CN103213940B - One makes material have two kinds of infiltrating methods of difference based on micro-nano-scale - Google Patents
One makes material have two kinds of infiltrating methods of difference based on micro-nano-scale Download PDFInfo
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- CN103213940B CN103213940B CN201310084326.2A CN201310084326A CN103213940B CN 103213940 B CN103213940 B CN 103213940B CN 201310084326 A CN201310084326 A CN 201310084326A CN 103213940 B CN103213940 B CN 103213940B
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- 238000000034 method Methods 0.000 title claims abstract description 13
- 239000000463 material Substances 0.000 title claims abstract description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000011248 coating agent Substances 0.000 claims abstract description 16
- 238000000576 coating method Methods 0.000 claims abstract description 16
- 229920002120 photoresistant polymer Polymers 0.000 claims abstract description 12
- 239000002086 nanomaterial Substances 0.000 claims abstract description 11
- OVZXZCHMYYOSKH-UHFFFAOYSA-N fluoro-tris(1,1,2,2,2-pentafluoroethoxy)silane Chemical compound FC(F)(F)C(F)(F)O[Si](F)(OC(F)(F)C(F)(F)F)OC(F)(F)C(F)(F)F OVZXZCHMYYOSKH-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000758 substrate Substances 0.000 claims abstract description 9
- 239000000126 substance Substances 0.000 claims abstract description 5
- 238000001771 vacuum deposition Methods 0.000 claims abstract description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 18
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 239000011159 matrix material Substances 0.000 claims description 2
- 239000010409 thin film Substances 0.000 abstract description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 abstract 1
- 229910000077 silane Inorganic materials 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000010408 film Substances 0.000 description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 5
- 229910052710 silicon Inorganic materials 0.000 description 5
- 239000010703 silicon Substances 0.000 description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 244000020998 Acacia farnesiana Species 0.000 description 3
- 235000010643 Leucaena leucocephala Nutrition 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 230000003075 superhydrophobic effect Effects 0.000 description 2
- 238000009736 wetting Methods 0.000 description 2
- 238000000018 DNA microarray Methods 0.000 description 1
- 238000012271 agricultural production Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- XPBBUZJBQWWFFJ-UHFFFAOYSA-N fluorosilane Chemical compound [SiH3]F XPBBUZJBQWWFFJ-UHFFFAOYSA-N 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 230000005661 hydrophobic surface Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
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Abstract
一种基于微纳米尺度使材料具有两种不同浸润性的方法，属于微纳薄膜技术领域。对基体进行清洗，并涂上光刻胶，制备微纳结构，进行真空镀膜，镀膜厚度几十纳米到几微米，镀膜后用丙酮清洗掉光刻胶，然后将其浸泡在全氟三乙氧基甲硅烷酒精溶液中，使得全氟三乙氧基甲硅烷进入原光刻胶的所在微纳结构中，拿出后用酒精清洗；用化学方法去除掉表面镀的镀膜，即在基体上得到微纳尺寸两种不同浸润性的表面。本发明可以通过微纳结构的尺寸和面积比例来调节宏观表面的浸润性。The invention discloses a method for making materials have two different wettability based on the micro-nano scale, and belongs to the technical field of micro-nano thin films. Clean the substrate, apply photoresist, prepare micro-nano structure, and conduct vacuum coating. The thickness of the coating is tens of nanometers to several microns. In the silane alcohol solution, make perfluorotriethoxysilane enter into the micro-nano structure of the original photoresist, take it out and clean it with alcohol; remove the coating on the surface by chemical method, that is, get micro-nano structure on the substrate Dimensions Two surfaces with different wettability. The invention can adjust the wettability of the macroscopic surface through the size and area ratio of the micro-nano structure.
Description
技术领域technical field
本发明涉及一种在不同材料表面制备微纳米尺寸，使其具有两种不同浸润性的方法，该方法制备简单，可以应用于浸润性的理论及实验的研究，属于微纳薄膜技术领域。The invention relates to a method for preparing micro-nano dimensions on the surface of different materials to make them have two different wettability. The method is simple to prepare and can be applied to theoretical and experimental research on wettability, belonging to the technical field of micro-nano thin films.
背景技术Background technique
润湿性(又称浸润性，Wettability)是固体表面的重要特征之一，无论在人们的日常生活当中还是在工农业生产中它都发挥着重要的作用。润湿性能的应用极其广泛，像微电子工业、印刷工业、造纸工业、交通行业乃至新材料的合成制备以及医药，生物芯片方面无不与润湿性能有着密切的关系。Wettability (also known as wettability, Wettability) is one of the important characteristics of solid surfaces, and it plays an important role in people's daily life and in industrial and agricultural production. The application of wetting properties is extremely wide, such as microelectronics industry, printing industry, paper industry, transportation industry, and even the synthesis and preparation of new materials, as well as medicine, and biochips are all closely related to wetting properties.
Cassie和Baxter[12]在研究了大量自然界中超疏水表面的过程中提出了复合接触的概念，他们认为液滴在粗糙表面上的接触是一种复合接触。微细结构化的表面因为结构尺度小于表面液滴的尺度，当表面疏水性较强时，Cassie认为在疏水表面上的液滴并不能填满粗糙表面上的凹槽，在液珠下面将有截留的空气在，于是表观上的液固接触面其实由固体和气体共同组成表面的润湿性能是由其表面的化学组成和微观形貌共同决定的。Cassie and Baxter [12] proposed the concept of compound contact in the process of studying a large number of superhydrophobic surfaces in nature. They believed that the contact of liquid droplets on rough surfaces is a compound contact. Because the structure scale of the microstructured surface is smaller than that of the surface droplet, when the surface is highly hydrophobic, Cassie believes that the droplet on the hydrophobic surface cannot fill the groove on the rough surface, and there will be interception under the droplet. The air is present, so the apparent liquid-solid contact surface is actually composed of solid and gas, and the wettability of the surface is determined by the chemical composition and microscopic morphology of the surface.
在理论工作研究方面，尽管一些基本的理论已经得到初步的验证并开始被广大研究者所认同，但是这些问题大多还只停留在超疏水大接触角度的形成及稳定性机制上，这些现象的内在原理得到了很大的推动和进步。但是对于微观尺寸内两种浸润性对固体表面的浸润性影响到目前为止还没有涉及。所以研究两种浸润性在不同接触份数下的整体浸润性很有必要。In terms of theoretical work research, although some basic theories have been initially verified and have begun to be recognized by the majority of researchers, most of these problems still only stay on the formation and stability mechanisms of superhydrophobic large contact angles. The principle has been greatly promoted and advanced. However, the influence of the two kinds of wettability on the solid surface wettability in the microscopic scale has not been involved so far. Therefore, it is necessary to study the overall wettability of the two kinds of wettability under different contact fractions.
发明内容Contents of the invention
本发明所要解决的问题是，提供一种使微观表面达到两种浸润性的材料的制作方法，通过在其表面形貌的构造，在不同形貌上实现不同的浸润性，从而研究其对材料整体的宏观浸润性影响。The problem to be solved by the present invention is to provide a method for making a material that achieves two types of wettability on the microscopic surface. Overall macroscopic invasiveness effects.
为了解决上述问题，本发明所采用的技术方案是制备尺寸不同的方形形貌的结构，在基体上对其进行光刻、曝光，然后在其上镀上一层薄膜，用丙酮对其光刻胶进行清洗，得到所需的形貌。然后把镀有薄膜的基体放在全氟三乙氧基甲硅烷酒精溶液浸泡，用酒精清洗。然后用化学方法去掉上面镀的薄膜。即可得到所需要的微观领域两种浸润性形貌的材料。In order to solve the above-mentioned problems, the technical scheme adopted in the present invention is to prepare structures of square shapes with different sizes, photoetch and expose them on the substrate, and then coat a layer of thin film on it, and photoetch them with acetone The gel was cleaned to obtain the desired morphology. Then soak the film-coated substrate in perfluorotriethoxysilane alcohol solution and clean it with alcohol. Then use chemical methods to remove the above-plated film. The material with two kinds of wettability morphology in the required microscopic domain can be obtained.
本发明一种基于微纳米尺度使材料具有两种不同浸润性的方法，其特征在于，包括以下步骤：The present invention is a method for making materials have two different wettability based on the micro-nano scale, which is characterized in that it comprises the following steps:
（1）纯基体分别用甲苯、丙酮、乙醇进行超声，用去粒子水冲洗干净；(1) Ultrasonic the pure matrix with toluene, acetone, and ethanol respectively, and rinse it with particle-free water;
（2）在基体上均匀涂一层光刻胶，经过烘烤、曝光，显影得到微纳结构的表面形貌；(2) Evenly coat a layer of photoresist on the substrate, after baking, exposure, and development to obtain the surface morphology of the micro-nano structure;
（3）对步骤（2）得到的基体进行真空镀膜，镀膜厚度几十纳米到几微米，镀膜材料为任意可实现的能用化学方法除去的材料，镀膜后用丙酮清洗掉光刻胶，然后将其浸泡在全氟三乙氧基甲硅烷酒精溶液中，使得全氟三乙氧基甲硅烷进入原光刻胶的所在微纳结构中，全氟三乙氧基甲硅烷酒精溶液浓度优选为1wt%，拿出后用酒精清洗；一般氟硅烷浓度不同，浸泡时间不同。(3) Carry out vacuum coating on the substrate obtained in step (2), the coating thickness is tens of nanometers to several microns, the coating material is any material that can be removed by chemical methods, and the photoresist is cleaned with acetone after coating, and then It is soaked in the perfluorotriethoxysilane alcohol solution, so that the perfluorotriethoxysilane enters the micro-nano structure of the original photoresist, and the concentration of the perfluorotriethoxysilane alcohol solution is preferably 1wt%, take it out and clean it with alcohol; Generally, the concentration of fluorosilane is different, and the soaking time is different.
（4）用化学方法去除掉步骤（3）表面镀的镀膜，即在基体上得到微纳尺寸两种不同浸润性的表面。(4) Chemically remove the coating on the surface of step (3), that is, two different wettability surfaces of micro-nano size are obtained on the substrate.
与已有技术相比，本发明的特征在于，在一种表面微观实现两种不同的浸润性。本发明可以通过微纳结构的尺寸和面积比例来调节宏观表面的浸润性，本发明也可验证Wenzel和Cassie理论。Compared with the prior art, the present invention is characterized in that two different wettability are realized on one surface microscopically. The invention can adjust the wettability of the macroscopic surface through the size and area ratio of the micro-nano structure, and the invention can also verify the theory of Wenzel and Cassie.
附图说明Description of drawings
图1为实施例1所得样品的镀膜后的金相照片，深颜色灰黑色方格的接触角为65°，其余的接触角为27°；Fig. 1 is the metallographic photograph after the coating of the sample gained in embodiment 1, the contact angle of dark color gray black square is 65 °, and all the other contact angles are 27 °;
图2为实施例1水滴在所制备的不同方形份数表面的接触角，左图对应图1左图，右图对应图1的右图。Fig. 2 is the contact angle of the water droplets prepared in Example 1 on the surface of different square fractions, the left figure corresponds to the left figure of Fig. 1, and the right figure corresponds to the right figure of Fig. 1.
具体实施方式detailed description
以下用两个实施例子来进一步介绍本发明，但本发明并不限于以下实施例。The following two implementation examples are used to further introduce the present invention, but the present invention is not limited to the following examples.
实施例1：Example 1:
（1）纯硅片分别用甲苯、丙酮、乙醇进行超声15min，用去粒子水冲洗干净。(1) Ultrasonic the pure silicon wafer with toluene, acetone, and ethanol for 15 minutes, and rinse it with particle-free water.
（2）在其上均匀涂一层正光刻胶，厚度约为1微米。经过烘烤、用掩膜曝光，显影得到微纳结构的表面形貌。(2) Apply a layer of positive photoresist evenly on it, with a thickness of about 1 micron. After baking, exposure with a mask, and development, the surface morphology of the micro-nano structure is obtained.
（3）对得到的硅片进行真空铝镀膜，镀膜厚度几十纳米到几微米不等，镀膜后用丙酮清洗掉光刻胶，然后将其浸泡在1wt%全氟三乙氧基甲硅烷酒精溶液浸泡3h，拿出后用酒精清洗。(3) Vacuum aluminum coating is carried out on the obtained silicon wafer, the thickness of the coating film ranges from tens of nanometers to several microns. After coating, the photoresist is cleaned with acetone, and then soaked in 1wt% perfluorotriethoxysilane alcohol Soak the solution for 3 hours, take it out and clean it with alcohol.
（4）用氢氧化钠腐蚀去除掉表面镀的铝薄膜，即在硅上得到微纳尺寸两种不同浸润性的表面。(4) The aluminum film plated on the surface is removed by etching with sodium hydroxide, that is, two different wettability surfaces of micro-nano size are obtained on the silicon.
实施例2：Example 2:
（1）纯钨片分别用甲苯、丙酮、乙醇进行超声15min，用去粒子水冲洗干净。(1) Ultrasonic the pure tungsten sheet with toluene, acetone, and ethanol for 15 minutes respectively, and rinse it with particle-free water.
（2）在其上均与涂一层正光刻胶，厚度约为1微米。经过烘烤、用掩膜曝光，显影得到微纳结构的表面形貌。(2) Apply a layer of positive photoresist on it, with a thickness of about 1 micron. After baking, exposure with a mask, and development, the surface morphology of the micro-nano structure is obtained.
（3）对得到的硅片进行真空铝镀膜，镀膜厚度几十纳米到几微米不等，镀膜后用丙酮清洗掉光刻胶，然后将其浸泡在全氟三乙氧基甲硅烷酒精溶液浸泡1h，拿出后用酒精清洗。(3) Vacuum aluminum coating is carried out on the obtained silicon wafer, the thickness of the coating film ranges from tens of nanometers to several microns. After coating, the photoresist is washed off with acetone, and then soaked in perfluorotriethoxysilane alcohol solution 1h, take it out and clean it with alcohol.
（4）用氢氧化钠腐蚀去除掉表面镀的铝薄膜，即在硅上得到微纳尺寸两种不同浸润性的表面。(4) The aluminum film plated on the surface is removed by etching with sodium hydroxide, that is, two different wettability surfaces of micro-nano size are obtained on the silicon.
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| CN1598695A (en) * | 2003-07-14 | 2005-03-23 | Jsr株式会社 | Method for forming pattern, and optical element |
| CN1697598A (en) * | 1998-05-14 | 2005-11-16 | 精工爱普生株式会社 | Substrate for forming specific pattern and manufacturing method thereof |
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| CN1815686A (en) * | 2004-12-17 | 2006-08-09 | 株式会社半导体能源研究所 | Semiconductor device and manufacturing method thereof |
| CN101475173A (en) * | 2009-01-20 | 2009-07-08 | 吉林大学 | Method for preparing super-hydrophobic antireflex micron and nano composite structure surface |
| CN101968565A (en) * | 2010-09-27 | 2011-02-09 | 徐州雷奥医疗设备有限公司 | Method for improving imaging quality of endoscope |
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| CN1697598A (en) * | 1998-05-14 | 2005-11-16 | 精工爱普生株式会社 | Substrate for forming specific pattern and manufacturing method thereof |
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| JP2006108506A (en) * | 2004-10-07 | 2006-04-20 | Seiko Epson Corp | Film pattern forming method and substrate manufacturing method |
| CN1815686A (en) * | 2004-12-17 | 2006-08-09 | 株式会社半导体能源研究所 | Semiconductor device and manufacturing method thereof |
| CN101475173A (en) * | 2009-01-20 | 2009-07-08 | 吉林大学 | Method for preparing super-hydrophobic antireflex micron and nano composite structure surface |
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Effective date of registration: 20200921 Address after: 061000 Chenquan Industrial Zone, Xian County, Cangzhou City, Hebei Province Patentee after: HEBEI MORTMAIN RUBBER AND PLASTIC TECHNOLOGY Co.,Ltd. Address before: Room 1424, Floor 4, Peony Pioneer Building, No. 2 Garden Road, Haidian District, Beijing, 100191 Patentee before: Beijing Zhonglian Technology Service Co.,Ltd. Effective date of registration: 20200921 Address after: Room 1424, Floor 4, Peony Pioneer Building, No. 2 Garden Road, Haidian District, Beijing, 100191 Patentee after: Beijing Zhonglian Technology Service Co.,Ltd. Address before: 100124 Chaoyang District, Beijing Ping Park, No. 100 Patentee before: Beijing University of Technology |
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Application publication date: 20130724 Assignee: Beijing Hongyi Shunfa Construction Equipment Leasing Co.,Ltd. Assignor: HEBEI MORTMAIN RUBBER AND PLASTIC TECHNOLOGY Co.,Ltd. Contract record no.: X2022980021410 Denomination of invention: A method based on micro nano scale to make materials have two different wettability Granted publication date: 20160406 License type: Common License Record date: 20221115 |
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