CN116176074A - 一种用于监测压电的复合膜 - Google Patents

一种用于监测压电的复合膜 Download PDF

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CN116176074A
CN116176074A CN202211613962.5A CN202211613962A CN116176074A CN 116176074 A CN116176074 A CN 116176074A CN 202211613962 A CN202211613962 A CN 202211613962A CN 116176074 A CN116176074 A CN 116176074A
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composite
monitoring
nanofiber
piezoelectricity
layer
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刘宇清
刘通
杨旭红
杨婷
万成伟
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Suzhou University
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Abstract

本发明属于功能复合纳米纤维膜技术领域，具体涉及一种用于监测压电的复合膜。该多层复合功能膜包含对喷混合静电纺单元膜，经磁控溅射金属颗粒与丝蛋白纳米纤维膜连接。复合体中具有固体电解质薄膜，上层结构体具有三维杂乱结构、高比面积和孔隙率，下层结构体具有一定的生物相容性和生物力学强度。本发明将丝蛋白纳米纤维膜置于底部，进行磁控溅射沉积，选用材料极性相似，层状之间有较高的亲和力，使得整个膜层与层之间连接紧密，既能保证连接牢固度，又不会对复合体功能性造成影响。本发明结构设计合理，能够实现单电极压电对人体行为变化的监测，制备出具有稳定性好，热尺寸收缩率小，拉伸强度大的复合纳米纤维膜。

Description

一种用于监测压电的复合膜
技术领域
本发明属于功能复合纳米纤维膜技术领域，具体涉及一种用于监测压电的复合膜。
背景技术
智能化纺织材料是近年来备受关注的复合材料之一，可穿戴智能纺织品具有良好的便携性，功耗低等优势进而极大的提高了工作效率，具有巨大的发展前景，目前被广泛应用于以收集血压、心电和血氧饱和等各种生理指标。目前以新型柔性智能纺织品如织物键盘，以及柔性薄膜电子材料对功能性复合膜提出了应用的迫切需求，柔性智能材料以静电纺为载体，构成透气、可拉伸、传递电信号的一体化结构。利用高分子纳米纤维，例如聚乳酸、聚酰亚胺、聚偏氟乙烯、聚氨酯等本身就具有抗菌、隔热、防水等优势，其次高分子纳米纤维是一种极好的载体，能够将纳米材料附着在表面。
对喷压电一体化多层膜的结构以导电、透气、生物力学强度为重要参数指标之一，对于单层静电纺纤维膜很难达到上述效果，专利申请号为CN202110216388.9对纳米纤维膜采用喷胶复合，实现上下层的连接，但采用喷胶连接使得复合体存在不透气、亲肤性差的问题。
专利申请号为CN201510505147.0实现了具有某些功能性的纳米纤维复合面料的制备，通过纺出纳米纤维，堆积成为无纺布，在经过材料复合之后通过压光处理获得纳米纤维无纺布底膜，但导致利用现有纳米纤维与基底的复合工艺可能会导致功能性纳米纤维层不能太薄、功能性纳米纤维层与基底的复合强度不够。
专利申请号为CN202210078721.9：将共聚物纳米纤维悬浮液均匀喷涂于基材表面，干燥后，得到纳米纤维膜；将所得纳米纤维膜经等离子体处理。通过对的纳米纤维膜进行改性处理，使丙烯酸均匀结合在纳米纤维膜表面，经活化镀铜处理，所得柔性导电膜，但在镀铜会产生不均匀、导电性差、镀层容易脱落等问题。
申请专利号CN202210646057.3温敏胶将三层不同的纤维层平铺叠合在一起，利用离子-电子界面的双电层效应和微凸起结构双重增敏，达到了信息传递的功能，在使用过程中会产生一定的电压差，只将金属粒子磁控溅射沉积在微凸起结构上，但在使用过程中导电粒子位置发生改变，灵敏度下降。
专利申请号CN202210891010.3通过接收辊转动，第一静电纺丝注射器和第二静电纺丝注射器进行纺丝，实现不同材料的同时纺丝，得到了与隔膜一体化的材料，但喷射一定厚度后会导致电子传输效率下降。
发明内容
基于现有技术中电子传输效率低，不均匀、导电性差、镀层容易脱落和纤维层不能太薄、功能性纳米纤维层与基底的复合强度不够等问题，本发明意图使用磁控溅射沉积将混合纳米纤维膜表面形成一层浅浅的金属银粒子膜，增强了原混纺纳米纤维膜的导电能力。
为了解决上述技术问题，本发明提供了一种用于监测压电的复合膜，包括混合静电纺纳米纤维层和丝蛋白纳米纤维层；所述丝蛋白纳米纤维层通过热粘合的方法贴合于所述混合静电纺纳米纤维层的表面；
所述混合静电纺纳米纤维层包括如下制备步骤：
S1：将纺丝液A喷射于接收辊上面，得到纤维层；
S2：于所述纤维层的表面喷射纺丝液B，得到复合纤维层；其中，纤维层和复合纤维层的厚度比为1-3：4；
S3：于所述复合纤维层的表面通过磁控溅射的方法沉积纳米银膜，得到复合静电纺循环单元薄膜；
S4：重复步骤S1-S3，得到所述混合静电纺纳米纤维层；
所述纺丝液A的溶质为PAN和PU，所述纺丝液B的溶质为PVDF。
优选的，所述纤维层为15-40μm。
优选的，所述纺丝液B中，PVDF的浓度为12-20wt％。
优选的，所述纺丝液A中，PAN和PU的浓度均为12-20wt％。
优选的，所述步骤S4中，重复步骤S1-S3的次数为1-10次。
优选的，所述磁控溅射采用体积比为1-2：1-3的Ar和N2的混合气氛。
优选的，所述丝蛋白纳米纤维层由浓度为14-20wt％的再生蚕丝蛋白溶液通过静电纺丝得到。
优选的，所述接收辊的转速为10-200r/min。
优选的，所述纳米银膜的厚度为30-500nm。
优选的，所述步骤S1中，纺丝液A的纺丝条件为：纺丝电压12-18kV，进射速率为0.7-1.5mL/h，距离为10-15cm。
优选的，所述步骤S2中，纺丝液B的纺丝条件为：纺丝电压为13-17kV，进射速率为0.5-1.2mL/h，距离为12-17cm。
优选的，所述纳米银与混合静电纺纳米纤维层的厚度比为3-5：100。
优选的，所述磁控溅射的工作混合气压为1-3Pa、功率10-20W。
优选的，所述步骤S4中，热粘合的温度为60-180℃，压力为20-150MPa。
本发明制备得到的用于监测压电的复合膜能够实现单电极压电对人体行为变化的监测，同时具备透气、可拉伸的效果。
本发明的技术方案相比现有技术具有以下优点：
1.本发明采用对喷静电纺将两种不同溶液混合为纳米纤维膜利用原料之间的协同增效，使聚合物纺丝溶液保持良好的粘度，将三种不同的物质均质化应用到一层纳米纤维膜，赋予一层纳米纤维膜不同的功能，磁控溅射沉积将混合纳米纤维膜表面形成一层浅浅的金属银粒子膜，增强了原混纺纳米纤维膜的导电能力，对电信号的变化更加敏感，利用压电产生电压差，对人体行为进行监测。通过热粘合将混纺纳米纤维膜与丝蛋白纳米纤维膜连接，利用丝蛋白的生物相容性，将丝蛋白纳米纤维与人体皮肤表面直接接触，从而形成一个多层的混合纳米纤维膜，纳米纤维膜具有三维杂乱结构和较大的孔隙率，透气透湿能力较好。通过热粘合将复合纳米纤维膜连为一体，增强了纤维之间的抱合力，提高整体稳定性，延长使用寿命。
2.底部采用蚕丝蛋白材料作为基底，蚕丝蛋白材料本身就具有较高的透气性和抗汗湿性能，结合纤维结构的高透气性，相比于仅具有纤维结构的压力传感器，本发明的传感器具有更高的透气性，具备更好的柔性，采用磁控溅射沉积，丝蛋白膜的表面粒子分散和负载效果更好。
3.发明采用多层纳米纤维膜结构有效提高结构体的耐用能力，同时，不同功能结构有效扩大了其使用范围。增加连接牢固度，得到的复合膜在纺制过程中均匀混合，规律排列，两侧PAN，PU复合结构纤维膜对中间的PVDF膜起到支撑和连接作用。在经过热处理之后PVDF有部分熔融，与两面的复合膜出现黏结现象，纤维膜整体变得更加质密，更适合应用于电子传输，协同增效，能够实现单电极压电对人体运动变化产生的微小信号进行监测，同时具备可拉伸的效果。
4.利用PAN作为聚合物基体材料，PVDF在(PAN，PU)纳米纤维纺丝薄膜中均匀分布，PU对复合膜整体性进行保护，通过多层循环有效增加压电敏感性以及压电电压，有效增加了复合膜的使用厚度，从而适应不同的使用环境。
附图说明
图1为对喷静电纺丝的流程示意图。
图2为用于监测压电的复合膜的循环结构示意图。
图3为用于监测压电的复合膜与丝蛋白结合结构示意图。
图4为用于检测压电的复合膜的结构图。
图5为用于检测压电的纳米纤维形态示意图。
图6为磁控溅射银粒子示意图。
附图标记说明：1-接收辊，2-第一注射泵，3-第二注射泵，4-第一高压发生器，5-第二高压发生器，6-混合纤维复合层，601-PAN、PU纳米纤维层，602-PVDF纳米纤维层，603-纳米银膜，7-丝蛋白纳米纤维层，8-复合膜。
具体实施方式
下面结合附图和具体实施例对本发明作进一步说明，以使本领域的技术人员可以更好地理解本发明并能予以实施，但所举实施例不作为对本发明的限定。
根据标准GB/T5453-1997《纺织品织物透气性的测试》对纳米纤维膜的透气性能进行测试。对压电材料施外力，利用静电计采集获得被测压电薄膜的电压信号大小，示波器所采集电压波形图。从Instron测试上述固化样品的剪粘合强度，十字头速度为5mm/分钟，重复测试三次。利用拉伸强度试验机进行拉伸性能测试，选用5KN传感器，夹头间距为100mm，拉伸速度为100mm/min，检测断裂强力。
实施例1
(1)将PVDF溶解于DMF溶剂中，在配制好的溶液中加入磁石，然后在室温下磁力搅拌14h，直至完全溶解得到质量分数为12％的纺丝液B；
同时，将PAN和PU溶解于DMF溶剂中，在配制好的溶液中加入磁石，然后在室温下磁力搅拌12h，直至完全溶解得到包括12wt％PAN溶液和18wt％PU溶液的纺丝液A。
将纺丝液A置于第一注射泵2中，纺丝液B置于第二注射泵3中，置于接收轮两侧；其中纺丝液A的第一高压发生器5纺丝电压为14kV，进射速率为1mL/h，距离为10cm，喷涂纺丝液B的第二高压发生器4纺丝电压为17kV，进射速率为0.9mL/h，距离为12cm；设置接收辊1转速为100r/min，纤维层和复合纤维层的厚度比为2：4；将纺丝液A喷射于接收辊上面，得到纤维层；于所述纤维层的表面喷射纺丝液B，得到复合纤维层。
(2)将纳米银于100mL/min的Ar/N2(所述Ar与N2的流量比为2:3)的混合气氛中，调节混合气压为2Pa，使用功率为10W的直流电源，对频电源，开启电源使靶材起辉，将银颗粒镀到复合膜上层，得到混合膜。将上述步骤(1)到(3)循环10次。
(4)制备质量分数为17％的再生蚕丝蛋白溶液，设置喷丝器转速2500rpm，电压7kV，输网帘转速45rpm，得到丝蛋白纳米纤维层7，以混合静电纺纳米纤维层6沉积有纳米银膜603的所在面为接收面，加入TPU纳米颗粒粘结剂进行多层热粘合，热处理的温度为70℃，压力为120MPa。
通过合成用于监测压电的复合膜，测得该复合膜的粘合强度为11.25MPa，拉伸强度为43.5MPa，电压差为10.6v，透气性能为31.97mm/s。
实施例2
(1)将PVDF溶解于DMF溶剂中，在配制好的溶液中加入磁石，然后在室温下磁力搅拌14h，直至完全溶解得到质量分数为12％的纺丝液B；
同时，将PAN和PU溶解于DMF溶剂中，在配制好的溶液中加入磁石，然后在室温下磁力搅拌10h，直至完全溶解得到包括10wt％PAN溶液和18wt％PU溶液的纺丝液A。
(2)其中纺丝液B的纺丝电压为15kV，进射速率为0.8mL/h，距离为13cm；纺丝液A的纺丝电压为13kV，进射速率为1.2mL/h，距离为10cm，纤维层和复合纤维层的厚度比为3：4，设置接收辊转速为100r/min，将纺丝液A喷射于接收辊上面，得到纤维层；于所述纤维层的表面喷射纺丝液B，得到复合纤维层。
(3)将纳米银于100mL/min的Ar/N2(所述Ar与N2的流量比为2:3)的混合气氛中，调节混合气压为2.5Pa，使用功率为20W的直流电源，对频电源，开启电源使靶材起辉，将银颗粒镀到复合膜上层，得到混合膜。将上述步骤(1)到(3)循环5次。
(4)制备质量分数为17％的再生蚕丝蛋白溶液，设置喷丝器转速2700rpm，电压7kV，输网帘转速50rpm，得到丝蛋白纳米纤维层7，以混合静电纺纳米纤维层6沉积有纳米银膜603的所在面为接收面，加入TPU纳米颗粒粘结剂进行多层热粘合，热处理的温度为80℃，热粘合的压力为150MPa。
通过合成用于监测压电的复合膜，测得该复合膜的粘合强度为10.06MPa，拉伸强度为37MPa，电压差为8.8v，透气性能为23.47mm/s。
实施例3
(1)将PVDF溶解于DMF溶剂中，在配制好的溶液中加入磁石，然后在室温下磁力搅拌12h，直至完全溶解得到质量分数为12％的纺丝液B；
同时，将PAN和PU溶解于DMF溶剂中，在配制好的溶液中加入磁石，然后在室温下磁力搅拌12h，直至完全溶解得到包括10wt％PAN溶液和18wt％PU溶液的纺丝液A。
(2)其中纺丝液B的纺丝电压为15kV，进射速率为0.9mL/h，距离为12cm；纺丝液A的纺丝电压为14kV，进射速率为0.9mL/h，距离为10cm，纤维层和复合纤维层的厚度比为1：4，设置接收辊转速为200r/min，将纺丝液A喷射于接收辊上面，得到纤维层；于所述纤维层的表面喷射纺丝液B，得到复合纤维层。
(3)将纳米银于100mL/min的Ar/N2(所述Ar与N2的流量比为1:1)的混合气氛中，调节混合气压为3Pa，使用功率为10W的直流电源，对频电源，开启电源使靶材起辉，将银颗粒镀到复合膜上层，得到混合膜。将上述步骤(1)到(3)循环5次。
(4)制备质量分数为17％的再生蚕丝蛋白溶液，设置喷丝器转速2700rpm，电压7kV，输网帘转速45rpm，得到丝蛋白纳米纤维层7，以混合静电纺纳米纤维层6沉积有纳米银膜603的所在面为接收面，加入TPU纳米颗粒粘结剂进行多层热粘合，热处理的温度为110℃，热粘合的压力为100MPa。
通过合成用于监测压电的复合膜，测得该复合膜的粘合强度为10.06MPa，拉伸强度为31.7MPa，电压差为9.2v，透气性能为21.54mm/s。
实施例4
(1)将PVDF溶解于DMF溶剂中，在配制好的溶液中加入磁石，然后在室温下磁力搅拌12h，直至完全溶解得到质量分数为10％的纺丝液B；
同时，将PAN和PU溶解于DMF溶剂中，在配制好的溶液中加入磁石，然后在室温下磁力搅拌12h，直至完全溶解得到包括10wt％PAN溶液和10wt％PU溶液的纺丝液A。
(2)其中纺丝液B的纺丝电压为13kV，进射速率为0.5mL/h，距离为12cm；纺丝液A的纺丝电压为12kV，进射速率为0.7mL/h，距离为10cm，纤维层和复合纤维层的厚度比为2：4，设置接收辊转速为100r/min，将纺丝液A喷射于接收辊上面，得到纤维层；于所述纤维层的表面喷射纺丝液B，得到复合纤维层。
(3)将纳米银于100mL/min的Ar/N2(所述Ar与N2的流量比为2:3)的混合气氛中，调节混合气压为2Pa，使用功率为20W的直流电源，对频电源，开启电源使靶材起辉，将银颗粒镀到复合膜上层，得到混合膜。将上述步骤(1)到(3)循环10次。
(4)制备质量分数为17％的再生蚕丝蛋白溶液，设置喷丝器转速2700rpm，电压7kV，输网帘转速45rpm，得到丝蛋白纳米纤维层7，以混合静电纺纳米纤维层6沉积有纳米银膜603的所在面为接收面，加入TPU纳米颗粒粘结剂进行多层热粘合，热处理的温度为60℃，热粘合的压力为110MPa。
通过合成用于监测压电的复合膜，测得该复合膜的粘合强度为9.76MPa，拉伸强度为32.5MPa，电压差为10.2v，透气性能为29.96mm/s。
实施例5
(1)将PVDF溶解于DMF溶剂中，在配制好的溶液中加入磁石，然后在室温下磁力搅拌12h，直至完全溶解得到质量分数为20％的纺丝液B；
同时，将PAN和PU溶解于DMF溶剂中，在配制好的溶液中加入磁石，然后在室温下磁力搅拌12h，直至完全溶解得到包括20wt％PAN溶液和20wt％PU溶液的纺丝液A。
(2)其中纺丝液B的纺丝电压为17kV，进射速率为1.2mL/h，距离为17cm；纺丝液A的纺丝电压为18kV，进射速率为1.5mL/h，距离为15cm，设置接收辊转速为50r/min，纤维层和复合纤维层的厚度比为3：4，将纺丝液A喷射于接收辊上面，得到纤维层；于所述纤维层的表面喷射纺丝液B，得到复合纤维层。
(3)将纳米银于100mL/min的Ar/N2(所述Ar与N2的流量比为3:1)的混合气氛中，调节混合气压为1.5Pa，使用功率为15W的直流电源，对频电源，开启电源使靶材起辉，将银颗粒镀到复合膜上层，得到混合膜。将上述步骤(1)到(3)循环10次。
(4)制备质量分数为17％的再生蚕丝蛋白溶液，设置喷丝器转速2700rpm，电压7kV，输网帘转速45rpm，得到丝蛋白纳米纤维层9，以混合静电纺纳米纤维层6沉积有纳米银膜603的所在面为接收面，加入TPU纳米颗粒粘结剂进行多层热粘合，热处理的温度为180℃，热粘合的压力为130MPa。
通过合成用于监测压电的复合膜，测得该复合膜的粘合强度为10.76MPa，拉伸强度为39.6MPa，电压差为8.3v，透气性能为19.57mm/s。
对比例1
与实施例1相比改变纺丝电压8kV，热粘合温度，将制得的对喷混纺纳米纤维膜在230℃下进行热压，其余条件不变。
纺纱电压下降，纳米纤维成膜性较差，通过提高温度热压，将纳米纤维发生膜质化，造成纤维之间抱合力下降，结构变化，造成压差改变，纺丝电压减小，纳米纤维膜无序性增强，影响纤维整体导电率，测得该复合膜的粘合强度为10.11MPa，拉伸强度为28.5MPa，电压差为4.5V，透气性能为27.63mm/s。
对比例2
与实施例1相比，改变接收辊速度与溶液浓度，提高接收辊速度为500r/min，在纺膜时物质间混合更加均匀，设定25wt％PAN溶液和25wt％PU的溶液A的浓度，增加纺膜时的物质接触，制成三维多孔纳米纤维膜，其余条件不变。
PAN，PU在过程中比例有所改变，成模性变差，测得该复合膜的粘合强度为6.23MPa，拉伸强度为22.4MPa，电压差为4.7V，透气性率为16.45mm/s。
对比例3
将实施例1中纺丝液A和纺丝液B混合，通过流延成膜法在玻璃板上自然干燥3-5天成膜，得到具有一定力学强度的复合膜。
该复合膜中各物质无序排列，孔隙率减少，压电信号不明显。测得该复合膜的粘合强度为4.58MPa，拉伸强度11.8MPa，电压差为2.1V，透气性率为8.46mm/s。
效果评价1
为验证本发明所得的技术效果，分别对实施例1、实施例2、实施例3、对比例1和对比例2所得复合膜进行测试，具体结果如表1所示：
表1各实施例与对比例的性能测试表
Figure BDA0004001353250000081
本发明采用对喷静电纺将两种不同溶液混合为纳米纤维膜利用原料之间的协同增效，使聚合物纺丝溶液保持良好的粘度，将三种不同的物质均质化应用到一层纳米纤维膜，赋予一层纳米纤维膜不同的功能，磁控溅射沉积将混合纳米纤维膜表面形成一层浅浅的金属银粒子膜，增强了原混纺纳米纤维膜的导电能力，对电信号的变化更加敏感，利用压电产生电压差，对人体行为进行监测。通过热粘合将混纺纳米纤维膜与丝蛋白纳米纤维膜连接，利用丝蛋白的生物相容性，将丝蛋白纳米纤维与人体皮肤表面直接接触，从而形成一个多层的混合纳米纤维膜，纳米纤维膜具有三维杂乱结构和较大的孔隙率，透气透湿能力较好。通过热粘合将复合纳米纤维膜连为一体，增强了纤维之间的抱合力，提高整体稳定性，延长使用寿命。
显然，上述实施例仅仅是为清楚地说明所作的举例，并非对实施方式的限定。对于所属领域的普通技术人员来说，在上述说明的基础上还可以做出其它不同形式变化或变动。这里无需也无法对所有的实施方式予以穷举。而由此所引申出的显而易见的变化或变动仍处于本发明创造的保护范围之中。

Claims (10)

1.一种用于监测压电的复合膜，其特征在于，包括混合静电纺纳米纤维层和丝蛋白纳米纤维层；所述丝蛋白纳米纤维层通过热粘合的方法贴合于所述混合静电纺纳米纤维层的表面；
所述混合静电纺纳米纤维层包括如下制备步骤：
S1：将纺丝液A喷射于接收辊上面，得到纤维层；
S2：于所述纤维层的表面喷射纺丝液B，得到复合纤维层；其中，纤维层和复合纤维层的厚度比为1-3：4；
S3：于所述复合纤维层的表面通过磁控溅射的方法沉积纳米银膜，得到复合静电纺循环单元薄膜；
S4：重复步骤S1-S3，得到所述混合静电纺纳米纤维层；
所述纺丝液A的溶质为PAN和PU，所述纺丝液B的溶质为PVDF。
2.如权利要求1所述的用于监测压电的复合膜，其特征在于，所述步骤S4中，重复步骤S1-S3的次数为1-10次。
3.如权利要求1所述的用于监测压电的复合膜，其特征在于，所述纳米银膜与混合静电纺纳米纤维层的厚度比为3-5：100。
4.如权利要求1所述的用于监测压电的复合膜，其特征在于，所述磁控溅射采用体积比为1-2：1-3的Ar和N2的混合气氛。
5.如权利要求1所述的用于监测压电的复合膜，其特征在于，所述磁控溅射的工作混合气压为1-3Pa，功率10-20W。
6.如权利要求1所述的用于监测压电的复合膜，其特征在于，所述纳米银膜的厚度为30-500nm。
7.如权利要求1所述的用于监测压电的复合膜，其特征在于，所述丝蛋白纳米纤维层由浓度为14-20wt％的再生蚕丝蛋白溶液通过静电纺丝得到。
8.如权利要求1所述的用于监测压电的复合膜，其特征在于，所述纺丝液B中PVDF的浓度为12-20wt％，所述纺丝液A中PAN和PU的浓度均为12-20wt％。
9.如权利要求1所述的用于监测压电的复合膜，其特征在于，所述热粘合的温度为60-180℃。
10.如权利要求1所述的用于监测压电的复合膜，其特征在于，所述热粘合的压力为20-150MPa。
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