CN115369647A - 一种多功能胶原纤维基柔性可穿戴传感材料的制备方法 - Google Patents
一种多功能胶原纤维基柔性可穿戴传感材料的制备方法 Download PDFInfo
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Abstract
本发明公开了一种多功能胶原纤维基柔性可穿戴传感材料的制备方法,首先,利用1H,1H,2H,2H‑全氟‑十二烷基三乙氧基硅烷、去离子水、氢氧化氨和乙醇对SiO2进行改性;采用导电聚合物单体和氧化剂对胶原纤维进行处理,再将含有乙酸乙酯、炭黑、改性SiO2、1H,1H,2H,2H‑全氟‑十二烷基三乙氧基硅烷、聚二甲基硅氧烷前驱体和固化剂的悬浮液喷涂到胶原纤维上;最后,将胶原纤维浸入到混合溶液中固化,即可。本发明制备的胶原纤维基柔性可穿戴传感材料,具有优异的机械性能、导电性、柔韧性、生物相容性、超双疏性、阻燃性、电磁屏蔽性能、光热转换性能和应变传感性能。
Description
技术领域
本发明属于高分子材料制备技术领域,具体涉及一种多功能胶原纤维基柔性可穿戴传感材料的制备方法。
背景技术
随着可穿戴电子设备的发展,柔性应变传感器已经引起了广泛的关注,因为它们通过将拉伸和压缩应变转变成电信号来捕捉姿势和监测各种人体活动,这使其适用于个性化健康监测、人机界面、软体机器人等方面。几十年来,具有各种转导机制的柔性应变传感器已被成功开发,包括压电、电容、压阻率等。其中,压阻式应变传感器因其结构设计简单、器件制备方便、数据易于可视化而被广泛探索。
一般来说,压阻式应变传感器通过将导电纳米材料分散在柔性聚合物基体中形成渗流网络。为了解决传感器在较宽的检测范围内可能出现的非线性响应以及导电通路的不可逆变化引起的大滞后行为,压阻式应变传感器的导电通路上的微观结构被设计出来。到目前为止,为了提高柔性应变传感器的灵敏度和响应范围,设计了各种微结构的柔性基材,包括纤维、皱纹、阵列、泡沫、纺织品、纸张、电纺薄膜等。虽然这种策略在提高性能方面被证明是有希望的,但复杂微纳米结构的构建不仅会使装置的制备复杂化,也会使实现大规模生产具有挑战性。此外,从实际应用效果来看,生物相容性、高灵敏度、高稳定性、高耐久性、低成本制造、佩戴舒适也是压阻式应变传感器工程面临的巨大挑战。因此,寻找一种更合适的基材来制备具有特殊内在微结构和显著应用性能的柔性应变传感器是非常重要的。
来自动物皮肤的胶原纤维拥有独特的三维网络结构和分层结构。除了能够避免微观结构的构建,其具有内在微观结构的胶原纤维,可以与人类皮肤极其匹配,在表面吸附导电和其他功能性纳米材料,以及在内部形成具有微观结构的导电通道。基于胶原纤维的柔性应变传感器的电阻会因为纤维的分离或压缩而发生变化,而渗流网络与胶原纤维之间可忽略的相对滑动可赋予传感器低滞后、快速响应和良好的稳定性。胶原纤维的同质分层结构将改善电子信号和传感器变形之间的线性关系。此外,经过鞣制后,预期的透气性、生物相容性、防腐和抗菌性能确保了基于胶原纤维的柔性应变传感器的佩戴舒适性和储存稳定性。上述优点使胶原纤维成为制备柔性可穿戴传感材料的合适基材。
发明内容
本发明的目的在于提供一种多功能胶原纤维基柔性可穿戴传感材料的制备方法,制备出的胶原纤维基传感材料具有良好的机械性能、导电性及生物相容性。
本发明所采用的技术方案是,一种多功能胶原纤维基柔性可穿戴传感材料的制备方法,首先利用1H,1H,2H,2H-全氟-十二烷基三乙氧基硅烷、去离子水、氢氧化氨和乙醇对SiO2进行改性,制备得到疏水性SiO2纳米颗粒;然后,采用导电聚合物单体溶液和氧化剂溶液对胶原纤维进行处理,再将含有乙酸乙酯、炭黑、疏水性SiO2纳米颗粒、1H,1H,2H,2H-全氟-十二烷基三乙氧基硅烷、聚二甲基硅氧烷前驱体和固化剂的悬浮液喷涂到胶原纤维上;最后,将胶原纤维浸入到含有乙酸乙酯、1H,1H,2H,2H-全氟-十二烷基三乙氧基硅烷、聚二甲基硅氧烷前驱体和固化剂的混合溶液中,固化后制备得到多功能胶原纤维基柔性可穿戴传感材料。
本发明的特点还在于,
具体按照以下步骤实施:
步骤1、制备疏水性SiO2纳米颗粒;
步骤2、制备多功能胶原纤维基柔性可穿戴传感材料,具体为:
步骤2.1,将0.1-5份的导电聚合物单体和1-20份的氧化剂分别溶解在100份的去离子水中,制备得到导电聚合物单体溶液和氧化剂溶液;
步骤2.2,将胶原纤维在室温下浸泡在导电聚合物单体溶液中并连续搅拌1h,之后在5℃下将胶原纤维在氧化剂溶液中浸泡0.1-6h,再用蒸馏水清洗胶原纤维并在室温下干燥;
步骤2.3,在100份的乙酸乙酯中加入0.05-1份的炭黑、0.1-10份的疏水性SiO2纳米颗粒、0.1-10份的1H,1H,2H,2H-全氟-十二烷基三乙氧基硅烷、0.1-10份的聚二甲基硅氧烷前驱体和0.01-1份的固化剂,室温下搅拌2h后得到混合悬浮液;
步骤2.4,将混合悬浮液通过喷枪喷涂到步骤2.2的胶原纤维上,并在60℃下固化0.01-1h;
步骤2.5,将0.1-10份的1H,1H,2H,2H-全氟-十二烷基三乙氧基硅烷、0.1-10份的聚二甲基硅氧烷前驱体和0.01-1份的固化剂加入100份的乙酸乙酯中,室温下搅拌1h后得到混合溶液;
步骤2.6,将步骤2.4中的胶原纤维浸泡在混合溶液中,浸泡时间为0.01-1h,之后在60℃下固化0.01-6h,得到多功能胶原纤维基柔性可穿戴传感材料。
步骤1中,具体为:
首先,将0.1-10份的1H,1H,2H,2H-全氟-十二烷基三乙氧基硅烷滴加到含有5.00-20.00份的去离子水、1-10份的氢氧化氨、0.1-10份的SiO2纳米颗粒和100份的乙醇的混合溶液中,在40℃下磁力搅拌24h,得到SiO2分散液;然后,以10000转每分钟对分散液进行离心处理10min,再用乙醇对沉淀物进行1-5次洗涤,最后,将离心沉淀物在60℃下真空干燥12h,得到疏水性SiO2纳米颗粒。
步骤2.1中,导电聚合物单体为聚吡咯、聚苯胺、聚吲哚和聚乙炔中的任意一种或多种。
步骤2.1中,氧化剂为非金属单质、含有变价元素的高价化合物中的任意一种或两种;非金属单质为F2、Cl2、O2、Br2、I2、S、Si中的任意一种;含有变价元素的高价化合物为KMnO4、KClO3、HNO3、MnO2、H2O2、FeCl3中的任意一种。
本发明的有益效果在于:
(1)本发明方法采用的胶原纤维基材来源于动物的皮,具有资源丰富、廉价易得、可再生和可生物降解等优点,可以替代部分合成纤维,而有效地节约化石资源和保护生态环境;
(2)本发明制备的多功能胶原纤维基柔性可穿戴传感材料,具有优异的机械性能、导电性、柔韧性、生物相容性、超双疏性、阻燃性、电磁屏蔽性能、光热转换性能和应变传感性能等,在智能服装、可穿戴电子设备、人机交互和人工智能等方面具有一定的应用前景;
(3)本发明的胶原纤维基柔性可穿戴传感材料,其制备工艺简单,操作流程简便,条件温和,有利于批量化生产。
附图说明
图1为实施例1制得的多功能胶原纤维基柔性可穿戴传感材料的外观图。
图2为实施例1制得的多功能胶原纤维基柔性可穿戴传感材料的扫描电子显微镜图(一);
图3为实施例1制得的多功能胶原纤维基柔性可穿戴传感材料的扫描电子显微镜图(二);
图4为实施例1制得的多功能胶原纤维基柔性可穿戴传感材料和不同种类液体的照片图;
图5为实施例1制得的多功能胶原纤维基柔性可穿戴传感材料在手指弯曲时的实时电阻变化图;
图6为实施例1制得的多功能胶原纤维基柔性可穿戴传感材料在人体跳跃、步行、慢跑和快跑时的实时电阻变化图。
具体实施方式
下面结合附图和具体实施方式对本发明进行详细说明。
本发明一种多功能胶原纤维基柔性可穿戴传感材料的制备方法,首先利用1H,1H,2H,2H-全氟-十二烷基三乙氧基硅烷、去离子水、氢氧化氨和乙醇对SiO2进行改性,制备得到疏水性SiO2纳米颗粒。然后,采用导电聚合物单体溶液和氧化剂溶液对胶原纤维进行处理,再将含有乙酸乙酯、炭黑、疏水性SiO2纳米颗粒、1H,1H,2H,2H-全氟-十二烷基三乙氧基硅烷、聚二甲基硅氧烷前驱体和固化剂的悬浮液喷涂到胶原纤维上。最后,将胶原纤维浸入到含有乙酸乙酯、1H,1H,2H,2H-全氟-十二烷基三乙氧基硅烷、聚二甲基硅氧烷前驱体和固化剂的混合溶液中,固化后制备得到多功能胶原纤维基柔性可穿戴传感材料;
采用具有层级结构和三维网络结构的胶原纤维为基材,利用原位聚合方式引入导电聚合物,使用导电炭黑增加结构导电性,引入疏水性SiO2纳米颗粒增加纤维表面粗糙结构,并应用氟硅烷以降低材料表面能,从而制备得到多功能胶原纤维基柔性可穿戴传感材料。
具体按照以下步骤实施:
步骤1、制备疏水性SiO2纳米颗粒;
具体为:首先,将0.1-10份的1H,1H,2H,2H-全氟-十二烷基三乙氧基硅烷滴加到含有5.00-20.00份的去离子水、1-10份的氢氧化氨、0.1-10份的SiO2纳米颗粒和100份的乙醇的混合溶液中,在40℃下磁力搅拌24h,得到SiO2分散液;然后,以10000转每分钟对分散液进行离心处理10min,再用乙醇对沉淀物进行1-5次洗涤,最后,将离心沉淀物在60℃下真空干燥12h,得到疏水性SiO2纳米颗粒;
步骤2、制备多功能胶原纤维基柔性可穿戴传感材料,具体为:
步骤2.1,将0.1-5份的导电聚合物单体和1-20份的氧化剂分别溶解在100份的去离子水中,制备得到导电聚合物单体溶液和氧化剂溶液;
导电聚合物单体为聚吡咯、聚苯胺、聚吲哚和聚乙炔中的任意一种或多种;
氧化剂为非金属单质、含有变价元素的高价化合物中的任意一种或两种;
非金属单质为F2、Cl2、O2、Br2、I2、S、Si中的任意一种;
含有变价元素的高价化合物为KMnO4、KClO3、HNO3、MnO2、H2O2、FeCl3中的任意一种;
步骤2.2,将尺寸为12cm×25cm的胶原纤维在室温下浸泡在200mL的导电聚合物单体溶液中并连续搅拌1h,之后在5℃下将胶原纤维在200mL的氧化剂溶液中浸泡0.1-6h,再用蒸馏水清洗胶原纤维并在室温下干燥;
胶原纤维是来源于天然动物皮中的未处理或经过鞣制处理的胶原纤维,或者基于胶原及其衍生物制得的胶原纤维。
步骤2.3,在100份的乙酸乙酯中加入0.05-1份的炭黑、0.1-10份的疏水性SiO2纳米颗粒、0.1-10份的1H,1H,2H,2H-全氟-十二烷基三乙氧基硅烷、0.1-10份的聚二甲基硅氧烷前驱体和0.01-1份的固化剂,室温下搅拌2h后得到混合悬浮液;
步骤2.4,将混合悬浮液通过喷枪喷涂到步骤2.2的胶原纤维上,并在60℃下固化0.01-1h;
步骤2.5,将0.1-10份的1H,1H,2H,2H-全氟-十二烷基三乙氧基硅烷、0.1-10份的聚二甲基硅氧烷前驱体和0.01-1份的固化剂加入100份的乙酸乙酯中,室温下搅拌1h后得到混合溶液;
步骤2.6,将步骤2.4中的胶原纤维浸泡在混合溶液中,浸泡时间为0.01-1h,之后在60℃下固化0.01-6h,得到多功能胶原纤维基柔性可穿戴传感材料。
实施例1
步骤1、制备疏水性SiO2纳米颗粒;
首先,将1.00质量份的1H,1H,2H,2H-全氟-十二烷基三乙氧基硅烷滴加到含有10.00质量份的去离子水、4.00质量份的氢氧化氨、2.00质量份的SiO2纳米颗粒和100.00质量份的乙醇的混合溶液中,在40.0℃下磁力搅拌24.0h后得到SiO2分散液。然后,以10000转每分钟对分散液进行离心处理10分钟,再用乙醇对沉淀物进行3次洗涤。最后,将离心沉淀物在60.0℃真空干燥12.0h后得到疏水性SiO2纳米颗粒。
步骤2、多功能胶原纤维基柔性可穿戴传感材料的制备;
首先,分别将1.71质量份的吡咯和13.00质量份的三氯化铁分别溶解在100.00质量份的去离子水中制备吡咯溶液和三氯化铁溶液。其次,将尺寸为12cm×25cm的胶原纤维在室温下浸泡在200.0mL的吡咯溶液中并连续搅拌1.0h,并在5.0℃下将胶原纤维在200.0mL的三氯化铁溶液中浸泡2.0h,再用蒸馏水清洗胶原纤维并在室温下干燥。接着,在100.00质量份的乙酸乙酯中加入0.40质量份的炭黑、0.40质量份的疏水性SiO2纳米颗粒、0.40质量份的1H,1H,2H,2H-全氟-十二烷基三乙氧基硅烷、0.40质量份的聚二甲基硅氧烷前驱体和0.04质量份的固化剂,室温下搅拌2.0h后得到混合悬浮液。然后,将悬浮液通过喷枪喷涂到上述胶原纤维上,并在60.0℃下固化0.1h。之后,将1.00质量份的1H,1H,2H,2H-全氟-十二烷基三乙氧基硅烷、1.00质量份的聚二甲基硅氧烷前驱体和0.10质量份的固化剂加入100.00质量份的乙酸乙酯中,室温下搅拌1.0h后得到混合溶液。最后,将上述胶原纤维浸入混合溶液0.1h,再在60.0℃下进一步固化3.0h后制备得到多功能胶原纤维基柔性可穿戴传感材料。
图1为实施例1制得的多功能胶原纤维基柔性可穿戴传感材料的外观图,通过观察可知,制得的胶原纤维呈现均匀的黑色,表明了导电聚合物的良好分布。
图2和图3为实施例1制得的多功能胶原纤维基柔性可穿戴传感材料的扫描电子显微镜图。通过观察可知,制得的胶原纤维表面显示出具有明显层次的粗糙结构,这是由于改性SiO2和炭黑的存在增加了胶原纤维表面的粗糙度。
图4为实施例1制得的多功能胶原纤维基柔性可穿戴传感材料和不同种类液体的照片图。通过观察可知,水、棕榈油、橙汁、绿茶、牛奶、可乐、咖啡和甘油均在胶原纤维上呈现球状分布,这是因为改性SiO2和炭黑增加了纤维表面的粗糙结构,而1H,1H,2H,2H-全氟-十二烷基三乙氧基硅烷和聚二甲基硅氧烷降低了材料的表面能,从而赋予了胶原纤维良好的拒水拒油性。
图5为实施例1制得的多功能胶原纤维基柔性可穿戴传感材料在手指弯曲时的实时电阻变化。通过观察可知,随着手指持续地弯曲,电流呈现循环的变化,表明胶原纤维具有良好的导电性能和传感性能。
图6为实施例1制得的多功能胶原纤维基柔性可穿戴传感材料在人体跳跃、步行、慢跑和快跑时的实时电阻变化。通过观察可知,电阻在人体运动时呈现规律性变化;同时,随着人体运动状态的改变,电阻也呈现相应的特征变化,也表明该胶原纤维具有良好的导电性能和传感性能。
实施例2
步骤1,制备疏水性SiO2纳米颗粒;
首先,将1.20质量份的1H,1H,2H,2H-全氟-十二烷基三乙氧基硅烷滴加到含有12.00质量份的去离子水、4.30质量份的氢氧化氨、2.30质量份的SiO2纳米颗粒和100.00质量份的乙醇的混合溶液中,在40.0℃下磁力搅拌24.0h后得到SiO2分散液。然后,以10000转每分钟对分散液进行离心处理10分钟,再用乙醇对沉淀物进行3次洗涤。最后,将离心沉淀物在60.0℃真空干燥12.0h后得到疏水性SiO2纳米颗粒。
步骤2,多功能胶原纤维基柔性可穿戴传感材料的制备:
首先,分别将2.00质量份的苯胺和15.00质量份的二氧化锰分别溶解在100.00质量份的去离子水中制备吡咯溶液和二氧化锰溶液。其次,将尺寸为12cm×25cm的胶原纤维在室温下浸泡在200.0mL吡咯溶液中并连续搅拌1.0h,并在5.0℃下将胶原纤维在200.0mL的二氧化锰溶液中浸泡2.0h,再用蒸馏水清洗胶原纤维并在室温下干燥。接着,在100.00质量份的乙酸乙酯中加入0.45质量份的炭黑、0.45质量份的疏水性SiO2纳米颗粒、0.45质量份的1H,1H,2H,2H-全氟-十二烷基三乙氧基硅烷、0.45质量份的聚二甲基硅氧烷前驱体和0.04质量份的固化剂,室温下搅拌2.0h后得到混合悬浮液。然后,将悬浮液通过喷枪喷涂到上述胶原纤维上,并在60.0℃下固化0.5h。之后,将1.50质量份的1H,1H,2H,2H-全氟-十二烷基三乙氧基硅烷、1.50质量份的聚二甲基硅氧烷前驱体和0.15质量份的固化剂加入100.00质量份的乙酸乙酯中,室温下搅拌1.0h后得到混合溶液。最后,将上述胶原纤维浸入混合溶液0.2h,再在60.0℃下进一步固化3.0h后制备得到多功能胶原纤维基柔性可穿戴传感材料。
实施例3
步骤1、制备疏水性SiO2纳米颗粒;
首先,将1.00质量份的1H,1H,2H,2H-全氟-十二烷基三乙氧基硅烷滴加到含有10.00质量份的去离子水、4.00质量份的氢氧化氨、2.00质量份的SiO2纳米颗粒和100.00质量份的乙醇的混合溶液中,在40.0℃下磁力搅拌24.0h后得到SiO2分散液。然后,以10000转每分钟对分散液进行离心处理10分钟,再用乙醇对沉淀物进行3次洗涤。最后,将离心沉淀物在60.0℃真空干燥12.0h后得到疏水性SiO2纳米颗粒。
步骤2、多功能胶原纤维基柔性可穿戴传感材料的制备:
首先,分别将1.90质量份的吡咯和14.00质量份的三氯化铁分别溶解在100.00质量份的去离子水中制备吡咯溶液和三氯化铁溶液。其次,将尺寸为12cm×25cm的胶原纤维在室温下浸泡在200.0mL的吡咯溶液中并连续搅拌1.0h,并在5.0℃下将胶原纤维在200.0mL的三氯化铁溶液中浸泡2.5h,再用蒸馏水清洗胶原纤维并在室温下干燥。接着,在100.00质量份的乙酸乙酯中加入0.50质量份的炭黑、0.50质量份的疏水性SiO2纳米颗粒、0.50质量份的1H,1H,2H,2H-全氟-十二烷基三乙氧基硅烷、0.50质量份的聚二甲基硅氧烷前驱体和0.04质量份的固化剂,室温下搅拌2.0h后得到混合悬浮液。然后,将悬浮液通过喷枪喷涂到上述胶原纤维上,并在60.0℃下固化0.2h。之后,将1.50质量份的1H,1H,2H,2H-全氟-十二烷基三乙氧基硅烷、1.50质量份的聚二甲基硅氧烷前驱体和0.15质量份的固化剂加入100.00质量份的乙酸乙酯中,室温下搅拌1.0h后得到混合溶液。最后,将上述胶原纤维浸入混合溶液0.2h,再在60.0℃下进一步固化3.0h后制备得到多功能胶原纤维基柔性可穿戴传感材料。
实施例4
步骤1、制备疏水性SiO2纳米颗粒;
首先,将1.50质量份的1H,1H,2H,2H-全氟-十二烷基三乙氧基硅烷滴加到含有13.00质量份的去离子水、4.60质量份的氢氧化氨、2.40质量份的SiO2纳米颗粒和100.00质量份的乙醇的混合溶液中,在40.0℃下磁力搅拌24.0h后得到SiO2分散液。然后,以10000转每分钟对分散液进行离心处理10分钟,再用乙醇对沉淀物进行5次洗涤。最后,将离心沉淀物在60.0℃真空干燥12.0h后得到疏水性SiO2纳米颗粒。
步骤二、多功能胶原纤维基柔性可穿戴传感材料的制备:
首先,分别将1.95质量份的苯胺和14.50质量份的过氧化氢分别溶解在100.00质量份的去离子水中制备吡咯溶液和过氧化氢溶液。其次,将尺寸为12cm×25cm的胶原纤维在室温下浸泡在200.0mL的吡咯溶液中并连续搅拌1.0h,并在5.0℃下将胶原纤维在200.0mL的过氧化氢溶液中浸泡2.5h,再用蒸馏水清洗胶原纤维并在室温下干燥。接着,在100.00质量份的乙酸乙酯中加入0.50质量份的炭黑、0.50质量份的疏水性SiO2纳米颗粒、0.50质量份的1H,1H,2H,2H-全氟-十二烷基三乙氧基硅烷、0.50质量份的聚二甲基硅氧烷前驱体和0.04质量份的固化剂,室温下搅拌2.0h后得到混合悬浮液。然后,将悬浮液通过喷枪喷涂到上述胶原纤维上,并在60.0℃下固化0.2h。之后,将1.50质量份的1H,1H,2H,2H-全氟-十二烷基三乙氧基硅烷、1.50质量份的聚二甲基硅氧烷前驱体和0.15质量份的固化剂加入100.00质量份的乙酸乙酯中,室温下搅拌1.0h后得到混合溶液。最后,将上述胶原纤维浸入混合溶液0.2h,再在60.0℃下进一步固化3.0h后制备得到多功能胶原纤维基柔性可穿戴传感材料。
实施例5
步骤1、制备疏水性SiO2纳米颗粒;
首先,将1.50质量份的1H,1H,2H,2H-全氟-十二烷基三乙氧基硅烷滴加到含有14.00质量份的去离子水、5.00质量份的氢氧化氨、3.00质量份的SiO2纳米颗粒和100.00质量份的乙醇的混合溶液中,在40.0℃下磁力搅拌24.0h后得到SiO2分散液。然后,以10000转每分钟对分散液进行离心处理10分钟,再用乙醇对沉淀物进行5次洗涤。最后,将离心沉淀物在60.0℃真空干燥12.0h后得到疏水性SiO2纳米颗粒。
步骤2、多功能胶原纤维基柔性可穿戴传感材料的制备:
首先,分别将2.50质量份的吡咯和17.00质量份的二氧化锰分别溶解在100.00质量份的去离子水中制备吡咯溶液和二氧化锰溶液。其次,将尺寸为12cm×25cm的胶原纤维在室温下浸泡在200.0mL的吡咯溶液中并连续搅拌1.0h,并在5.0℃下将胶原纤维在200.0mL的二氧化锰溶液中浸泡3.0h,再用蒸馏水清洗胶原纤维并在室温下干燥。接着,在100.00质量份的乙酸乙酯中加入0.55质量份的炭黑、0.55质量份的疏水性SiO2纳米颗粒、0.55质量份的1H,1H,2H,2H-全氟-十二烷基三乙氧基硅烷、0.55质量份的聚二甲基硅氧烷前驱体和0.05质量份的固化剂,室温下搅拌2.0h后得到混合悬浮液。然后,将悬浮液通过喷枪喷涂到上述胶原纤维上,并在60.0℃下固化0.2h。之后,将1.50质量份的1H,1H,2H,2H-全氟-十二烷基三乙氧基硅烷、2.00质量份的聚二甲基硅氧烷前驱体和0.20质量份的固化剂加入100.00质量份的乙酸乙酯中,室温下搅拌1.0h后得到混合溶液。最后,将上述胶原纤维浸入混合溶液0.2h,再在60.0℃下进一步固化3.0h后制备得到多功能胶原纤维基柔性可穿戴传感材料。
本发明的方法,基于结构设计和聚合物合成,以胶原纤维、导电聚合物单体、氧化剂、氟硅烷、疏水性SiO2纳米颗粒等为原料,结合原位聚合法以及喷涂和浸渍的操作工艺制备得到多功能胶原纤维基柔性可穿戴传感材料。制备出的胶原纤维基传感材料具有良好的机械性能、导电性、柔韧性、生物相容性、超双疏性、阻燃性、电磁屏蔽性能、光热转换性能和应变传感性能等。
Claims (5)
1.一种多功能胶原纤维基柔性可穿戴传感材料的制备方法,其特征在于,首先利用1H,1H,2H,2H-全氟-十二烷基三乙氧基硅烷、去离子水、氢氧化氨和乙醇对SiO2进行改性,制备得到疏水性SiO2纳米颗粒;然后,采用导电聚合物单体溶液和氧化剂溶液对胶原纤维进行处理,再将含有乙酸乙酯、炭黑、疏水性SiO2纳米颗粒、1H,1H,2H,2H-全氟-十二烷基三乙氧基硅烷、聚二甲基硅氧烷前驱体和固化剂的悬浮液喷涂到胶原纤维上;最后,将胶原纤维浸入到含有乙酸乙酯、1H,1H,2H,2H-全氟-十二烷基三乙氧基硅烷、聚二甲基硅氧烷前驱体和固化剂的混合溶液中,固化后制备得到多功能胶原纤维基柔性可穿戴传感材料。
2.根据权利要求1所述的一种多功能胶原纤维基柔性可穿戴传感材料的制备方法,其特征在于,具体按照以下步骤实施:
步骤1、制备疏水性SiO2纳米颗粒;
步骤2、制备多功能胶原纤维基柔性可穿戴传感材料,具体为:
步骤2.1,将0.1-5份的导电聚合物单体和1-20份的氧化剂分别溶解在100份的去离子水中,制备得到导电聚合物单体溶液和氧化剂溶液;
步骤2.2,将胶原纤维在室温下浸泡在导电聚合物单体溶液中并连续搅拌1h,之后在5℃下将胶原纤维在氧化剂溶液中浸泡0.1-6h,再用蒸馏水清洗胶原纤维并在室温下干燥;
步骤2.3,在100份的乙酸乙酯中加入0.05-1份的炭黑、0.1-10份的疏水性SiO2纳米颗粒、0.1-10份的1H,1H,2H,2H-全氟-十二烷基三乙氧基硅烷、0.1-10份的聚二甲基硅氧烷前驱体和0.01-1份的固化剂,室温下搅拌2h后得到混合悬浮液;
步骤2.4,将混合悬浮液通过喷枪喷涂到步骤2.2的胶原纤维上,并在60℃下固化0.01-1h;
步骤2.5,将0.1-10份的1H,1H,2H,2H-全氟-十二烷基三乙氧基硅烷、0.1-10份的聚二甲基硅氧烷前驱体和0.01-1份的固化剂加入100份的乙酸乙酯中,室温下搅拌1h后得到混合溶液;
步骤2.6,将步骤2.4中的胶原纤维浸泡在混合溶液中,浸泡时间为0.01-1h,之后在60℃下固化0.01-6h,得到多功能胶原纤维基柔性可穿戴传感材料。
3.根据权利要求2所述的一种多功能胶原纤维基柔性可穿戴传感材料的制备方法,其特征在于,所述步骤1中,具体为:
首先,将0.1-10份的1H,1H,2H,2H-全氟-十二烷基三乙氧基硅烷滴加到含有5.00-20.00份的去离子水、1-10份的氢氧化氨、0.1-10份的SiO2纳米颗粒和100份的乙醇的混合溶液中,在40℃下磁力搅拌24h,得到SiO2分散液;然后,以10000转每分钟对分散液进行离心处理10min,再用乙醇对沉淀物进行1-5次洗涤,最后,将离心沉淀物在60℃下真空干燥12h,得到疏水性SiO2纳米颗粒。
4.根据权利要求2所述的一种多功能胶原纤维基柔性可穿戴传感材料的制备方法,其特征在于,所述步骤2.1中,导电聚合物单体为聚吡咯、聚苯胺、聚吲哚和聚乙炔中的任意一种或多种。
5.根据权利要求2所述的一种多功能胶原纤维基柔性可穿戴传感材料的制备方法,其特征在于,所述步骤2.1中,氧化剂为非金属单质、含有变价元素的高价化合物中的任意一种或两种;非金属单质为F2、Cl2、O2、Br2、I2、S、Si中的任意一种;含有变价元素的高价化合物为KMnO4、KClO3、HNO3、MnO2、H2O2、FeCl3中的任意一种。
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