CN109989180A - 一种纳米压电复合膜的制备方法 - Google Patents

一种纳米压电复合膜的制备方法 Download PDF

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CN109989180A
CN109989180A CN201711465492.1A CN201711465492A CN109989180A CN 109989180 A CN109989180 A CN 109989180A CN 201711465492 A CN201711465492 A CN 201711465492A CN 109989180 A CN109989180 A CN 109989180A
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冯章启
严珂
李通
袁旭
史传梅
夏一鹭
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Nanjing University of Science and Technology
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Abstract

本发明公开了一种纳米压电复合膜的制备方法。包括如下步骤：将氧化石墨分散在乙醇溶液中，超声一定时间使其分散均匀；利用静电纺丝装置对聚偏二氟乙烯‑三氟乙烯溶液进行纺丝，制备聚偏二氟乙烯‑三氟乙烯纳米纤维；将制得聚偏二氟乙烯‑三氟乙烯纳米纤维浸润在分散有氧化石墨烯的乙醇溶液中，以一定速度进行提拉，即得到氧化石墨烯/聚偏二氟乙烯‑三氟乙烯纳米复合膜。本发明的工艺简单，得到的复合膜保留了聚偏二氟乙烯‑三氟乙烯纳米纤维的压电效应，并改善了材料表面的亲水性，可用于细胞培养支架。

Description

一种纳米压电复合膜的制备方法
技术领域
本发明属于膜材料制备技术领域，尤其涉及一种纳米压电复合膜的制备方法。
背景技术
静电纺丝技术是一种利用高压静电场制备连续微纳米纤维的方法，具有高效快捷、成本低廉、工艺可控且环保无污染的优良特点。近年来，随着纳米科技的成熟和进步，以及科研工作者对纳米材料的关注和重视，静电纺丝技术获得了突飞猛进的发展，成为有效制备微纳米材料的主要途径之一。
近年来，以聚偏二氟乙烯(PVDF)为代表的压电高分子材料得到了广泛的关注。压电高分子材料不仅具有良好的压电性能，还具备传统压电陶瓷无法比拟的弹性、可塑性等优势。经过机械拉伸和电场极化的PVDF塑性薄膜具有灵敏度高、生物相容性好及复杂环境稳定性优良等特点，这些特点使压电高分子材料在传感驱动材料方面有着广泛的应用。研究表明，在PVDF中加入三氟乙烯(TrFE)，即为聚偏二氟乙烯-三氟乙烯(P(VDF-TrFE))，可以改善材料中的β晶体结构，提高聚合物薄膜的压电性能，进一步拓展压电高分子材料的应用范围。
虽然聚偏二氟乙烯-三氟乙烯(P(VDF-TrFE))纳米纤维具有良好的压电性能，但其表面为疏水性质，普通的改性手段可能会对其中的β相造成破坏，导致其压电性能大幅度下降，这些缺点均阻碍了其在细胞培养方面的进一步发展。
发明内容
本发明的目的在于解决现有聚偏二氟乙烯-三氟乙烯(P(VDF-TrFE))纳米纤维表面高度疏水、改性易破坏晶型等缺点，提供了一种复合纳米压电薄膜的制备方法，该复合膜具有既保留了聚偏二氟乙烯-三氟乙烯(PVDF-TrFE)纳米纤维的压电效应，同时又使其表面具备了一定的亲水性，在细胞培养方面显示了优越的前景。
为了达到上述目的，本发明公开了一种纳米压电复合膜的制备方法，包括以下具体步骤：
步骤1：配置乙醇的水溶液，将氧化石墨烯在乙醇水溶利进行超声分散，至分散液均匀、无分层、无明显颗粒；
步骤2：配置N,N二甲基甲酰胺溶与丙酮的混合溶液，将聚偏二氟乙烯-三氟乙烯(PVDF-TrFE)加入N,N二甲基甲酰胺溶与丙酮的混合溶液中，搅拌至溶液均匀澄清，再离心以出去溶液中的气泡；
步骤3：利用静电纺丝设备对步骤2中制得的聚偏二氟乙烯-三氟乙烯(PVDF-TrFE)溶液进行纺丝，制备得到聚偏二氟乙烯-三氟乙烯(PVDF-TrFE)纳米纤维；
步骤4：将步骤3中制得的聚偏二氟乙烯-三氟乙烯(PVDF-TrFE)纳米纤维全部浸润在步骤1中制得的含有氧化石墨烯的乙醇水溶液，利用恒流注射泵进行提拉，进行烘干，即得到氧化石墨烯/聚偏二氟乙烯-三氟乙烯纳米复合膜。
优选地，步骤1中乙醇水溶液体积分数为40-70％，超声时间为2-6h。
优选地，步骤1中氧化石墨烯溶液的浓度为1mg/ml～3mg/ml。
优选地，步骤2中N,N二甲基甲酰胺溶与丙酮的比例为3：2。
优选地，步骤2中聚偏二氟乙烯-三氟乙烯与溶液的质量分数比为20％。
优选地，步骤3中电纺条件为：电压18kV，接收距离15cm，溶液流速为1.0ml/h，针头为21号。
优选地，步骤4中恒流注射泵的提拉速度为0.33ml/h。
与现有技术相比，本发明具有以下显著优点：
(1)本发明的工艺简单，原料易得。
(2)本发明制克服了材料疏水所带来的负载能力薄弱的问题。
(3)本发明的制备方法为细胞培养提供了可行的方法，为考量压电效应与细胞之间的作用带来可能。
附图说明
图1为本发明制得的氧化石墨烯/聚偏二氟乙烯-三氟乙烯纳米复合膜SEM图。
图2为本发明制得的聚偏二氟乙烯-三氟乙烯纳米纤维压电性能测试图。
图3为本发明制得的复合纤维膜上培养肝癌细胞的SEM图。
具体实施方式
下面结合具体实施例以及附图，进一步阐明本发明。
首先，配置10ml70％的乙醇溶液，将10mg氧化石墨烯置于70％乙醇溶液中，进行超声分散，氧化石墨烯溶液的浓度为1mg/ml，分散时间为4h，确保氧化石墨烯已经均匀分散在乙醇溶液中。随后，配置聚偏二氟乙烯-三氟乙烯的纺丝溶液，溶剂为N,N二甲基甲酰胺溶与丙酮，两种溶剂的体积比例为3：2。将0.2g聚偏二氟乙烯-三氟乙烯置与溶剂中，超声2h加速溶解，利用静电纺丝装置进行纺丝，承接片为玻璃。纺丝5min，取出承接片，固定在恒流注射泵上，并保证载有纤维的玻璃片完全浸没在分散有氧化石墨烯的乙醇溶液中，以0.33ml/h的速度进行提拉。提拉结束后，将玻璃片取下置于烘箱中进行干燥，即得到氧化石墨烯/聚偏二氟乙烯-三氟乙烯纳米压电复合膜。利用制备的纳米压电复合膜培养肝癌细胞，以验证所制备的膜在细胞培养方面的应用，如图1-3所示，图1为本发明制得的氧化石墨烯/聚偏二氟乙烯-三氟乙烯纳米复合膜SEM图。图2为本发明制得的聚偏二氟乙烯-三氟乙烯纳米纤维压电性能测试图。图3为本发明制得的复合纤维膜上培养肝癌细胞的SEM图可以看出的是，经过3天的培养，细胞在膜上表现出了良好的粘附性和形貌。

Claims (7)

1.一种纳米压电复合膜的制备方法，其特征在于，包括如下具体步骤：
步骤1：配置乙醇的水溶液，将氧化石墨烯在乙醇水溶利进行超声分散，至分散液均匀、无分层、无明显颗粒；
步骤2：配置N,N二甲基甲酰胺溶与丙酮的混合溶液，将聚二氟乙烯-三氟乙烯加入N,N二甲基甲酰胺溶与丙酮的混合溶液中，搅拌至溶液均匀澄清，再离心以出去溶液中的气泡；
步骤3：利用静电纺丝设备对步骤2中制得的聚偏二氟乙烯-三氟乙烯溶液进行纺丝，制备得到聚偏二氟乙烯-三氟乙烯纳米纤维；
步骤4：将步骤3中制得的聚偏二氟乙烯-三氟乙烯纳米纤维全部浸润在步骤1中制得的含有氧化石墨烯的乙醇水溶液，利用恒流注射泵进行提拉，进行烘干，即得到氧化石墨烯/聚偏二氟乙烯-三氟乙烯纳米复合膜。
2.如权利要求1中所述的纳米压电复合膜的制备方法，其特征在于，步骤1中乙醇水溶液体积分数为40-70％，超声时间为2-6h。
3.如权利要求1中所述的纳米压电复合膜的制备方法，其特征在于，步骤1中氧化石墨烯溶液的浓度为1mg/ml～3mg/ml。
4.如权利要求1中所述的纳米压电复合膜的制备方法，其特征在于，步骤2中N,N二甲基甲酰胺溶与丙酮的溶液体积比例为3：2。
5.如权利要求1中所述的纳米压电复合膜的制备方法，其特征在于，步骤2中聚偏二氟乙烯-三氟乙烯与溶剂的质量分数比例为20％。
6.如权利要求1中所述的纳米压电复合膜的制备方法，其特征在于，步骤3中，电纺条件为：电压18kV，接收距离15cm，溶液流速为1.0ml/h，针头为21号。
7.如权利要求1中所述的纳米压电复合膜的制备方法，其特征在于，步骤4中恒流注射泵的提拉速度为0.33ml/h。
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CN111869951A (zh) * 2020-06-23 2020-11-03 西安理工大学 一种口罩过滤层的制备方法
CN111869951B (zh) * 2020-06-23 2022-09-27 山西洁康惠医疗器械有限公司 一种口罩过滤层的制备方法
CN112226839A (zh) * 2020-10-16 2021-01-15 武汉智达纺织科技有限公司 一种氧化石墨烯改性聚偏氯乙烯压电织物及其制备方法

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