CN106009014A - 玻璃模版法制备超疏水聚四氟乙烯薄膜的方法 - Google Patents
玻璃模版法制备超疏水聚四氟乙烯薄膜的方法 Download PDFInfo
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Abstract
本发明公开了玻璃模版法制备超疏水聚四氟乙烯薄膜的方法,它是采用激光刻蚀、等离子体刻蚀或氧化还原法,制备粗糙度为1.5‑10微米的毛玻璃模版,将5‑35%的聚四氟乙烯乳液,涂在毛玻璃模版毛化一面,干燥后,固化,在温度降到10‑50℃时揭下薄膜。通过使用微米级的毛玻璃模版,利用固化时聚四氟乙烯的薄膜表面产生的内应力,获得了纳米级超疏水表面微结构的聚四氟乙烯薄膜,模版无磨损;解决了模版压印技术中,压印模版和聚合物薄膜之间粘接严重,模版重复使用率低的问题,可生产更大面积的纳米级超疏水薄膜;且基底厚可达10微米,避免了气相电化学反应,导致的金属表面锈蚀,生产过程中只有干燥和固化,没有任何排放,环保。
Description
技术领域
本发明属疏水材料技术领域,具体涉及玻璃模版法制备超疏水聚四氟乙烯薄膜的方法。
背景技术
超疏水表面是指静态接触角大于150度,滚动角小于10度的具有微米-纳米级结构特殊表面。这种表面具有自洁防污的基本性能,是人造的荷叶表面。可以广泛的用于电力、航洋、石油化工、航空、风电、太阳能光伏板等广泛的领域。主要解决:(1)自洁功能,防止表面污渍和污染;(2)防腐蚀作用:由于其超疏水在其表面与水接触面形成一层空气隔膜,所以更高改善其防腐蚀性能。
目前虽然有一些涂层或者低表面能的薄膜,如聚四氟乙烯薄膜、聚氨酯薄膜等能够具有一定的防污和自洁的功能,但其自洁和防污的功能非常有限。
超疏水表面虽然可以通过以下三种方式来实现:1)表面结构构造(化学腐蚀、激光刻蚀或者模版压印等)外加低表面能修饰,如专利:CN201210388555.9 ;2)涂料方法:直接利用传统的喷涂设备将超疏水涂料喷涂或者涂覆在其工件表面,干燥和固化后形成超疏水表面如中国专利:CN201110278149.2;CN201210286775.0;CN201210466649.3;还有美国的超级干商品和Neverwet商品;3)申请人曾利用聚四氟乙烯乳液和锌的水溶液及其氯化钠的混合水溶液,涂覆在其工件表面,通过原位加热和洗涤处理,获得超疏水薄膜(中国发明专利:CN201410315176.6)。
超疏水表面的难点和关键是:大面积低成本的构造微米纳米技术,提高超疏水表面的机械强度和化学耐用性(耐腐蚀性和耐水浸泡性能),虽然一般的超疏水表面(不论是涂层型还是改性型)有一定的耐腐蚀性(防腐蚀性能),但由于表面层的多孔性,很容易导致气相电化学反应,导致金属表面的锈蚀,所以其防腐蚀性能非常有限(参见文献:Wang, Li,Jieyi Yang, Yan Zhu, Zhenhua Li, Tao Sheng, Y. M. Hu, and De-Quan Yang. "AStudy of the Mechanical and Chemical Durability of Ultra-Ever DrySuperhydrophobic Coating on Low Carbon Steel Surface." Colloids and SurfacesA: Physicochemical and Engineering Aspects, 497(2016)17-27. )。
粗糙表面的压印技术(杨得全等“一种利用热喷涂模板法制备超疏水聚合物表面的方法”,CN 201210388555.9),机械耐用性好,解决了气相电化学反应,导致金属表面锈蚀的问题。但是压印模版和聚合物薄膜之间粘接严重,压印模版的重复使用率较低;不能制造大面积单块薄膜,操作也比较困难。
发明内容
本发明的目的是为了解决粗糙表面的压印超疏水聚合物薄膜,压印模版和聚合物薄膜之间粘接严重,压印模版易磨损,重复使用率低,单次生产面积小的问题,而提供一种玻璃模版法制备超疏水聚四氟乙烯薄膜的方法。
一种毛玻璃模版,它的粗糙度为1.5-10微米;
所述的粗糙度为:1.5-5微米;
它采用激光刻蚀、等离子体刻蚀或氧化还原法制备的;
所述的氧化还原法,采用的氧化还原混合液包括:15-35%的浓度为40-60%的硫酸、盐酸或硝酸、5-15%氢氟酸、40-60%的浓度为5-10%乙醇、0.03-0.06%硝酸铵;上述各组份之和为100%;
所述的氧化还原法,采用的氧化还原混合液为100g五倍子酸 、305ml乙醇胺、140ml水、1.3g吡嗪、0.24mlFC129;
(2)所述的氧化还原法,采用的氧化还原混合液包括:50g 浓度为68%HNO3、30g浓度为55%HF、30 g CH3 COOH、0.6gBr2;
玻璃模版法制备超疏水聚四氟乙烯薄膜的方法,它包括:
1)将5-35%的聚四氟乙烯乳液,涂在粗糙度为1.5-10微米的毛玻璃模版毛化一面;
2)90-110℃干燥;
3)300-360℃固化;
4)缓慢降温后,在10-50℃的温度下揭下聚四氟乙烯薄膜;
步骤1)所述的聚四氟乙烯乳液涂抹厚度为10-20微米。
步骤2)所述的干燥温度为100℃,时间为30-100分钟;
步骤如果)所述的固化时间为20-40分钟。
本发明提供了玻璃模版法制备超疏水聚四氟乙烯薄膜的方法,它是采用激光刻蚀、等离子体刻蚀或氧化还原法,制备粗糙度为1.5-10微米的毛玻璃模版,将5-35%的聚四氟乙烯乳液,涂在毛玻璃模版毛化一面,90-110℃干燥30-100min后,放入300-360℃固化20-40min,缓慢降温后,在温度降到10-50℃时揭下薄膜。通过使用微米级的毛玻璃模版,利用固化时聚四氟乙烯的薄膜表面产生的内应力,获得了纳米级超疏水表面微结构的聚四氟乙烯薄膜,使薄膜表面微结构更加稳定,模版无磨损;解决了模版压印技术中,压印模版和聚合物薄膜之间粘接严重,模版重复使用率低的问题,可生产更大面积的纳米级超疏水薄膜;且基底厚可达10微米,贴在金属表面时,避免了气相电化学反应,导致的金属表面锈蚀。生产过程中只有干燥和固化,没有任何排放,环保。
附图说明
图1 传统方法制备超疏水表面的流程图;
图2 玻璃模版法制备超疏水聚四氟乙烯薄膜的流程图;
图3 为典型的毛玻璃模版表面电镜照片;
图4 为玻璃模版法制备超疏水聚四氟乙烯薄膜表面微结构和与水接触情况电子显镜照片。
具体实施方式
实施例1
1. 毛玻璃模版的制备:(1)用氧化还原方法制作毛玻璃,采用15-35%浓度为40-60%的硫酸(或者盐酸、硝酸)作为氧化剂、5-15%氢氟酸作为还原剂、40-60%的浓度为5-10%乙醇作为缓冲剂、0.03-0.06%硝酸铵为催化剂的混合液,室温下(20-30℃)浸泡1-2个小时,(2)取出玻璃用水清洗表面残余物;(3)干燥玻璃表面得到毛化的玻璃。
2. 用10%的聚四氟乙烯乳液(浙江巨化)刷涂或者辊涂在玻璃板上毛化的一面;
3. 将载有聚四氟乙烯乳液的毛玻璃在90-110℃下干燥30-100min;
4. 将干燥的载有聚四氟乙烯膜的玻璃板放入300-360℃的烘箱中固化30min;
5. 缓慢降温至100℃,拿出固化的玻璃板;
6. 在10-50℃的温度下轻轻拨拉出聚四氟乙烯薄膜,获得单面是超疏水的聚四氟乙烯薄膜,其静态接触角为157度,滚动角为4度;
7. 玻璃模版可以重复使用多次。
实施例2
1. 毛化玻璃模版制备:(1)配置氧化还原混合液体,包括:100g五倍子酸 、305ml乙醇胺、 140ml水 、 1.3g吡嗪、 0.24mlFC129(2)将玻璃置于液体中,室温下(20-30℃)浸泡1-2个小时,取出;(3)水洗清洁表面,(4)干燥其毛化的玻璃表面;
2. 用25%的聚四氟乙烯乳液(浙江巨化)刷涂或者辊涂在玻璃板上毛化的一面;
3. 将载有聚四氟乙烯乳液的毛玻璃在100℃下干燥60min;
4. 将干燥的载有聚四氟乙烯膜的玻璃板放入320℃的烘箱中固化20min;
5. 缓慢降温至100℃,拿出固化的玻璃板;
6. 在25℃的温度下轻轻拨拉出聚四氟乙烯薄膜,获得单面是超疏水的聚四氟乙烯薄膜,其表面的静态接触角为154度,滚动角为5度;
7. 玻璃模版可以重复使用多次。
实施例3
1. 制备毛化玻璃模版:(1)配置氧化还原混合液体,包括:50g HNO3[68%] 、30gHF[55%]、 CH3 COOH 30 g、 0.6gBr2;(2)将玻璃置于液体中,室温下浸泡2小时,取出;(3)水洗清洁表面,(4)干燥其毛化的玻璃表面;
2.用35%的聚四氟乙烯乳液(浙江巨化)刷涂或者辊涂在玻璃板上毛化的一面;
3. 将载有聚四氟乙烯乳液的毛玻璃在100℃下干燥30min;
4. 将干燥的载有聚四氟乙烯膜的玻璃板放入300℃的烘箱中固化40min;
5. 缓慢降温至100℃,拿出固化的玻璃板;
6. 在50℃的温度下轻轻拨拉出聚四氟乙烯薄膜,获得单面是超疏水的聚四氟乙烯薄膜,其表面静态接触角为163度,滚动角为6度;
7. 玻璃模版可以重复使用多次。
Claims (10)
1.一种毛玻璃模版,它的粗糙度为1.5-10微米。
2.根据权利要求1所述的一种毛玻璃模版,其特征在于:所述的粗糙度为1.5-5微米。
3.根据权利要求1或2所述的一种毛玻璃模版,其特征在于:它是采用激光刻蚀、等离子体刻蚀或氧化还原法制备的。
4.根据权利要求3所述的一种毛玻璃模版,其特征在于:所述的氧化还原法,采用的氧化还原混合液为:15-35%的浓度为40-60%的硫酸、盐酸或硝酸、5-15%氢氟酸、40-60%的浓度为5-10%乙醇、0.03-0.06%硝酸铵;上述各组份之和为100%。
5.根据权利要求3所述的一种毛玻璃模版,其特征在于:所述的氧化还原法,采用的氧化还原混合液为100g五倍子酸 、305ml乙醇胺、140ml水、1.3g吡嗪、0.24mlFC129。
6.根据权利要求3所述的一种毛玻璃模版,其特征在于:所述的氧化还原法,采用的氧化还原混合液包括:50g 浓度为68%HNO3、 30g浓度为55%HF、30 g CH3 COOH、0.6gBr2。
7.玻璃模版法制备超疏水聚四氟乙烯薄膜的方法,它包括:
1)将5-35%的聚四氟乙烯乳液,涂在粗糙度为1.5-10微米的毛玻璃模版毛化一面;
2)90-110℃干燥;
3)300-360℃固化;
4)缓慢降温后,在10-50℃的温度下揭下聚四氟乙烯薄膜。
8.根据权利要求7所述的玻璃模版法制备超疏水聚四氟乙烯薄膜的方法,其特征在于:步骤1)所述的聚四氟乙烯乳液涂抹厚度为10-20微米。
9.根据权利要求8所述的玻璃模版法制备超疏水聚四氟乙烯薄膜的方法,其特征在于:步骤2)所述的干燥温度为100℃,时间为30-100分钟。
10.根据权利要求8或9所述的玻璃模版法制备超疏水聚四氟乙烯薄膜的方法,其特征在于:步骤3)所述的固化时间为20-40分钟。
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