CN111320768A - 一种水凝胶应变传感器的制备方法 - Google Patents
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Abstract
本发明公开了一种水凝胶应变传感器的制备方法,将N‑丙烯酰基甘氨酰胺单体、氯化锂完全溶解在去离子水中,然后加入光引发剂1173,充分搅拌后超声去除气泡得到水凝胶前驱液;将水凝胶前驱液倒入隔绝氧气的密闭模具中,并置于紫外箱内光照得到超分子离子水凝胶;将超分子离子水凝胶放置在氯化锂溶液中充分浸泡,浸泡时间为1‑3天,去除水凝胶制备过程中带入的杂质;将充分浸泡后的水凝胶清洗干净,将表面干燥,裁剪成长条状结构,在两端安装导电铜电极组装成水凝胶应变传感器。整个制备过程安全可靠,工艺简单高效,材料性能优异且生物相容性良好,适合在人体皮肤外表使用,可广泛应用于柔性机器人、柔性电子皮肤、实时健康监测等领域。
Description
技术领域
本发明涉及智能材料的技术领域,尤其是指一种水凝胶应变传感器的制备方法。
背景技术
模拟人造皮肤电子设备具有各种功能的独特组合,可以通过将各种物理或化学刺激转换为电子信号来模仿人类皮肤的柔韧性和敏感性。由于它们的广泛使用,例如软机器人、生物医学假体、个人医疗保健监视等,它们引起了越来越多的关注。传统上,这些智能设备是通过复合弹性基材(例如PDMS)和导电填料(金属颗粒,碳纳米管,导电聚合物)来制造的。它们被称为电子皮肤,是因为它们通过电子传输信号。但是,这种导体通常是不透明的,因为导电电子会阻碍光的传输,这限制了它们在可调谐光学器件中需要透明性的某些设备中的应用。因此,提出了离子水凝胶来解决该问题。水凝胶是由固相和液相组成的三维聚合物网络。聚合物网络有助于其弹性,而水相则充当导电离子的载体,这类似于人体细胞外基质的功能。由于这些优异的特性,离子水凝胶兼具生物相容性,可拉伸性,透明性和导电性,使其成为人造软电子产品的优秀候选者。
聚N-丙烯酰基甘氨酰胺复合氯化锂形成一种无毒无害的离子导电水凝胶,分子侧链上形成丰富的双酰胺键氢键交联点,这给水凝胶提供了高强度和优异的拉伸性能;氯化锂为设备提供了稳定的导电介质,且离子导电水凝胶透光性好,透明度高,在光学性能方面相比电子导电水凝胶有绝对优势。本发明体系有望成功应用在可穿戴领域。
发明内容
本发明的目的在于克服现有技术的缺点和不足,提出了一种高强度新型的水凝胶应变传感器的制备方法,制得的水凝胶应变传感器具有高强度,高透明度,稳定的电信号传输能力,可用于拉伸应变和压缩应力的检测。同时,水凝胶高拉伸性极大扩大了传感器对信号的检测范围,可实现微小和大幅度的人体运动的实时监测;整个制备过程安全可靠,工艺简单高效,材料性能优异且生物相容性良好,适合在人体皮肤外表使用,可广泛应用于柔性机器人、柔性电子皮肤、实时健康监测等领域。
为实现上述目的,本发明所提供的技术方案为:一种水凝胶应变传感器的制备方法,该方法利用超分子聚合物聚N-丙烯酰基甘氨酰胺分子侧链密集的双氢键物理交联形成高强度的水凝胶,与导电介质氯化锂复合,采用一步溶胶-凝胶法原位制备成高强度、高透明度的离子导电水凝胶,其具体包括以下步骤:
1)将N-丙烯酰基甘氨酰胺单体、氯化锂完全溶解在去离子水中,然后加入光引发剂1173(2-羟基-2-甲基-1-苯基-1-丙酮),充分搅拌后超声去除气泡得到水凝胶前驱液;
2)将步骤1)获得的水凝胶前驱液倒入隔绝氧气的密闭模具中,并置于紫外箱内光照得到超分子离子水凝胶;
3)将步骤2)获得的超分子离子水凝胶放置在氯化锂溶液中充分浸泡,浸泡时间为1-3天,去除水凝胶制备过程中带入的杂质;
4)将充分浸泡后的水凝胶清洗干净,将表面干燥,裁剪成长条状结构,在两端安装导电铜电极组装成水凝胶应变传感器。
在步骤1)中,所述N-丙烯酰基甘氨酰胺单体的质量分数为30%,这相对于N-丙烯酰基甘氨酰胺单体加去离子水的质量;所述氯化锂的质量分数为0.4wt%-1.2%,这相对于N-丙烯酰基甘氨酰胺单体加去离子水的质量。
在步骤1)中,所述光引发剂1173的质量分数为2%,这相对于N-丙烯酰基甘氨酰胺单体的质量。
在步骤1)中,搅拌条件是利用磁力搅拌器搅拌1分钟-5分钟,超声时间为5分钟。
在步骤2)中,所述模具为方形模具,其组成为两片方形的全透光玻璃片中间夹有1mm厚的硅橡胶片,所述硅橡胶片为中空状,镂空部位尺寸为6cm×6cm的正方形。
在步骤2)中,紫外光照射时间为40分钟,照射强度为15mW/cm2-30mW/cm2。
在步骤3)中,用于浸泡水凝胶的氯化锂溶液的质量分数为0.4%-1.2%。
在步骤3)中,浸泡过程中每天更新氯化锂溶液3次。
在步骤4)中,将水凝胶表面干燥是用氮气吹拂水凝胶表面2-5min使其干燥。
在步骤4)中,所述长条状尺寸为4cm×1.5cm。
本发明与现有技术相比,具有如下优点与有益效果:
1、本发明利用了超分子聚合物聚N-丙烯酰基甘氨酰胺复合导电介质氯化锂制备出了离子导电水凝胶,该导电水凝胶被用来组装成柔性的可穿戴传感器,集高强度、高透明度、优异机械强度、大拉伸率、稳定的信号传输能力等多功能于一体。
2、本发明使用的水凝胶体系成胶不需要加入交联剂,减少有毒物质的使用,生物相容性良好。
3、本发明工艺简单,原材料来源广泛,材料机械性能和电信号传输性能均非常优异,在柔性传感器中有广泛的应用前景。
附图说明
图1是本发明实施例1-5中制备的含有不同的氯化锂浓度导电水凝胶的应力应变曲线图。
图2是本发明实施例3中制备的导电水凝胶被组装为应变传感器监测手指弯曲角度的电阻变化曲线图。
图3是本发明实施例3中制备的导电水凝胶被组装为压力传感器监测人体脉搏跳动的电阻变化曲线图。
具体实施方式
下面结合具体实施例对本发明作进一步说明。
实施例1
取3gN-丙烯酰基甘氨酰胺单体溶于7ml的去离子水中充分搅拌至完全溶解,加入0.04g氯化锂再次振荡至完全溶解得到透明溶液;接着加入50ul光引发剂1173,充分振荡使其分散在溶液中;将上述溶液超声5分钟去除气泡得到水凝胶预聚液;将预聚液倒入预先制备好的模具中,模具尺寸为:两片完全透光的玻璃片中夹着1mm厚的镂空硅橡胶,镂空部分尺寸为6cm×6cm;将上述装有预聚液的模具放入紫外光照箱中以15mW/cm2的紫外光强度照射40分钟;得到的水凝胶放入浓度为0.4wt%的氯化锂溶液中浸泡三天,每天更换三次新鲜的氯化锂溶液。将浸泡三天后的水凝胶清洗干净,用吹风机吹干水凝胶表面,裁剪成尺寸为4cm×1.5cm的长条状结构,在水凝胶两端安装导电铜电极组装成水凝胶应变传感器。
实施例2
取3gN-丙烯酰基甘氨酰胺单体溶于7ml的去离子水中充分搅拌至完全溶解,加入0.08g氯化锂再次振荡至完全溶解得到透明溶液;接着加入50ul光引发剂1173,充分振荡使其分散在溶液中;将上述溶液超声5分钟去除气泡得到水凝胶预聚液;将预聚液倒入预先制备好的模具中,模具尺寸为:两片完全透光的玻璃片中夹着1mm厚的镂空硅橡胶,镂空部分尺寸为6cm×6cm;将上述装有预聚液的模具放入紫外光照箱中以15mW/cm2的紫外光强度照射40分钟;得到的水凝胶放入浓度为0.8wt%的氯化锂溶液中浸泡三天,每天更换三次新鲜的氯化锂溶液。将浸泡三天后的水凝胶清洗干净,用吹风机吹干水凝胶表面,裁剪成尺寸为4cm×1.5cm的长条状结构,在水凝胶两端安装导电铜电极组装成水凝胶应变传感器。
实施例3
取3gN-丙烯酰基甘氨酰胺单体溶于7ml的去离子水中充分搅拌至完全溶解,加入0.12g氯化锂再次振荡至完全溶解得到透明溶液;接着加入50ul光引发剂1173,充分振荡使其分散在溶液中;将上述溶液超声5分钟去除气泡得到水凝胶预聚液;将预聚液倒入预先制备好的模具中,模具尺寸为:两片完全透光的玻璃片中夹着1mm厚的镂空硅橡胶,镂空部分尺寸为6cm×6cm;将上述装有预聚液的模具放入紫外光照箱中以15mW/cm2的紫外光强度照射40分钟;得到的水凝胶放入浓度为1.2wt%的氯化锂溶液中浸泡三天,每天更换三次新鲜的氯化锂溶液。将浸泡三天后的水凝胶清洗干净,用吹风机吹干水凝胶表面,裁剪成尺寸为4cm×1.5cm的长条状结构,在水凝胶两端安装导电铜电极组装成水凝胶应变传感器,用透明胶带将水凝胶固定在志愿者的食指上来测试手指弯曲的角度,如图2所示,志愿者的食指分别弯曲0°、30°、60°、90°得到相对应的水凝胶应变传感器相对阻抗变化曲线,用3M胶带将水凝胶应变传感器固定在志愿者的手腕上来测试人体运动前后的脉搏跳动次数,如图3所示。
实施例4
取3gN-丙烯酰基甘氨酰胺单体溶于7ml的去离子水中充分搅拌至完全溶解,加入0.16g氯化锂再次振荡至完全溶解得到透明溶液;接着加入50ul光引发剂1173,充分振荡使其分散在溶液中;将上述溶液超声5分钟去除气泡得到水凝胶预聚液;将预聚液倒入预先制备好的模具中,模具尺寸为:两片完全透光的玻璃片中夹着1mm厚的镂空硅橡胶,镂空部分尺寸为6cm×6cm;将上述装有预聚液的模具放入紫外光照箱中以15mW/cm2的紫外光强度照射40分钟;得到的水凝胶放入浓度为1.6wt%的氯化锂溶液中浸泡三天,每天更换三次新鲜的氯化锂溶液。将浸泡三天后的水凝胶清洗干净,用吹风机吹干水凝胶表面,裁剪成尺寸为4cm×1.5cm的长条状结构,在水凝胶两端安装导电铜电极组装成水凝胶应变传感器。
实施例5
取3gN-丙烯酰基甘氨酰胺单体溶于7ml的去离子水中充分搅拌至完全溶解,加入0.2g氯化锂再次振荡至完全溶解得到透明溶液;接着加入50ul光引发剂1173,充分振荡使其分散在溶液中;将上述溶液超声5分钟去除气泡得到水凝胶预聚液;将预聚液倒入预先制备好的模具中,模具尺寸为:两片完全透光的玻璃片中夹着1mm厚的镂空硅橡胶,镂空部分尺寸为6cm×6cm;将上述装有预聚液的模具放入紫外光照箱中以15mW/cm2的紫外光强度照射40分钟;得到的水凝胶放入浓度为2.0wt%的氯化锂溶液中浸泡三天,每天更换三次新鲜的氯化锂溶液。将浸泡三天后的水凝胶清洗干净,用吹风机吹干水凝胶表面,裁剪成尺寸为4cm×1.5cm的长条状结构,在水凝胶两端安装导电铜电极组装成水凝胶应变传感器。
参见图1所示,为水凝胶在不同氯化锂浓度下的应力应变曲线比较,由图中可知,混合1.2wt%浓度氯化锂的水凝胶力学性能最佳。
以上所述之实施例子只为本发明之较佳实施例,并非以此限制本发明的实施范围,故凡依本发明之形状、原理所作的变化,均应涵盖在本发明的保护范围内。
Claims (10)
1.一种水凝胶应变传感器的制备方法,其特征在于:该方法利用超分子聚合物聚N-丙烯酰基甘氨酰胺分子侧链密集的双氢键物理交联形成高强度的水凝胶,与导电介质氯化锂复合,采用一步溶胶-凝胶法原位制备成高强度、高透明度的离子导电水凝胶,其具体包括以下步骤:
1)将N-丙烯酰基甘氨酰胺单体、氯化锂完全溶解在去离子水中,然后加入光引发剂1173,充分搅拌后超声去除气泡得到水凝胶前驱液;
2)将步骤1)获得的水凝胶前驱液倒入隔绝氧气的密闭模具中,并置于紫外箱内光照得到超分子离子水凝胶;
3)将步骤2)获得的超分子离子水凝胶放置在氯化锂溶液中充分浸泡,浸泡时间为1-3天,去除水凝胶制备过程中带入的杂质;
4)将充分浸泡后的水凝胶清洗干净,将表面干燥,裁剪成长条状结构,在两端安装导电铜电极组装成水凝胶应变传感器。
2.根据权利要求1所述的一种水凝胶应变传感器的制备方法,其特征在于:在步骤1)中,所述N-丙烯酰基甘氨酰胺单体的质量分数为30%,这相对于N-丙烯酰基甘氨酰胺单体加去离子水的质量;所述氯化锂的质量分数为0.4wt%-1.2%,这相对于N-丙烯酰基甘氨酰胺单体加去离子水的质量。
3.根据权利要求1所述的一种水凝胶应变传感器的制备方法,其特征在于:在步骤1)中,所述光引发剂1173的质量分数为2%,这相对于N-丙烯酰基甘氨酰胺单体的质量。
4.根据权利要求1所述的一种水凝胶应变传感器的制备方法,其特征在于:在步骤1)中,搅拌条件是利用磁力搅拌器搅拌1分钟-5分钟,超声时间为5分钟。
5.根据权利要求1所述的一种水凝胶应变传感器的制备方法,其特征在于:在步骤2)中,所述模具为方形模具,其组成为两片方形的全透光玻璃片中间夹有1mm厚的硅橡胶片,所述硅橡胶片为中空状,镂空部位尺寸为6cm×6cm的正方形。
6.根据权利要求1所述的一种水凝胶应变传感器的制备方法,其特征在于:在步骤2)中,紫外光照射时间为40分钟,照射强度为15mW/cm2-30mW/cm2。
7.根据权利要求1所述的一种水凝胶应变传感器的制备方法,其特征在于:在步骤3)中,用于浸泡水凝胶的氯化锂溶液的质量分数为0.4%-1.2%。
8.根据权利要求1所述的一种水凝胶应变传感器的制备方法,其特征在于:在步骤3)中,浸泡过程中每天更新氯化锂溶液3次。
9.根据权利要求1所述的一种水凝胶应变传感器的制备方法,其特征在于:在步骤4)中,将水凝胶表面干燥是用氮气吹拂水凝胶表面2-5min使其干燥。
10.根据权利要求1所述的一种水凝胶应变传感器的制备方法,其特征在于:在步骤4)中,所述长条状尺寸为4cm×1.5cm。
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