CN113215822B - 一种基于取向纳米纤维的多功能可拉伸透气传感材料 - Google Patents
一种基于取向纳米纤维的多功能可拉伸透气传感材料 Download PDFInfo
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Abstract
本发明公开一种基于取向纳米纤维的多功能可拉伸透气传感材料。通过静电纺丝技术调控纳米纤维膜的形貌结构,设计具有取向结构的导电离子液体/柔性高分子的纳米纤维膜,并通过沿着垂直于纳米纤维取向方向制备电极获得具有优异传感性能的高分子基可拉伸应变/温度传感材料。本发明利用静电纺丝技术制备了具有多孔结构的纳米纤维膜,透气性好,提高了传感器件佩戴时的舒适性,此外,通过巧妙地调整纺丝工艺(主要是提高滚筒接收器的转速)制备了具有纳米纤维取向分布的纤维膜,提高了传感器件应变/温度传感的灵敏性和重复性。
Description
技术领域
本发明属于高分子复合材料领域,涉及一种基于取向结构纳米纤维膜的多功能可拉伸 透气传感材料。
背景技术
随着电子皮肤、人机交互、可穿戴电子设备等新兴领域的迅速发展,作为核心部件的 柔性、可拉伸、可穿戴的应变/温度传感材料成为人们关注的热点。传统的应变/温度传感 材料多由金属或半导体等刚性材料制成,其较差的柔韧性、可拉伸性以及延展性使材料的 应用受到局限。研究显示,将导电材料与柔性高分子复合是制备柔性传感材料的有效途径。 目前研究较多的高分子基柔性应变/温度传感材料主要是由无机纳米粒子,例如碳系材料 (炭黑、碳纳米管、石墨烯等)和金属材料(银粒子、银纳米线等),填充的柔性高分子导电复合材料。然而,由于无机材料与高分子基体之间的相容性普遍较差,在高分子基体(尤其是高粘度的柔性高分子)内无机材料分布不均匀,并且构筑的导电网络杂乱无章, 温度和应变刺激下导电通路的演变不可逆,导致材料的应变/温度响应行为的稳定性和可 重复性较差。此外,由于无机纳米粒子与高分子的热膨胀系数差异大,高分子基柔性温度 传感材料往往呈现非单调的电信号响应。这些问题严重阻碍了高分子基柔性温度传感材料和柔性应变传感材料的实际应用。
离子液体(IL)是一类由阴阳离子组成的室温熔融盐,具有低熔点、低挥发性、低密度、高离子导电率、抗菌性等独特优势,在高分子材料改性、功能材料的制备等诸多领域 受到广泛关注。与无机纳米填料相比,离子液体不仅具有优异的导电率,并且可通过氢键 作用、偶极作用、质子化作用等与高分子链相互作用,提高其在高分子基体中的分散。因 此,将离子液体作为传感组分为制备高性能的高分子基柔性传感材料提供了新的思路。此 外,静电纺丝技术能够将离子液体/高分子复合之后的基材,进一步纺丝制备成透气性强、 柔性、适合可穿戴器件的传感材料,对可穿戴器件产业的发展具有重要意义。
发明内容
本发明的目的是解决现有的无机导电纳米粒子填充高分子基柔性传感材料存在的应 变/温度响应行为的稳定性和可重复性较差、温度响应信号非单调变化的问题,发展基于 离子导电机制的高分子基多功能可拉伸透气传感材料,并利用静电纺丝技术调控纳米纤维 膜的形貌结构,最终获得透气性好、应变/温度响应行为的稳定性和可重复性好、温度响 应信号单调变化的高分子基可拉伸应变/温度传感材料。
本发明通过以下技术方案实现:
通过静电纺丝技术调控纳米纤维膜的形貌结构,设计具有取向结构的导电离子液体/ 柔性高分子的纳米纤维膜,并通过沿着垂直于纳米纤维取向方向制备电极获得具有优异传 感性能的高分子基可拉伸透气应变/温度传感材料。
一种基于取向纳米纤维的多功能可拉伸透气传感材料采用以下方案一方法制备得到:
步骤(1):将柔性高分子基体加入到有机溶剂中,搅拌后得到均一的高分子溶液;
步骤(2):上述高分子溶液利用静电纺丝纺成具有取向结构的纳米纤维膜;
步骤(3):将具有取向结构的纳米纤维膜在导电离子液体中超声,然后在真空烘箱中干燥,获得复合纳米纤维膜;
作为优选,所述超声时间为30-100min,超声温度为18-35℃,超声功率为120W, 频率为40KHz。
作为优选,所述真空烘箱的温度为30-70℃,时间为12-24h。
步骤(4):将干燥好的复合纳米纤维膜裁剪成矩形样条,在纤维膜上沿着垂直于纳米纤维取向方向的两端粘附电极后得到基于取向结构纳米纤维膜的多功能可拉伸透气传感器件。
一种基于取向纳米纤维的多功能可拉伸透气传感材料采用以下方案二方法制备得到:
步骤(1):将柔性高分子基体加入到有机溶剂中,搅拌后得到均一的高分子溶液;
步骤(2):将导电离子液体加入到步骤一得到的高分子溶液中,机械搅拌均匀得到混合溶液;
步骤(3):将步骤(2)得到的混合溶液静电纺丝纺成具有取向结构的复合纳米纤维膜;
步骤(4):将干燥好的复合纳米纤维膜裁剪成矩形样条,在纤维膜上沿着垂直于纳米纤维取向方向的两端粘附电极后得到基于取向结构纳米纤维膜的多功能可拉伸透气传感器件。
作为优选,所述柔性高分子基体为聚偏氟乙烯(PVDF)、热塑性聚氨酯(TPU)、苯乙烯类热塑性弹性体(SBS、SEBS、SEPS及以上共混物)、热塑性聚烯烃类弹性体(TPO)、 聚酯弹性体(TPEE)中的一种或多种;
作为优选,所述有机溶剂为柔性高分子的相应良溶剂;
作为优选,所述高分子溶液的浓度为15-30wt%;
作为优选,所述离子液体与柔性高分子的质量比为(1:9)-(2:1);
作为优选,所述静电纺丝所用纺丝针头的型号为18G-22G;
作为优选,所述静电纺丝注射速度为0.01-1mm/min;
作为优选,所述静电纺丝的电压为15-25KV,针头距离收集装置间的间距为10-20cm, 采用滚筒作为收集装置,滚筒的转速为2500-3000rpm,温度在18-35℃,其环境湿度在 30%以下。
作为优选,所述具有取向结构的纳米纤维膜的厚度为0.05-2mm。
作为优选,所述导电离子液体为1-乙基-3-甲基咪唑四氟硼酸盐、N-甲基,甲氧基乙 基吡咯烷双三氟甲磺酰亚胺盐、1-乙基-3-甲基咪唑双氟磺酰亚胺盐、N-甲基丙基哌啶双 三氟甲磺酰亚胺盐、1-乙基-3-甲基咪唑双三氟甲磺酰亚胺盐、1-丁基-3-甲基咪唑双三氟 甲磺酰亚胺盐和1-己基-3-甲基咪唑双三氟甲磺酰亚胺盐中的一种或多种;
作为优选,所述电极材料为导电铜片,粘合剂为导电银浆。
本发明的另一个目的是提供上述基于取向纳米纤维的多功能可拉伸透气传感材料在 应变、温度传感器上的应用。
本发明的有益效果是:
1.本发明选取离子液体作为传感组分,制备基于离子导电机制的高分子基可拉伸透 气应变/温度传感材料,消除了以无机导电纳米粒子为传感组分的高分子基传感 复合材料存在的传感性能稳定性、重复性差,温度响应信号非单调变化的问题;
2.本发明利用静电纺丝技术制备了具有多孔结构的纳米纤维膜,透气性好,提高了 传感器件佩戴时的舒适性,此外,通过巧妙地调整纺丝工艺(主要是提高滚筒接 收器的转速)制备了具有纳米纤维取向分布的纤维膜,提高了传感器件应变/温 度传感的灵敏性和重复性。
附图说明
图1是实施例1制备的纳米纤维取向分布的复合纤维膜的扫描电镜图;
图2是取向纳米纤维膜表面电极的制备示意图;其中(a)为沿着垂直于纳米纤维取向方向的样条两端制备电极,(b)为沿着纳米纤维取向方向的样条两端制备电极;
图3是实施例1、对照例1、对照例2制备的复合纳米纤维膜电阻变化相对值随应变的变化;
图4是实施例1、对照例1、对照例2制备的复合纳米纤维膜电阻变化相对值随温度的变化;
图5是实施例2、对照例3、对照例4、对照例5制备的复合材料电阻变化相对值随 应变的变化;其中(a)的横坐标为应变,(b)的横坐标为循环次数;
图6是实施例2、对照例3、对照例4、对照例5制备的复合材料电阻变化相对值随 温度的变化;
图7是对照例2制备的纳米纤维无规的复合纤维膜的扫描电镜图;
具体实施方式
下面结合附图来进一步对本发明进行描述,但应当理解,以下的描述只为了更好的 说明本发明的特点和优点,而不是对本发明权利要求的限制。
实施例1
将5g PVDF加入到溶剂DMF中,搅拌后得到PVDF质量分数为20%的均一PVDF溶液。然后将PVDF溶液置于10ml注射器(针头型号为18G)中,以0.05mm/min的注射速度, 在20KV高压条件下静电纺丝(注射器针头距离滚筒接收器的距离为20cm,滚筒转速为 2500rpm,湿度为30%,温度为25℃),得到纳米纤维取向分布的纤维膜。然后将该纤维 膜置于10g 1-丁基-3-甲基咪唑双三氟甲磺酰亚胺盐溶液中25℃下120W,40KHz超声30 min,然后在真空烘箱中50℃干燥18h,获得复合纳米纤维膜,纤维膜的形貌结构如附图 1所示。在该纤维膜上沿着垂直于纳米纤维取向方向的样条两端粘附电极(电极材料为导 电铜片,粘合剂为导电银浆,如附图2a所示),制备传感器件V-IL/PVDF,并对所制得的 传感器件进行应变传感性能和温度传感性能测试,如附图3,4所示。
实施例2
将5g TPU加入到四氢呋喃(THF)与N,N-二甲基甲酰胺(DMF)的混合溶剂DMF/THF中,搅拌后得到TPU质量分数为25%的均一TPU溶液。然后将2.2g 1-己基-3-甲基咪唑 双三氟甲磺酰亚胺盐加入到TPU溶液中,机械搅拌均匀后得到混合溶液。将上述混合溶液 置于10ml注射器(针头型号为20G)中,以0.02mm/min的注射速度,在25KV高压条 件下静电纺丝(注射器针头距离滚筒接收器的距离为15cm,滚筒转速为2800rpm,湿度 为25%,温度为23℃),得到纳米纤维取向分布的纤维膜。在该纤维膜上沿着垂直于纳米 纤维取向方向的样条两端粘附电极(电极材料为导电铜片,粘合剂为导电银浆,如附图2a所示),制备传感器件V-IL/TPU,并对所制得的传感器件进行应变传感性能和温度传感 性能测试,如附图5,6所示。
对照例1
将5g PVDF加入到溶剂DMF中,搅拌后得到PVDF质量分数为20%的均一PVDF溶液。然后将PVDF溶液置于10ml注射器(针头型号为18G)中,以0.05mm/min的注射速度, 在20KV高压条件下静电纺丝(注射器针头距离滚筒接收器的距离为20cm,滚筒转速为 2500rpm,湿度为30%,温度为25℃),得到纳米纤维取向分布的纤维膜。然后将该纤维 膜置于10g 1-丁基-3-甲基咪唑双三氟甲磺酰亚胺盐溶液中25℃下120W,40KHz超声 30min,然后在真空烘箱中50℃干燥18h,获得复合纳米纤维膜。在该纤维膜上沿着纳米 纤维取向方向的样条两端粘附电极(电极材料为导电铜片,粘合剂为导电银浆,如附图 2b所示),制备传感器件P-IL/PVDF,并对所制得的传感器件进行应变传感性能和温度传 感性能测试,如附图3,4所示。
对照例2
将5g PVDF加入到溶剂DMF中,搅拌后得到PVDF质量分数为20%的均一PVDF溶液。然后将PVDF溶液置于10ml注射器(针头型号为18G)中,以0.05mm/min的注射速度, 在20KV高压条件下静电纺丝(注射器针头距离滚筒接收器的距离为20cm,滚筒转速为 40rpm,湿度为30%,温度为25℃),得到纳米纤维无规分布的多孔纤维膜,纤维膜的形 貌结构如附图7所示。然后将该纤维膜置于10g 1-丁基-3-甲基咪唑双三氟甲磺酰亚胺 盐溶液中25℃下120W,40KHz超声30min,然后在真空烘箱中50℃干燥18h,获得复 合纳米纤维膜。在该纤维膜的样条两端粘附电极(电极材料为导电铜片,粘合剂为导电银 浆),制备传感器件R-IL/PVDF,并对所制得的传感器件进行应变传感性能和温度传感性 能测试,如附图3,4所示。
对照例3
将5g TPU加入到混合溶剂DMF/THF中,搅拌后得到TPU质量分数为25%的均一TPU溶液。然后将3g 1-己基-3-甲基咪唑双三氟甲磺酰亚胺盐加入到TPU溶液中,机械搅拌 均匀后得到混合溶液。将上述混合溶液置于10ml注射器(针头型号为20G)中,以0.02 mm/min的注射速度,在25KV高压条件下静电纺丝(注射器针头距离滚筒接收器的距离 为15cm,滚筒转速为2800rpm,湿度为25%,温度为23℃),得到纳米纤维取向分布的 纤维膜。在该纤维膜上沿着纳米纤维取向方向的样条两端粘附电极(电极材料为导电铜片, 粘合剂为导电银浆,如附图2b所示),制备传感器件P-IL/TPU,并对所制得的传感器件 进行应变传感性能和温度传感性能测试,如附图5,6所示。
对照例4
将5g TPU加入到混合溶剂DMF/THF中,搅拌后得到TPU质量分数为20%的均一TPU溶液。 然后将2.2g 1-己基-3-甲基咪唑双三氟甲磺酰亚胺盐加入到TPU溶液中,机械搅拌均匀后得 到混合溶液。将上述混合溶液置于10ml注射器(针头型号为20G)中,以0.15mm/min的注 射速度,在20KV高压条件下静电纺丝(注射器针头距离滚筒接收器的距离为20cm,滚筒转 速为40rpm,湿度为30%,温度为25℃),得到纳米纤维无规分布的纤维膜。在该纤维膜的 样条两端粘附电极(电极材料为导电铜片,粘合剂为导电银浆),制备传感器件R-IL/TPU,并 对所制得的传感器件进行应变传感性能和温度传感性能测试,如附图5,6所示。
对照例5
将5g TPU溶于DMF中,搅拌后得到TPU的均一溶液;将2.2g 1-己基-3-甲基咪唑 双三氟甲磺酰亚胺盐溶于DMF中,搅拌后得到均匀的IL溶液;将IL溶液加入到TPU溶液 中,机械搅拌均匀后得到混合溶液。然后将混合溶液静置1h;再将静置后的IL/TPU溶液 倒入模具中,60℃下挥发24h,得到IL/TPU导电薄膜,样条两端粘附电极(电极材料 为导电铜片,粘合剂为导电银浆),制备传感器件IL/TPU,并对所制得的传感器件进行应 变传感性能和温度传感性能测试,如附图5,6所示。
如图1所示,以高速转动的滚筒为纳米纤维接收器时,可以获得纳米纤维取向分布的 离子液体与柔性高分子的复合纤维膜。
如图3所示,在具有取向结构的纤维膜上裁制矩形样条,当沿着垂直于纳米纤维取向 方向的样条两端粘附电极并制备传感器件时,传感器件(V-IL/PVDF)的应变灵敏性要明显大于沿着纳米纤维取向方向的样条两端粘附电极所制备得传感器件(P-IL/PVDF,对照例1),也大于在无规的纤维膜上裁制矩形样条所制备的传感器件(R-IL/PVDF对照例2)。
如图4所示,相对于对照例1,2,实施例1沿着垂直于纳米纤维取向方向的样条两端粘附电极所制备传感器件(V-IL/PVDF)的温度传感的灵敏性最高。
如图5所示,在具有取向结构的纤维膜上裁制矩形样条,当沿着垂直于纳米纤维取向 方向的样条两端粘附电极并制备传感器件时,传感器件(V-IL/TPU)的应变灵敏性和应变 响应范围要明显大于沿着纳米纤维取向方向的样条两端粘附电极所制备得传感器件
(P-IL/TPU,对照例3),也大于在无规的纤维膜上裁制矩形样条所制备的传感器件(R-IL/TPU对照例4)和非透气的IL/TPU传感器件(对照例5),如图5a所示。同时也 发现沿着垂直于纳米纤维取向方向的样条两端粘附电极所制备传感器件的应变传感行为 的重复性和稳定性也更好,如图5b所示。
如图6所示,相对于其他三种传感器件,实施例2沿着垂直于纳米纤维取向方向的样 条两端粘附电极所制备传感器件得温度传感的灵敏性最高。
如图7所示,以低速转动的滚筒为纳米纤维接收器时,获得纳米纤维无规分布的纤维 膜。
由测试结果分析可知:通过调控纳米纤维膜的形貌结构,制备具有取向结构的离子液 体与柔性高分子的纳米纤维膜,并在垂直于纳米纤维取向方向粘附电极制备的传感器件具 有最佳的应变传感性能和温度传感性能。
最后,需要注意的是,以上列举的仅是本发明的具体实施例。显然,本发明不限于以 上实施例,还可以有很多变形。本领域的普通技术人员能从本发明公开的内容中直接导出 或联想到的所有变形,均应认为是本发明的保护范围。
Claims (8)
1.一种基于取向纳米纤维的多功能可拉伸透气传感材料在应变温度传感器上的应用,其特征在于所述基于取向纳米纤维的多功能可拉伸透气传感材料采用以下方法制备得到:
步骤(1):将柔性高分子基体加入到有机溶剂中,搅拌后得到均一的高分子溶液;
步骤(2):上述高分子溶液利用静电纺丝纺成具有取向结构的纳米纤维膜;所述静电纺丝采用滚筒作为收集装置,滚筒的转速为2500-3000 rpm;
步骤(3):将具有取向结构的纳米纤维膜在导电离子液体中超声,然后在真空烘箱中干燥,获得复合纳米纤维膜;
步骤(4):将干燥好的复合纳米纤维膜裁剪成矩形样条,在纤维膜上沿着垂直于纳米纤维取向方向的两端粘附电极即可。
2.根据权利要求1所述的应用,其特征在于步骤(3)所述超声时间为30-100 min,超声温度为18-35 °C,超声功率为120 W,频率为40 KHz。
3.根据权利要求1所述的应用,其特征在于步骤(3)所述真空烘箱的温度为30-70 °C,时间为12-24 h。
4.根据权利要求1所述的应用,其特征在于所述柔性高分子基体为聚偏氟乙烯PVDF、聚氨酯类热塑性弹性体TPU、苯乙烯类热塑性弹性体、聚烯烃类热塑性弹性体、聚酯类热塑性弹性体中的一种或多种。
5.根据权利要求1所述的应用,其特征在于所述高分子溶液的浓度为15-30 wt%。
6.根据权利要求1所述的应用,其特征在于所述静电纺丝注射速度为0.01-1mm/min。
7.根据权利要求1所述的应用,其特征在于所述静电纺丝的电压为15-25 KV,针头距离收集装置间的间距为10-20 cm,温度在18-35 °C,其环境湿度在30%以下。
8.根据权利要求1所述的应用,其特征在于所述导电离子液体为1-乙基-3-甲基咪唑四氟硼酸盐、N-甲基甲氧基乙基吡咯烷双三氟甲磺酰亚胺盐、1-乙基-3-甲基咪唑双氟磺酰亚胺盐、N-甲基丙基哌啶双三氟甲磺酰亚胺盐、1-乙基-3-甲基咪唑双三氟甲磺酰亚胺盐、1-丁基-3-甲基咪唑双三氟甲磺酰亚胺盐和1-己基-3-甲基咪唑双三氟甲磺酰亚胺盐中的一种或多种。
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