CN109295419A - 一种制备具有树枝状结构的超疏水表面的方法 - Google Patents

一种制备具有树枝状结构的超疏水表面的方法 Download PDF

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CN109295419A
CN109295419A CN201811070934.7A CN201811070934A CN109295419A CN 109295419 A CN109295419 A CN 109295419A CN 201811070934 A CN201811070934 A CN 201811070934A CN 109295419 A CN109295419 A CN 109295419A
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metal film
solution
metal
photoresist layer
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王清
徐双双
王宁
郑旭
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Shandong University of Science and Technology
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Abstract

本发明公开了一种制备具有树枝状结构的超疏水表面的方法，包括以下步骤：S1,对基底的表面进行超声清洗、干燥；S2，在S1所得基底的表面真空蒸镀金属膜；S3,将S2所得基底浸入金属置换溶液，以使S2所得金属膜的外表面与所述金属置换溶液发生金属置换反应；S4,将S3所得产品取出、冲洗并干燥，即得。本发明通过真空蒸镀技术与置换反应相结合，使制得的超疏水表面粗糙度均匀，疏水性优良，与基底的粘附力更强，结构的机械稳定性更好，制备过程中不使用挥发性溶剂，不会对环境和人体造成污染和危害，绿色环保。

Description

一种制备具有树枝状结构的超疏水表面的方法
技术领域
本发明涉及疏水表面领域，具体涉及一种制备具有树枝状结构的超疏水表面的方法。
背景技术
超疏水的研究源于“荷叶效应”，一般来说，超疏水表面的接触角大于150°，滚动角小于10°。超疏水具有特殊的表面浸润性，因此，超疏水表面在油水分离、自清洁、防腐防污等领域具有极其广泛的应用。
材料表面的超疏水性不但受到材料表面能的影响，还受到表面粗糙程度的控制。目前制备超疏水表面的方法有很多，包括喷涂法、刻蚀法、模板法、等离子处理法、溶胶凝胶法等，其中最广泛的方法之一就是利用喷涂法对材料表面进行粗糙度处理。但是利用喷涂法制备的超疏水表面与基底粘结力差，疏水性不足，制备过程中使用的挥发性溶剂危害人体健康、污染环境，同时喷涂法也会使得材料大量浪费，造成经济损失。
以喷涂法处理玻璃基底为例，由于要求被喷涂的涂料的黏度比较小，因此喷涂的纳米颗粒与玻璃基底粘附力不足，造成制备的超疏水表面机械稳定性差；纳米颗粒的堆积难以实现大面积、高质量的控制，因此导致利用喷涂法制备的超疏水表面粗糙度不均匀，造成制备的超疏水表面疏水性不足；为了保证喷涂溶液能够有效喷涂，需要添加易挥发的涂料溶剂，既污染环境，不利于人体健康，又浪费涂料，造成经济损失。
发明内容
为克服现有技术存在的上述不足，本发明提供一种制备具有树枝状结构的超疏水表面的方法，由该方法制得的超疏水表面与基底的粘附力强，机械稳定性好，综合性能优越。本发明通过以下技术方案实现：一种制备具有树枝状结构的超疏水表面的方法，包括以下步骤：
S1,对基底的表面进行超声清洗、干燥；
S2，在S1所得基底的表面真空蒸镀金属膜；
S3,将S2所得基底浸入金属置换溶液，以使S2所得金属膜的外表面与所述金属置换溶液发生金属置换反应；
S4,将S3所得产品取出、冲洗并干燥，即得。
优选的，在S1中，所述基底为透光的玻璃或塑料；在S2中，包括以下分步骤：
S2a、在S1所得基底的单侧表面涂覆光刻胶层；
S2b、对S2a所述光刻胶层进行光刻、显影、冲洗干燥处理，以形成镂空的微纳结构的图案；
S2c、对S2b所得基底的光刻胶层侧真空蒸镀金属膜；
S2d、对S2c所得光刻胶层进行反向光刻，以及显影、冲洗、干燥处理，以去除光刻胶层，并得到镂空的微纳结构的金属膜。
优选的，在S2a中，将S1所得基底放在运胶机上，使用微量移液器将紫外光刻胶滴在所述基底的表面后，匀胶两次。
优选的，在S4中，S3所得产品还通过含有硬脂酸的溶液进行化学改性处理。
优选的，在S2中，所述金属膜为铜膜；在S3中，所述金属置换溶液为含有0.01mol/L硝酸银的溶液。
优选的，在S4中，化学改性所用溶液为含有0.01mol/L硬脂酸的乙醇溶液，改性时间为2h。
本发明通过真空蒸镀技术与置换反应相结合，使制得的超疏水表面粗糙度均匀，疏水性优良，与基底的粘附力更强，结构的机械稳定性更好，制备过程中不使用挥发性溶剂，不会对环境和人体造成污染和危害，绿色环保。
附图说明
下面结合附图和具体实施例对本发明作进一步详细说明。
图1为本发明实施例一的制备流程结构示意图；
图2为真空蒸镀膜设备示意图；
图3为本发明实施例二的制备流程结构示意图。
图中各标号对应如下，玻璃基底1，铜膜2，超疏水表面3，紫外光刻胶4，光源5，真空罩6，基片台7，蒸发舟8，铜靶材9。
具体实施方式
下面结合具体实施方式对本发明进行进一步的描述：
实施例1
如图1和图2所示，第一步，真空蒸镀铜膜
1、取一玻璃基底1(图1A)，尺寸为2cm×3cm，依次用丙酮、乙醇、去离子水超声清洗10min；
2、设置真空蒸镀设备的冷水循环装置；
3、打开真空罩6，将所要蒸镀的铜靶材9放入蒸发舟8，将玻璃基底1置于基片台7上并固定；
4、真空操作；
5、设置镀膜参数，开始镀膜操作；
6、镀膜完成后(图1B)，将蒸镀铜膜2后的玻璃基底1取出。
第二步，置换反应
1、配置浓度为0.01mol/L的硝酸银溶液；
2、将镀铜基底浸入到配置好的硝酸银溶液中反应10min，反应后缓慢取出，置于空气中自然干燥。
第三步，化学改性
1、配置浓度为0.01mol/L的硬脂酸的乙醇溶液；
2、将干燥后的玻璃基底1放入配置好的硬脂酸的乙醇溶液中改性2h，改性后，用乙醇冲洗，然后置于空气中自然干燥，即可制得具有树枝状结构的超疏水表面3(图1C)。
通过化学改性，降低了基底的表面能，使得基底具有更加优越的超疏水性能。
应当理解的是，本实施例的玻璃基底1也可以变化为塑料的方式实施。
实施例2
如图2和图3所示，第一步，紫外光刻
(1)根据需要，预先设计出将要光刻的图案；
(2)取一玻璃基底1(图3A)，具体尺寸为2cm×3cm，将其依次在丙酮、乙醇、去离子水中超声清洗并干燥；
(3)将清洗干净的玻璃基底1放在匀胶机上，使用微量移液器在玻璃基底1上滴入AZ5214E型紫外光刻胶4(正胶)，匀胶分两次，转速和时间分别设置为500rpm/min和10s以及4000rpm/min和30s；
(4)将匀胶完成后的玻璃基底1放在无掩膜光刻机上按照预先设计好的图案通过光源5进行光刻(图3B)；
(5)光刻完成后，立即放入显影液中进行显影40s，显影完成后用去离子水冲洗并干燥(图3C)；
第二步，真空蒸镀铜膜
1、设置真空蒸镀设备的冷水循环装置；
2、打开真空罩6，将所要蒸镀的铜靶材9放入蒸发舟8内，将玻璃基底1置于基片台7上并固定；
3、真空操作；
4、设置镀膜参数，开始镀膜操作；
5、镀膜完成后，将蒸镀铜膜2后的具有微米级结构的玻璃基底1取出(图3D)。
第三步，再次进行紫外光刻
1、将镀膜后的具有微米级结构的玻璃基底1重新放置在无掩膜光刻机上，玻璃基底1朝向上方，有微米级结构的一侧朝向下方，继续按照预先设计好的图案进行紫外光刻(图3E)；
2、光刻完成后，立即放入显影液中进行显影40s，显影完成后用去离子水冲洗并干燥(图3F)。
第四步，置换反应
1、配置浓度为0.01mol/L的硝酸银溶液；
2、将镀铜基底浸入到配置好的硝酸银溶液中反应10min，反应后缓慢取出，置于空气中自然干燥。
第五步，化学改性
1、配置浓度为0.01mol/L的硬脂酸的乙醇溶液；
2、将干燥后的基底放入配置好的硬脂酸的乙醇溶液中改性2h，改性后，用乙醇冲洗，然后置于空气中自然干燥，即可制得具有树枝状结构的超疏水表面3(图3G)。
本实施例通过两次光刻，可以有选择性地生成微纳结构，得到局部镀铜表面，可使制得的成品具有优越的疏水性能。
上述实施例利用真空镀膜技术在基底上蒸镀一层铜膜，由于蒸镀技术是通过加热蒸发铜靶材使铜靶材凝固并沉积在基底表面，铜膜厚度均匀可控，因此使得蒸镀完成后的铜膜与基底粘附力强；然后，将蒸镀上一层铜膜的基底与硝酸银溶液进行置换反应，置换反应后得到具有树枝状结构的超疏水表面，其树枝状结构使得其与镀铜基底的粘附性也很强，表面粗糙度也很均匀，因此，大大提高了超疏水表面的机械稳定性和疏水均一性；通过硬脂酸的乙醇溶液对基底进行化学改性，在树枝状结构表面自组装形成了一层硬脂酸膜，进一步降低了基底的表面能，使得基底具有更加优越的超疏水性能。在制备过程中，不使用易挥发的有害溶剂，对人和环境不会造成危害和污染。
应当理解的是，对本领域普通技术人员来说，可以根据上述说明加以改进或变换，而所有这些改进和变换都应属于本发明所附权利要求的保护范围。
上面对本发明专利进行了示例性的描述，显然本发明专利的实现并不受上述方式的限制，只要采用了本发明专利的方法构思和技术方案进行的各种改进，或未经改进将本发明专利的构思和技术方案直接应用于其它场合的，均在本发明的保护范围内。

Claims (6)

1.一种制备具有树枝状结构的超疏水表面的方法，其特征在于，包括以下步骤：
S1,对基底的表面进行超声清洗、干燥；
S2，在S1所得基底的表面真空蒸镀金属膜；
S3,将S2所得基底浸入金属置换溶液，以使S2所得金属膜的外表面与所述金属置换溶液发生金属置换反应；
S4,将S3所得产品取出、冲洗并干燥，即得。
2.根据权利要求1所述的方法，其特征在于，在S1中，所述基底为透光的玻璃或塑料；在S2中，包括以下分步骤：
S2a、在S1所得基底的单侧表面涂覆光刻胶层；
S2b、对S2a所述光刻胶层进行光刻、显影、冲洗干燥处理，以形成镂空的微纳结构的图案；
S2c、对S2b所得基底的光刻胶层侧真空蒸镀金属膜；
S2d、对S2c所得光刻胶层进行反向光刻，以及显影、冲洗、干燥处理，以去除光刻胶层，并得到镂空的微纳结构的金属膜。
3.根据权利要求2所述的方法，其特征在于，在S2a中，将S1所得基底放在运胶机上，使用微量移液器将紫外光刻胶滴在所述基底的表面后，匀胶两次。
4.根据权利要求1所述的方法，其特征在于，在S4中，S3所得产品还通过含有硬脂酸的溶液进行化学改性处理。
5.根据权利要求1所述的方法，其特征在于，在S2中，所述金属膜为铜膜；在S3中，所述金属置换溶液为含有0.01mol/L硝酸银的溶液。
6.根据权利要求4所述的方法，其特征在于，在S4中，化学改性所用溶液为含有0.01mol/L硬脂酸的乙醇溶液，改性时间为2h。
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