CN112108346A - 一种用于纳米金属的防腐涂层及其制备方法 - Google Patents
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Abstract
本发明公开了一种用于纳米金属的防腐涂层及其制备方法,该防腐涂层包括高聚物涂层和二维材料涂层,高聚物涂层置于易氧化贵金属纳米结构表面,再经二维材料转移之后,在金属纳米结构表面形成高聚物‑二维材料纳米涂层,高聚物涂层为聚乙烯吡咯烷酮(PVP)层、聚甲基丙烯酸甲酯(PMMA)层和聚二甲基硅氧烷(PDMS)层中的任意一种,二维材料为石墨烯或六方氮化硼(hBN)。本发明制备的高聚物‑二维材料混合涂层,可实现对易氧化金属纳米材料的防护,利于纳米结构的长期稳定使用。
Description
技术领域
本发明涉及纳米金属及防腐技术领域,尤其涉及用于易氧化金属纳米材料的防腐涂层及其制备方法。
背景技术
随着信息技术的高速发展,金属纳米材料在高集成度纳米光电器件、生物传感、柔性器件等领域有重要应用。然而,由于在空气中金属纳米粒子表面极易氧化,其在实际生产与生活中的应用受到极大限制。不同于块状金属,纳米金属材料容易受到防腐涂层厚度的影响,而采用现有的涂层技术所获得的涂层厚度较厚,不可避免地影响金属纳米材料原本的物理特性。因此,现需提供一种对易氧化金属纳米材料本身物理属性影响最小的纳米级厚度的防腐涂层材料,使其成为用于易氧化纳米材料的氧化防护。
具有原子层厚度、疏水性、阻隔性、极好的化学稳定性和高温稳定性等独特性质的二维材料如石墨烯、hBN在材料防腐领域有重要应用。然而,二维材料在制备和转移的过程中会不可避免地引入缺陷,这将不利于金属纳米材料的长久有效防护。将高聚物纳米涂层置于金属纳米结构表面,然后将二维材料转移至高聚物涂层之上,可以实现对金属纳米结构的长久稳定保护。基于高聚物和二维材料纳米涂层保护金属纳米结构,提供了一种抑制金属纳米材料氧化的方法,必将推动金属纳米材料的广泛应用,促进材料科学、信息、传感等学科的发展。
发明内容
本发明要解决的技术问题在于针对现有技术中的不足,提供一种能有效抑制金属纳米材料腐蚀的基于高聚物和二维材料的纳米涂层及其制备方法。
本发明提供了如下技术方案:
一种用于纳米金属的防腐涂层,包括高聚物涂层和二维材料涂层,所述高聚物涂层置于易氧化贵金属纳米结构表面,再经二维材料转移之后,在金属纳米结构表面形成高聚物-二维材料纳米涂层。高聚物涂层为聚乙烯吡咯烷酮(PVP)层、聚甲基丙烯酸甲酯(PMMA)层和聚二甲基硅氧烷(PDMS)层中的任意一种,所述二维材料为石墨烯或六方氮化硼(hBN)。
进一步的,所述高聚物涂层厚度小于20nm。
进一步的,所述二维材料可以采用化学气相沉积(CVD)方法或剥离方法制备,所述高聚物涂层材料采用旋涂方法制备。
进一步的,所述二维材料层数为单层或多层。
进一步的,所述易氧化贵金属纳米结构有银纳米结构、铜纳米结构、铝纳米结构、铁纳米结构。
一种用于纳米金属的防腐涂层的制备方法,包括以下步骤:
(1)将金属纳米结构通过滴加、旋涂、蒸镀、磁控溅射或者印刷方法置于干净的基底表面,或将基底浸泡至含有金属纳米结构的均匀分散液中;
(2)在上述基底表面旋涂高聚物纳米涂层;
(3)将二维材料转移到旋涂有高聚物涂层的金属纳米结构的基底表面,自然晾干,然后将其置于10%H2和N2的混合气体中150-200℃下退火1-3h。
与现有技术相比该发明的有益效果如下:在高聚物纳米涂层和二维材料涂层的共同作用下,金属纳米结构表面不能与外界环境直接接触,利于金属纳米结构的长期稳定;防腐涂层对金属纳米结构原本的物理属性影响小,有利于基于金属纳米结构高性能器件的广泛研发与应用;该方法工艺简单、性价比高,在纳米材料防腐应用领域具有很好的发展前景。
附图说明
图1为一种基于高聚物-二维材料防腐涂层保护的金属纳米结构示意图。
图中,各标号所代表的部件如下:
1、基底;2、金属纳米结构;3、高聚物纳米涂层;4、二维材料涂层。
具体实施方式
下面结合具体的实施例,对本发明的技术方案进行清楚、完整的描述。显然,所描述的实施例仅仅是本发明的一部分实施例。基于本发明中的实施例,本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
实施例1
铜纳米薄膜—PVP—hBN:采用电子束蒸发镀膜方法制备厚度为60nm的铜纳米薄膜,具体过程如下:将厚度为1mm的洁净玻璃基底(25mm×25mm)置于镀膜机中,当腔体真空达到1×10-7bar时,将膜生长速率控制在~2A/s,通过校准的石英微晶天平来监测蒸镀薄膜的厚度。需要注意的是,在镀铜膜之前,需将1.5nm厚的铬膜(膜生长速率:~0.6A/s)蒸镀在玻璃基底上,用作玻璃基底与铜膜之间的粘合剂。然后将厚度小于20nm的高聚物PVP(2%PVP,溶剂:去离子水,PVP分子量:1300000)涂层旋涂置于上述铜纳米薄膜结构表面,其中旋涂转速为6000r/min,旋涂时间为2min。最后,通过电化学分层方法将1×1cm2的单层CVDhBN转移至上述基底结构表面,具体过程为:首先,将PMMA溶液旋涂于采用CVD方法生长有hBN的铁箔表面,然后在1mol/L的NaOH溶液中对铁箔表面的PMMA/hBN进行电化学鼓泡剥离,将剥离后的PMMA/hBN膜转移至去离子水中,使用去离子水反复多次洗涤涂有PMMA层的hBN;然后将其转移至含有高聚物PVP涂层的铜纳米薄膜结构表面,自然干燥后,使用丙酮浸泡3分钟去除hBN上涂覆的PMMA层,自然晾干。然后将其置于10%H2和N2的混合气体中150℃下退火2h。
实施例2
银纳米线—PMMA—双层石墨烯:首先,将银纳米线结构置于干净的硅片基底表面。然后,将厚度小于10nm的高聚物PMMA(0.1%PMMA,溶剂:氯苯)涂层旋涂置于上述银纳米线结构表面,120℃下烘烤3分钟。其中旋涂转速为8000r/min,旋涂时间为2min。最后,先后两次将1×1cm2的单层CVD石墨烯转移至上述银纳米线结构表面,具体过程为:首先,将PMMA溶液旋涂于采用CVD方法生长有石墨烯的铁箔表面,使用等离子体清洗机(气体:Ar/O2,清洗时长:20s)除去铜箔背面(无石墨烯的那一面)的污染物、氧化物;然后使用25g/l的过硫酸铵溶液刻蚀掉铜箔;使用去离子水反复多次洗涤附有PMMA的石墨烯;然后将其转移至含高聚物PMMA涂层的银纳米线结构表面,在120℃下干燥5分钟后,使用丙酮浸泡3分钟去除石墨烯上涂覆的PMMA层,自然晾干。然后将其置于10%H2和N2的混合气体中200℃下退火3h。然后,采用上述相同的步骤,进行第二次转移单层CVD石墨烯,在银纳米线结构表面形成PMMA-双层石墨烯纳米涂层。
实施例3
银纳米薄膜—PDMS—双层hBN:采用电子束蒸发镀膜方法制备厚度为50nm的银纳米薄膜,具体过程如下:将厚度为1mm的洁净玻璃基底(25mm×25mm)置于镀膜机中,当腔体真空达到1×10-7bar时,将膜生长速率控制在~5A/s,通过校准的石英微晶天平来监测蒸镀薄膜的厚度。需要注意的是,在镀银膜之前,需将1.5nm厚的铬膜(膜生长速率:~0.6A/s)蒸镀在玻璃基底上,用作玻璃基底与银膜之间的粘合剂。然后将厚度小于20nm的高聚物PDMS(使用硅油稀释PDMS(硅油和PDMS的质量比为1:1))涂层旋涂置于上述银纳米薄膜结构表面,其中旋涂转速为8000r/min,旋涂时间为2min。最后,先后两次通过电化学分层方法将1×1cm2的单层CVD hBN转移至上述基底结构表面,具体过程为:首先,将PMMA溶液旋涂于采用CVD方法生长有hBN的铁箔表面,然后在1mol/L的NaOH溶液中对铁箔表面的PMMA/hBN进行电化学鼓泡剥离,将剥离后的PMMA/hBN膜转移至去离子水中,使用去离子水反复多次洗涤涂有PMMA层的hBN;然后将其转移至含有高聚物PDMS涂层的银纳米薄膜结构表面,自然干燥后,使用丙酮浸泡3分钟去除hBN上涂覆的PMMA层,自然晾干。然后将其置于10%H2和N2的混合气体中150℃下退火2h。然后,采用与上述相同的步骤,进行第二次转移单层CVD hBN,在银纳米薄膜表面形成PDMS-双层hBN纳米涂层。
Claims (6)
1.一种用于纳米金属的防腐涂层,其特征在于,包括高聚物涂层和二维材料涂层,所述高聚物涂层置于易氧化贵金属纳米结构表面,再经二维材料转移之后,在金属纳米结构表面形成高聚物-二维材料纳米涂层,所述高聚物涂层为聚乙烯吡咯烷酮(PVP)层、聚甲基丙烯酸甲酯(PMMA)层和聚二甲基硅氧烷(PDMS)层中的任意一种,所述二维材料为石墨烯或六方氮化硼(hBN)。
2.根据权利要求1所述的一种用于纳米金属的防腐涂层,其特征在于,所述高聚物涂层厚度小于20nm。
3.根据权利要求1所述的一种用于纳米金属的防腐涂层,其特征在于,所述二维材料可以采用化学气相沉积(CVD)方法或剥离方法制备,所述高聚物涂层材料采用旋涂方法制备。
4.根据权利要求1所述的一种用于纳米金属的防腐涂层,其特征在于,所述二维材料层数为单层或多层。
5.根据权利要求1所述的一种用于纳米金属的防腐涂层,其特征在于,所述易氧化贵金属纳米结构有银纳米结构、铜纳米结构、铝纳米结构、铁纳米结构。
6.权利要求1-5任意一项所述的用于纳米金属的防腐涂层的制备方法,其特征在于,包括以下步骤:
(1)将金属纳米结构通过滴加、旋涂、蒸镀、磁控溅射或者印刷方法置于干净的基底表面,或将基底浸泡至含有金属纳米结构的均匀分散液中;
(2)在上述基底表面旋涂高聚物纳米涂层;
(3)将二维材料转移到旋涂有高聚物涂层的金属纳米结构的基底表面,自然晾干,然后将其置于10%H2和N2的混合气体中150-200℃下退火1-3h。
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