CN104476895A - Method for constructing multistage ordered microstructure by combination of template imprinting and surface wrinkling - Google Patents
Method for constructing multistage ordered microstructure by combination of template imprinting and surface wrinkling Download PDFInfo
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- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 claims 10
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Abstract
本发明提供了一种模板压印和表面起皱相结合构筑多级有序微结构的方法;首先在洁净的玻璃基底旋涂聚乙烯亚胺的水溶液,干燥后继续旋涂聚苯乙烯(PS)的四氢呋喃溶液。在水浴环境下,将该PS薄膜转移到拉伸的聚二甲基硅氧烷(PDMS)基底上,形成PDMS/PS软硬复合体系。在该样品上加盖预先制备的皱纹模板后加热,在冷却过程中PDMS/PS双层体系形成一级形貌。然后将预拉伸的PDMS回缩,PDMS/PS双层体系形成二级皱纹形貌。通过改变模板压印得到的一级形貌与表面起皱得到的二级形貌相交角度,控制复合形貌的各向异性。本方法成本低,过程简单,重复性好,实现了在PDMS基底上构筑精确可控的多级有序微结构。
The invention provides a method for constructing a multi-level ordered microstructure by combining template imprinting and surface wrinkling; first, an aqueous solution of polyethylenimine is spin-coated on a clean glass substrate, and after drying, spin-coating polystyrene (PS ) in tetrahydrofuran. In a water bath environment, the PS film was transferred to a stretched polydimethylsiloxane (PDMS) substrate to form a PDMS/PS soft-hard composite system. The sample was covered with a pre-prepared wrinkle template and then heated, and the PDMS/PS bilayer system formed a first-order morphology during the cooling process. Then the pre-stretched PDMS was retracted, and the PDMS/PS bilayer system formed a secondary wrinkled morphology. The anisotropy of the composite topography is controlled by changing the intersection angle between the primary topography obtained by template imprinting and the secondary topography obtained by surface wrinkling. The method has the advantages of low cost, simple process and good repeatability, and realizes the construction of an accurate and controllable multi-level ordered microstructure on the PDMS substrate.
Description
技术领域technical field
本发明涉及聚合物薄膜表面的微结构加工技术,特别是模板压印和表面起皱相结合构筑多级有序微结构的方法;具体涉及一种PDMS/PS(聚二甲基硅氧烷/聚苯乙烯)双层体系制备复合形貌的工艺方法。The present invention relates to the microstructure processing technology of the polymer film surface, especially the method for constructing the multi-level ordered microstructure by combining template embossing and surface wrinkling; Polystyrene) double-layer system preparation method of composite morphology.
背景技术Background technique
自然界中动植物表面天然存在的微纳复合结构已经引起了科学家们广泛的关注。通过向自然界的学习,使我们了解到高级结构,即微纳复合结构,对材料性能的影响,促使我们加深对材料表面加工作用的理解。近年来,功能性微纳复合结构的可控制备引起了各个领域的广泛研究。总的来说,表面形貌的制备技术主要有以下两种:“自上而下”(Top-down)方法和“自下而上”(Bottom-up)方法。“自上而下”就是利用机械和刻蚀技术使材料的尺寸逐渐减小,并达到微米、纳米尺度,如软刻蚀技术;“自下而上”则是由小分子级尺寸运用化学合成以达到寡分子或高分子的纳米级尺寸,即应用原子或分子创造有机和无机结构,如自组装技术。目前,微米尺度的功能性材料表面的制备方法已经取得了很大的进展,但不使用刻蚀技术而对材料表面进行图案化仍是一项挑战。本文结合“自上而下”和“自下而上”两种技术,在聚合物薄膜表面构筑微图案。The naturally occurring micro-nano composite structures on the surface of animals and plants in nature have attracted widespread attention of scientists. By learning from nature, we understand the impact of advanced structures, that is, micro-nano composite structures, on the properties of materials, which prompts us to deepen our understanding of the surface processing of materials. In recent years, the controllable preparation of functional micro-nano composite structures has attracted extensive research in various fields. Generally speaking, there are two main techniques for preparing surface topography: "Top-down" method and "Bottom-up" method. "Top-down" is to use mechanical and etching technology to gradually reduce the size of the material and reach the micron and nanometer scale, such as soft etching technology; "bottom-up" is to use chemical synthesis of small molecular size In order to achieve the nanoscale size of oligomolecules or polymers, that is, the application of atoms or molecules to create organic and inorganic structures, such as self-assembly technology. At present, great progress has been made in the fabrication of micron-scale functional material surfaces, but patterning material surfaces without using etching techniques remains a challenge. In this paper, "top-down" and "bottom-up" techniques are combined to construct micropatterns on the surface of polymer films.
发明内容Contents of the invention
针对上述现有技术,本发明提供模板压印和表面起皱相结合构筑多级有序微结构的方法。本发明选用PDMS为基底,与转移得到的PS薄膜构成软硬复合体系。利用简单的操作方式构筑了两级复合形貌,并做到了通过改变模板的加盖角度等实验参数,实现对复合形貌进行精确的调控。Aiming at the above-mentioned prior art, the present invention provides a method for constructing a multi-level ordered microstructure by combining template imprinting and surface wrinkling. The present invention selects PDMS as the substrate, and forms a soft-hard composite system with the transferred PS film. The two-level composite morphology was constructed by using a simple operation method, and the precise control of the composite morphology was realized by changing the experimental parameters such as the capping angle of the template.
本发明的技术方案如下:Technical scheme of the present invention is as follows:
一种模板压印和表面起皱相结合构筑多级有序微结构的方法,包括以下步骤:A method for constructing a multi-level ordered microstructure by combining template imprinting and surface wrinkling, comprising the following steps:
(1)将PDMS弹性体固定到拉伸台上,按照预拉伸率为2-10%进行拉伸,一部分拉伸的PDMS用于制备皱纹模板,一部分拉伸的PDMS用于转移PS薄膜;(1) Fix the PDMS elastomer on the stretching table, stretch according to the pre-stretch ratio of 2-10%, a part of the stretched PDMS is used to prepare a wrinkle template, and a part of the stretched PDMS is used to transfer the PS film;
(2)将用于制备皱纹模板的拉伸的PDMS,经过氧等离子体处理5-30分钟,回缩后得到带有规整形貌的皱纹模板;(2) The stretched PDMS used to prepare the wrinkle template is treated with oxygen plasma for 5-30 minutes, and the wrinkle template with a regular appearance is obtained after retraction;
(3)在水浴环境下,将玻璃基底上旋涂的PS薄膜转移到步骤(1)的用于转移PS薄膜的拉伸的PDMS上,形成PDMS/PS双层体系,真空条件下进行干燥;(3) In a water bath environment, the PS film spin-coated on the glass substrate is transferred to the stretched PDMS used to transfer the PS film in step (1), forming a PDMS/PS double-layer system, and drying under vacuum conditions;
(4)将步骤(2)制备的皱纹模板以不同角度加盖到经过步骤(3)中真空干燥过的PDMS/PS双层体系上,90-120摄氏度下加热0.5-2小时后冷却到室温,将皱纹模板揭掉,得到一级形貌;(4) Cover the wrinkle template prepared in step (2) on the PDMS/PS bilayer system vacuum-dried in step (3) at different angles, heat at 90-120 degrees Celsius for 0.5-2 hours and then cool to room temperature , remove the wrinkle template to obtain the first-level topography;
(5)将步骤(4)获得的具有一级形貌的PDMS/PS/双层体系回缩,产生二级皱纹形貌,最终制备了两级复合形貌。(5) The PDMS/PS/bilayer system with the first-order morphology obtained in step (4) was retracted to produce a second-order wrinkled morphology, and finally a two-stage composite morphology was prepared.
其中PDMS弹性体可以采用现有技术的任何方法制备;同时也可以采用如下方法制备:将PDMS预聚体和交联剂按质量比为(5-20):1混合后,用玻璃棒充分搅拌形成均匀的预聚物,将此预聚物在循环水式多用真空泵中脱气后倒入培养皿中,加热交联。Wherein the PDMS elastomer can be prepared by any method of the prior art; at the same time, it can also be prepared by the following method: the PDMS prepolymer and the crosslinking agent are mixed according to the mass ratio of (5-20): 1, and then fully stirred with a glass rod A uniform prepolymer is formed, and the prepolymer is degassed in a circulating water multi-purpose vacuum pump and then poured into a petri dish for heating and crosslinking.
玻璃基底上旋涂PS薄膜可以采用现有技术的任何方法制备;同时也可以采用如下方法制备:在洁净的玻璃基底上旋涂质量分数为1wt%的聚乙烯亚胺的水溶液,干燥后继续旋涂质量分数为1-5wt%聚苯乙烯的四氢呋喃溶液。Spin coating PS thin film on glass substrate can adopt any method of prior art to prepare; Also can adopt following method to prepare simultaneously: on clean glass substrate, spin coating mass fraction is the aqueous solution of 1wt% polyethyleneimine, continues to spin after drying The tetrahydrofuran solution whose mass fraction is 1-5wt% polystyrene is coated.
步骤(1)中,用PDMS弹性体的拉伸率控制一级、二级形貌的周期;步骤(2)中,氧等离子体处理时间控制皱纹模板周期,进而调控一级形貌的周期;步骤(4)中,用皱纹模板的不同加盖角度调控两级形貌的相对取向,加热温度和时间调控一级形貌的高度。In step (1), the period of the primary and secondary morphology is controlled by the stretching ratio of the PDMS elastomer; in step (2), the oxygen plasma treatment time controls the period of the wrinkle template, thereby regulating the period of the primary morphology; In step (4), different capping angles of the wrinkle template are used to control the relative orientation of the two-level features, and the heating temperature and time are used to control the height of the first-level features.
该方法首先在洁净的玻璃基底旋涂聚乙烯亚胺(PEI)的水溶液,干燥后继续旋涂聚苯乙烯(PS)的四氢呋喃溶液。在水浴环境下,将该PS薄膜转移到拉伸的聚二甲基硅氧烷(PDMS)基底上,形成PDMS/PS软硬复合体系。在该样品上加盖预先制备的皱纹模板后加热,在冷却过程中PDMS/PS双层体系形成一级形貌。然后将预拉伸的PDMS回缩,PDMS/PS双层体系形成二级皱纹形貌。通过改变模板压印得到的一级形貌与表面起皱得到的二级形貌相交角度,控制复合形貌的各向异性。本方法成本低,过程简单,重复性好,实现了在PDMS基底上构筑精确可控的多级有序微结构。In the method, an aqueous solution of polyethyleneimine (PEI) is firstly spin-coated on a clean glass substrate, and then spin-coats a tetrahydrofuran solution of polystyrene (PS) after drying. In a water bath environment, the PS film was transferred to a stretched polydimethylsiloxane (PDMS) substrate to form a PDMS/PS soft-hard composite system. The sample was covered with a pre-prepared wrinkle template and then heated, and the PDMS/PS bilayer system formed a first-order morphology during the cooling process. Then the pre-stretched PDMS was retracted, and the PDMS/PS bilayer system formed a secondary wrinkled morphology. The anisotropy of the composite topography is controlled by changing the intersection angle between the primary topography obtained by template imprinting and the secondary topography obtained by surface wrinkling. The method has the advantages of low cost, simple process and good repeatability, and realizes the construction of an accurate and controllable multi-level ordered microstructure on the PDMS substrate.
与现有技术相比,本发明的有益效果是:Compared with prior art, the beneficial effect of the present invention is:
该技术成本低、精度高、操作简便、应用范围广。精细调控了PDMS弹性体表面的图案化微结构的形貌,避免了自上而下方法中昂贵仪器的使用、复杂的工艺条件、和苛刻的实验参数等缺点,也避免了从下而上方法中图案规整度相对较差和尺寸范围小等不足。采用本发明的方法制得的微结构在在光学、微电子、传感器、生物医学等很多领域有着广泛的应用前景。The technology has the advantages of low cost, high precision, easy operation and wide application range. The morphology of the patterned microstructure on the surface of the PDMS elastomer is finely regulated, avoiding the disadvantages of using expensive instruments, complicated process conditions, and harsh experimental parameters in the top-down method, and also avoiding the disadvantages of the bottom-up method The regularity of the medium pattern is relatively poor and the size range is small. The microstructure prepared by the method of the invention has wide application prospects in many fields such as optics, microelectronics, sensors, and biomedicine.
附图说明Description of drawings
图1为本发明实施例1中一级、二级形貌相交角度为0度的复合结构的光学显微镜图片;Figure 1 is an optical microscope picture of a composite structure with a primary and secondary morphology intersection angle of 0 degrees in Example 1 of the present invention;
图2为本发明实施例2中一级、二级形貌相交角度为40度的复合结构的光学显微镜图片;Fig. 2 is an optical microscope picture of a composite structure with a primary and secondary morphology intersection angle of 40 degrees in Example 2 of the present invention;
图3为本发明实施例3中一级、二级形貌相交角度为90度的复合结构的光学显微镜图片。Fig. 3 is an optical microscope picture of a composite structure with a primary and secondary morphology intersection angle of 90 degrees in Example 3 of the present invention.
具体实施方式Detailed ways
下面结合具体实施方式对本发明作进一步详细地描述。The present invention will be further described in detail below in combination with specific embodiments.
实施例1:Example 1:
一种模板压印和表面起皱相结合构筑多级有序微结构的方法,包括以下步骤:A method for constructing a multi-level ordered microstructure by combining template imprinting and surface wrinkling, comprising the following steps:
(1)将PDMS弹性体固定到拉伸台上,预拉伸率为10%,用于制备皱纹模板;拉伸率为5%,用于转移PS薄膜;(1) Fix the PDMS elastomer on the stretching table with a pre-stretch rate of 10% for preparing a wrinkle template; a stretch rate of 5% for transferring the PS film;
(2)将用于制备皱纹模板的拉伸的PDMS,经过氧等离子体处理10分钟,回缩后得到带有规整形貌的皱纹模板;(2) The stretched PDMS used to prepare the wrinkle template is treated with oxygen plasma for 10 minutes, and the wrinkle template with a regular shape is obtained after retraction;
(3)在水浴环境下,将玻璃基底上旋涂2wt%PS薄膜转移到步骤(1)的用于转移PS薄膜的拉伸的PDMS上,形成PDMS/PS双层体系,真空条件下进行干燥;(3) In a water bath environment, transfer the spin-coated 2wt% PS film on the glass substrate to the stretched PDMS used to transfer the PS film in step (1) to form a PDMS/PS double-layer system, and dry it under vacuum conditions ;
(4)将步骤(2)制备的皱纹模板以与PDMS拉伸方向成90度角加盖到经过步骤(3)中真空干燥过的PDMS/PS双层体系上,90摄氏度下加热2小时后冷却到室温,将皱纹模板揭掉,得到一级形貌;(4) Cover the wrinkle template prepared in step (2) on the PDMS/PS bilayer system that has been vacuum-dried in step (3) at an angle of 90 degrees to the PDMS stretching direction, and heat it at 90 degrees Celsius for 2 hours Cool to room temperature, remove the wrinkle template, and obtain the first-order morphology;
(5)将步骤(4)获得的具有一级形貌的PDMS/PS/双层体系回缩,产生二级皱纹形貌,最终制备了两级复合形貌。复合形貌如图1所示,其中图1为光学显微镜图片。(5) The PDMS/PS/bilayer system with the first-order morphology obtained in step (4) was retracted to produce a second-order wrinkled morphology, and finally a two-stage composite morphology was prepared. The composite morphology is shown in Figure 1, where Figure 1 is an optical microscope picture.
实施例2:Example 2:
(1)将PDMS弹性体固定到拉伸台上,预拉伸率为5%,用于制备皱纹模板;拉伸率为10%,用于转移PS薄膜;(1) Fix the PDMS elastomer on the stretching table, the pre-stretch rate is 5%, and it is used to prepare the wrinkle template; the stretch rate is 10%, and it is used to transfer the PS film;
(2)将用于制备皱纹模板的拉伸的PDMS,经过氧等离子体处理10分钟,回缩后得到带有规整形貌的皱纹模板;(2) The stretched PDMS used to prepare the wrinkle template is treated with oxygen plasma for 10 minutes, and the wrinkle template with a regular shape is obtained after retraction;
(3)在水浴环境下,将玻璃基底上旋涂3wt%PS薄膜转移到步骤(1)的用于转移PS薄膜的拉伸的PDMS上,形成PDMS/PS双层体系,真空条件下进行干燥;(3) In a water bath environment, transfer the spin-coated 3wt% PS film on the glass substrate to the stretched PDMS used to transfer the PS film in step (1) to form a PDMS/PS double-layer system, and dry it under vacuum conditions ;
(4)将步骤(2)制备的皱纹模板以与PDMS拉伸方向成50度角加盖到经过步骤(3)中真空干燥过的PDMS/PS双层体系上,105摄氏度下加热1小时后冷却到室温,将皱纹模板揭掉,得到一级形貌;(4) Cover the wrinkle template prepared in step (2) on the PDMS/PS bilayer system that has been vacuum-dried in step (3) at an angle of 50 degrees to the PDMS stretching direction, and heat it at 105 degrees Celsius for 1 hour Cool to room temperature, remove the wrinkle template, and obtain the first-order morphology;
(5)将步骤(4)获得的具有一级形貌的PDMS/PS/双层体系回缩,产生二级皱纹形貌,最终制备了两级复合形貌。复合形貌如图2所示,其中图2为光学显微镜图片。(5) The PDMS/PS/bilayer system with the first-order morphology obtained in step (4) was retracted to produce a second-order wrinkled morphology, and finally a two-stage composite morphology was prepared. The composite morphology is shown in Figure 2, where Figure 2 is an optical microscope picture.
实施例3:Example 3:
(1)将PDMS弹性体固定到拉伸台上,预拉伸率为5%,用于制备皱纹模板;拉伸率为5%,用于转移PS薄膜;(1) Fix the PDMS elastomer on the stretching table with a pre-stretch rate of 5%, which is used to prepare a wrinkle template; a stretch rate of 5%, which is used to transfer the PS film;
(2)将用于制备皱纹模板的拉伸的PDMS,经过氧等离子体处理15分钟,回缩后得到带有规整形貌的皱纹模板;(2) The stretched PDMS used to prepare the wrinkle template was treated with oxygen plasma for 15 minutes, and a wrinkle template with a regular shape was obtained after retraction;
(3)在水浴环境下,将玻璃基底上旋涂2wt%PS薄膜转移到步骤(1)的用于转移PS薄膜的拉伸的PDMS上,形成PDMS/PS双层体系,真空条件下进行干燥;(3) In a water bath environment, transfer the spin-coated 2wt% PS film on the glass substrate to the stretched PDMS used to transfer the PS film in step (1) to form a PDMS/PS double-layer system, and dry it under vacuum conditions ;
(4)将步骤(2)制备的皱纹模板以与PDMS拉伸方向成0度角加盖到经过步骤(3)中真空干燥过的PDMS/PS双层体系上,120摄氏度下加热0.5小时后冷却到室温,将皱纹模板揭掉,得到一级形貌;(4) Cover the wrinkle template prepared in step (2) on the PDMS/PS bilayer system that has been vacuum-dried in step (3) at an angle of 0 degrees to the PDMS stretching direction, and heat it at 120 degrees Celsius for 0.5 hours Cool to room temperature, remove the wrinkle template, and obtain the first-order morphology;
(5)将步骤(4)获得的具有一级形貌的PDMS/PS/双层体系回缩,产生二级皱纹形貌,最终制备了两级复合形貌。复合形貌如图3所示,其中图3为光学显微镜图片。(5) The PDMS/PS/bilayer system with the first-order morphology obtained in step (4) was retracted to produce a second-order wrinkled morphology, and finally a two-stage composite morphology was prepared. The composite morphology is shown in Figure 3, where Figure 3 is an optical microscope picture.
实施例4:Example 4:
(1)将PDMS弹性体固定到拉伸台上,预拉伸率为10%,用于制备皱纹模板;拉伸率为3%,用于转移PS薄膜;(1) Fix the PDMS elastomer on the stretching table with a pre-stretch rate of 10% for preparing a wrinkle template; a stretch rate of 3% for transferring the PS film;
(2)将用于制备皱纹模板的拉伸的PDMS,经过氧等离子体处理30分钟,回缩后得到带有规整形貌的皱纹模板;(2) The stretched PDMS used to prepare the wrinkle template was treated with oxygen plasma for 30 minutes, and a wrinkle template with a regular appearance was obtained after retraction;
(3)在水浴环境下,将玻璃基底上旋涂4wt%PS薄膜转移到步骤(1)的用于转移PS薄膜的拉伸的PDMS上,形成PDMS/PS双层体系,真空条件下进行干燥;(3) In a water bath environment, transfer the spin-coated 4wt% PS film on the glass substrate to the stretched PDMS used to transfer the PS film in step (1) to form a PDMS/PS double-layer system, and dry it under vacuum ;
(4)将步骤(2)制备的皱纹模板以与PDMS拉伸方向成45度角加盖到经过步骤(3)中真空干燥过的PDMS/PS双层体系上,95摄氏度下加热1小时后冷却到室温,将皱纹模板揭掉,得到一级形貌;(4) Cover the wrinkle template prepared in step (2) on the PDMS/PS bilayer system that has been vacuum-dried in step (3) at an angle of 45 degrees to the PDMS stretching direction, and heat it at 95 degrees Celsius for 1 hour Cool to room temperature, remove the wrinkle template, and obtain the first-order morphology;
(5)将步骤(4)获得的具有一级形貌的PDMS/PS/双层体系回缩,产生二级皱纹形貌,最终制备了两级复合形貌。(5) The PDMS/PS/bilayer system with the first-order morphology obtained in step (4) was retracted to produce a second-order wrinkled morphology, and finally a two-stage composite morphology was prepared.
综上,本发明方法主要是将聚苯乙烯(PS)薄膜转移到拉伸的PDMS基底,得到PDMS/PS软硬复合体系。通过模板压印和表面起皱相结合的方法依次构筑一级形貌、二级形貌。实验中可以通过调控一级、二级形貌的相交角度,改变复合形貌的各向异性。本发明方法将自上而下的模板压印和从下而上的表面起皱结合起来,保留了各自方法的优点。In summary, the method of the present invention mainly transfers the polystyrene (PS) film to the stretched PDMS substrate to obtain a PDMS/PS soft-hard composite system. The combination of template imprinting and surface wrinkling is used to construct the first-order morphology and the second-order morphology in sequence. In the experiment, the anisotropy of the composite morphology can be changed by adjusting the intersection angle of the primary and secondary morphology. The method of the present invention combines top-down stencil imprinting and bottom-up surface wrinkling, retaining the advantages of each method.
尽管上面结合图对本发明进行了描述,但本发明并不局限于上述的具体实施方案,上述的具体实施方式仅仅是示意性的,而不是限制性的,本领域的普通技术人员在本发明的启示下,在不脱离本发明宗旨的情况下,还可以作出很多变形,这些均属于本发明的保护之内。Although the present invention has been described above in conjunction with the drawings, the present invention is not limited to the above-mentioned specific embodiments, and the above-mentioned specific embodiments are only illustrative and not restrictive. Under the inspiration, many modifications can be made without departing from the gist of the present invention, and these all belong to the protection of the present invention.
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Publication number | Priority date | Publication date | Assignee | Title |
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102491254A (en) * | 2011-12-14 | 2012-06-13 | 天津大学 | Method for wrinkling polydimethylsiloxane (PDMS) elastomer in selective area |
CN102794904A (en) * | 2012-07-13 | 2012-11-28 | 天津大学 | Preparation method and application of PDMS (polydimethylsiloxane) surface double-layer selected area wrinkle |
CN103373703A (en) * | 2013-07-04 | 2013-10-30 | 天津大学 | Method for forming double-layer orderly-arranged nanoparticles by utilizing polymers as templates |
KR20140007589A (en) * | 2012-07-09 | 2014-01-20 | 한국기초과학지원연구원 | Method for transfering pleated microstructure and method for measuring electrical characteristics of the same |
-
2014
- 2014-12-05 CN CN201410736080.7A patent/CN104476895B/en not_active Expired - Fee Related
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102491254A (en) * | 2011-12-14 | 2012-06-13 | 天津大学 | Method for wrinkling polydimethylsiloxane (PDMS) elastomer in selective area |
KR20140007589A (en) * | 2012-07-09 | 2014-01-20 | 한국기초과학지원연구원 | Method for transfering pleated microstructure and method for measuring electrical characteristics of the same |
CN102794904A (en) * | 2012-07-13 | 2012-11-28 | 天津大学 | Preparation method and application of PDMS (polydimethylsiloxane) surface double-layer selected area wrinkle |
CN103373703A (en) * | 2013-07-04 | 2013-10-30 | 天津大学 | Method for forming double-layer orderly-arranged nanoparticles by utilizing polymers as templates |
Non-Patent Citations (2)
Title |
---|
杨扬: "表面皱纹区域化制备以及模板应用", 《中国硕士学位论文全文数据库 工程科技Ⅰ辑》, 15 August 2012 (2012-08-15) * |
邱鑫: "基于嵌段聚合物的高级皱纹结构的制备", 《中国硕士学位论文全文数据库 工程科技Ⅰ辑》, 15 August 2014 (2014-08-15), pages 34 - 35 * |
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