Paint & Coatings Industry >

2018 , Vol. 48 >Issue 11: 79 - 87

DOI: https://doi.org/10.12020/j.issn.0253-4312.2018.11.79

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Research Progress in Self-Healing Superhydrophobic Multifunctional Synergistic Coatings

  • Yanfang Qiao ,
  • Liqiang Wang * ,
  • Xiaowei Liu
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  • Advanced equipment manufacturing technology laboratory of Jiangsu Province,Department of Packaging Engineering, Jiangnan University, Wuxi,Jiangsu 214122,China

Received date: 2018-09-19

  Online published: 2018-12-19

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Copyright reserved © 2018
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Abstract

Self-healing superhydrophobic coatings can extend the service life of coatings, which is one of the hottest research topics in recent years. The mechanism of superhydrophobic self-healing coatings is summarized, including the restoration of surface morphology and the supplement of low surface energy components. The recovery of surface topography can be achieved through dynamic chemical bonding and gas compensation. The supplement of low surface energy components relies on the surface energy to drive the underlying low surface energy components to migrate to the surface of the coating under stimulus conditions. At present, there are new research directions such as the use of shape memory alloys for self-healing large-scale surface structures, reducing dependence on external stimuli to achieve autonomous self-healing processes, self-repairing with molecular structures, and self-healing multi-layer slippery liquid infused porous surface (SLIPS) design. The synergic effect of the multiple functions is introduced, which promotes the overall performance of the coating to be optimal. The synergic effect of superhydrophobic self-healing multifunctional fiber, superhydrophobic anticorrosive self-healing coating and superhydrophobic conductive self-healing coating are introduced. This provides new ideas for the design of multifunctional coatings. Finally, the prospects of the self-healing superhydrophobic coatings are put forward.

Key words： self-healing; restoring surface morphology; immigration of low surface energy components; superhydrophobic; multifunctional; synergic effect

Cite this article

Yanfang Qiao , Liqiang Wang , Xiaowei Liu . Research Progress in Self-Healing Superhydrophobic Multifunctional Synergistic Coatings[J]. Paint & Coatings Industry, 2018 , 48(11) : 79 -87 . DOI: 10.12020/j.issn.0253-4312.2018.11.79

受荷叶启发,人们将像水滴在荷叶表面成球形不能润湿铺展开的表面称为超疏水表面,即水的静态接触角CA>150°,滑动角SA<10°[1]。超疏水涂层可广泛应用于防污[2,3,4]、自清洁[5,6]、油水分离[7,8,9]等方面。但在实际使用过程中,涂层表面易受到机械、化学破坏,使得疏水性能下降。通过研究自然界的非润湿性植物(如荷叶),研究人员发现受损植物可以通过再生表面蜡层来恢复其超疏水性,其被定义为自修复功能[10]。人们希望获得像荷叶一样可以在表面遭受破坏后分泌低表面能物质实现自修复,得到一种动态、稳定的智能涂层。自修复超疏水性能可在涂层被破坏后实现超疏水性能的恢复从而延长涂层的使用寿命[11,12]。
自修复超疏水涂层研究引起了研究者的广泛关注并取得了一定成果。Golovin等[13]对超疏水自修复提出了粘合剂和填充物之间的混溶参数S*和表面的超疏水势P* 2个评估设计指标。目前制备的超疏水涂层可在机械冲击、磨损[14,15]、等离子处理[16,17]等破坏后实现较好的超疏水性能自修复。但仍存在着如何修复大尺度结构损伤、优化修复次数及条件、简化制备工艺、配方更环保等方面的挑战。
随着基材应用环境的复杂,单一功能的涂层往往不能很好的满足实际应用。于是人们开始赋予涂层更多功能,多功能涂层应用越来越广泛,如超疏水防腐涂层[18]、超疏水抑菌涂层[19,20]、超疏水导电涂层[21]等。多功能涂层的多个功能之间不是简单的功能叠加,而应该相互配合相互协同,使得涂层整体性能达到最优效果。多功能涂层设计时可考虑各功能间协同作用,从上而下对涂层进行设计。

1 自修复超疏水涂层修复原理

当实现超疏水的2个条件:表面结构和低表面能物质其中一个遭受破坏时,涂层的疏水性能会下降[22,23,24,25,26]。恰当的表面形貌可将更多的空气截留在水滴底部减小固液接触面积,从而提高接触角,降低滑动角[27];低表面能物质可以有效降低涂层的表面能[28]。但在实际使用过程中疏水涂层的表面易受到机械磨损、化学腐蚀、紫外线辐射等,使得表面结构破坏、低表面能物质丧失,导致涂层的疏水性能下降[29,30]。据此对超疏水性能的自修复可从恢复被破坏的表面形貌和补充低表面能物质两方面进行。

1.1 表面形貌的修复

恰当的表面形貌即合适的粗糙度是实现超疏水表面的一个必要条件,通常疏水表面形貌由微米/纳米粒子构成,形成分级结构[31,32]。涂层在使用过程中易受到机械磨损、划切等,使得原有表面形貌改变导致疏水性能下降。如何实现表面形貌的恢复是自修复的一个研究难点,尤其是减少对外界刺激的依赖实现自主修复以及修复大尺度结构损伤。
1.1.1 物质的变形
基材进行内部自我修复可通过不同种类动态共价键和非共价键作用来实现,如Dies-Alder反应[33,34]、二硫键动态交换[35,36]、主客体相互作用[37,38]、金属配位作用[39,40]等。基材自修复能力在宏观上表现为:当涂层的表面形貌破坏后,在一定刺激下(温度、湿度等),可通过变形、溶胀、流动来恢复原有形貌,实现超疏水性能的自修复。
形状记忆聚合物(shape memory polymer,SMP)是能够在特定的刺激条件下(如热、光等),从临时形状自发恢复到永久形状的一种刺激响应性材料[41]。这种材料特性为实现疏水涂层表面形貌被破坏后的恢复提供了设计思路。Qian等[42]采用环氧基形状记忆聚合物在钢条上制备了可通过加热实现超疏水性能自修复的涂层。修复的机制是当加热后温度高于环氧基聚合物的玻璃化温度,分子链被“激活”,在内应力的驱使下环氧基形状记忆聚合物恢复到初始形状[43]。
如何不依靠外界刺激实现涂层形貌的自主修复,使得涂层更加智能是新的研究方向。Das等[44]利用形状记忆聚合物与改性氨基氧化石墨烯以共价键结合得到了具有自修复性能的超疏水涂层。在对涂层施加压力后表面形貌改变,超疏水性能下降;当外界压力撤去后,无需外界刺激,涂层可自行恢复原有表面形貌。该设计提供了生物弹性界面,通过压力使得涂层在亲水表面和疏水表面间转换。涂层的自修复程度与时间成线性增长关系:在施加188 kPa的压力下涂层表面形貌被压平,撤去压力24 h后形貌恢复至72%。涂层表面形貌受压力破坏后无需外界刺激可进行自主修复,但所需自修复时间较长。
具有遇水溶胀特性的材料也可用来实现表面形貌的自修复,该自修复进程所需的外界刺激条件简单易实现。白宁宁[45]通过喷涂法制备了聚甲基丙烯酸甲酯(PMMA)/硬脂酸锌(ZNO)/硬脂酸(STA)自修复超疏水复合涂层。当涂层经受雨水冲刷后,表面形貌被压平,将其浸泡在水中超疏水性得到恢复。修复机制是PMMA在水中溶胀恢复了被雨水冲刷而压平的粗糙表面,这种破坏-自修复循环最少可进行4次。但未进行机械磨损实验,若具有自修复性能的PMMA被磨损,自修复性能会随之下降。
可修复大尺度结构损伤使超疏水涂层更好地应用于实际中是自修复涂层研究的难点。武梦春[46]通过制备聚己内酯(PCL)/聚乙烯醇(PVA)膜,该复合膜具有热修复性能,再将导电的银纳米线与膜结合,并沉积一层银纳米粒子和1H,1H,2H,2H-全氟癸硫醇(PFDT)得到具有自修复能力的超疏水膜。涂层表面的银纳米线(AgNWs)和银纳米粒子(AgNPs)提供了合适的粗糙度。位于底层的PCL/PVA膜作为结构层提供了热修复能力。该膜的自修复机制如图1所示。当涂层表面受到机械划痕损伤后,向涂层施加低电压,表层导电银纳米线和粒子将电能转化为热能,热量传导至底层。当温度高于PCL/PVA膜的熔点,膜开始熔融,向切口处流动使得伤口全部愈合或者变小。但其制备工艺较为复杂,先在基材上涂覆热修复层(PCL/PVA复合膜),再滴涂银纳米线溶液(提供导电性),最后沉积具有超疏水性的功能层(银纳米粒子和PFDT)。该涂层虽然对大规模的机械划痕造成的结构损伤具有很好的自修复功能,但是对于机械磨损造成的损伤未进行进一步研究。
图1 PFDT/AgNPs-AgNWs/PCL/PVA膜自修复示意图

Fig.1 Schematic illustration of restoring superhydrophobicity of the PFDT/AgNPs-AgNWs/PCL/PVA film

通过材料的变形一般可实现表面形貌因压平、划切造成损伤的自修复。这类破坏未减少涂层的表面物质,然而当涂层经受机械磨损后,通过材料的变形则不能实现形貌的恢复。这时需要表面结构的再生来维持涂层的原有形貌,恢复超疏水性能。
1.1.2 物质的再生
构造表面形貌是为了通过具有一定粗糙度的表面将更多的空气保存在表面凹处,使得液滴从Wenzel状态转换到非润湿的Cassie-Baster状态[47,48]。涂层表面的气体补偿也是实现超疏水性能自修复的一种方式。Cheek等[49]通过导电超疏水表面的电解反应得到氢气进行气体补偿,对超疏水表面实行自修复。Liu等[50]制备了具有SiO2包覆Na2CO3的多孔核壳结构的超疏水自修复涂层。Na2CO3在酸性条件下会产生CO2气体,对涂层表面进行气体补偿,防止水滴浸润涂层表面。这种方法实现的自修复稳定性较差,可与其他超疏水自修复方法结合,作为超疏水性能自修复的一种辅助增强手段。

1.2 低表面能物质的修复

水在材料表面的润湿性受材料表面能的影响,表面能越低,润湿性越差,疏水性越好[51,52]。当涂层表面低表面能物质受机械磨损减少或化学试剂降解后,疏水性能下降。低表面能物质的补充通常是将其储存在基材中,然后通过外界刺激将低表面能物质迁移到表层[13,20]。
1.2.1 低表面能物质的迁移
低表面能物质迁移的原因是当涂层表层的低表面能物质丧失后,为了维持界面表面能最低即在自由能的驱使下,低表面能物质会向涂层表面迁移以降低表面能[53,54]。
Tu等[55]通过将TiO2与水性全氟烷基甲基丙烯酸共聚物(PMC)乳液混合喷涂至乙烯基封端聚二甲基硅氧烷(PDMS)预处理的木材上,得到在紫外线照射下能够自修复的超疏水涂层。如图2所示,自修复机理为当表层低表面能物质在紫外照射降解后通过加热使得PDMS迁移到涂层表面再形成一层新的低表面能物质以维持超疏水性。该涂层的制备采用了水性PMC,污染小,但采用的全氟化合物难降解,对动植物有一定毒性[56]。自修复超疏水涂层配方的环保性是研究的一个重难点。
图2 PMC/TiO2/PDMS超疏水膜自修复机理

Fig.2 Self-healing mechanism of the PMC/TiO2/PDMS superhydrophobic film

利用分子结构框架实现超疏水及自修复性能是研究的新趋势[57]。Qiang等[58]利用三官能度乙烯基全氟癸醇(PFDO)、乙烯基封端聚二甲基硅氧烷(PDMS)和八乙烯基多面体低聚倍半硅氧烷(POSS)组成的溶液,采用浸渍的方法制得自修复超疏水纤维。如图3所示,该浸渍液中PFDO作为低表面能物质,PDMS可提供一定的粗糙度,POSS分子具有多面体笼型结构,PFDO、PDMS可通过自由基结合在POSS的8个顶点上形成PFDO-PDMS结构分子。当纤维受磨损后表面的PFDO、PDMS减少,疏水性能下降;在加热后,PFDO-PMDS的分子迁移到涂层表面,同时降低了表面自由能,恢复了表面粗糙度,形成超疏水性能的自修复。
图3 涂层分子结构及修复原理示意图

Fig.3 Schematic diagram of the molecular structure of coating and self-healing mechanism

目前对机械磨损造成的表面形貌破坏实现自修复的研究较少,为了降低设计难度和成本,可通过提高表面形貌对机械磨损的抵抗能力,只针对低表面能物质的补充进行自修复。有机硅机械强度高、耐磨性好,具有良好的热稳定性[59]。将含氟化合物与有机硅结合起来得到的氟硅化合物具有良好的疏水性和耐高低温性能[60]。Zhang等[61]利用溶胶-凝胶法加上纳米颗粒制得了耐磨自修复超疏水涂层。该涂层利用支链硫醇-烯基氟烷基硅烷(T-FAS)作为粘合剂将纳米颗粒与基材牢固结合。涂层在经受砂纸打磨、划切等机械破坏后表面形貌基本不变,通过加热将底层的氟化链迁移到表面实现超疏水性能的自修复。
1.2.2 润滑液流动
Wong等[62]模仿猪笼草表面结构,首次提出具有自修复性能的光滑浸渍多孔表面SLIPS(slippery liquid infused porous surfaces),该设计通过在多孔基材表面浸渍一层润滑液使其具有自修复超疏水性能。基材经受机械磨损后,润滑液在表面能驱动的毛细管作用下填充被破坏的间隙实现超疏水性能的自修复。如图4(a)所示,环氧树脂基材的SLIPS在经受50 mm长的机械划伤后,在150 ms内可实现自修复。图4(b)为涂层表面所受累积损伤与接触角滞后散点图。检测液为癸烷[表面能(23.6±0.1)mN/m,约5 μL],图中误差线表示至少3次独立测量的标准偏差。涂层表面在补充润滑液后(红色箭头所示),当经受累积破坏面积(受损面积/全部面积)达到20%时仍然具有很好的超疏水能力。SLIPS在受到小面积机械损伤时,可通过润滑液的流动实现自主修复;当受损面积较大时,可通过补充润滑液恢复超疏水性能。
图4 SLIPS对物理损伤自修复能力检测结果

Fig.4 Self-healing ability test result of SLIPS on physical damage

在SLIPS设计中,润滑液起着十分重要的作用,当多孔基材浸渍的润滑液蒸发或者由于机械破坏而丧失时会使得超疏水性能下降。如何使润滑液稳定地维持在多孔基材内受到研究者的关注。Tenjimbayashi等[63]针对SLIPS中润滑液易因蒸发、机械损伤等因素而消耗,设计了润滑剂夹层的三层表面LIMITS(lubricant-inserted microporous triple-layered surface),该团队采用相分离技术将润滑剂夹在两层亲油多孔基材中,使其通过不断分泌来实现自修复。该方法为先在铁基材上结合聚偏二氟乙烯六氟丙烯共聚物(PVDF-HFP)得到超亲油多孔表面SPS (self-standing porous surface),再将其浸润在润滑剂中得到润滑液浸润的光滑表面LIS(lubricant-infused surface),最后再将一层SPS覆盖在LIS得到LIMITS。如图5所示,相比于传统的LIS,LIMITS降低了润滑剂因蒸发而损耗的可能性,同时润滑剂储存在多孔的亲油层SPS中,可通过自分泌来补充表面润滑剂,这种多层设计可更加长久地维持超疏水性能。但是该方法所采用的工艺步骤较多,同时需要两层多孔表面,增加了涂层厚度。
图5 传统润滑剂浸渍表面和润滑剂夹层的三层表面对比

Fig.5 Comparison of conventional LIS and LIMITS

对于从补充低表面能物质和修复机械受损基材这2个方面进行的超疏水涂层的自修复,可以使得涂层的超疏水性能更加稳定,延长涂层的使用寿命。自修复超疏水涂层的设计有时会将溶胶-凝胶法、SLIPS设计、仿生荷叶设计、记忆合金等多种设计思路和方法结合起来,以获得更稳定的超疏水自修复涂层[64,65,66,67]。但由于配方的环保性、价格以及工艺步骤等问题,自修复超疏水涂层大规模生产应用较少。

2 多功能协同作用涂层的应用

为了使涂层在实际应用中能达到更好的效果,越来越多的涂层不再仅具有单一功能,多功能涂层受到越来越广泛的关注。并且多个功能不是简单的叠加,而是达到1+1>2的协同作用。涂层的自修复超疏水性能可以和其他性能如抑菌性、防腐蚀性、导电性等协同作用,从而提高涂层的各方面性能。

2.1 超疏水自修复多功能纤维

疏水性能在纤维纺织领域有着重要的应用,其可为纤维提供油水分离[68,69]、自清洁[70,71]等性能。为满足不同应用场合的需求,纤维可能还要具有抗菌、着色牢固等性能。武梦春[46]通过浸蘸的方法设计了着色牢固抗菌超疏水自修复纤维。该研究中利用不同颜色的纳米银粒子对纤维进行染色,同时银粒子提供了抗菌性能。但纳米银粒子与纤维的结合强度低,通过表面修饰F-POSS分子再将纳米银粒子与疏水涂层结合,既可提高银粒子与纤维的结合强度,又可使得纤维获得超疏水自修复性能。该设计的自修复机理为:当纤维表面受磨损后,表层的低表面能物质分解,底层的F-POSS通过湿度诱导在表面能的驱动下迁移到表层实现超疏水性能的恢复。实验表明,纤维可经受16个“O2等离子处理-自修复循环周期”后依然能保持其超疏水性能。但随着O2等离子处理的次数增加所需的自修复时间增长,这是由于基材底层可迁移的F-POSS随着自修复次数的增加而逐渐减少。
该设计中引入的F-POSS一方面提高了涂层中Ag粒子与纤维的结合强度,另一方面也引入了自修复性能。从整体上提高了涂层的抗菌性能、色牢度、疏水性能。

2.2 超疏水防腐蚀自修复涂层

水是参与金属腐蚀的一个重要因素,若能避免金属与水的直接接触可以减缓腐蚀进程。越来越多的研究者将实现自修复超疏水涂层作为得到可靠耐久防腐蚀涂层的一个突破口。
Qian等[42]研究了基于腐蚀缓蚀剂BAT和环氧基形状记忆合金聚合物(SMP)双重作用的超疏水防腐蚀自修复涂层。考虑实际应用中会存在基材受损后在SMP自修复进程被触发前却已暴露在腐蚀性环境中的情况。在这种情况下,基材中包埋的BAT腐蚀缓蚀剂可以有效地吸附在暴露的基材表面形成一层阻隔膜,抑制腐蚀进程。同时,受损基材间隙中存在的腐蚀产物会影响SMP的形状恢复。将受划切损伤的基材在质量分数3.5%NaCl溶液中浸泡不同时长,然后在60 ℃下加热20 min,观察切口间隙的愈合和耐腐蚀情况。实验表明,不含BAT的受损基材在NaCl溶液中浸泡3 d后不能热修复,其耐腐蚀性也明显下降;含5%BAT的受损基材在NaCl溶液中浸泡5 d后仍能热修复,其耐腐蚀性无明显下降,但浸泡7 d后受损基材不能进行热修复,耐腐蚀性也明显下降。这是由于BAT能有效抑制腐蚀,减少腐蚀产物的生成,有利于SMP的热修复。
该研究中BAT与SMP协同作用,BAT抑制腐蚀产物的生成有利于SMP实现自愈合;SMP的自愈合性能降低了基材暴露在环境中的概率,两者相互促进从整体上提高了涂层的防腐蚀性能。

2.3 超疏水导电自修复涂层

涂层是广泛使用的改善材料表面性能的一种方法,但基底聚集的电子会导致涂层脱落[72]。导电涂层由于能有效去除聚集的电子而受到广泛关注[73,74]。将导电性和超疏水性结合起来获得多功能涂层可应用于电子产品包装[75]、生物传感器[76]等方面。
Chen等[21]通过将光催化TiO2纳米粒子、石墨粒子、氟化聚硅氧烷和甲基三(甲基乙基酮肟)硅烷共混配制成溶液喷涂到基材上得到超疏水导电自修复涂层。该设计中TiO2纳米粒子和石墨粒子不仅提供了超疏水表面所需的粗糙度,也赋予了涂层导电性和光催化性。同时涂层中TiO2和石墨粒子构成的表面由于自相似结构仍然保持着分级结构,在表面磨损后仍能较好地保持原有的表面微观结构[77]。所以只需通过底层氟化物在表面能的驱动下迁移补充表面磨损消耗的低表面能物质便可实现超疏水性的自修复。实验表明,该涂层可经受6次10 kPa的机械磨损-修复循环。TiO2和石墨粒子的引入使得涂层具有牢固的表面微观结构,降低了实现超疏水性自修复的难度;同时也使得涂层兼具导电性能。并且整个涂层制作工艺简单,降低了成本。

3 结 语

超疏水性能应用广泛,而自修复性能又极大地延长了超疏水涂层的使用寿命。通过低表面能物质的补偿和表面形貌的恢复这2个方面可实现超疏水性能的自修复。现阶段研究对恢复因磨损而造成表面形貌破坏的方法较少,同时多数自修复进程需要外界刺激。如何修复大尺度结构损伤、优化自修复条件,同时使得整个配方更加环保,工艺简单,是该领域未来研究的重点。对于多功能涂层进行设计,使各功能间相互协调,相互促进,达到涂层整体性能最优,将是自修复超疏水多功能涂层研究的发展方向。

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