CN114001637B - 双模芯鞘结构弹性应力发光导电应变传感器的制备方法 - Google Patents
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Abstract
本发明公开了一种双模芯鞘结构弹性应力发光导电应变传感器的制备方法：将纳米导电颗粒与高分子材料混合，机械搅拌后超声，使导电粒子充分分散在高分子材料基体中，并除去混合物中的气泡；用注射器以恒定的速度将混合物注射到氯化钙溶液中，得到导电纤维；将应力发光粉ZnS:Mn2+与PDMS混合，机械搅拌后超声分散，然后将所得混合物注入到含有导电纤维的模具中并固化。双模纤维的结构是利用固化好的导电纤维穿入到模具中注入应力发光高分子混合物再次固化实现的芯鞘结构。该双模导电应力发光纤维基于应力发光材料应用在应力传感器上，在人工智能的应力检测、人造皮肤、可穿戴产品等各个领域具有非常广泛的应用前景。
Description
技术领域
本发明涉及一种芯鞘结构导电弹性应力发光传感器及其制备方法，属于智能可穿戴技术领域。
背景技术
用于测量物体受力变形所产生的应变大小的传感器被称为应变传感器，传统应变传感器分为电阻式应力传感器和电容式应力传感器，应变是一个在各个领域中经常用到的物理量，在结构设计、地质勘探和航空航天等领域都需要对应变进行测量并实时检测，在智能穿戴领域也有广泛的应用包括健康监测和运动的检测等。未来的应变传感器的研究将会在传感器的多信号的鉴定与分离、高稳定低延迟以及多功能性方面展开，从而提升和优化应变传感器的性能，实现在智能穿戴领域多功能的应用。对于传统应变传感器的改善，研究者们进行了传感器制备方法的探究，通过选材，结构设计，性能优化等，如微加工技术、薄膜技术和厚膜技术以及对传感器机制的探究。陈建文等利用PDMS结合碳纳米管制备了具有良好透明度和传感范围的超薄导电碳纳米管层的透明应变传感器[Composites Science andTechnology,2020,186:107938]；Singh等通过研究应变对原始石墨烯和掺杂石墨烯的电子特性的影响制备了超灵敏的高性能应变传感器[ACS Applied Electronic Materials,2020,2(2):523]。传统的应变传感器虽然得到了广泛的应用，但也存在着其固有的局限性，如扩展性差，单模式传感等。随着基于聚合物纳米复合材料的发展，新型可拉伸双模应变传感器有望解决以上限制。
发明内容
本发明所要解决的技术问题是：提供一种同时具有非接触式光学测量和接触式传感器测量的双模芯鞘结构弹性应力发光导电应变传感器及其制备方法，该材料弹性应力发光强度高，制备工艺简单，成本低廉，可对不同形式的机械力信号如压缩、拉伸、碰撞、摩擦等即时响应，既可以产生肉眼可见的光信号又可以提供电阻变化产生的电流信号来反映产生的应力及应变的大小。
为了解决上述技术问题，本发明提供了一种双模芯鞘结构弹性应力发光导电应变传感器的制备方法，包括以下步骤：
步骤1)：将纳米导电颗粒与高分子材料混合，机械搅拌后超声，使导电粒子充分分散在高分子材料基体中，并除去混合物中的气泡；用注射器以恒定的速度将混合物注射到氯化钙溶液中，得到导电纤维；
步骤2)：将应力发光粉ZnS:Mn2+与PDMS混合，机械搅拌后超声分散，然后将所得混合物注入到含有步骤1)所得导电纤维的模具中并固化，即得双模芯鞘结构弹性应力发光导电应变传感器。
优选地，所述步骤1)中纳米导电颗粒与高分子材料的质量比为1:19-4:6；氯化钙溶液的质量浓度为10％-40％。
优选地，所述步骤1)中的纳米导电颗粒采用石墨粉、石墨烯、碳纳米管、导电有机物，或者石墨烯与碳纳米管的混合物；高分子材料采用海藻酸钠、聚二甲基硅氧烷、聚氨酯或橡胶。
更优选地，所述的导电有机物为聚苯胺或聚吡咯。
优选地，所述步骤1)中机械搅拌的时间为20-30分钟，超声的时间为1-2 小时。
优选地，所述步骤2中)的应力发光粉ZnS:Mn2+采用固相反应法合成；应力发光粉ZnS:Mn2+与PDMS的体积比为0.5:1-1:1。
更优选地，所述应力发光粉ZnS:Mn2+的制备方法为：将硫化锌、碳酸锰按混合，用酒精湿磨均匀，然后在氮气的氛围下在管式炉中加热反应，反应结束后随炉降温并研磨均匀即可。
进一步地，所述硫化锌、碳酸锰的质量比为1:0.001-1:0.05；加热反应的工艺参数为：以10℃的升温速率升温至900℃-1100℃，然后反应5-6小时。
优选地，所述步骤2中)固化的温度为60℃-90℃，时间为2小时。
本发明中的芯鞘结构中具有高度柔性和可拉伸性能的应力发光导电纤维可以在应力的作用下直接将机械能转换成光能，其发光的强度可以通过发光粉的含量以及应力的施加方式进行调节，纤维所发光的颜色也可以通过使用不同种类的发光粉及其混合物进行调节。而且由于纤维独特的一维结构，应力发光纤维可以很容易编织成为可穿戴的应力发光织物。
测量应变有很多方法，如非接触式光学测量法和接触式传感器测量法。本发明中采用芯鞘结构的双模芯鞘结构弹性应力发光导电应变传感器外层采用的应力发光纤维结构可以实现非接触式光学测量，而内部芯层结构则是纳米导电纤维结构可以实现接触式传感器的方法测量应变。当传感器被粘贴于被测点表面时，随着结构变形，贴附点产生的应变就会由于压阻效应使导电纤维电阻发生变化，产生电信号并由引出线输出。转换并反馈成应变信号，进一步就可以检测应变的大小。这种结构可以有效的解决传统应变传感器单模式传感以及扩产性差的问题。
与现有技术相比，本发明的技术效果是：
内层将导电的纳米颗粒与高分子基体混合制成纳米颗粒/高分子复合纤维控制导电纳米填料含量在导电渗透阈值之上，致使导电纳米填料间相互连接，形成宏观导电网络，应变发生后纤维的电阻值发生变化实现接触式传感器测量。外层应力发光粉与高分子基体混合制成应力发光粉/高分子复合壳层，应变发生后内部发光粉由于受力而发光，而且发光强度会随形变量大小而不同从而实现非接触式光学测量。这种芯鞘结构能够同时具有非接触式光学测量和接触式传感器测量的双模特性，而且具有良好的可重复性。
附图说明
图1为双模芯鞘结构弹性应力发光导电应变传感器结构图；
图2为各锰离子浓度合成的应力发光粉的XRD图谱；
图3为各锰离子浓度合成的应力发光粉的荧光光谱图；
图4为合成的锰离子浓度为0.5％应力发光粉的SEM图；
图5为纤维五厘米长度不同掺杂比的电阻值图；
图6为10％的石墨烯碳纳米管掺杂的纤维拉伸电阻变化曲线。
具体实施方式
为使本发明更明显易懂，兹以优选实施例，并配合附图作详细说明如下。
实施例1
制备导电纤维的纳米填料为石墨烯和碳纳米管的1：1混合物，将混合均匀的纳米填料以3:7的质量比与高分子基体海藻酸钠混合并搅拌均匀。然后把搅拌好的混合物进行超声3小时使填料均匀的混合到高分子基体中。
把得到的混合物加入到注射器中以湿法纺织的工艺将混合液以相同的速度注射到质量分数为30％的氯化钙溶液中完成固化形成交联网络结构，完成导电纤维的制备。
制备发光粉时采用硫化锌和碳酸锰为原料分别按照化学计量比1:0.1％； 1:0.3％；1:0.5％；1:1％；1:3％；1:5％混合均匀分别分组为S1-S6，把混合物转移到研钵中加入少量乙醇充分研磨20分钟，得到混合均匀的粉体。
把研磨均匀的粉体放入干燥箱中干燥2小时并再次充分研磨。然后把粉体转移到氧化铝坩埚中在氮气氛围下在管式炉中以10℃/min的速度加热到1050℃并保温6小时，随炉降温后得到发光粉。把粉体在玛瑙研钵中研磨30min得到高发光效率粒径均匀的应力发光粉。
将应力发光粉与PDMS以1：1的体积比混合均匀后进行超声分散3小时然后以PDMS:固化剂＝10:1的质量比加入固化剂并搅拌均匀。把加入固化剂的应力发光粉高分子基体的混合物注入到含有导电纤维的模具中，在80℃的真空干燥箱中3h完成固化。得到双模芯鞘结构弹性应力发光导电应变纤维，然后把纤维固定到织物或者是柔性板上得到双模芯鞘结构弹性应力发光导电应变传感器。
从图2可以看出S1-S6六组的XRD图谱均与标准硫化锌PDF卡片 PDF#75-1534衍射峰的位置一致，说明每个样品均形成规则的立方结构。Mn2+的离子的半径与Zn2+离子的半径接近，说明掺杂的离子占据Zn2+离子的格位，同时没有使晶格结构发生变化。
同时由图3的荧光光谱的纵向对比可以看出随着锰离子浓度的增大发光强度呈现出先增大后减小的趋势，只有比例为1:1％时亮度的极值呈现出忽然降低的现象，而掺杂比例为1:0.5％的S3的亮度峰值最大。由图3的荧光光谱的横向对比可以看出六组发光粉的激发光谱的波长基本上都分布在578nm附近，同时 S3、S4、S5三组在493附近也出现了较小的峰，整体都表现出橙色的光。
由图4的扫描电镜图片可以看出发光粉的粒径较小比表面积较大容易与 PDMS混合均匀实现高灵敏应力发光。
实施例2
制备导电纤维的纳米填料为石墨烯和碳纳米管的1：1混合物，将混合均匀的纳米填料分别以1:19；1:9；2:8；3:7；4:6的质量比与高分子基体海藻酸钠混合并搅拌均匀。然后把搅拌好的混合物进行超声2-3小时使填料均匀的混合到高分子基体中。
把得到的混合物加入到注射器中以湿法纺织的工艺将混合液以相同的速度注射到质量分数为30％的氯化钙溶液中完成固化形成交联网络结构，完成导电纤维的制备。
制备发光粉时采用硫化锌和碳酸锰为原料按照化学计量比1:0.5％混合均匀，把混合物转移到研钵中加入少量乙醇充分研磨20分钟，得到混合均匀的粉体。
把研磨均匀的粉体放入干燥箱中干燥2小时并再次充分研磨。然后把粉体转移到氧化铝坩埚中在氮气氛围下在管式炉中以10℃/min的速度加热到1050摄氏度并保温六小时，随炉降温后得到发光粉。把粉体在玛瑙研钵中研磨30min得到高发光效率粒径均匀的应力发光粉。
将应力发光粉与PDMS以1：1的体积比混合均匀后进行超声分散3小时然后以PDMS:固化剂＝10:1的质量比加入固化剂并搅拌均匀。把加入固化剂的应力发光粉高分子基体的混合物注入到含有导电纤维的模具中，在80℃的真空干燥箱中3h完成固化。得到双模芯鞘结构弹性应力发光导电应变纤维，然后把纤维固定到织物或者是柔性板上得到双模芯鞘结构弹性应力发光导电应变传感器。
从图5可以看出石墨烯与碳纳米管的不同的掺杂浓度会使导电纤维的电阻不同，随着石墨烯和碳纳米管含量的增加纤维的电阻在明显下降，碳纳米管的一维线性结构与石墨烯二维纳米结构相互连接共同构成了纤维的导电通路。而且当填料的含量超过30％时，纤维的电阻下降趋势没有之前下降得快，所以石墨烯与碳纳米管的含量在30％时较为适宜。图5的右上角为导电纤维作为导线点亮LED 灯珠的数码照片。
Claims (3)
1.一种双模芯鞘结构弹性应力发光导电应变传感器的制备方法，其特征在于，包括以下步骤：
步骤1)：将纳米导电颗粒与高分子材料混合，机械搅拌后超声，使导电粒子充分分散在高分子材料基体中，并除去混合物中的气泡；用注射器以恒定的速度将混合物注射到氯化钙溶液中，得到导电纤维；所述纳米导电颗粒与高分子材料的质量比为1:19-4:6；氯化钙溶液的质量浓度为10％-40％；所述的纳米导电颗粒采用石墨粉、石墨烯、碳纳米管、聚苯胺或聚吡咯，或者石墨烯与碳纳米管的混合物；高分子材料采用海藻酸钠、聚二甲基硅氧烷、聚氨酯或橡胶；
步骤2)：将应力发光粉ZnS:Mn2+与PDMS混合，机械搅拌后超声分散，然后将所得混合物注入到含有步骤1)所得导电纤维的模具中并固化，即得双模芯鞘结构弹性应力发光导电应变传感器；所述应力发光粉ZnS:Mn2+采用固相反应法合成；应力发光粉ZnS:Mn2+与PDMS的体积比为0.5:1-1:1；所述应力发光粉ZnS:Mn2+的制备方法为：将硫化锌、碳酸锰按混合，用酒精湿磨均匀，然后在氮气的氛围下在管式炉中加热反应，反应结束后随炉降温并研磨均匀即可；所述硫化锌、碳酸锰的质量比为1:0.001-1:0.05；加热反应的工艺参数为：以10℃的升温速率升温至900℃-1100℃，然后反应5-6小时。
2.如权利要求1所述的双模芯鞘结构弹性应力发光导电应变传感器的制备方法，其特征在于，所述步骤1)中机械搅拌的时间为20-30分钟，超声的时间为1-2小时。
3.如权利要求1所述的双模芯鞘结构弹性应力发光导电应变传感器的制备方法，其特征在于，所述步骤2中)固化的温度为60℃-90℃，时间为2小时。
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