CN111468372A - 一种超浸润硅油型液体灌注表面的制备方法 - Google Patents
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Abstract
本发明公开了一种超浸润硅油型液体灌注表面的制备方法，是将坡缕石粉末与十八烷基三甲氧基硅烷分散在乙醇中形成混合液，再加入磷酸铝粘结剂水溶液，然后于20~30℃搅拌10~20 min，得到均匀的悬浮液；利用喷涂法将上述悬浮液喷涂在镁片表面，于110~120℃下加热1.5~2.0 h，使涂层完全交联和固化得到APT‑OTMS‑AP涂层；将硅油滴加到超疏水性的APT‑OTMS‑AP涂层表面，静置得到超浸润硅油型液体灌注表面。该液体灌注表面制备过程简单、原料廉价且环保，并具有极强的疏水性、优异的耐磨性和抗冲击性，即使在通过砂纸打磨以及砂石冲击后仍然保持较高水平的疏水性。此外，该液体灌注表面还具有良好的防腐蚀性能。
Description
技术领域
本发明属于涂层技术领域，涉及一种超浸润硅油型液体灌注表面的制备方法。
背景技术
随着自然的演化，生物体形成了具有复杂的功能性特殊结构、图案或纹理。受猪笼草的启发，2011年Aizenberg首次提出了一种合成的液体注入的多孔表面，并证实它不同于莲花效应。由于润滑油的注入，超疏水表面的气体阻挡层被液体阻挡层所取代。气体阻挡层不能像液体注入的多孔表面中的润滑层那样有效地承受恶劣的外部环境。因此，与具有亚稳态的超疏水表面相比，液体注入技术获得的光滑液体注入多孔表面更稳定。此外，与超疏水表面相比，液体注入的光滑多孔表面表现出更优越的液体排斥、防结冰、防污、防腐蚀、压力稳定性和自愈合性能。
近年来，人们开发了各种性能的液体注入型多孔材料。例如，李等人成功制备了一种金属多孔结构，通过进一步的修饰和灌注，获得了光滑的液体注入多孔表面，表现出良好的耐腐蚀和自愈合性能。陈等人利用聚酰胺6与硅油结合，采用飞秒激光直写法制备了光滑的液体注入多孔表面，具有稳定的液体排斥性和自愈性。
但是，这些光滑的注液多孔表面总是从具有粗糙多孔结构的表面建立的，这意味着它们不可避免地面临着超疏水表面的脆弱性。因此，仍然有必要寻找有效且稳定的粘合剂以增强机械强度。另外，这些表面的制造过程麻烦并且受到基板的限制，并且不可避免地涉及利用含氟材料，该材料昂贵并且对人体健康和环境有害。而坡缕石（APT）与过去报道的人工制造的多孔结构不同，它是一种天然的多孔无机矿物。因此，使用APT直接建立多孔表面并进行液体注入是一条非常方便和有效的途径。此外，由于APT表面的反应性羟基，很容易用粘合剂形成稳定和坚固的结构，并且APT的低成本和高可用性也提高了实际工程应用的潜力。
发明内容
本发明的目的是提供一种超浸润硅油型液体灌注表面的制备方法。
一、硅油型液体灌注表面的制备及表征
本发明硅油型液体灌注表面的制备方法，包括以下工艺步骤：
（1）将坡缕石粉末与十八烷基三甲氧基硅烷（OTMS）分散在乙醇中形成混合液，再加入磷酸铝（AP）粘结剂水溶液，然后于20~30℃搅拌10~20 min，得到均匀的悬浮液；
（2）利用喷涂法将上述悬浮液喷涂在镁片表面，于110~120℃下加热1.5~2.0 h，使涂层完全交联和固化得到APT-OTMS-AP涂层；
（3）将硅油滴加到超疏水性的APT-OTMS-AP涂层表面，静置得到超浸润硅油型液体灌注表面。
所述坡缕石粉末与十八烷基三甲氧基硅烷的质量比为2:1~3:1。
所述磷酸铝粘结剂与坡缕石粉末的质量比为3.7:1~4.3:1。
所述静置时间为0.5~1.0 h。
图1为原始镁片（a）和本发明制备的APT-OTMS-AP涂层表面不同放大倍数（b、c）下的SEM图。由图b可以看出，镁片已经被APT-OTMS-AP完全覆盖，形成了具有微纳米级的分层粗糙结构。由图c可以观察到APT-OTMS-AP涂层表面具有许多特殊的花状微观结构，而这些花状微观结构是由AP粘结剂和大量的纳米级坡缕石棒构成。
图2为APT和APT-OTMS-AP涂层表面的红外光谱图（a），APT-OTMS-AP涂层表面的EDS分析图（b）。由图a可以看出，对APT粉末和APT-OTMS-AP涂层表面的红外光谱进行分析，APT-OTMS-AP涂层表面的红外光谱出现了OTMS的特征衍射峰，这说明APT粉末成功地被OTMS修饰。由图b可以看出，APT-OTMS-AP涂层表面所含元素（C、O、Al、P和Si）分布在涂层表面，这说明APT-OTMS-AP已经成功地覆盖在镁片上。从图3可以看出，APT表现出类似于Brunauer等人描述的IV型吸附和解吸等温线，其中在相对压力下吸收体积的增加表示介孔特征。定量得到的结构参数表明，ATP的孔径达到3.678 nm，BET表面积大，为370.12 m2/g，这有利于其对润滑剂的吸附。
二、硅油型液体灌注表面的特殊浸润性能
1、浸润性测试
对水和不同液滴的接触角和滚动角测试：将APT-OTMS-AP涂层表面和硅油型液体灌注表面水平放在接触角测量仪器上。分别取4μL油和不同液体进行测量。
测试结果：图4a为不同液滴在制备的APT-OTMS-AP涂层表面的浸润性，接触角均大于150°，而滚动角小于10°。由图4a可见，APT-OTMS-AP涂层表面在空气中具有优异的超疏水性。然而，APT-OTMS-AP涂层表面不能有效地排斥某些复杂的混合物或有机液体，甚至这些液体也可能粘附在APT-OTMS-AP涂层的表面，如牛奶，乙二醇等。在用硅油进行灌注后，所制备的表面对水滴呈现出106°的接触角和5°的滑动角。如图4b所示，相对APT-OTMS-AP涂层表面来说，不同液体在硅油型液体灌注表面的接触角有所降低，而滑动角基本不变。但对于一些复杂的混合物或有机液体在硅油型液体灌注表面上仍具有较低的滑动角，这表明硅油型液体灌注表面具有优异的液体排斥性和普遍性，而这也是APT-OTMS-AP涂层表面所不具有的。
2、机械稳定性测试
测试方法：利用SiC砂纸（800目）和不同质量砂子（20~120 g）对硅油型液体灌注基底的APT-OTMS-AP涂层表面进行了磨损试验，并对不同磨损次数后的接触角进行了测定。
测试结果：APT-OTMS-AP涂层表面在800目SiC砂纸上连续磨损100个循环（图5a），表现出优异的机械性能，并保持大于150°的接触角（图5b）。这种优异的机械性能归因于AP粘结剂的官能团与APT表面上的氧（镁）原子之间的氢（配位）键。同时，图5c为抗冲击性的测试过程，在测试过程中漏斗内20~120 g的砂子从20 cm高落下并撞击APT-OTMS-AP涂层表面。试验结果如图5d所示，在经受不同重量砂子的冲击后，APT-OTMS-AP涂层表面仍保持超疏水性，接触角仍然保持在150°以上。这种现象进一步表明APT-OTMS-AP涂层具有优异的机械稳定性，同时它还为硅油型液体灌注表面的制备提供了稳定的基础，并赋予硅油型液体灌注表面优异的机械性能。
3、防腐蚀性能测试
测试方法：通过电化学工作站在3.5 wt % NaCl溶液中将镁片、APT-OTMS-AP涂层和硅油型液体灌注表面浸泡2小时。
测试结果：图6为镁片、APT-OTMS-AP涂层和硅油型液体灌注表面的极化曲线。由图6可见，与原始镁片相比，浸泡在3.5 wt % NaCl溶液中2小时的硅油型液体灌注表面和APT-OTMS-AP涂层表面的腐蚀电流密度明显降低了2个数量级和1个数量级，这表明硅油型液体灌注表面相对于APT-OTMS-AP涂层具有更优异的防腐蚀性能。同时，硅油型液体灌注表面的腐蚀电位比镁片和APT-OTMS-AP涂层的更大，进一步表明硅油型液体灌注表面具有更好的耐腐蚀性。因此，从腐蚀电流密度和腐蚀电位的比较可以看出，硅油型液体灌注表面涂层对于提高镁片的耐腐蚀性是最有效的。
综上所述，本发明利用表面富含大量羟基的坡缕石为原料，通过十八烷基三甲氧基硅烷修饰，并结合磷酸铝粘结剂成功制备出具有一定机械耐久性的超疏水液体灌注表面。该液体灌注表面制备过程简单、原料廉价且环保，并表现出极强的疏水性以及较好的耐久性，即使在通过砂纸打磨以及砂石冲击后仍然保持较高水平的疏水性。此外，该液体灌注表面还具有良好的防腐蚀性能。
附图说明
图1分别为原始镁片（a）和本发明制备的APT-OTMS-AP涂层表面不同放大倍数（b、c）下的SEM图。
图2为APT和本发明制备的APT-OTMS-AP涂层表面的红外光谱图（a），APT-OTMS-AP涂层表面的EDS分析图（b）。
图3为APT的吸附和解吸等温线。
图4为本发明制备的APT-OTMS-AP涂层表面（a）和硅油型液体灌注表面（b）的浸润性测试图及接触角和滚动角柱状图。
图5为本发明制备的APT-OTMS-AP涂层的砂纸摩擦测试的示意图（a）和砂纸摩擦试验对它的接触角的影响（b）；砂流冲击试验的示意图（c）和砂流冲击循环对APT-OTMS-AP涂层接触角的影响（d）。
图6为镁片、APT-OTMS-AP涂层和硅油型液体灌注表面的极化曲线。
具体实施方式
下述通过具体实施例对本发明硅油型液体灌注表面的具体制备方法及性能作进一步说明。
实施例1、超浸润硅油型液体灌注表面的制备
（1）悬浮液的制备：在室温下，先将1g坡缕石粉末与0.44 g十八烷基三甲氧基硅烷分散在15 mL乙醇中形成混合液，再加入20mL浓度为0.35~0.45 g/mL的磷酸铝粘结剂水溶液，然后于20~30℃搅拌10~20 min，得到均匀的悬浮液；
（2）APT-OTMS-AP涂层表面的制备：用喷枪将所制备的悬浮液均匀喷涂在已预处理的镁片上；再将所得的镁片放置在干燥箱中，在110~120℃下加热1.5~2.0 h，使涂层完全交联和固化来获得具有超疏水APT-OTMS-AP涂层；
（3）硅油型液体灌注表面的制备：将硅油滴加到所制备的超疏水性APT-OTMS-AP涂层表面，使硅油进入微纳米级分层多孔结构中以得到液体灌注表面。再静置1h，硅油完全注入后，将样品垂直放置来除去过量的硅油，从而得到液体灌注表面。
实施例2、浸润性测试
将实施例1制备的APT-OTMS-AP涂层表面和硅油型液体灌注表面水平放在接触角测量仪器上，分别取4 μL油和不同液体进行测量。APT-OTMS-AP涂层表面的接触角均大于150°，而滚动角小于10°，不同液体在硅油型液体灌注表面的接触角有所降低，而滑动角基本不变，对于一些复杂的混合物或有机液体（如牛奶、乙二醇）在硅油型液体灌注表面上仍具有较低的滚动角，这表明硅油型液体灌注表面具有优异的液体排斥性和普遍性（见图4）。
实施例3、机械性能测试
将实施例1制备的APT-OTMS-AP涂层水平放置在800目SiC砂纸表面，并将500g砝码放置在样品上方，然后用镊子来回拖动。然后将进行过不同循环次数磨损测试的APT-OTMS-AP涂层进行接触角测定。随着循环磨损100次以后，其接触角依然大于150°。将APT-OTMS-AP涂层倾斜放置，从20 cm高处将漏斗内20~120 g的砂子落下并撞击APT-OTMS-AP涂层表面。在经受不同重量砂子的冲击后，APT-OTMS-AP涂层表面仍保持超疏水性，接触角仍然保持在150°以上（见图5）。
实施例4、防腐蚀性能测试
通过电化学工作站在3.5 wt % NaCl溶液中将实施例1制备镁片、APT-OTMS-AP涂层和硅油型液体灌注表面浸泡2小时，然后测试极化曲线。从腐蚀电流密度和腐蚀电位的比较可以看出，硅油型液体灌注表面涂层对于提高镁板的耐腐蚀性是最有效的（见图6）。
Claims (4)
1.一种超浸润硅油型液体灌注表面的制备方法，包括以下工艺步骤：
（1）将坡缕石粉末与十八烷基三甲氧基硅烷分散在乙醇中形成混合液，再加入磷酸铝粘结剂水溶液，然后于20~30℃搅拌10~20 min，得到均匀的悬浮液；
（2）利用喷涂法将上述悬浮液喷涂在镁片表面，于110~120℃下加热1.5~2.0 h，使涂层完全交联和固化得到APT-OTMS-AP涂层；
（3）将硅油滴加到超疏水性的APT-OTMS-AP涂层表面，静置得到超浸润硅油型液体灌注表面。
2.如权利要求1所述超浸润硅油型液体灌注表面的制备方法，其特征在于：所述坡缕石粉末与十八烷基三甲氧基硅烷的质量比为2:1~3:1。
3.如权利要求1所述超浸润硅油型液体灌注表面的制备方法，其特征在于：所述磷酸铝粘结剂与坡缕石粉末的质量比为3.7:1~4.3:1。
4.如权利要求1所述超浸润硅油型液体灌注表面的制备方法，其特征在于：所述静置时间为0.5~1.0 h。
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