CN106871775B - 碳系材料-高分子聚合物应变敏感薄膜及制备方法 - Google Patents

碳系材料-高分子聚合物应变敏感薄膜及制备方法 Download PDF

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CN106871775B
CN106871775B CN201710076583.XA CN201710076583A CN106871775B CN 106871775 B CN106871775 B CN 106871775B CN 201710076583 A CN201710076583 A CN 201710076583A CN 106871775 B CN106871775 B CN 106871775B
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film
carbon
high molecular
molecular polymer
rigid substrate
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CN106871775A (zh
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太惠玲
叶学亮
袁震
郭睿
蒋亚东
黎威志
杜晓松
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University of Electronic Science and Technology of China
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Abstract

本发明公开了一种碳系材料‑高分子聚合物应变敏感薄膜及制备方法，涉及一种碳系材料柔性应变敏感薄膜制备方法，其目的在于提供一种碳系材料‑高分子聚合物应变敏感薄膜及制备方法，解决单一碳材料应变薄膜灵敏度差、稳定性不佳的问题。该碳系材料‑高分子聚合物应变敏感薄膜由碳系敏感薄膜、高分子聚合物薄膜通过层层自组装工艺形成多层复合薄膜。制备方法包括以下步骤：基片表面清洗与亲水、疏水处理；配置碳系材料和高分子聚合物分散液；通过层层自组装工艺将高分子聚合物和碳系材料层层组装生长在基片上；将复合薄膜从刚性基底转移到柔性基底；在复合物薄膜表面两端用导电银浆接入电极，再用柔性薄膜进行封装。

Description

碳系材料-高分子聚合物应变敏感薄膜及制备方法
技术领域
本发明涉及一种基于碳系材料柔性应变敏感薄膜制备方法，具体地指一种层层自组装制备柔性碳系复合应变薄膜的工艺方法。
背景技术
应变传感器因其具有测量分辨率高、测量范围宽、不受电磁干扰、耐腐蚀、抗冲击振动、抗疲劳、使用寿命长等优点，使其在航空航天、机械、电力、化工、建筑、医疗健康、汽车工业等多个领城有着十分广泛的应用。柔性应变传感器不仅可以克服传统应变传感器的刚性、脆性等缺点，而且还可以弯折甚至卷绕，极大地拓展了应变传感器在生物医学领域、仿生机器人领域、智能电子领域、材料结构缺陷监测等领域的运用。
目前用于制备柔性应变敏感薄膜的材料主要包括：碳系材料(石墨烯、碳管等)和金属系材料(AuNWs、AgNWs、ZnONWs、Pt等)，其中碳系纳米材料因具有良好的导电性、高比表面积、优良力学特性等优点，使其被广泛地用于各类功能敏感薄膜材料。目前应变敏感薄膜制备方法主要包括：化学气相沉积、原位自组装、喷涂、浸渍法、静电纺丝法。专利CN104257359A公开了一种基于碳材料-柔性高分子聚合物复合敏感材料柔性应变传感器制备方法，将碳材料和柔性高分子聚合物粘稠状混合物作为敏感材料涂覆在纺织物上，得到三维纳米结构敏感层；其制备特征在于将两种材料粘稠溶液按一定配比直接混合，得到粘稠状混合物，该制备过程简单易于操作，但存在复合材料均匀性及膜层生长可控性差等问题。专利CN103076031A公开了一种利用静电纺丝法制备的柔性可拉伸应变传感器，将配置的导电聚合物纺丝溶液注入针管，利用静电纺丝装置将纺丝溶液沉积在柔性收集基底上，该方法制备的柔性可拉伸应变传感器具有较好的灵敏度和稳定性，但存在着装置成本较高、操作复杂等问题。专利CN104406513A公开了一种石墨烯基表面应变传感器制备方法，将氧化石墨烯喷涂在基板上，利用化学还原或紫外光照射氧化石墨烯得到石墨烯薄膜，粘贴电极后，再喷涂一层高分子溶液，该方法制备的应变传感器应变系数为5，相较于同类应变传感器灵敏度较低，且制备工艺可控性差。
发明内容
基于上述柔性应变敏感薄膜在制备过程中出现的诸如：薄膜制备装置成本高昂、操作复杂、制备工艺可控性差、薄膜性能差、实用价值低等问题。本发明提供一种碳系材料-高分子聚合物应变敏感薄膜及制备方法，解决单一碳材料应变薄膜灵敏度差、稳定性不佳等问题。
本发明采用的技术方案如下：
一种碳系材料-高分子聚合物应变敏感薄膜，包括多层碳系敏感薄膜、多层高分子聚合物薄膜，所述碳系敏感薄膜与高分子聚合物薄膜依次通过层层自组装工艺形成多层复合薄膜。
其中，所述碳系敏感薄膜所使用的碳材料为石墨烯、氧化石墨烯、氧化还原石墨烯、石墨烯量子点、石墨烯纳米片、碳纳米管、碳纳米纤维、纳米多孔碳或纳米石墨中的一种或几种的组合。
其中，所述高分子聚合物薄膜所使用的材料为一种可溶于水或醇且具有黏粘特性的材料，包括聚乙烯亚胺(PEI)、聚丙烯酰胺(PAAM)或聚乙烯吡咯烷酮(PVP)等。
一种碳系材料-高分子聚合物应变敏感薄膜的制备方法，包括以下步骤：
①对刚性基底表面依次进行清洗、亲水、疏水处理；
②配置分散均匀的碳系材料分散液，配置分散均匀的高分子聚合物分散液；
③将步骤①中疏水处理后的刚性基底依次、重复浸渍在高分子聚合物分散液和碳系材料分散液中，通过层层自组装工艺在刚性基底上制备多层复合薄膜；
④将步骤③中制备的多层复合薄膜从刚性基底转移到柔性基底上；
⑤在复合薄膜表面两端用导电银浆接入两个电极，并用柔性薄膜进行封装。
其中，步骤①中，清洗处理的步骤为：将刚性基底依次在丙酮、乙醇和去离子水中超声清洗10-30min，氮气吹干；亲水处理的步骤为：将清洗后的刚性基底依次放入浓硫酸、双氧水中超声清洗各15-30min，氮气吹干；疏水处理的步骤为：将经过亲水处理过的刚性基底放入烧杯中，滴加TMCS溶液并密封烧杯口，将烧杯放入恒温水箱并在60℃-80℃下水浴40-60min，氮气吹干。此处疏水处理的目的是便于后期将复合薄膜从刚性基底转移到柔性基底，得到完整柔性复合薄膜。
其中，步骤②中，配置碳系材料分散液和高分子聚合物分散液时，需要辅以超声分散处理20-40min，磁力搅拌处理10-20min。
其中，步骤③中，层层自组装工艺为：将疏水处理后的刚性基底浸渍在高分子聚合物溶液中生长2-5min后取出，用去离子水洗净后N2吹干，在刚性基底表面生长一层高分子聚合物薄膜；随后将刚性基底浸渍在碳系材料溶液中生长2-5min后取出，用去离子水洗净后N2吹干，在聚合物薄膜上生长一层碳系敏感薄膜。依次重复上述过程步骤多次，最终在刚性基底上形成多层复合薄膜。
其中，步骤④中，复合薄膜转移过程中：通过利用具有良好粘附性且熔点高的高分子胶状材料(如二甲基硅氧烷(PDMS))，将多层复合薄膜转移到柔性基底上。
其中，步骤⑤中，电极材料包括铜线、金、银、碳纳米管或石墨烯等，电极引出方式为粘贴或印刷。柔性封装薄膜的材料为PDMS、聚乙烯或聚酰亚胺等材料中的任一种。
综上所述，由于采用了上述技术方案，本发明的有益效果是：
1、本发明中，碳系材料与高分子聚合物组成新的纳米复合敏感材料体系，在充分发挥碳系材料本身大比表面积、优良力学性能及导电能力等优势的同时，高分子聚合物可极大地提升碳系材料薄膜与柔性基底的附着度，从而提高薄膜的应变恢复性能与稳定性；此外，高分子聚合物可有效改善碳系材料的分散性，有利于均匀导电网络的形成，因此可改善单一碳系应变敏感材料灵敏度差的问题。
2、本发明中，利用层层自组装工艺制备应变敏感薄膜，通过逐层交替沉积的方法,借助各层分子间的弱相互作用(如静电引力、氢键、配位键等)，使层与层间自发缔和形成结构完整、性能稳定、具有某种特定功能的分子聚集体或超分子结构；同时还可通过调节自组装薄膜层数、材料以及复合薄膜界面来进一步优选应变复合薄膜最佳性能参数。该工艺操作过程简单、设备要求低、原理可靠，制备的传感器灵敏度高、应变系数大、柔韧性好、成本低、环境友好。
3、本发明中，对刚性基底进行疏水处理，目的是便于后期将复合薄膜从刚性基底转移到柔性基底，以得到完整的柔性复合薄膜。不直接采用柔性可拉伸材料的原因在于二个方面：其一，柔性材料基底在亲水处理过程中绝大多数会被浓硫酸腐蚀；其二，自组装过程中柔性基底会悬浮在溶液中不能完全被浸渍，在清洗和吹干过程中也难以控制。
附图说明
图1为本发明涉及的层层自组装工艺流程图；
图2为本发明涉及的石墨烯基复合薄膜的扫描电镜(SEM)图；
图3为本发明涉及的一种石墨烯基复合薄膜的傅里叶红外光谱吸收图；
图4为本发明涉及的一种石墨烯基复合薄膜断层处原子力显微镜(AFM)图；
图5为本发明涉及的一种石墨烯基复合薄膜厚度变化图；
图6为本发明制备的一种石墨烯基柔性应变传感器的响应曲线；
图7为不同应变大小下石墨烯基柔性复合薄膜电阻相对变化率的变化关系曲线；
图8为手指弯曲前后柔性复合薄膜电阻相对变化率的变化关系曲线。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白，以下结合附图及实施例，对本发明进行进一步详细说明。应当理解，此处所描述的具体实施例仅用以解释本发明，并不用于限定本发明。
一种碳系材料-高分子聚合物应变敏感薄膜，包括多层碳系敏感薄膜、多层高分子聚合物薄膜。该碳系敏感薄膜所使用的碳材料为石墨烯、氧化石墨烯、氧化还原石墨烯、石墨烯量子点、石墨烯纳米片、碳纳米管、碳纳米纤维、纳米多孔碳或纳米石墨中的一种或几种的组合；该高分子聚合物薄膜所使用的材料为一种可溶于水或醇且具有黏粘特性的材料，优选聚乙烯亚胺(PEI)、聚丙烯酰胺(PAAM)或聚乙烯吡咯烷酮(PVP)。多层碳系敏感薄膜、多层高分子聚合物薄膜通过层层自组装工艺形成多层复合薄膜，该复合薄膜中的碳系敏感薄膜和高分子聚合物薄膜是以“……—碳系敏感薄膜—高分子聚合物薄膜—碳系敏感薄膜—高分子聚合物薄膜—……—碳系敏感薄膜—高分子聚合物薄膜—碳系敏感薄膜—高分子聚合物薄膜—……”的形式设置。
一种碳系材料-高分子聚合物应变敏感薄膜的制备方法，包括以下步骤：
①对刚性基底表面依次进行清洗、亲水、疏水处理。
在对刚性基底进行清洗处理时，其步骤为：将刚性基底依次在丙酮、乙醇和去离子水中超声清洗10-30min，氮气吹干。在对刚性基底进行亲水处理时，其步骤为：将清洗后的刚性基底依次放入浓硫酸、双氧水中超声清洗各15-30min，氮气吹干。在对刚性基底进行疏水处理时，其步骤为：将经过亲水处理过的刚性基底放入烧杯中，滴加TMCS溶液并密封烧杯口，将烧杯放入恒温水箱并在60℃-80℃下水浴40-60min，氮气吹干。
②配置分散均匀的碳系材料分散液，配置分散均匀的高分子聚合物分散液。
在该步骤中，配置碳系材料分散液和高分子聚合物分散液时，需要辅以超声分散处理20-40min，磁力搅拌处理10-20min；也可以单独进行超声分散处理或者磁力搅拌处理。
③将步骤①中疏水处理后的刚性基底依次、重复浸渍在高分子聚合物分散液和碳系材料分散液中，通过层层自组装工艺在刚性基底上制备多层复合薄膜。
该层层自组装工艺为：将疏水处理后的刚性基底浸渍在高分子聚合物溶液中生长2-5min后取出，用去离子水洗净后N2吹干，在刚性基底表面生长一层高分子聚合物薄膜；随后将刚性基底浸渍在碳系材料溶液中生长2-5min后取出，用去离子水洗净后N2吹干，在聚合物薄膜上生长一层碳系敏感薄膜。依次重复上述过程步骤多次，最终在刚性基底上形成多层复合薄膜。
④将步骤③中制备的复合薄膜从刚性基底转移到柔性基底上。
在复合薄膜转移过程中：通过利用具有良好粘附性且熔点高的高分子胶状材料将多层复合薄膜转移到柔性基底上，该高分子胶状材料可选用二甲基硅氧烷(PDMS)。
⑤在复合薄膜表面两端用导电银浆引入两个电极，并用柔性薄膜进行封装。
电极材料为铜线、金、银、碳纳米管或石墨烯，电极引出方式为粘贴或印刷，柔性封装薄膜材料为PDMS、聚乙烯或聚酰亚胺。
实施例1
本实施例以石墨烯-聚乙烯亚胺复合薄膜作为敏感层制备石墨烯基柔性应变传感器，其具体工艺步骤为：
(1)选用玻璃作为薄膜生长基底，分别用丙酮、无水乙醇、去离子水超声清洗玻璃基片各10-30min，然后依次用浓硫酸、双氧水、去离子水各超声清洗15-30min，使半亲水半疏水玻璃表面完全亲水，洗净后氮气吹干。将装有完全亲水玻璃基片的支片架放入干净烧杯，滴加适量TMCS溶液并密封烧杯口，将烧杯放入恒温水箱，在65℃水浴40-60分钟，得到完全疏水玻璃基底。
(2)将2mg/ml氧化石墨烯溶液和去离子水按照1:2-1:3体积比例配置，并超声分散处理20-40min，使得氧化石墨烯均匀分散。将黄色黏稠状PEI液体溶于去离子水，配置1％w/v-5％w/v PEI溶液，并超声分散处理20-40min，使得PEI溶液分散均匀。
(3)将硅烷化处理后的玻璃基片放入1％w/v-5％w/vPEI溶液中浸渍生长2-3min，取出用去离子水清洗，然后用N2吹干；随后将玻璃基片放入浓度为0.25mg/ml-1mg/ml氧化石墨烯溶液中浸渍生长2-3min，取出用去离子水清洗，然后用N2吹干。依次重复上述过程层层组装PEI薄膜和氧化石墨烯薄膜，制备出多层复合敏感薄膜。
(4)将聚二甲基硅氧烷主剂和固化剂按照10:1质量比称重，混合后成分搅拌10-20min，至大量气泡产生，将装有混合液的烧杯放入真空箱，在-0.05MPa--0.01MPa下脱泡10-20分钟，得到PDMS前驱液。利用旋涂工艺将PDMS前驱液旋涂到多层复合敏感薄膜玻璃基片上，调节旋涂机的旋转转速(500rmp-800rmp)和旋转时间(9s-30s)，制备出厚度不一的柔性基底。将旋涂有PDMS的玻璃基片放入真空干燥箱中，在60℃-70℃下烘烤40-60min。将玻璃基片从干燥箱中取出，待玻璃基片温度恢复到室温时，将PDMS从玻璃基片上机械剥离，复合薄膜被转移到PDMS上，制备出柔性复合薄膜。
(5)将柔性复合薄膜放入气氛炉中，220℃退火2h，将氧化石墨烯还原成石墨烯，利用导电银浆将铜线作为电极镀在石墨烯基柔性复合薄膜表面，封装制备出石墨烯基柔性应变传感器。
本发明对制备的柔性复合薄膜的应变敏感性能进行测试，结果显示柔性复合薄膜的电阻随着弯曲或拉伸程度的变化而变化，重复性好、响应大、灵敏度高、在小应变下仍具有较大应变系数。
本实施案例中的层层自组装工艺制备多层复合薄膜工艺流程图如图1所示。图2为复合薄膜表面形貌图，可见复合薄膜呈波纹褶皱形貌。图3为复合薄膜的傅里叶红外吸收光谱，可见，在3385cm-1附近的-OH官能团吸收峰明显消失，1314cm-1和1413cm-1附近的C-OH吸收峰明显消失，说明氧化石墨烯被充分还原。图4给出了自组装两层石墨烯复合薄膜AFM断面图，图中白色区域为复合薄膜，黑色区域为基底，可见敏感薄膜从玻璃基片成功转移到了PDMS柔性基底，单层复合薄膜的厚度估算为4nm，如图5所示。
本实施例将封装好的石墨烯基柔性应变传感器两端固定，利用动态应变测试平台，设置运动平台各参数，拉伸应变传感器。石墨烯基柔性应变传感器的电阻随着薄膜的拉伸，电阻发生急剧变化，利用keithley2700信号采集器采集电阻阻值数据。测试应变大小与电阻响应曲线，可用于人体生理参数(血压、心率、脉搏)和运动状态(手指膝盖活动)实时监测。
本实施例利用动态测试平台，在薄膜两端施加拉伸力使其发生形变，以固定拉伸形变石墨烯复合薄膜应变片保持10s，随后动态平台运动到原位释放拉伸形变保持10s使其恢复原状，如此以20s为一个测试周期，反复循环几十个周期，如图6所示；从图中可以明显看出石墨烯复合薄膜拉伸形变时，电阻急剧增大，说明该传感器对拉伸应变具有高灵敏和高稳定特性；图7给出了在不同拉伸应变下石墨烯基复合薄膜电阻相对变化率(△R/R0)的变化关系，从图中可以看出薄膜拉伸形变增大时，电阻增大，相对电阻变化率与应变大小成线性关系。在本实施例中，制备的柔性应变敏感薄膜可运用于人体运动状态监测。图8给出了手指微弱弯曲前后电阻相对变化率变化曲线，从图中可以看出该复合薄膜具有良好的响应和稳定性，可被运用于对人体运动状态实时监测。
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明的保护范围之内。

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1.一种碳系材料-高分子聚合物应变敏感薄膜的制备方法，其特征在于，包括以下步骤：
①对刚性基底表面依次进行清洗、亲水及疏水处理；
将刚性基底依次在丙酮、乙醇和去离子水中超声清洗10-30min，氮气吹干；亲水处理的步骤为：将清洗后的刚性基底依次放入浓硫酸、双氧水中超声清洗各15-30min，氮气吹干；疏水处理的步骤为：将经过亲水处理过的刚性基底放入烧杯中，滴加适量三甲基氯硅烷(TMCS)溶液并密封烧杯口，将烧杯放入恒温水箱并在60℃-80℃下水浴40-60min，氮气吹干
②配置分散均匀的碳系材料分散液，配置分散均匀的高分子聚合物分散液；
配置碳系材料分散液和高分子聚合物材料分散液时，需要辅以超声分散处理20-40min，磁力搅拌处理10-20min；
③将步骤①中疏水处理后的刚性基底依次、重复浸渍在高分子聚合物分散液、碳系材料分散液中，通过层层自组装工艺在基底上制备多层复合薄膜；
层层自组装工艺为：将疏水处理后的刚性基底浸渍在高分子聚合物溶液中生长2-5min后取出，用去离子水洗净后N2吹干，在刚性基底表面生长一层高分子聚合物薄膜；随后将刚性基底浸渍在碳系材料溶液中生长2-5min后取出，用去离子水洗净后N2吹干，在聚合物薄膜上生长一层碳系敏感薄膜；依次重复上述过程步骤多次，最终在刚性基底上形成多层复合薄膜；依次重复上述过程步骤多次，最终在刚性基底上形成多层复合薄膜，复合薄膜中的碳系敏感薄膜和高分子聚合物薄膜是以“……—碳系敏感薄膜—高分子聚合物薄膜—碳系敏感薄膜—高分子聚合物薄膜—……—碳系敏感薄膜—高分子聚合物薄膜—碳系敏感薄膜—高分子聚合物薄膜—……”的形式设置；
④将步骤③中制备的多层复合薄膜从刚性基底转移到柔性基底上；
所述复合薄膜转移过程中：通过利用具有良好粘附性且熔点高的高分子胶状材料，将多层复合薄膜转移到柔性基底上；
⑤在复合薄膜表面两端用导电银浆引入两个电极，并用柔性薄膜进行封装；
电极材料包括铜线、金、银、碳纳米管或石墨烯，电极引出方式为粘贴或印刷，柔性封装薄膜的材料为PDMS、聚乙烯或聚酰亚胺材料中的任一种；
所述高分子聚合物薄膜所使用的材料为一种可溶于水或醇且具有黏粘特性的高分子材料，高分子聚合物薄膜所使用的材料为聚乙烯亚胺(PEI)、聚丙烯酰胺(PAAM)或聚乙烯吡咯烷酮(PVP)。
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