directly by using two-block copolymer based on template and many in electric field of the present invention, its basic principle is: the orientation and the form of conduction template (surface field) by having the chemical surface figure and electric field acting in conjunction regulation and control di-block copolymer microphase-separated, impel the di-block copolymer microphase-separated to carry out controlled orderly arrangement to a certain extent, directly assemble out nanostructured.Compare with the single game control technique, apply the combination in two kinds of outfields, control the orientations of block copolymer microcell with the twin shaft driving force, can avoid the decay of self assembly ordered nano micro-structural, many defectives of self assembly ordered nano-structure have been reduced simultaneously, and can effectively shorten the time of self assembly, realize the manufacturing of large tracts of land, long-range order nanostructured.In order to realize the multiplexing of template and can to repeat manufacturing with the uniformity nanostructured, use for reference the principle of nano impression, template is inverted on block copolymer, rear pattern plate is finished in self assembly and block copolymer is separated from each other (being equivalent to the demoulding of nano impression).This realizes the multiplexing of template on the one hand, on the other hand owing to there is not the existence of force of impression, template is little with section copolymer adhesiveness, be easy to the demoulding, avoided nano impression because polymer and template adhesion or the adhesion that bigger force of impression causes, cause demoulding difficulty, and the many defectives that not exclusively cause owing to filling.This is different from nano impression fully based on the shaping principle that pressure-driven causes resist to be out of shape, and has overcome adhesion of metallic mold for nano-imprint and resist and filling and has not exclusively waited technical barrier.
Template and electric field induce the apparatus and method of the direct assembling nanostructure of block copolymer as follows.Whole device is made up of four parts: the conduction template with chemical surface figure; Di-block copolymer PS-b-PMMA; The substrate of conductionization; DC electric field (its anode links to each other with template, and negative electrode links to each other with substrate).Template is made up of conductive layer and mould with chemical surface figure, and the chemical surface figure has preference or good wellability mutually to di-block copolymer PMMA, and the infiltration of PS phase is then shown as neutrality.Template and electric field are induced the concrete grammar of the direct assembly nanostructured of di-block copolymer:
(1). di-block copolymer PS-b-PMMA is spin-coated on the conductive substrates (substrate); Between conductive die and substrate, apply DC electric field subsequently, and carry out annealing in process, induce di-block copolymer generation microphase-separated down in template and electric field, and be orientated and arrange, directly assemble out the nanostructured of high-sequential according to the direction of design;
(2). template is removed, adopt degree of depth UV exposure then, crosslinking curing PS phase when degraded PMMA is identical;
(3). remove the PMMA phase, copy the feature structure of template at PS on mutually.
The made nanostructured
xWith
yDirection character depends on the graphic feature on the template,
zGrowth to character shape is controlled by extra electric field and di-block copolymer primary coat thickness.
This method can be transferred to pattern image on substrate or other functional material further combined with technologies such as " deposition ", " electroforming ", " etching ", " Lift-off ", realizes the making of function nano structure (metal or nonmetal).
The notable feature of this method is: it is the nanometer manufacture method that a kind of " from top to bottom " and " from bottom to top " combine for (1); (2) can realize the inferior 10nm(Sub-10nm of large tracts of land, long-range order) manufacturing of structure; (3) the self assembly time is short; Template can be reused (this had not only realized repeating with conforming manufacturing but also greatly reducing production cost of nanostructured); (4) this method is particularly suitable for the manufacturing of high density and nanostructureds such as cyclic array nano-pore, nano-pillar and stratiform; (5) have that cost is low, uniformity and favorable repeatability, be fit to the advantage that mass is made.
Description of drawings
Fig. 1 is that template of the present invention and electric field are induced the assembling nanostructure directly by using two-block copolymer process route chart.
Fig. 2 a is that template of the present invention and electric field induce di-block copolymer directly to assemble the apparatus and method schematic diagram of layered nano-structure.
Fig. 2 b is that template of the present invention and electric field induce di-block copolymer directly to assemble the apparatus and method schematic diagram of layered nano-structure.
Fig. 2 c is that template of the present invention and electric field induce di-block copolymer directly to assemble the apparatus and method schematic diagram of layered nano-structure.
Fig. 3 a is that the present invention has the structure of chemical surface figure conduction template and makes schematic diagram.
Fig. 3 b is that the present invention has the structure of chemical surface figure conduction template and makes schematic diagram.
Fig. 3 c is that the present invention has the structure of chemical surface figure conduction template and makes schematic diagram.
Fig. 3 d is that the present invention has the structure of chemical surface figure conduction template and makes schematic diagram.
Fig. 3 e is that the present invention has the structure of chemical surface figure conduction template and makes schematic diagram.
Fig. 3 f is that the present invention has the structure of chemical surface figure conduction template and makes schematic diagram.
Wherein, 1. the conduction template, 2. di-block copolymer PS-b-PMMA, 21.PS phase, 22.PMMA phase, 3. substrate, 4. DC electric field, 5. silicon substrate, 6. conductive metal layer, 7 have the mould of the chemical surface figure of modification, 71. there is not the self assembled monolayer PETS of modification, 72. the self assembled monolayer PETS after the modification, 8. tin indium oxide ITO, 9. photoresist.
The specific embodiment
The present invention is described in further detail below in conjunction with drawings and Examples.
Among Fig. 2 a-Fig. 2 c, it comprises the substrate 3 and the DC electric field 4 of a conduction template 1 with chemical surface figure, di-block copolymer PS-b-PMMA2, conductionization, wherein di-block copolymer PS-b-PMMA2 places between conduction template 1 and the substrate 3, conduction template 1 is connected with the anode of DC electric field 4, and 3 negative electrodes with DC electric field 4 of substrate are connected.
Wherein, substrate 3 is made up of the conductive metal layer of laying on silicon substrate 5 and the silicon substrate 56, and conductive metal layer 6 is connected with the negative electrode of DC electric field 4.
Di-block copolymer PS-b-PMMA2 21 22 is made of with PMMA mutually mutually PS.
The processing technology routine of inducing assembling nanostructure directly by using two-block copolymer based on template and electric field comprises referring to Fig. 1: 1. conduct electricity the manufacturing of template 1; 2. substrate 3 preliminary treatment; 3. spin coating di-block copolymer PS-b-PMMA2 in substrate 3; 4. apply DC electric field 4 and the direct assembling nanostructure of annealing in process; 5. remove conduction template 1; 6. degree of depth UV exposure degraded PMMA crosslinked PS mutually 21 22 time mutually; 7. remove the PMMA phase 22 of di-block copolymer PS-b-PMMA2; 8. PS phase figure is transferred to substrate or other functional material.
The present invention is with the embodiment that is made as perpendicular to substrate 3 layered nano-structures, and Fig. 2 a-Fig. 2 c is based on the apparatus and method schematic diagram of manufacturing of the present invention perpendicular to the layered nano-structure of substrate.Concrete manufacturing process steps:
1) manufacturing of conduction template
The conduction template 1 that the present invention uses is made up of with the mould 7 with chemical surface figure of modification tin indium oxide ITO8, mould chemistry surfacial pattern (surface field) 22 has preference or good wellability mutually to di-block copolymer PMMA, to PS mutually 21 infiltration then show as neutrality.Fig. 3 a-Fig. 3 f is that the present invention has structure and the schematic diagram of fabrication technology that chemical surface figure conduction template is made.This template is a conductive layer with tin indium oxide (ITO), the chemical surface figure is a matrix material with self assembled monolayer Phenylethyltrichlorosilane (PETS), handle by the graphics field being carried out chemical modification, make this zone preference PMMA phase 22, promptly PMMA mutually 22 is had good imbibition characteristic, to PS mutually 21 infiltration then show as neutrality.The concrete manufacture method of template: (a) among Fig. 3 a, be substrate, form self assembled monolayer PETS thereon with tin indium oxide ITO8; (b) among Fig. 3 b, spin coating photoresist 9 on self assembled monolayer PETS; (c) among Fig. 3 c, obtain groove after electron beam exposure, the development and accommodate a meter structure graph; (d) among Fig. 3 d, the figure chemical modification of exposure is handled, and makes it the 22 self assembled monolayer PETS72 that have after good wellability (with soft X-ray irradiation, exposure figure is modified, this zone preference PMMA phase 22 in oxygen atmosphere) becomes modification mutually to PMMA; (e) among Fig. 3 e, remove photoresist, unexposed figure (self assembled monolayer that does not have modification is PETS71) keeps neutral to di-block copolymer.Template vertical view after completing is shown in Fig. 3 f.
2) substrate 3 preliminary treatment
For non-conductive substrate 3, need generate one deck conductive metal layer 6 thereon, make substrate have electric conductivity.Present embodiment is substrate with the silicon substrate (Gold-coatedsiliconsubstrate) that coats gold.
3) spin coating di-block copolymer PS-b-PMMA2
Spin coating di-block copolymer PS-b-PMMA2(volume fraction in substrate 3
fBe 0.7), its thickness is 1 μ m.
4) apply DC electric field 4 and the direct assembling nanostructure of annealing in process
Apply the DC electric field 30V/ μ m perpendicular to substrate 3 between conduction template 1 and substrate 3, its anode links to each other with conduction template 1, and negative electrode links to each other with substrate 3.And under 170 ℃, annealed 10 hours, microphase-separated takes place in di-block copolymer PS-b-PMMA2, directly assembles out the layered nano-structure perpendicular to substrate 3.
5) the conduction template removes
The conduction template is separated with di-block copolymer PS-b-PMMA2, removes template.
6) PMMA of degree of depth UV exposure degraded di-block copolymer PS-b-PMMA2 crosslinking curing PS mutually 21 22 time mutually;
(dosage is 25J/cm in the DUV exposure
2), in degraded PMMA phase 22 while crosslinking curing PS phase 21.
7) remove PMMA phase 22
The use glacial acetic acid soaked 2 hours, and the PMMA phase 22 after decomposing is removed in dissolving.
8) PS phase figure is transferred to substrate or other functional material
By technologies such as " etching ", " deposition ", " electroforming ", " Lift-off " pattern image is transferred on substrate or other functional material, realized the making of function nano structure (metal or nonmetal).
DC electric field 4 scopes that the present invention applies between conduction template 1 and substrate 3 are 30～40V/ μ m;
Of the present invention can also use vacuum aluminum-coated on the poly-phthalimide film (AluminizedKapton, Kapton/AI) or silicon (Silicon) be substrate.
The annealing temperature that the present invention uses must be higher than the glass transition temperature (be 105 ℃ for PS promptly, PMMA is 115 ℃) of di-block copolymer two phase-splittings, and annealing temperature adopts 160 ℃～190 ℃.
Claims (8)
1. the device of an assembling nanostructure directly by using two-block copolymer, it is characterized in that, it comprises the substrate and the DC electric field of a conduction template with chemical surface figure, polystyrene-poly methyl methacrylate PS-b-PMMA di-block copolymer, conductionization, wherein di-block copolymer PS-b-PMMA places between conduction template and the substrate, the conduction template is connected with the anode of DC electric field, and substrate then is connected with the negative electrode of DC electric field.
2. the device of assembling nanostructure directly by using two-block copolymer as claimed in claim 1 is characterized in that, described substrate is made up of the conductive metal layer of laying on silicon layer and the silicon layer, and conductive metal layer is connected with the negative electrode of DC electric field.
3. the device of assembling nanostructure directly by using two-block copolymer as claimed in claim 1, it is characterized in that, described conduction template is made up of conductive layer and the mould with chemical surface figure of modification, conductive layer is connected with anode, the chemical surface figure has preference or wellability mutually to di-block copolymer PMMA, then is neutral to the infiltration of PS phase.
4. a method that adopts the described assembling nanostructure directly by using two-block copolymer of claim 1 is characterized in that, it is from top to bottom a kind of and the nanometer manufacture method that combines from bottom to top, and its concrete steps are:
1) makes the conduction template;
2) to substrate pretreatment;
3) spin coating di-block copolymer PS-b-PMMA in substrate;
4) apply the direct assembling nanostructure of DC electric field and annealing in process;
5) remove the conduction template, the template of will conducting electricity is separated with di-block copolymer;
Crosslinking curing PS phase when 6) degree of depth UV exposure degraded PMMA is identical;
7) remove the PMMA phase;
8) PS phase figure is transferred to substrate.
5. template as claimed in claim 4 and electric field are induced the method for assembling nanostructure directly by using two-block copolymer, it is characterized in that, and in the described step 3), in substrate during spin coating di-block copolymer PS-b-PMMA, its volume fraction
fBe 0.6-0.8, its thickness is 1-3 μ m.
6. template as claimed in claim 4 and electric field are induced the method for assembling nanostructure directly by using two-block copolymer, it is characterized in that, in the described step 4), between conduction template and substrate, apply DC electric field 30～40V/ μ m perpendicular to substrate, its anode links to each other with the conduction template, and negative electrode links to each other with substrate, and anneals 8-12 hour down at 160 ℃～190 ℃, di-block copolymer generation microphase-separated is directly assembled out the layered nano-structure perpendicular to substrate; Nanostructured
xWith
yDirection character depends on the graphic feature on the template,
zGrowth to character shape is controlled by extra electric field and di-block copolymer primary coat thickness.
7. template as claimed in claim 4 and electric field are induced the method for assembling nanostructure directly by using two-block copolymer, it is characterized in that, in the described step 6), adopt the DUV exposure, and dosage is 25J/cm
2, the time for exposure is 2-5 minute, thereby in degraded PMMA crosslinking curing PS phase when identical.
8. template as claimed in claim 4 and electric field are induced the method for assembling nanostructure directly by using two-block copolymer, it is characterized in that, in the described step 7), remove the PMMA phase time and use glacial acetic acid to soak 2-4 hour, thereby the PMMA phase after decomposing is removed in dissolving.
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| CN102915907A (en) * | 2011-08-02 | 2013-02-06 | 中芯国际集成电路制造(北京)有限公司 | Semiconductor device manufacturing method |
| CN103035510A (en) * | 2011-10-08 | 2013-04-10 | 中芯国际集成电路制造(上海)有限公司 | Contact through hole etching method |
| CN103515191A (en) * | 2012-06-20 | 2014-01-15 | 中芯国际集成电路制造(上海)有限公司 | Semiconductor structure and forming method thereof |
| CN104181770A (en) * | 2014-09-10 | 2014-12-03 | 青岛理工大学 | Method for manufacturing micro/nano composite structure based on 4D printing and nanoimprint lithography |
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| US10633533B2 (en) | 2014-09-30 | 2020-04-28 | Lg Chem, Ltd. | Block copolymer |
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| CN102915907A (en) * | 2011-08-02 | 2013-02-06 | 中芯国际集成电路制造(北京)有限公司 | Semiconductor device manufacturing method |
| CN102915907B (en) * | 2011-08-02 | 2015-05-13 | 中芯国际集成电路制造(北京)有限公司 | Semiconductor device manufacturing method |
| CN103035510B (en) * | 2011-10-08 | 2015-08-19 | 中芯国际集成电路制造(上海)有限公司 | Contact through hole lithographic method |
| CN103035510A (en) * | 2011-10-08 | 2013-04-10 | 中芯国际集成电路制造(上海)有限公司 | Contact through hole etching method |
| CN103515191A (en) * | 2012-06-20 | 2014-01-15 | 中芯国际集成电路制造(上海)有限公司 | Semiconductor structure and forming method thereof |
| CN103515191B (en) * | 2012-06-20 | 2016-05-25 | 中芯国际集成电路制造(上海)有限公司 | Semiconductor structure and forming method thereof |
| CN104181770A (en) * | 2014-09-10 | 2014-12-03 | 青岛理工大学 | Method for manufacturing micro/nano composite structure based on 4D printing and nanoimprint lithography |
| CN107077066A (en) * | 2014-09-30 | 2017-08-18 | 株式会社Lg化学 | The method for manufacturing patterned substrate |
| US10633533B2 (en) | 2014-09-30 | 2020-04-28 | Lg Chem, Ltd. | Block copolymer |
| CN107077066B (en) * | 2014-09-30 | 2021-04-02 | 株式会社Lg化学 | Method of manufacturing patterned substrate |
| CN107077066B9 (en) * | 2014-09-30 | 2021-05-14 | 株式会社Lg化学 | Method of manufacturing patterned substrate |
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| CN101837950B (en) | 2012-09-05 |
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