CN103576447A - Fluorine-containing polymer ultraviolet nano-coining template and preparation method thereof - Google Patents
Fluorine-containing polymer ultraviolet nano-coining template and preparation method thereof Download PDFInfo
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- CN103576447A CN103576447A CN201310543038.9A CN201310543038A CN103576447A CN 103576447 A CN103576447 A CN 103576447A CN 201310543038 A CN201310543038 A CN 201310543038A CN 103576447 A CN103576447 A CN 103576447A
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Abstract
The invention provides a fluorine-containing polymer ultraviolet nano-coining template and a preparation method thereof. The template is composed of a substrate and a fluorine-containing polymer coining structure layer located on the substrate, wherein the substrate is made of quartz or fluorine-containing polymer. The preparation method is implemented through coating a CYTOP (cyclic transparent optical polymer) polymer solution on the quartz substrate by way of spin coating, removing residual fluorine-containing solvents in the CYTOP polymer solution subjected to spin coating through heated evaporation, and coining a CYTOP solid membrane on the quartz substrate by using a coining female template in hot nano-coining form on a nano-coining machine; or pouring the CYTOP polymer solution on the coining female template, and after the solution is automatically flattened by flowing and fills the stricture of the female template, removing residual fluorine-containing solvents in the CYTOP polymer solution through heated evaporation, thereby obtaining a CYTOP solid membrane; and finally, separating the coining female template from the CYTOP solid membrane so as to obtain the fluorine-containing polymer ultraviolet nano-coining template. By using the ultraviolet nano-coining template disclosed by the invention, an anti-sticking treatment process in the preparation of the nano-coining template can be omitted, and the problem that the anti-sticking effect of a template after being coined many times is reduced can be solved.
Description
Technical field
The invention belongs to micro-nano manufacture field, be specifically related to a kind of fluoropolymer template that can be used for ultraviolet nanometer impression and preparation method thereof.
Background technology
Nanometer embossing is that first a kind of S.Y.Chou professor of brand-new nano-pattern clone method ，You Princeton University proposed in nineteen ninety-five.Because it has high resolving power, high yield, the advantage such as low-cost, and be included into the development blueprint of international semiconductor, cause various countries researchist's extensive concern.Except at semiconductor applications, nanometer embossing is also widely used in biomedicine, information storage, subwavelength optical element, the numerous areas such as nanoelectronics.
Nanometer embossing, from the time that occurs only having so far the short more than ten years, also has a lot of key issues to need further to study and solve.In nanometer embossing, the most important thing is nano-imprinting apparatus, nano-imprint stamp and nano impression glue.Wherein the impact of the product confrontation nano-imprint process of nano-imprint stamp is most important.High-specific surface area due to nano-pattern, nano-imprint stamp is in the knockout course of imprint process, meeting and nano impression glue produce very strong interaction force, therefore nano-imprint stamp conventionally need to carry out release treatment and reduce this interaction force before impression, thereby realized the demoulding smoothly.The release treatment on nano-imprint stamp surface is generally at template surface generation one deck silicon fluoride molecular layer, to realize the reduction of template surface free energy by the method for gas phase or liquid phase, thereby reduces the acting force to impression glue in impression.But this method need to be carried out pre-service to template conventionally, make template surface generate the silicon hydroxyl that can react with silicon fluoride, and need to keep dry in antiseized process, technique is loaded down with trivial details, and after multi-impression, anti-adhesion effects has decline to a certain degree.In addition, this class reagent of silicon fluoride is conventionally expensive and have toxicity.
On the other hand, the people such as Lee [D.Y.Khang, H.Kang, T.Kim, H.H.Lee, Nano Lett.4 (4), 633 (2004)] template that adopts the AF2400 of fluorinated polymer material Du Pont directly to make nano impression, not only saved the technique of release treatment, and multi-impression still can keep good anti-adhesion effects.But this material has higher glass transition temperature, therefore prepare the higher temperature and pressure of nano-imprint stamp needs of this polymkeric substance.
Summary of the invention
In view of above situation, the object of the invention is to solve the antiseized problem of template in nano impression, provide a kind of and be easy to fluoropolymer ultraviolet nanometer impression block without release treatment and preparation.Another object of the present invention is to provide the preparation method of this template.
For achieving the above object, the technical scheme that ultraviolet nanometer impression block of the present invention is taked is:
A ultraviolet nanometer impression block, it is comprised of substrate and the fluoropolymer stamping structure layer being positioned on substrate, and described substrate is quartz or fluoropolymer self.
Described fluoropolymer is the material of trade name CYTOP.It has lower glass transition temperature, high ultraviolet transmittance, and can be dissolved in specific containing in fluorous solvent.Commodity CYTOP is the CYTOP polymer solution (AGC Chemicals, Japan) being dissolved in containing fluorous solvent, and concentration 9% obtains CYTOP solid film and with the making of nano-imprint stamp by spin-coating or the method for building film forming.
Described quartz substrate, between 1 to 3 millimeter, has high ultraviolet transmittance and high surface smoothness.The substrate that the surfaces such as CYTOP solid film and quartz have silicon hydroxyl to exist has fine adhesive capacity.
The preparation method of ultraviolet nanometer impression polymer template of the present invention is divided into two kinds of situations, comprises the following steps respectively:
(1) when substrate is quartz, spin coating CYTOP polymer solution in quartz substrate; By heating evaporation, remove remnants in the CYTOP polymer solution of spin coating containing fluorous solvent, obtain CYTOP solid film; On nano marking press, with impression caster, the mode with hot nano impression impresses the CYTOP solid film in quartz substrate again; Finally, after impression completes, separated impression caster and CYTOP solid film, obtain being positioned at the fluoropolymer ultraviolet nanometer impression block in quartz substrate;
(2) when substrate is fluoropolymer self, CYTOP polymer solution is cast on impression caster, treat its automatic levelling the structure of filling up caster; By heating evaporation, remove the fluorous solvent that contains in solution, obtain CYTOP solid film; Finally, careful separation CYTOP solid film and impression caster, obtain being positioned at CYTOP polymkeric substance from the fluoropolymer ultraviolet nanometer impression block as substrate.
Utilize above-mentioned fluoropolymer ultraviolet nanometer impression block, without release treatment, just can be directly used in ultraviolet nanometer impression, technique specifically comprises the following steps: (1) utilizes sol evenning machine on required substrate, evenly to apply one deck ultraviolet stamping glue; (2) by described fluoropolymer ultraviolet nanometer impression block, with structural plane, the mode facing to ultraviolet glue is laid on substrate, forms impression combination; (3) for the fluoropolymer ultraviolet nanometer impression block being positioned in quartz substrate, impression combination is placed on marking press platform, apply certain pressure, and with the ultraviolet mercury lamp certain hour that exposes, make ultraviolet stamping glue fully curing; (4) for the fluoropolymer ultraviolet nanometer impression block being positioned on fluoropolymer self substrate, by the capillary force of micro-nano structure and the absorption affinity of ultraviolet glue, template and substrate are fitted naturally, again this combination is placed on to 1 minutes that exposes under ultraviolet mercury lamp, makes ultraviolet stamping glue fully curing; (5) take template off, complete moulding process.
The invention provides a kind of new ultra-violet nano-imprint stamp without release treatment and preparation method thereof, the beneficial effect compared with prior art having is:
(1) fluoropolymer ultraviolet nanometer impression block of the present invention, adopts hard fluoropolymer CYTOP to make stamping structure layer, can obtain high-resolution nanostructured, as shown in Figure 5.
(2) fluoropolymer ultraviolet nanometer impression block of the present invention hard fluoropolymer CYTOP used has lower glass transition temperature (105 ℃), therefore can under lower temperature impression, with the hot padding of impression caster, obtain.
(3) fluoropolymer ultraviolet nanometer impression block of the present invention also can, without any substrate (with polymkeric substance from as substrate), obtain by build the way of film forming at impression caster, thereby not need marking press to prepare template.
(4) fluoropolymer ultraviolet nanometer impression block of the present invention, just can be directly used in ultraviolet nanometer impression without release treatment, and because structural sheet itself is fluoropolymer, so after multi-impression, anti-adhesion effects can not decline.This has solved the antiseized problem in nano impression, has simplified technique, has reduced cost, has improved product yield.
Accompanying drawing explanation
Fig. 1: quartz substrate fluoropolymer ultraviolet nanometer impression block schematic diagram;
Fig. 2: polymkeric substance self is made substrate fluoropolymer ultraviolet nanometer impression block schematic diagram;
Fig. 3: quartz substrate fluoropolymer ultraviolet nanometer impression block preparation flow schematic diagram;
Fig. 4: utilize quartz substrate fluoropolymer template to carry out ultraviolet nanometer impression schematic diagram; 5: quartz substrate fluoropolymer ultraviolet nanometer impression block; 6: ultraviolet stamping glue; 7: silicon substrate.
Fig. 5: utilize quartz substrate fluoropolymer template to carry out the electron scanning micrograph of ultraviolet nanometer impression, (a) 440nm cycle, 220nm live width optical grating construction silicon caster; (b) the 440nm cycle, 220nm live width optical grating construction fluoropolymer template; (c) used the 440nm cycle of 20 times 220nm live width optical grating construction fluoropolymer template; (d) the 440nm cycle of utilizing fluoropolymer template ultraviolet nanometer impression to obtain, 220nm live width optical grating construction.
Fig. 6: utilize quartz substrate fluoropolymer template to carry out the electron scanning micrograph of ultraviolet nanometer impression, (a) 400nm cycle, outer ring diameter 300nm, live width 50nm, height 40nm, circular ring structure silicon caster; (b) circular ring structure fluoropolymer template; (c) utilize fluoropolymer template ultraviolet nanometer impression to obtain circular ring structure; (d) the atomic force microscope figure corresponding with figure (a); (e) the atomic force microscope figure corresponding with figure (c); (f) transversal place Cross Section Morphology in figure (d); (g) transversal place Cross Section Morphology in figure (e).
Fig. 7: utilize quartz substrate fluoropolymer template to carry out the electron scanning micrograph of ultraviolet nanometer impression, (a) the 200nm cycle, 100nm live width pore space structure, in figure, the upper right corner is structure for amplifying; (b) the 400nm cycle, 200nm live width lattice structure, in figure, the upper right corner is structure for amplifying.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in further detail:
The structure of fluoropolymer ultraviolet nanometer impression block of the present invention is shown in Fig. 1 and Fig. 2, and fluoropolymer CYTOP is as template rigid structural layer 2, and underlying substrate is that piezoid 1 or CYTOP polymkeric substance 3 are own.
The concrete making step of the fluoropolymer ultraviolet nanometer impression block of the present embodiment:
1. quartz substrate fluoropolymer ultraviolet nanometer impression block making step is as shown in Figure 3, specific as follows:
(1) CYTOP polymkeric substance 3 solution are dropped on clean piezoid 1, utilize sol evenning machine that CYTOP film is evenly coated on piezoid 1, film thickness is according to caster nano-pattern size Selection suitable thickness and controlled by sol evenning machine rotating speed, and the piezoid that even glue is applied to CYTOP film is placed on hot platform and is heated to 150 ℃ to maintain 1 hour residual containing fluorous solvent to remove.
(2) structural plane of impression caster 4 is contacted and is adjacent to the CYTOP film on piezoid 1, again this combination is placed on nano marking press impression platform and carries out hot nano impression, the rear pattern of pressure of first heating, imprint parameters: 170 ℃ of temperature, pressure 0.1-0.5MPa, temperature retention time 5 minutes, 5 minutes pressure-maintaining and heat-preservation time.After having impressed, careful separation caster 4 and piezoid 1 obtain quartz substrate fluoropolymer ultraviolet nanometer impression block.
2. the fluoropolymer ultraviolet nanometer impression block making step of polymkeric substance self substrate:
CYTOP polymer solution is cast on impression caster structural plane, then caster is placed on to hot platform is heated to 150 ℃ and maintains 4 hours to remove containing fluorous solvent and to leave one deck CYTOP solid film at caster structural plane.Careful separation caster and CYTOP solid film, obtain the fluoropolymer ultraviolet nanometer impression block of polymkeric substance self substrate.Fluoropolymer template thickness determines by building solution liquid layer thickness.
Fluoropolymer ultraviolet nanometer impression block prepared by the present embodiment utilization carries out ultraviolet nanometer imprint process step as shown in Figure 4:
(1) utilize sol evenning machine on silicon substrate 7 with 1600 revs/min, within 40 seconds, evenly apply one deck ultraviolet stamping glue 6.
(2) by the fluoropolymer ultraviolet nanometer impression block of making, with structural plane, the mode facing to ultraviolet glue is laid on substrate, forms impression combination.
(3) for quartz substrate fluoropolymer ultraviolet nanometer impression block 5, combination is placed on marking press platform, applies 0.3MPa pressure, with ultraviolet mercury lamp 1 minutes that exposes, make ultraviolet stamping 6 glue fully curing.
(4) for polymkeric substance self substrate fluoropolymer ultraviolet nanometer impression block, by the capillary force of micro-nano structure and the absorption affinity of ultraviolet glue, template and substrate are fitted naturally, then this combination is placed on to 1 minutes that exposes under ultraviolet mercury lamp, make ultraviolet stamping glue fully curing.
(5) take template off, complete moulding process.
Claims (5)
1. a fluoropolymer ultraviolet nanometer impression block, is characterized in that, described template is comprised of substrate and the fluoropolymer stamping structure layer being positioned on substrate, and described substrate is quartz or fluoropolymer self.
2. a kind of fluoropolymer ultraviolet nanometer impression block according to claim 1, is characterized in that, described fluoropolymer is the material of trade name CYTOP.
3. a kind of fluoropolymer ultraviolet nanometer impression block according to claim 1 and 2, is characterized in that, the thickness of described quartz substrate, between 1 to 3 millimeter, has high ultraviolet transmittance; Described fluoropolymer self substrate thickness is between 0.05 to 0.1 millimeter.
4. the preparation method of a kind of fluoropolymer ultraviolet nanometer impression block as claimed in claim 1, it is characterized in that, first buy the material of trade name CYTOP, is the CYTOP polymer solution being dissolved in containing fluorous solvent, concentration is 9%, and the method comprises the following steps:
(1) when substrate is quartz, spin coating CYTOP polymer solution in quartz substrate; By heating evaporation, remove remnants in the CYTOP polymer solution of spin coating containing fluorous solvent, obtain CYTOP solid film; On nano marking press, with impression caster, the mode with hot nano impression impresses the CYTOP solid film in quartz substrate again; Finally, after impression completes, separated impression caster and CYTOP solid film, obtain being positioned at the fluoropolymer ultraviolet nanometer impression block in quartz substrate;
(2) when substrate is fluoropolymer self, CYTOP polymer solution is cast on impression caster, treat its automatic levelling the structure of filling up caster; By heating evaporation, remove the fluorous solvent that contains in solution, obtain CYTOP solid film; Finally, careful separation CYTOP solid film and impression caster, obtain being positioned at CYTOP polymkeric substance from the fluoropolymer ultraviolet nanometer impression block as substrate.
5. utilize the nano-imprint process of a kind of fluoropolymer ultraviolet nanometer impression block as claimed in claim 1, it is characterized in that, described fluoropolymer ultraviolet nanometer impression block can be directly used in ultraviolet nanometer impression without release treatment, and technique specifically comprises the following steps: (1) utilizes sol evenning machine on required substrate, evenly to apply one deck ultraviolet stamping glue;
(2) by described fluoropolymer ultraviolet nanometer impression block, with structural plane, the mode facing to ultraviolet glue is laid on substrate, forms impression combination;
(3) for the fluoropolymer ultraviolet nanometer impression block being positioned in quartz substrate, impression combination is placed on marking press platform, apply certain pressure, and with the ultraviolet mercury lamp certain hour that exposes, make ultraviolet stamping glue fully curing;
(4) for the fluoropolymer ultraviolet nanometer impression block being positioned on fluoropolymer self substrate, by the capillary force of micro-nano structure and the absorption affinity of ultraviolet glue, template and substrate are fitted naturally, again this combination is placed on to 1 minutes that exposes under ultraviolet mercury lamp, makes ultraviolet stamping glue fully curing;
(5) take template off, complete moulding process.
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| CN107643652A (en) * | 2017-10-31 | 2018-01-30 | 武汉华星光电技术有限公司 | Nano-imprint stamp and preparation method thereof and application |
| CN107844027A (en) * | 2017-09-28 | 2018-03-27 | 边捷 | A kind of high-resolution overlength 1-dimention nano pattern preparation method |
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| CN107844027A (en) * | 2017-09-28 | 2018-03-27 | 边捷 | A kind of high-resolution overlength 1-dimention nano pattern preparation method |
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Application publication date: 20140212 |