CN103676473A - Method for preparing metal pattern on curved surface by combining nano-imprinting with wet etching - Google Patents
Method for preparing metal pattern on curved surface by combining nano-imprinting with wet etching Download PDFInfo
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- CN103676473A CN103676473A CN201310551957.0A CN201310551957A CN103676473A CN 103676473 A CN103676473 A CN 103676473A CN 201310551957 A CN201310551957 A CN 201310551957A CN 103676473 A CN103676473 A CN 103676473A
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- 229910052751 metal Inorganic materials 0.000 title claims abstract description 55
- 239000002184 metal Substances 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 45
- 238000001039 wet etching Methods 0.000 title claims abstract description 24
- 239000003292 glue Substances 0.000 claims abstract description 17
- 238000001704 evaporation Methods 0.000 claims abstract description 15
- 230000008020 evaporation Effects 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 12
- 238000004528 spin coating Methods 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 9
- 229920000642 polymer Polymers 0.000 claims description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 7
- 239000001301 oxygen Substances 0.000 claims description 7
- 229910052760 oxygen Inorganic materials 0.000 claims description 7
- 238000001020 plasma etching Methods 0.000 claims description 7
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 6
- 229910052737 gold Inorganic materials 0.000 claims description 6
- 239000010931 gold Substances 0.000 claims description 6
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 6
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 239000011651 chromium Substances 0.000 claims description 5
- 229910052804 chromium Inorganic materials 0.000 claims description 5
- 229910052802 copper Inorganic materials 0.000 claims description 5
- 239000010949 copper Substances 0.000 claims description 5
- 238000007747 plating Methods 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- 239000010703 silicon Substances 0.000 claims description 5
- 239000000243 solution Substances 0.000 claims description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- 238000005566 electron beam evaporation Methods 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 3
- 239000000853 adhesive Substances 0.000 claims description 3
- 230000001070 adhesive effect Effects 0.000 claims description 3
- 239000004411 aluminium Substances 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 3
- 239000000178 monomer Substances 0.000 claims description 3
- 229910052709 silver Inorganic materials 0.000 claims description 3
- 239000004332 silver Substances 0.000 claims description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 2
- 229910016874 Fe(NO3) Inorganic materials 0.000 claims description 2
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- 229960000583 acetic acid Drugs 0.000 claims description 2
- 238000009835 boiling Methods 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 239000012362 glacial acetic acid Substances 0.000 claims description 2
- 239000003999 initiator Substances 0.000 claims description 2
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-M acrylate group Chemical group C(C=C)(=O)[O-] NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims 2
- 238000005530 etching Methods 0.000 abstract description 5
- 230000003287 optical effect Effects 0.000 abstract description 5
- 239000000835 fiber Substances 0.000 abstract description 3
- 230000007547 defect Effects 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000000992 sputter etching Methods 0.000 abstract 2
- 238000001723 curing Methods 0.000 description 11
- 238000010276 construction Methods 0.000 description 6
- 239000000758 substrate Substances 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000004049 embossing Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 229920001169 thermoplastic Polymers 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical group COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 229920005573 silicon-containing polymer Polymers 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000004642 Polyimide Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 101100460147 Sarcophaga bullata NEMS gene Proteins 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- HGAZMNJKRQFZKS-UHFFFAOYSA-N chloroethene;ethenyl acetate Chemical compound ClC=C.CC(=O)OC=C HGAZMNJKRQFZKS-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001312 dry etching Methods 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 238000001883 metal evaporation Methods 0.000 description 1
- 238000000059 patterning Methods 0.000 description 1
- 238000001259 photo etching Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 239000004926 polymethyl methacrylate Substances 0.000 description 1
- -1 polypropylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 230000004304 visual acuity Effects 0.000 description 1
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- Shaping Of Tube Ends By Bending Or Straightening (AREA)
- Diffracting Gratings Or Hologram Optical Elements (AREA)
Abstract
The invention discloses a method for preparing a metal pattern on a curved surface by combining nano-imprinting with wet etching. The method comprises the following steps: firstly, evaporating one layer of metal on the curved surface; then imprinting a pattern on the metal by a transferring method; etching to remove a residual layer by a reaction ion etching method; etching the metal to a base by taking imprinting glue as a mask; and then removing the imprinting glue on the upper layer of the metal pattern by using the reaction ion etching to obtain the metal pattern. The method disclosed by the invention is simple and feasible; an ion lifting process is replaced on a plane to prepare the metal pattern; compared with a common ion lifting process, the integrity of the pattern is not easy to damage and the defects are reduced; the metal pattern is prepared on the curved surface and the process of preparing the pattern on the curved surface cannot be realized by the ion lifting process. The method has a wide application prospect in the fields of production of a fiber Bragg grating, a refraction/diffraction mixed optical element, a nano electromechanical system and the like.
Description
Technical field
The present invention relates to a kind of nanometer embossing that utilizes and in conjunction with wet etching, on curved surface, prepare the method for metal pattern.
Background technology
At curved surface and complex topography surface, prepare the concern that nanostructured is more and more subject to people recently, especially more and more extensive in the application in the fields such as artificial compound eye, semisphere electronic eyes camera, photovoltaic device, image sensor array, micro-executive component and Fibre Optical Sensor.Nineteen ninety-five, after people's invention nanometer embossings such as Steven Y.Chou, nanometer embossing relies on the advantages such as its high-level efficiency, high resolving power and low cost in microstructure making field, attracted many scientific research personnel and engineering technical personnel's concern.Although current many micro-nano process technologies can both be prepared on planar substrate surface patterning nanostructured, these technology are mostly not suitable for preparing nano-pattern at nonplanar substrate surface.Therefore need the curved surface nano-pattern preparation method of a kind of with low cost, reliable in quality of exploitation badly.By elastic body soft template, can on curved surface, impress out various nano-patterns at present, but so far, no matter be which kind of photoetching or stamping technique, all metal pattern can not be transferred to curved surface and get on.
The preparation technology of now conventional metal pattern realizes by lifting off technique.This technique is to adopt thermoplastic polymer for lifting off layer, on thermoplastic-polymer solution spin coating and substrate, then direct heat impresses, or the siliceous thermosetting of spin coating impresses glue again on it, by reactive ion etching, remove remnant layer, after evaporation metal, in organic solvent, utilize the dissolubility of thermoplastic polymer and remove the metal on residual polymer, thereby obtaining suprabasil metal pattern.Lift off technique and need to obtain and lift off uniformly layer, and on curved surface, be impossible utilize the technique of spin coating to obtain uniform film; And utilize soft template to carry out curved surface impression, and can only impress glue with ultra-violet curing to impress, and impression glue has formed cross-linked network after solidifying under ultraviolet lighting, thereby cannot be dissolved in again among organic solvent, cannot realize and lifting off.
Summary of the invention
For deficiency of the prior art, the object of the invention is to propose a kind of method of preparing metal construction on curved surface.
The method of preparing metal construction on curved surface that the present invention proposes is in conjunction with wet etching method based on ultraviolet nanometer impression.Be characterized in first evaporation layer of metal film on curved surface, then on metal film, by two transfer methods, adopt soft impression block stamping structure ultra-violet curing, etching is removed remnant layer, expose after metal, using remaining polymkeric substance as etch mask again, wet etching metal, then obtain final metal construction after removing polymer mask by reactive ion etching.
The concrete technical scheme of the present invention is as follows:
Nano impression is prepared the method for metal pattern on curved surface in conjunction with wet etching, concrete steps are as follows:
1) first curved-surface materials surface is cleaned up with deionized water, the dry rear method evaporation layer of metal film on curved-surface materials that passes through electron beam evaporation plating or magnetron sputtering, metal can be gold, silver, copper, aluminium or chromium, and thickness is 1～100 nanometer;
2) at clean silicon chip surface spin coating one deck ultra-violet curing impression glue, this ultraviolet solidified nano impression glue for the performed polymer containing (methyl) acrylate group, containing the monomer of (methyl) acrylate group or the above two potpourri in being dissolved with ultraviolet initiator high boiling solvent solution;
3) flexible nano impression block is covered on the impression glue that spin coating is good, crosses and after 1-5 minute, to be covered on the curved surface that is coated with metal prepared by step 1), and ultra-violet curing;
4) after impression adhesive curing, surperficial impression soft template is removed, obtained the polymkeric substance stamping structure on curved surface, under stamping structure, have the uniform metallic film of one deck;
5) adopt oxygen plasma to carry out reactive ion etching, remove impression glue;
6) in corrosive liquid, take cure polymer carries out wet etching as mask;
7) with oxygen plasma, carry out reactive ion etching, remove curing polymkeric substance, thereby on curved surface, obtain metallic pattern.
When evaporation metal is gold or when silver-colored, the aqueous solution that consists of Fe(NO3)39H2O and thiocarbamide of wet etching liquid, its pH value is adjusted to as 1-5 with watery hydrochloric acid; When evaporation metal is copper, the aqueous solution that consists of iron chloride of wet etching liquid; When evaporation metal is chromium, the glacial acetic acid solution that consists of ammonium ceric nitrate of wet etching liquid.
The present invention is simple, both can substitute in the plane to lift off technique and prepare metal pattern, than the conventional integrality that lifts off the more survivable figure of technique and reduce the generation of defect; Can on curved surface, prepare metal pattern again, and prepare pattern on curved surface, lift off technique and cannot realize.Method of the present invention had both been utilized the ultra-violet curing of existing impression glue, can by the technique lifting off, on curved surface, not obtain high-resolution nano-pattern again, thereby for the preparation of various novel micro nanometer device elements lays the first stone, manufacturing bragg grating (fiber Bragg grating), roll over/spread out mixed optical element (Hybrid Optics), receive Mechatronic Systems (NEMS) field and have broad application prospects.Up to now, any report that not yet has this method.
Accompanying drawing explanation
Fig. 1 is method flow diagram of the present invention.
Embodiment
Below in conjunction with accompanying drawing, this method is further described.
The present invention proposes a kind of method prepared by novel metallic pattern, the method is by metal evaporation, on curved surface, plate equably layer of metal film, then the method impressing by two transfers on curved surface is prepared the microstructure of polymkeric substance on metallic film, afterwards, by reactive ion etching, remove remnant layer again and expose substrate, and take remaining polymkeric substance as mask carries out wet etching, the metal film of lower floor is eroded away to required figure.Concrete operation step is as follows:
(1) evaporation metal on curved surface
First on curved surface, adopt plating layer of metal, this metal can be gold, silver, copper, aluminium, chromium.Can adopt the method for electron beam evaporation plating, also can adopt the method for magnetron sputtering, the thickness of evaporation metal is 1～100 nanometer.
(2) two transfer methods imprinted pattern on curved surface
First on silicon chip, spin coating one deck ultra-violet curing impresses glue, and this impression glue can, with conventional various not siliceous liquid ultra-violet curing monomer or performed polymer, include but are not limited to CN975, CN996 etc.Then the soft template being made by dimethyl silicone polymer is covered thereon, after 1～5 minute, opened, and be covered on the curved surface that is coated with metal, and under high-pressure sodium lamp, irradiate and solidify under the condition of nitrogen protection.After impression adhesive curing, template is taken off, obtained the structure of polymkeric substance.
(3) wet etching is prepared metal construction on curved surface
Adopt oxygen plasma etch, the remnant layer of polymer architecture is removed, expose after lower metal, by metal placement and corrosive liquid, corrode to exposing after substrate, then remove polymkeric substance with oxygen plasma etch, obtain the metal pattern on curved surface.
The present embodiment is prepared golden optical grating construction in conjunction with wet etching at curved surface with nano impression.
The substrate with curved surface can be the plastics such as silicon, silicon dioxide, silicon nitride and tygon, polypropylene, polymethylmethacrylate, polyimide.First with electron beam evaporation plating, plate 30 nm of gold on curved surface, standby.
The CN975(Sartomer company that spin coating 80 nanometers contain 3% light trigger on silicon chip in addition), dimethyl silicone polymer soft template is covered thereon, its structure is optical grating construction, and the cycle is 550 nanometers, and gash depth is 110 nanometers.After 3 minutes, soft template is thrown off, then soft template is covered in and is coated with on golden curved surface, under nitrogen protection, 100 watts of high-pressure sodium lamp ultra-violet curings, after 15 minutes, are thrown off soft template, obtain impressing the structure of glue.
By the curved surface that impression has a structure above dry etching 15 seconds in oxygen plasma, remove the remnant layer of stamping structure, in etching liquid, wet etching is 5 minutes, and etching liquid is the Fe (NO that contains 50mmol/L
3)
3.9H
2the aqueous solution of O and 30mmol/L thiocarbamide.
Claims (5)
1. nano impression is prepared the method for metal pattern on curved surface in conjunction with wet etching, it is characterized in that, concrete steps are as follows:
1) first curved-surface materials surface is cleaned up with deionized water, dry rear by method evaporation layer of metal film on curved-surface materials of electron beam evaporation plating or magnetron sputtering;
2) at clean silicon chip surface spin coating one deck ultra-violet curing impression glue;
3) flexible nano impression block is covered on the impression glue that spin coating is good, crosses and after 1-5 minute, to be covered on the curved surface that is coated with metal prepared by step 1), and ultra-violet curing;
4) after impression adhesive curing, surperficial impression soft template is removed, obtained the polymkeric substance stamping structure on curved surface, under stamping structure, have the uniform metallic film of one deck;
5) adopt oxygen plasma to carry out reactive ion etching, remove impression glue;
6) in corrosive liquid, take cure polymer carries out wet etching as mask;
7) with oxygen plasma, carry out reactive ion etching, remove curing polymkeric substance, thereby on curved surface, obtain metallic pattern.
2. nano impression according to claim 1 is prepared the method for metal pattern on curved surface in conjunction with wet etching, it is characterized in that step 2) ultraviolet solidified nano of spin coating impression glue is for the performed polymer containing acrylate group, containing monomer or the solution of both potpourris in being dissolved with ultraviolet initiator high boiling solvent of acrylate group.
3. nano impression according to claim 1 is prepared the method for metal pattern on curved surface in conjunction with wet etching, it is characterized in that, the metal of step 1) institute evaporation is gold, silver, copper, aluminium or chromium.
4. nano impression according to claim 3 is prepared the method for metal pattern on curved surface in conjunction with wet etching, it is characterized in that, the thickness of evaporation metal is 1～100 nanometer.
5. according to the nano impression described in claim 3 or 4, in conjunction with wet etching, on curved surface, prepare the method for metal pattern, it is characterized in that, when evaporation metal is gold or when silver-colored, the aqueous solution that consists of Fe(NO3)39H2O and thiocarbamide of wet etching liquid, its pH value is adjusted to as 1-5 with watery hydrochloric acid; When evaporation metal is copper, the aqueous solution that consists of iron chloride of wet etching liquid; When evaporation metal is chromium, the glacial acetic acid solution that consists of ammonium ceric nitrate of wet etching liquid.
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| CN201310551957.0A CN103676473B (en) | 2013-11-08 | 2013-11-08 | The method that nano impression prepares metal pattern in conjunction with wet etching on curved surface |
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| CN201310551957.0A CN103676473B (en) | 2013-11-08 | 2013-11-08 | The method that nano impression prepares metal pattern in conjunction with wet etching on curved surface |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105448799A (en) * | 2015-11-25 | 2016-03-30 | 东莞同济大学研究院 | Curved surface film circuit manufacture method based on laser projection technology |
| CN105448800A (en) * | 2015-11-25 | 2016-03-30 | 东莞同济大学研究院 | Manufacturing method for curved surface film circuit based on 3D printing technology |
| CN105858591A (en) * | 2016-03-29 | 2016-08-17 | 中国科学院高能物理研究所 | Metal micro-structure and manufacturing method thereof |
| CN106185791A (en) * | 2016-07-14 | 2016-12-07 | 重庆大学 | A kind of manufacturing processing technic of local hydrophobic material |
| CN107572834A (en) * | 2016-07-04 | 2018-01-12 | 正达国际光电股份有限公司 | A kind of bend glass processing technology |
| CN108008599A (en) * | 2017-12-27 | 2018-05-08 | 青岛天仁微纳科技有限责任公司 | Method, apparatus and mould preparation method for three-dimension curved surface nanoscale coining |
| CN109256477A (en) * | 2018-09-20 | 2019-01-22 | 合肥鑫晟光电科技有限公司 | The production method and QLED display device of hole injection layer for QLED |
| WO2019056586A1 (en) * | 2017-09-20 | 2019-03-28 | 南方科技大学 | Method for preparing optical metasurface |
| CN114016025A (en) * | 2021-10-29 | 2022-02-08 | 株洲中车时代半导体有限公司 | Metal film transfer method |
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| CN105448800B (en) * | 2015-11-25 | 2018-11-30 | 东莞同济大学研究院 | A kind of production method of the curved surface thin film circuit based on 3D printing technique |
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| CN109256477A (en) * | 2018-09-20 | 2019-01-22 | 合肥鑫晟光电科技有限公司 | The production method and QLED display device of hole injection layer for QLED |
| CN109256477B (en) * | 2018-09-20 | 2020-05-26 | 合肥鑫晟光电科技有限公司 | Manufacturing method of hole injection layer for QLED and QLED display device |
| CN114016025A (en) * | 2021-10-29 | 2022-02-08 | 株洲中车时代半导体有限公司 | Metal film transfer method |
| CN114016025B (en) * | 2021-10-29 | 2024-04-19 | 株洲中车时代半导体有限公司 | Metal film transfer method |
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