CN100380139C - Biological template method for preparing antireflection film - Google Patents
Biological template method for preparing antireflection film Download PDFInfo
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- CN100380139C CN100380139C CNB200510136315XA CN200510136315A CN100380139C CN 100380139 C CN100380139 C CN 100380139C CN B200510136315X A CNB200510136315X A CN B200510136315XA CN 200510136315 A CN200510136315 A CN 200510136315A CN 100380139 C CN100380139 C CN 100380139C
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Abstract
The present invention provides a method for preparing an anti-reflection thin film by serving a biological nanometer structure existing in the natural world as a template by second order duplication. The used biological template comprises an insect compound eye and anti-reflection photonic crystal on the surface of each wing. Firstly, the biological nanometer structure serves as the template to evaporate metal in vacuum, and a minus structure corresponding to the biological template is obtained on a metal thin film; then, the metal minus structure is used as the template to cast organic polymer, and an organic polymer film of which the surface is provided with the nanometer structure consistent to the biological template is obtained after the organic polymer is solidified. The anti-reflection thin film preparation technique of the present invention has the advantages of simple process, low cost and high yield and can realize large-area nanostructure preparation. The prepared organic polymer film of which the surface is provided with the nanometer structure has strong anti-reflection effect, successfully imitates the anti-reflection function of the nanometer structure on the biological surface and has wide application on optics.
Description
Technical field
The present invention relates to a kind of new nanostructured technology of preparing, being specifically related to a kind of is template with the biological structure, prepares the method for anti-reflection structure by the method for duplicating, and belongs to field of nano material preparation.
Background technology
The many organism surfaces of nature have micro-nano structure, these structures are that biotic population has special biological function at nature through very long evolution differentiation, with their existence closely bound up (Pete Vukusic and J.Roy Sambles, nature 424 (2003) 852-855).For example, compound eye of some insect and wing surface have the coniform array nanostructured that regular hexagonal is arranged, be also referred to as photonic crystal, be illustrated in figure 1 as the electromicroscopic photograph of cicada's wings surface nano-structure, the base diameter of each circular cone is 150nm, and top diameter is 65nm, highly is about 400nm, become regular hexagonal array, centre distance is 190nm.Studies show that the coniform array nanostructured in this surface has very strong anti-reflection function in ultraviolet and visible light wave range, thereby reduce the identification of harmful animal it.Being similar to the coniform array nanostructured in cicada's wings surface and why having anti-reflection function, is because this structure forms the equivalent medium (J.Opt.Soc.Am.A, 8 (1991) 549, J.Opt.Soc.Am.A, 12 (1995) 333) of refraction coefficient gradual change at the interface.
The antireflection effect optically has widely uses, and for example, can be used for the surface treatment of devices such as lens, rearview mirror, display, solar cell, light sensor, to reduce the surface to reflection of light, strengthens seeing through or absorption of light wave.Though generally adopt at present the method for film interference to reduce the reflection of surface to light wave, existing bonding and hot bulging coefficient shortcoming such as do not match is having a strong impact on the stability and the persistence of its antireflection effect between film.By contrast, utilizing coniform array structure that anti-reflex treated is carried out on the surface is a well selection.Photoetching, electron beam lithography, focused-ion-beam lithography, reactive ion etching and nano impression nanostructured processing technology have been used to prepare anti-reflecting surface, but because equipment that these technology adopted relatively costliness and complex process are difficult to reach the requirement of producing low-costly and in high volume.
Summary of the invention
The object of the present invention is to provide a kind of anti-reflection film technology of preparing, directly the biological nano structure that exists with nature is a template, prepares the anti-reflection film with nanostructured by the method for duplicating.
The present invention is achieved through the following technical solutions.
It is as follows that the biological template legal system is equipped with the processing step of anti-reflection film: be template vacuum evaporation layer of metal film with the biological nano structure at first, obtain on metallic film and the corresponding minus structure of biological nano structure; Be that template is cast with organic polymer with metal minus structure then, after solidifying, obtain the organic polymeric antireflective film that the surface has the nanostructured consistent with biological template.
Wherein, used biological nano structure is present in many organism surfaces, for example compound eye of some insect and wing surface, and preferred biological nano structure comprises the compound eye of moth and the photonic crystal on cicada's wings surface.Be that material is when carrying out a level replication with the metal, usually the thick metallic film of vacuum evaporation one deck 300～500nm on biological template, with organic polymer glue metallic film is glued then and take off, obtain and the corresponding minus metal construction of biological surface structure, as shown in Figure 3.Be that material is when carrying out two level replications with the organic polymer, the minus metal construction that obtains with a level replication is a template, be cast with organic polymer toward its surface, and be cured by the heating or the method for ultraviolet irradiation, on metal form, take organic polymer thin film at last off, promptly obtain required anti-reflection film.As shown in Figure 4, just obtain the nanostructured consistent, realize accurately duplicating of biological surface nanostructured with biological template on the organic polymer thin film surface by above-mentioned two level replications.
According to the situation of biological template, use the nanostructured preparation that nanostructured technology of preparing of the present invention can realize big face.The used metal material of the present invention comprises that gold (Au), chromium (Cr), titanium (Ti), nickel (Ni) and aluminium (Al) etc. have the metal and the alloy material thereof of certain intensity and hardness; 10
-6Evaporation metal under the vacuum condition of mbar, evaporation speed are 0.15～0.50nm/s.The used organic polymer of the present invention comprise polymethylmethacrylate (polymethyl methacrylate, PMMA) and polyamine fat (polyurethane PU) waits and to have the higher elasticity modulus (＞1.2Gpa) organic polymer.The condition of cure of PMMA is 90～170 ℃ of baking 30～60min, and the condition of cure of PU is 8w ultra violet lamp 15min～30min.
Nanostructured anti-reflection film technology of preparing of the present invention, directly the photonic crystal with biological surface is a template, method by two level replications, realized accurately duplicating of biological surface nanostructured, avoided complicated traditional nanostructured processing technologys such as photoetching, electron beam lithography, focused-ion-beam lithography, reactive ion etching, the anti-reflection film that a kind of technology is simple, cost is low, productive rate is high technology of preparing is provided.Wherein, a level replication material therefor is for metal material commonly used, and is cheap and easy to get, and the template that can be used as two level replications repeats repeatedly to use, and can further reduce the technology cost; The condition of cure gentleness of two level replications does not need impressed pressure, and set time is short, is fit to produce in enormous quantities.Use technology of the present invention and can realize large-area nanostructured preparation.
Ultraviolet-visible (UV-Vis) optical characterisation shows, at the UV, visible light wave band, the organic polymer thin film that has surface nano-structure that the present invention is prepared has very strong anti-reflection effect, its reflectivity to ultraviolet-visible light only is about 1/3 of a structureless organic polymer thin film, successfully imitated the anti-reflection function of biological surface nanostructured, optically have widely and use, for example, can be used for lens, rearview mirror, display, solar cell, the surface treatment of devices such as light sensor, to reduce the surface, strengthen seeing through or absorption of light wave to reflection of light.
Description of drawings
Fig. 1 is the electromicroscopic photograph of cicada's wings surface nano-structure.
Fig. 2 is the process chart that biological template legal system of the present invention is equipped with the nanostructured anti-reflection film.
Fig. 3 be on the metallic film with the electromicroscopic photograph of the corresponding minus structure of biological surface nanostructured.
Fig. 4 is the electromicroscopic photograph of the organic polymer thin film nanostructured for preparing of the present invention.
Among the figure:
1---biological nano structure 2---organic gel
3---silicon base 4---metallic film
5---organic polymer thin film
Embodiment
(1) the cicada's wings ultrasonic cleaning 5min in acetone that will grow up, ultrasonic cleaning 2min in ultrapure water places the air air dry again.
(2) will clean and dried cicada's wings with organic gluing card in the silicon base surface, and place in the vacuum coating equipment, 10
-6The thick metal A u of evaporation 300nm under the vacuum condition of mbar.
(3) take out the sample of evaporation metal in the vacuum coating equipment, with EPO-TEK 377 organic gel metal A u film and another silicon base bonding with evaporation under the condition of 150 ℃ of curing 1hr, and the Au film is taken off next from the cicada's wings surface, obtain and the corresponding minus structure of cicada's wings surface structure at Au film surface (with the side of the tight card of cicada's wings), as shown in Figure 3.This metallic film is used as the template of two level replications.
(4) the Au film that step (3) is obtained places in the container of one 2 * 2 * 2cm, be dissolved in the PMMA solution (15wt%) of methyl phenyl ethers anisole toward its surface casting 1ml, leave standstill 10min under the room temperature condition, place 60 ℃ of bakings of baking oven 30min then, with evaporation organic solvent methyl phenyl ethers anisole.Then the PMMA film that solidifies is taken off from the Au film surface, obtained having the PMMA film of cicada's wings surface nano-structure, as shown in Figure 4.
(1) the cicada's wings ultrasonic cleaning 5min in acetone that will grow up, ultrasonic cleaning 2min in ultrapure water places the air air dry again.
(2) will clean and dried cicada's wings with organic gluing card in the silicon base surface, and place in the vacuum coating equipment, 10
-6The thick metal A u of evaporation 500nm under the vacuum condition of mbar.
(3) take out the sample of evaporation metal in the vacuum coating equipment, with EPO-TEK 377 organic gel metal A u film and another silicon base bonding with evaporation under the condition of 150 ℃ of curing 1hr, and the Au film taken off from the cicada's wings surface, obtain and the corresponding minus structure of cicada's wings surface structure at Au film surface (with the side of the tight card of cicada's wings).This metallic film is used as the template of two level replications.
(4) the Au film that step (3) is obtained places in the container of one 2 * 2 * 2cm, be dissolved in the PMMA solution (15wt%) of methyl phenyl ethers anisole toward its surface casting 1ml, leave standstill 10min under the room temperature condition, place 60 ℃ of bakings of baking oven 60min then, with evaporation organic solvent methyl phenyl ethers anisole.Then the PMMA film that solidifies is taken off from the Au film surface, obtained having the PMMA film of cicada's wings surface nano-structure.
(1) the cicada's wings ultrasonic cleaning 5min in acetone that will grow up, ultrasonic cleaning 2min in ultrapure water places the air air dry again.
(2) will clean and dried cicada's wings with organic gluing card in the silicon base surface, and place in the vacuum coating equipment, 10
-6The thick metal A u of evaporation 500nm under the vacuum condition of mbar.
(3) take out the sample of evaporation metal in the vacuum coating equipment, with EPO-TEK 377 organic gel metal A u film and another silicon base bonding with evaporation under the condition of 150 ℃ of curing 1hr, and the Au film taken off from the cicada's wings surface, obtain and the corresponding minus structure of cicada's wings surface structure at Au film surface (with the side of the tight card of cicada's wings).This metallic film is used as the template of two level replications.
(4) the Au film that step (3) is obtained places in the container of one 2 * 2 * 2cm, be dissolved in the PMMA solution (15wt%) of methyl phenyl ethers anisole toward its surface casting 1ml, leave standstill 10min under the room temperature condition, place 90 ℃ of bakings of baking oven 30min then, with evaporation organic solvent methyl phenyl ethers anisole.Then the PMMA film that solidifies is taken off from the Au film surface, obtained having the PMMA film of cicada's wings surface nano-structure.
(5) the metal A u film that obtains with step (3) is same template, and twice repeating step (4) obtains the PMMA film with spline structure.
(1) the cicada's wings ultrasonic cleaning 5min in acetone that will grow up, ultrasonic cleaning 2min in ultrapure water places the air air dry again.
(2) will clean and dried cicada's wings with organic gluing card in the silicon base surface, and place in the vacuum coating equipment, 10
-6The thick metal A u of evaporation 500nm under the vacuum condition of mbar.
(3) take out the sample of evaporation metal in the vacuum coating equipment, with EPO-TEK 377 organic gel metal A u film and another silicon base bonding with evaporation under the condition of 150 ℃ of curing 1hr, and the Au film taken off from the cicada's wings surface, obtain and the corresponding minus structure of cicada's wings surface structure at Au film surface (with the side of the tight card of cicada's wings).This metallic film is used as the template of two level replications.
(4) the Au film that step (3) is obtained places in the container of one 2 * 2 * 2cm, be dissolved in the PMMA solution (15wt%) of methyl phenyl ethers anisole toward its surface casting 1ml, leave standstill 10min under the room temperature condition, place 170 ℃ of bakings of baking oven 30min then, with evaporation organic solvent methyl phenyl ethers anisole.Then the PMMA film that solidifies is taken off from the Au film surface, obtained having the PMMA film of cicada's wings surface nano-structure.
(1) the cicada's wings ultrasonic cleaning 5min in acetone that will grow up, ultrasonic cleaning 2min in ultrapure water places the air air dry again.
(2) will clean and dried cicada's wings with organic gluing card in the silicon base surface, and place in the vacuum coating equipment, 10
-6The thick Metal Cr of evaporation 500nm under the vacuum condition of mbar.
(3) take out the sample of evaporation metal in the vacuum coating equipment, with EPO-TEK 377 organic gel Metal Cr film and another silicon base bonding with evaporation under the condition of 150 ℃ of curing 1hr, and the Metal Cr film is taken off next from the cicada's wings surface, obtain and the corresponding minus structure of cicada's wings surface structure at Cr film surface (with the side of the tight card of cicada's wings), as shown in Figure 8.This metallic film is used as the template of two level replications.
(4) the Cr film that step (3) is obtained places in the container of one 2 * 2 * 2cm, be dissolved in the PMMA solution (15wt%) of methyl phenyl ethers anisole toward its surface casting 1ml, leave standstill 10min under the room temperature condition, place 90 ℃ of bakings of baking oven 30min then, with evaporation organic solvent methyl phenyl ethers anisole.Then the PMMA film that solidifies is taken off from the Cr film surface, obtained having the PMMA film of cicada's wings surface nano-structure.
Embodiment 6
(1) the cicada's wings ultrasonic cleaning 5min in acetone that will grow up, ultrasonic cleaning 2min in ultrapure water places the air air dry again.
(2) will clean and dried cicada's wings with organic gluing card in the silicon base surface, and place in the vacuum coating equipment, 10
-6The thick metal Ti of evaporation 500nm under the vacuum condition of mbar.
(3) take out the sample of evaporation metal in the vacuum coating equipment, with EPO-TEK 377 organic gel metal Ti film and another silicon base bonding with evaporation under the condition of 150 ℃ of curing 1hr, and the metal Ti film is taken off next from the cicada's wings surface, obtain and the corresponding minus structure of cicada's wings surface structure at Ti film surface (with the side of the tight card of cicada's wings), as shown in Figure 9.This metallic film is used as the template of two level replications.
(4) the Ti film that step (3) is obtained places in the container of one 2 * 2 * 2cm, be dissolved in the PMMA solution (15wt%) of methyl phenyl ethers anisole toward its surface casting 1ml, leave standstill 10min under the room temperature condition, place 90 ℃ of bakings of baking oven 30min then, with evaporation organic solvent methyl phenyl ethers anisole.Then the PMMA film that solidifies is taken off from the Ti film surface, obtained having the PMMA film of cicada's wings surface nano-structure.
Embodiment 7
(1) the cicada's wings ultrasonic cleaning 5min in acetone that will grow up, ultrasonic cleaning 2min in ultrapure water places the air air dry again.
(2) will clean and dried cicada's wings with organic gluing card in the silicon base surface, and place in the vacuum coating equipment, 10
-6The metal Ni that evaporation 500nm is thick under the vacuum condition of mbar.
(3) take out the sample of evaporation metal in the vacuum coating equipment, with EPO-TEK 377 organic gel metal Ni film and another silicon base bonding with evaporation under the condition of 150 ℃ of curing 1hr, and metal Ni film is taken off next from the cicada's wings surface, obtain and the corresponding minus structure of cicada's wings surface structure at Ni film surface (with the side of the tight card of cicada's wings), as shown in figure 10.This metallic film is used as the template of two level replications.
(4) the Au film that step (3) is obtained places in the container of one 2 * 2 * 2cm, be dissolved in the PMMA solution (15wt%) of methyl phenyl ethers anisole toward its surface casting 1ml, leave standstill 10min under the room temperature condition, place 90 ℃ of bakings of baking oven 30min then, with evaporation organic solvent methyl phenyl ethers anisole.Then the PMMA film that solidifies is taken off from the Ni film surface, obtained having the PMMA film of cicada's wings surface nano-structure.
Embodiment 8
(1) the cicada's wings ultrasonic cleaning 5min in acetone that will grow up, ultrasonic cleaning 2min in ultrapure water places the air air dry again.
(2) will clean and dried cicada's wings with organic gluing card in the silicon base surface, and place in the vacuum coating equipment, 10
-6The thick metal A u of evaporation 500nm under the vacuum condition of mbar.
(3) take out the sample of evaporation metal in the vacuum coating equipment, with EPO-TEK 377 organic gel metal A u film and another silicon base bonding with evaporation under the condition of 150 ℃ of curing 1hr, and the Au film taken off from the cicada's wings surface, obtain and the corresponding minus structure of cicada's wings surface structure at Au film surface (with the side of the tight card of cicada's wings).This metallic film is used as the template of two level replications.
(4) the Au film that step (3) is obtained places in the container of one 2 * 2 * 2cm, toward its surface casting 0.5ml polyamine fat (PU) presoma, leave standstill 5min under the room temperature condition, place irradiation 30min curing under the 8w uviol lamp then, at last the polyamine membrane of lipoprotein that solidifies is taken off from the Au film surface, obtained having the polyamine membrane of lipoprotein of cicada's wings surface nano-structure.
Embodiment 9
Cicada's wings, embodiment 3 gained PMMA films and other the structureless PMMA film of system are carried out optical characterisation in ultraviolet and visible light wave range, and used optical instrument is the Lambda 950 ultraviolet-visibles-near infrared spectrophotometer of PerkinEmler company.Characterization result shows that at ultraviolet and visible light wave range, the reflectivity of embodiment 3 gained PMMA films is 36% of a non-structure PMMA film, illustrates that the PMMA film that application the technology of the present invention is duplicated has stronger antireflective property.
Claims (7)
1. the preparation method of an anti-reflection film, its step is as follows: be template vacuum evaporation layer of metal film with the biological nano structure at first, obtain on metallic film and the corresponding minus structure of biological nano structure; Be that template is cast with organic polymer with metal minus structure then, after solidifying, obtain the organic polymeric antireflective film that the surface has the nanostructured consistent with biological template, the compound eye that wherein said biological nano structure is a moth or the photonic crystal on cicada's wings surface.
2. preparation method as claimed in claim 1 is characterized in that: the material of described metallic film is selected from the alloy of gold, chromium, titanium, nickel, aluminium or above-mentioned metal.
3. preparation method as claimed in claim 1 is characterized in that: 10
-6Evaporation metal under the vacuum condition of mbar, evaporation speed are 0.15～0.50nm/s.
4. preparation method as claimed in claim 1 is characterized in that: described thickness of metal film is 300～500nm.
5. preparation method as claimed in claim 1 is characterized in that: described organic polymer is the organic polymer of elastic modulus greater than 1.2Gpa.
6. as the described preparation method of the arbitrary claim of claim 1～5, it is characterized in that: described organic polymer is a polymethylmethacrylate, and its condition of cure is 90～170 ℃ of baking 30～60min.
7. as the described preparation method of the arbitrary claim of claim 1～5, it is characterized in that: described organic polymer is a polyamine fat, and its condition of cure is 8w ultra violet lamp 15min～30min.
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101866958A (en) * | 2010-05-14 | 2010-10-20 | 河海大学常州校区 | Biomimetic antireflection film of solar cell and preparation method thereof |
| CN103576451A (en) * | 2013-11-08 | 2014-02-12 | 无锡英普林纳米科技有限公司 | Method for duplicating micro-nanostructure |
| CN104155710B (en) * | 2014-09-05 | 2017-02-15 | 山东理工大学 | Method for manufacturing large-area and high-accuracy thin film type grating device through whole butterfly wing |
| CN104178733B (en) * | 2014-09-05 | 2016-05-04 | 山东理工大学 | Lepidopterous insects wing is carried out to the method for full finned surface, high true to nature, large area microstructure replication |
| JP6623058B2 (en) * | 2015-12-18 | 2019-12-18 | デクセリアルズ株式会社 | Method for forming antireflection optical body and display panel |
| CN106526716B (en) * | 2016-11-22 | 2018-06-22 | 武汉华星光电技术有限公司 | A kind of production method and display device of micro-nano structure antireflective film |
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| US4322125A (en) * | 1978-05-11 | 1982-03-30 | International Standard Electric Corporation | Infra-red filter |
| CN85100175A (en) * | 1985-04-01 | 1986-07-30 | 电子工业部第十二研究所 | Casting grating method and casting grating |
| US6175439B1 (en) * | 1998-06-12 | 2001-01-16 | Ricoh Company, Inc. | Rotary body for a polygonal mirror type scanner and method of machining the same |
| US20020135847A1 (en) * | 2001-03-22 | 2002-09-26 | Seiko Epson Corporation | Manufacturing method of microstructure, manufacturing method and manufacturing device of electronic device |
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