CN113174580B - 一种基于湿度的薄膜褶皱形貌调控方法 - Google Patents

一种基于湿度的薄膜褶皱形貌调控方法 Download PDF

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CN113174580B
CN113174580B CN202110406947.2A CN202110406947A CN113174580B CN 113174580 B CN113174580 B CN 113174580B CN 202110406947 A CN202110406947 A CN 202110406947A CN 113174580 B CN113174580 B CN 113174580B
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刘锴
王恩泽
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Abstract

本发明公开了属于薄膜材料技术领域的一种基于湿度的薄膜褶皱形貌调控方法。所述方法具体步骤为：高温下在基底表面制备薄膜材料，冷却到室温得到基底‑薄膜材料；然后将基底‑薄膜材料置于湿度氛围中，薄膜开始形成褶皱形貌，保持后取出；得到具有褶皱形貌的薄膜材料。所述湿度氛围为40％～90％相对湿度，所述褶皱形貌包括六边形网络状褶皱形貌、平行电话线褶皱阵列形貌和分叉电话线褶皱网络形貌。本发明薄膜褶皱的形貌能通过调节基底种类、薄膜厚度和环境湿度进行调控；适用于更广泛的材料体系，且操作简便、可控性好；制备方法简单、环保，不需要使用有毒的有机溶剂；对于薄膜材料的基础研究和器件研发具有重要意义。

Description

一种基于湿度的薄膜褶皱形貌调控方法
技术领域
本发明属于薄膜材料技术领域，尤其涉及一种基于湿度的薄膜褶皱形貌调控方法。
背景技术
形成褶皱是薄膜材料释放自身应力的一种有效手段，这些褶皱可以形成具有一定空间分布规律的微纳结构，如人字形、棋盘形、迷宫形和网络状褶皱，可以用于构筑压力传感器、光栅结构和柔性器件等；此外，褶皱结构内部周期变化的应力场也会调控材料的电学、光学、磁学等多种性质，为基础研究和开发功能化器件提供了新的思路。但是目前常用的褶皱制备方法，如预应变法、溶胀法和液相收缩法等，主要是基于聚合物薄膜或聚合物基底，并不适用于需要经高温制备的薄膜材料体系。因此需要更为通用的方法制备并调控褶皱形貌，以推动基础研究和功能化器件开发。
发明内容
为了解决上述问题，本发明提出了一种基于湿度的薄膜褶皱形貌调控方法，具体步骤如下：
1)在300～1100℃下，在基底表面制备10～500nm厚的薄膜材料，冷却到室温得到基底-薄膜材料，薄膜和基底的热膨胀失配导致薄膜中具有残余压应力，但由于薄膜和基底结合力较强，此时薄膜保持平坦状态；
2)将步骤1)得到的基底-薄膜材料置于湿度氛围中，薄膜开始形成褶皱形貌，保持后取出；得到具有褶皱形貌的薄膜材料；所述湿度氛围为40％～90％相对湿度；所述形貌包括六边形网络状褶皱形貌、平行电话线褶皱阵列形貌或分叉电话线褶皱网络形貌。
当湿度氛围为40％～90％相对湿度，得到的褶皱形貌包括六边形网络状褶皱形貌、平行电话线褶皱阵列形貌和分叉电话线褶皱网络形貌；
当湿度氛围为40％～90％相对湿度，基底为蓝宝石，薄膜厚度为50～500nm，得到的褶皱形貌为六边形网络状褶皱形貌；
当湿度氛围为40％～90％相对湿度，基底为x切向的石英，薄膜厚度为50～150nm，得到的褶皱形貌包括平行电话线褶皱阵列形貌和分叉电话线褶皱网络形貌；
当湿度氛围为40％～60％相对湿度，基底为x切向的石英，薄膜厚度为50～150nm，得到的褶皱形貌为平行电话线阵列形貌；
当湿度氛围为60％～90％相对湿度，基底为x切向的石英，薄膜厚度为50～150nm，得到的褶皱形貌为分叉电话线褶皱网络形貌。
所述基底为亲水性基底或经处理后具有亲水性的基底，
所述处理过程采用食人鱼溶液(piranha溶液)，处理进行表面亲水处理；其中食人鱼溶液中，浓硫酸和双氧水的体积比3:1；
所述基底具体包括蓝宝石、石英、云母、玻璃、硅片或含氧化层的硅片。
所述基底表面制备薄膜的方法包括聚合物辅助沉积法、化学气相沉积法、溅射法或蒸镀法。
所述薄膜材料包括金属、金属氧化物、金属硫属元素化合物、金属碳化物、金属氮化物或金属碳氮化物。
在所述步骤2)中保持时间为1分钟～1小时。
所述步骤1)，基底在制备薄膜之前需要经过清洗，具体步骤为，依次用丙酮、异丙醇、去离子水清洗。
一种基于湿度的MoS2薄膜褶皱形貌调控方法，具体包含以下步骤：
1)依次用丙酮、异丙醇、去离子水清洗蓝宝石基底，并用浓硫酸和双氧水体积比3:1混合后的piranha溶液进行表面亲水处理；
2)在步骤1)获得的基底表面，旋涂聚合物辅助沉积法所需的含Mo元素的前驱体溶液，得到基底-前驱体薄膜；
3)在管式炉内加热到850℃硫化步骤2)得到的基底-前驱体薄膜，得到基底-MoS2薄膜；
4)将基底-MoS2薄膜置于相对湿度50％～80％的环境中，使MoS2薄膜与基底脱层，形成褶皱。
本发明的有益效果在于：
1.本发明与现有技术相比，适用于更广泛的材料体系，且操作简便、可控性好；制备方法简单、环保，不需要使用有毒的有机溶剂；对于薄膜材料的基础研究和器件研发具有重要意义。
2.薄膜褶皱的形貌能通过调节基底种类、薄膜厚度和环境湿度进行调控。
附图说明
图1为蓝宝石基底上～300nm厚的MoS2薄膜在80％相对湿度下得到的相邻节点之间距离为30μm的六边形网络状褶皱的光学照片。
图2为石英基底上～100nm厚的MoS2薄膜在50％相对湿度下得到的波长为10μm的平行电话线褶皱阵列的光学照片。
图3为石英基底上～100nm厚的MoS2薄膜在80％相对湿度下得到的波长为20μm的分叉电话线褶皱网络的光学照片。
图4为对比例1中在石英基底上～100nm厚的MoS2薄膜在干燥环境下保持平坦状态的光学照片。
具体实施方式
以下结合附图和具体实施例对本发明作进一步的详细说明：
实施例1
本实施例提供了一种在薄膜中获得网络状褶皱的方法，包括如下步骤：
将1g乙二胺四乙酸(EDTA)和2g钼酸铵加入20mL去离子水中，再加入2g聚乙烯亚胺(PEI，MW＝10000)，搅拌至溶液澄清后用截留量为10000的超滤离心管离心数次，得到含Mo的前驱体溶液。
依次用丙酮、异丙醇、去离子水清洗蓝宝石基底，并用piranha溶液(浓硫酸、双氧水体积比3:1混合)处理进行表面亲水处理；
1)在亲水处理后获得的基底表面，旋涂聚合物辅助沉积法所需的含Mo元素的前驱体溶液，得到基底-前驱体薄膜；
在管式炉内加热到850℃硫化基底-前驱体薄膜，得到基底-MoS2薄膜，其中MoS2薄膜厚度～300nm；
2)将基底-MoS2薄膜置于相对湿度50％～80％的环境中，使MoS2薄膜与基底脱层，形成如图1所示的相邻节点之间距离为30μm的六边形网络状褶皱形貌。
实施例2
本实施例提供了一种在薄膜中获得平行电话线褶皱阵列的方法，包括如下步骤：
将0.5g乙二胺四乙酸(EDTA)和1g钼酸铵加入20mL去离子水中，再加入1g聚乙烯亚胺(PEI，MW＝10000)，搅拌至溶液澄清后用截留量为10000的超滤离心管离心数次，得到含Mo的前驱体溶液。
依次用丙酮、异丙醇、去离子水清洗x切向的石英基底，并用piranha溶液(浓硫酸、双氧水体积比3:1混合)处理进行表面亲水处理；
1)在亲水处理获得的基底表面，旋涂聚合物辅助沉积法所需的含Mo元素的前驱体溶液，得到基底-前驱体薄膜；
在管式炉内加热到850℃硫化基底-前驱体薄膜，得到基底-MoS2薄膜，其中MoS2薄膜厚度～100nm；
2)将基底-MoS2薄膜置于相对湿度40％～50％的环境中，使MoS2薄膜与基底脱层，形成如图2所示的波长为10μm的平行电话线褶皱阵列形貌。
实施例3
本实施例提供了一种在薄膜中获得分叉电话线褶皱网络的方法，包括如下步骤：
将0.5g乙二胺四乙酸(EDTA)和1g钼酸铵加入20mL去离子水中，再加入1g聚乙烯亚胺(PEI，MW＝10000)，搅拌至溶液澄清后用截留量为10000的超滤离心管离心数次，得到含Mo的前驱体溶液。
依次用丙酮、异丙醇、去离子水清洗x切向的石英基底，并用piranha溶液(浓硫酸、双氧水体积比3:1混合)处理进行表面亲水处理；
1)在亲水处理获得的基底表面，旋涂聚合物辅助沉积法所需的含Mo元素的前驱体溶液，得到基底-前驱体薄膜；
在管式炉内加热到850℃硫化得到的基底-前驱体薄膜，得到基底-MoS2薄膜，其中MoS2薄膜厚度～100nm；
2)将基底-MoS2薄膜置于相对湿度80％～90％的环境中，使MoS2薄膜与基底脱层，形成如图3所示的波长为20μm的分叉电话线褶皱网络形貌。
对比例1
本对比例用于说明薄膜在未接触湿度前的形貌，包括如下步骤：
将0.5g乙二胺四乙酸(EDTA)和1g钼酸铵加入20mL去离子水中，再加入1g聚乙烯亚胺(PEI，MW＝10000)，搅拌至溶液澄清后用截留量为10000的超滤离心管离心数次，得到含Mo的前驱体溶液。
依次用丙酮、异丙醇、去离子水清洗x切向的石英基底，并用piranha溶液(浓硫酸、双氧水体积比3:1混合)处理进行表面亲水处理；
1)在亲水处理获得的基底表面，旋涂聚合物辅助沉积法所需的含Mo元素的前驱体溶液，得到基底-前驱体薄膜；
在管式炉内加热到850℃硫化得到的基底-前驱体薄膜，得到基底-MoS2薄膜，仍保持如图4所示的平坦无褶皱形貌，其中MoS2薄膜厚度～100nm。

Claims (6)

1.一种基于湿度的薄膜褶皱形貌调控方法，其特征在于，具体步骤如下：
1）在基底表面利用聚合物辅助沉积法处理含Mo元素的前驱体溶液，在300~1100 ℃下，制备10~500 nm厚的MoS2薄膜材料，冷却到室温得到基底-薄膜材料，薄膜和基底的热膨胀失配导致薄膜中具有残余压应力，但由于薄膜和基底结合力较强，此时薄膜保持平坦状态；
所述基底为蓝宝石或石英；使用前用体积比3:1的浓硫酸和双氧水混合后的食人鱼溶液进行表面亲水处理；
2）将步骤1）得到的基底-薄膜材料置于湿度氛围中，薄膜开始形成褶皱形貌，保持后取出；得到具有褶皱形貌的薄膜材料；
所述湿度氛围为40 %~ 90 %相对湿度；所述褶皱形貌包括六边形网络状褶皱形貌、平行电话线褶皱阵列形貌和分叉电话线褶皱网络形貌。
2.根据权利要求1所述一种基于湿度的薄膜褶皱形貌调控方法，其特征在于，所述湿度氛围为40 %~ 90 %相对湿度，基底为蓝宝石，薄膜厚度为50 ~ 500 nm，得到的褶皱形貌为六边形网络状褶皱形貌。
3.根据权利要求1所述一种基于湿度的薄膜褶皱形貌调控方法，其特征在于，所述湿度氛围为40 %~90 %相对湿度，基底为x切向的石英，薄膜厚度为50 ~ 150 nm，得到的褶皱形貌包括平行电话线褶皱阵列形貌或分叉电话线褶皱网络形貌。
4.根据权利要求3所述一种基于湿度的薄膜褶皱形貌调控方法，其特征在于，所述湿度氛围为40 %~60 %相对湿度，基底为x切向的石英，薄膜厚度为50 ~ 150 nm，得到的褶皱形貌为平行电话线阵列形貌。
5.根据权利要求3所述一种基于湿度的薄膜褶皱形貌调控方法，其特征在于，所述湿度氛围为60 %~90 %相对湿度，基底为x切向的石英，薄膜厚度为50 ~ 150 nm，得到的褶皱形貌为分叉电话线褶皱网络形貌。
6.根据权利要求1所述一种基于湿度的薄膜褶皱形貌调控方法，其特征在于，在所述步骤2）中保持时间为1分钟~1小时。
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