CN107474469A - 一种二硫化钼量子点修饰的柔性传感器电极的制备方法 - Google Patents
一种二硫化钼量子点修饰的柔性传感器电极的制备方法 Download PDFInfo
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Abstract
本发明涉及传感器电极材料领域,本发明公开了一种二硫化钼量子点修饰的柔性传感器电极的制备方法,通过溶液混合法制备柔性导电薄膜,其中以丙烯腈‑丁二烯‑苯乙烯树脂为柔性基底,以聚3,4‑乙烯二氧噻吩‑聚苯乙烯磺酸‑石墨烯为导电材料,并以二硫化钼量子点修饰电极,得到一种柔性传感器电极。本发明的传感器电极具有导电性能更加出色、灵敏度高、具有柔性的优点,可应用于医疗生物监测,环境和卫生监测等领域。
Description
技术领域
本发明涉及传感器电极材料领域,尤其涉及一种二硫化钼量子点修饰的柔性传感器电极的制备方法。
背景技术
传感器是人类自身对自然界各种感觉信息的探知,能够对不同信号和感知信息转化为可数字化、智能化的重要器件。在人类文明信息技术高速发展的过程中,传感器起到了越来越重的作用,是人类探索未知世界,同时也是人类了解现实世界,观察周边信息的重要手段之一。传感器是一种能把电、光、温度以及化学作用等非电学信号转化为电学信号的可调控的元器件。
石墨烯是一类新的碳二维纳米轻质材料,具有独特的单原子层二维晶体结构,大量的研究结果表明石墨烯具有已知材料最高的强度,大的比表面积比,优异的导电性和导热性等优异的性质,这些优异的性质也决定了它在诸如复合材料,电子器件,太阳能等诸多领域有着广泛的应用前景。
在传感器电极材料领域,现有技术中多数是将石墨烯复合到铂碳电极上,复合材料比较单一,导电性能不佳,存在缺陷,且不具有柔性,不能用于可穿戴设备,即不能更好地发挥传感器的实用价值,为此有必要开发出一种导电性能更加出色、与传统传感器相比具有更加优异的检测性能的柔性传感器电极材料。
发明内容
为了解决上述技术问题,本发明提供了一种二硫化钼量子点修饰的柔性传感器电极的制备方法。本发明的传感器电极具有导电性能更加出色、灵敏度高、具有柔性的优点,可应用于医疗生物监测,环境和卫生监测等领域。
本发明的具体技术方案为:一种二硫化钼量子点修饰的柔性传感器电极的制备方法,包括如下步骤:
(1)油性成膜溶液的配制:将丙烯腈-丁二烯-苯乙烯树脂添加到二氯甲烷溶液中,搅拌后静置使丙烯腈-丁二烯-苯乙烯树脂完全溶解,得到油性成膜溶液,待用。
丙烯腈-丁二烯-苯乙烯树脂具有耐低温性、耐热性、抗冲击性、电气性能及耐化学药品性优良,丙烯腈-丁二烯-苯乙烯树脂集合了三个单体的优良性能,即丙烯腈的耐热性、耐油性;丁二烯的耐冲击性;苯乙烯的光泽、成型性;是一种用途极广的柔性塑料。
(2)聚3,4-乙烯二氧噻吩-聚苯乙烯磺酸-石墨烯导电复合材料的制备:将石墨烯加入到聚苯乙烯磺酸溶液中,超声分散,然后加入3,4-乙烯二氧噻吩单体,并在搅拌条件下逐滴加入氯化铁溶液,继续搅拌反应10-14h,离心分离所得的墨绿色浆液,并分别用无水乙醇和蒸馏水反复清洗多次至洗涤液为无色,收集固体,70-80℃下真空干燥10-14h,得到聚3,4-乙烯二氧噻吩-聚苯乙烯磺酸-石墨烯导电复合材料。
将石墨烯加入到聚苯乙烯磺酸溶液中,超声分散,其目的是为了使石墨烯功能化,将聚苯乙烯磺酸负载于石墨烯上,并以功能化的石墨烯为载体原位聚合聚3,4-乙烯二氧噻吩,使其相互紧密结合。通过聚合的方法得到聚3,4-乙烯二氧噻吩-聚苯乙烯磺酸-石墨烯复合材料由于是通过化学键的作用相互结合在一起,大大提高了电子的迁移速率,比将聚3,4-乙烯二氧噻吩-聚苯乙烯磺酸溶液与石墨烯简单的物理混合导电性能要优越很多。
(3)水性导电溶液的配制:将步骤(2)所得的导电复合材料添加到水溶液中,超声分散,得到水性导电溶液,待用。
(4)高分子导电薄膜的制备:将步骤(3)所得的水性导电溶液和步骤(1)所得的油性成膜溶液进行混合,超声处理,得到混合均一的水油导电溶液,取水油导电溶液滴定于培养皿,放置20-28h后,自然干燥后得到高分子导电薄膜,掲下高分子导电薄膜后烘干。
(5)柔性传感器电极的制备:将步骤(4)所得的导电高分子薄膜剪裁成长条状样品,用固体石蜡和绝缘胶带将导电薄膜进行固定并对其部分区域进行覆盖。
(6)二硫化钼量子点的制备:将Na2MoO4·2H2O溶解于水中,超声4-6min;用盐酸调节pH至6-7;加入L-半胱氨酸和去离子水,超声4-6min;将溶液转移至反应釜进行水热反应,自然冷却后,离心,收集浅棕色的上清液,得到二硫化钼量子点。
二硫化钼是一种典型的过渡金属二维层状硫化物,单层的二硫化钼由-Mo-S原子层以共价键方式构成,层与层之间依靠较弱的范德华力结合。与具有二维层状结构的石墨烯不同,二硫化钼具有可调控的带隙结构。当块状的二硫化钼变为二硫化钼纳米片层时,二硫化钼的禁带宽度随着其层数的减小而增加。相比零带隙的石墨烯,单层二硫化钼表现出更为优异的物理化学特性,在光学器件、锂离子电池、光电催化、超级电容器、传感器等领域具有很高的应用前景,吸引了科研工作者的广泛关注。目前,关于二硫化钼的报道多停留在纳米片层范围,对于MoS2量子点的报道相对较少,相较于二硫化钼纳米片层,二硫化钼量子点具有更大的比表面积,更显著的边缘效应,使其在生物医学、光学成像、气体检测等领域更具潜力。在石墨烯和氧化锌纳米管阵列中掺杂二硫化钼量子点,大大得提高传感器灵敏度。
(7)二硫化钼量子点修饰的柔性传感器电极的制备:将步骤(6)所得的二硫化钼量子点加入到全氟磺酸树脂溶液中,超声分散均匀,然后再将其滴加到步骤(5)所得的导电高分子薄膜的未覆盖区域上,于室温下自然干燥,得到二硫化钼量子点修饰的柔性传感器电极。
本发明制备方法通过溶液混合法制备柔性导电薄膜,其中以丙烯腈-丁二烯-苯乙烯为柔性基底,以聚3,4-乙烯二氧噻吩-聚苯乙烯磺酸-石墨烯为导电材料,并以二硫化钼量子点修饰电极,得到一种柔性传感器电极。
在本发明中,聚3,4-乙烯二氧噻吩作为聚噻吩的衍生物,具有分子结构简单、能隙小、电导率高和透明度高等特点。被广泛应用于各领域。为解决聚3,4-乙烯二氧噻吩的不溶不熔性,聚苯乙烯磺酸被引入聚3,4-乙烯二氧噻吩,形成了分散性和加工性良好的聚3,4-乙烯二氧噻吩-聚苯乙烯磺酸悬浮液,聚3,4-乙烯二氧噻吩-聚苯乙烯磺酸水溶液具有良好的成膜性和环境稳定性。将石墨烯和聚3,4-乙烯二氧噻吩-聚苯乙烯磺酸掺杂在一起以得到导电性能优加的材料,并以丙烯腈-丁二烯-苯乙烯树脂为柔性塑料基底,得到性能十分优越的柔性透明导电薄膜,可作为可穿戴生物传感器电极,具有十分广阔的应用前景。为更进一步的提高导电薄膜的导电性和敏感性,本发明引入零维二硫化钼量子点,使其与传统的传感器电极相比具有更加优越的性能。
作为优选,步骤(1)中,所述油性成膜溶液中丙烯腈-丁二烯-苯乙烯树脂的质量分数为5%-20%。
作为优选,步骤(2)中,石墨烯与聚苯乙烯磺酸、聚3,4-乙烯二氧噻吩、氯化铁的质量比为1-2:1-2:1-3:1-3。
作为优选,步骤(3)中,超声分散的时间为25-35min,水性导电溶液中导电复合材料的质量分数为5%-20%。
作为优选,步骤(4)中,水性导电溶液和油性成膜溶液的体积比为0.1-1:1;超声处理时间为10-20min,烘干温度为60-70℃,干燥时间为1-2h。
作为优选,步骤(4)中,所述导电高分子薄膜剪裁后的尺寸为4*30mm,覆盖后其未覆盖区域的尺寸为4*6mm。
作为优选,步骤(6)中,将0.25-0.3g的Na2MoO4·2H2O溶解于25-30毫升的水中,所述盐酸的浓度为0.1M;所述L-半胱氨酸的加入量为0.5-0.55g,所述去离子水的加入量为45-55毫升。
作为优选,步骤(6)中,水热温度为190-210℃,水热时间为30-40h;离心转速为1800-2200rpm, 离心时间为50-70min。
作为优选,步骤(7)中,所述全氟磺酸树脂的浓度为0.4-0.6%,超声分散的时间为50-70min,二硫化钼量子点与全氟磺酸树脂溶液的用量比为0.5-1.5mg/mL。
与现有技术对比,本发明的有益效果是:
1、本发明以丙烯腈-丁二烯-苯乙烯树脂作为导电薄膜的基底,丙烯腈-丁二烯-苯乙烯树脂集合了三个单体的优良性能,即丙烯腈的耐热性、耐油性;丁二烯的耐冲击性;苯乙烯的光泽、成型性。使制备的导电薄膜具有十分的柔软性以及一定的拉伸性。
2、将石墨烯加入到聚苯乙烯磺酸溶液中,超声分散,其目的是为了使石墨烯功能化,将聚苯乙烯磺酸负载到石墨烯上,并以功能化的石墨烯为载体原位聚合聚3,4-乙烯二氧噻吩,使其相互紧密结合。通过聚合的方法得到聚3,4-乙烯二氧噻吩-聚苯乙烯磺酸-石墨烯复合材料由于是通过化学键的作用相互结合在一起,大大增加了电子的迁移速率,提高了薄膜的导电性。
3、二硫化钼是一种典型的过渡金属二维层状硫化物,相较于二硫化钼纳米片层,二硫化钼量子点具有更大的比表面积,更显著的边缘效应,使其在生物医学、光学成像、气体检测等领域更具潜力。在石墨烯和氧化锌纳米管阵列中掺杂二硫化钼量子点,大大得提高传感器灵敏度。
具体实施方式
下面结合实施例对本发明作进一步的描述。
实施例1:
(1)油性成膜溶液的配制
取1g的丙烯腈-丁二烯-苯乙烯树脂添加到20mL的二氯甲烷溶液中,搅拌后静置一天,使丙烯腈-丁二烯-苯乙烯树脂完全溶解到二氯甲烷溶液中,配制出质量分数为5%的丙烯腈-丁二烯-苯乙烯树脂溶液。
(2)聚3,4-乙烯二氧噻吩-聚苯乙烯磺酸-石墨烯导电复合材料的制备
取20mg的石墨烯(加入到20mL的聚苯乙烯磺酸溶液中,超声分散30min,然后加入3,4-乙烯二氧噻吩单体200uL,并在搅拌的情况下逐滴加入10mL、14mmoL/L氯化铁溶液,继续搅拌反应12h,离心分离所制备的墨绿色浆液,并分别用无水乙醇和蒸馏水反复清洗多次至洗涤液无色,收集固体于75℃下真空干燥12h,得到聚3,4-乙烯二氧噻吩-聚苯乙烯磺酸-石墨烯导电复合材料。
(3)水性导电溶液的配制
取1g的聚3,4-乙烯二氧噻吩-聚苯乙烯磺酸-石墨烯导电复合材料添加到20mL的水溶液中,超声分散30min,配制出质量分数为5%的聚3,4-乙烯二氧噻吩-聚苯乙烯磺酸-石墨烯溶液。
(4)高分子导电薄膜的制备
取1mL水性溶液和10mL的油性溶液进行混合,并用超声处理器进行超声处理15min,从而得到混合均一的水油(W/O)导电溶液,取3mL的导电混合液滴定于培养皿,放置24h后,自然干燥,掲下导电薄膜置于65℃恒温烘箱中烘干1.5h。
(5)柔性传感器电极的制备
将步骤(4)得到的导电高分子薄膜剪裁成4*30m的长条状样品,使用固体石蜡和绝缘胶带将导电薄膜的一段面积控制在4*6mm。
(6)二硫化钼量子点的制备
二硫化钼量子点的制备:将0.25gNa2MoO4·2H2O溶解在25mL水中,超声5min;用0.1M盐酸调节PH至6.5;加入0.5g L-半胱氨酸和50mL去离子水,超声5 min;将溶液转移至反应釜,200℃水热反应36h;自然冷却后,离心,转速2000rpm,60min,收集浅棕色的上清液,即为二硫化钼量子点。
(7)二硫化钼量子点修饰的柔性传感器电极
将步骤(6)得到的二硫化钼量子点1mg加入到1mL全氟磺酸树脂溶液(0.5%)中,使用超声机超声分散1h,将分散均匀的二硫化钼量子点滴加到步骤(5)的薄膜电极上,于室温下自然干燥,得到二硫化钼量子点修饰的柔性传感器电极。
实施例2:
(1)油性成膜溶液的配制
取1g的丙烯腈-丁二烯-苯乙烯树脂添加到20mL的二氯甲烷溶液中,搅拌后静置一天,使丙烯腈-丁二烯-苯乙烯树脂完全溶解到二氯甲烷溶液中,配制出质量分数为5%的丙烯腈-丁二烯-苯乙烯树脂溶液。
(2)聚3,4-乙烯二氧噻吩-聚苯乙烯磺酸-石墨烯导电复合材料的制备
取20mg的石墨烯加入到20mL的聚苯乙烯磺酸溶液中,超声分散30min,然后加入3,4-乙烯二氧噻吩单体200uL,并在搅拌的情况下逐滴加入10mL、14mmoL/L氯化铁溶液,继续搅拌反应12h,离心分离所制备的墨绿色浆液,并分别用无水乙醇和蒸馏水反复清洗多次至洗涤液无色,收集固体于75℃下真空干燥12h,得到聚3,4-乙烯二氧噻吩-聚苯乙烯磺酸-石墨烯导电复合材料。
(3)水性导电溶液的配制
取1g的聚3,4-乙烯二氧噻吩-聚苯乙烯磺酸-石墨烯导电复合材料添加到20mL的水溶液中,超声分散30min,配制出质量分数为5%的聚3,4-乙烯二氧噻吩-聚苯乙烯磺酸-石墨烯溶液。
(4)高分子导电薄膜的制备
取5mL水性溶液和10mL的油性溶液进行混合,并用超声处理器进行超声处理15min,从而得到混合均一的水油(W/O)导电溶液,取3mL的导电混合液滴定于培养皿,放置24h后,自然干燥,掲下导电薄膜置于65℃恒温烘箱中烘干1.5h。
(5)柔性传感器电极的制备
将步骤(4)得到的导电高分子薄膜剪裁成4*30m的长条状样品,使用固体石蜡和绝缘胶带将导电薄膜的一段面积控制在4*6mm。
(6)二硫化钼量子点的制备
二硫化钼量子点的制备:将0.25gNa2MoO4·2H2O溶解在25mL水中,超声5min;用0.1M盐酸调节PH至6.5;加入0.5g L-半胱氨酸和50mL去离子水,超声5 min;将溶液转移至反应釜,200℃水热反应36h;自然冷却后,离心,转速2000rpm,60min,收集浅棕色的上清液,即为二硫化钼量子点。
(7)二硫化钼量子点修饰的柔性传感器电极
将步骤(6)得到的二硫化钼量子点1mg加入到1mL全氟磺酸树脂溶液(0.5%)中,使用超声机超声分散1h,将分散均匀的二硫化钼量子点滴加到步骤(5)的薄膜电极上,于室温下自然干燥,得到二硫化钼量子点修饰的柔性传感器电极。
实施例3:
(1)油性成膜溶液的配制
取1g的丙烯腈-丁二烯-苯乙烯树脂添加到20mL的二氯甲烷溶液中,搅拌后静置一天,使丙烯腈-丁二烯-苯乙烯树脂完全溶解到二氯甲烷溶液中,配制出质量分数为5%的丙烯腈-丁二烯-苯乙烯树脂溶液。
(2)聚3,4-乙烯二氧噻吩-聚苯乙烯磺酸-石墨烯导电复合材料的制备
取20mg的石墨烯加入到20mL的聚苯乙烯磺酸溶液中,超声分散30min,然后加入3,4-乙烯二氧噻吩单体200uL,并在搅拌的情况下逐滴加入10mL、14mmoL/L氯化铁溶液,继续搅拌反应12h,离心分离所制备的墨绿色浆液,并分别用无水乙醇和蒸馏水反复清洗多次至洗涤液无色,收集固体于75℃下真空干燥12h,得到聚3,4-乙烯二氧噻吩-聚苯乙烯磺酸-石墨烯导电复合材料。
(3)水性导电溶液的配制
取1g的聚3,4-乙烯二氧噻吩-聚苯乙烯磺酸-石墨烯导电复合材料添加到20mL的水溶液中,超声分散30min,配制出质量分数为5%的聚3,4-乙烯二氧噻吩-聚苯乙烯磺酸-石墨烯溶液。
(4)高分子导电薄膜的制备
取10mL水性溶液和10mL的油性溶液进行混合,并用超声处理器进行超声处理15min,从而得到混合均一的水油(W/O)导电溶液,取3mL的导电混合液滴定于培养皿,放置24h后,自然干燥,掲下导电薄膜置于65℃恒温烘箱中烘干1.5h。
(5)柔性传感器电极的制备
将步骤(4)得到的导电高分子薄膜剪裁成4*30m的长条状样品,使用固体石蜡和绝缘胶带将导电薄膜的一段面积控制在4*6mm。
(6)二硫化钼量子点的制备
二硫化钼量子点的制备:将0.25gNa2MoO4·2H2O溶解在25mL水中,超声5min;用0.1M盐酸调节PH至6.5;加入0.5g L-半胱氨酸和50mL去离子水,超声5 min;将溶液转移至反应釜,200℃水热反应36h;自然冷却后,离心,转速2000rpm,60min,收集浅棕色的上清液,即为二硫化钼量子点。
(7)二硫化钼量子点修饰的柔性传感器电极
将步骤(6)得到的二硫化钼量子点1mg加入到1mL全氟磺酸树脂溶液(0.5%)中,使用超声机超声分散1h,将分散均匀的二硫化钼量子点滴加到步骤(5)的薄膜电极上,于室温下自然干燥,得到二硫化钼量子点修饰的柔性传感器电极。
本发明中所用原料、设备,若无特别说明,均为本领域的常用原料、设备;本发明中所用方法,若无特别说明,均为本领域的常规方法。
以上所述,仅是本发明的较佳实施例,并非对本发明作任何限制,凡是根据本发明技术实质对以上实施例所作的任何简单修改、变更以及等效变换,均仍属于本发明技术方案的保护范围。
Claims (9)
1.一种二硫化钼量子点修饰的柔性传感器电极的制备方法,其特征在于包括如下步骤:
(1)油性成膜溶液的配制:将丙烯腈-丁二烯-苯乙烯树脂添加到二氯甲烷溶液中,搅拌后静置使丙烯腈-丁二烯-苯乙烯树脂完全溶解,得到油性成膜溶液,待用;
(2)聚3,4-乙烯二氧噻吩-聚苯乙烯磺酸-石墨烯导电复合材料的制备:将石墨烯加入到聚苯乙烯磺酸溶液中,超声分散,然后加入3,4-乙烯二氧噻吩单体,并在搅拌条件下逐滴加入氯化铁溶液,继续搅拌反应10-14h,离心分离所得的墨绿色浆液,并分别用无水乙醇和蒸馏水反复清洗多次至洗涤液为无色,收集固体,70-80℃下真空干燥10-14h,得到聚3,4-乙烯二氧噻吩-聚苯乙烯磺酸-石墨烯导电复合材料;
(3)水性导电溶液的配制:将步骤(2)所得的导电复合材料添加到水溶液中,超声分散,得到水性导电溶液,待用;
(4)高分子导电薄膜的制备:将步骤(3)所得的水性导电溶液和步骤(1)所得的油性成膜溶液进行混合,超声处理,得到混合均一的水油导电溶液,取水油导电溶液滴定于培养皿,放置20-28h后,自然干燥后得到高分子导电薄膜,掲下高分子导电薄膜后烘干;
(5)柔性传感器电极的制备:将步骤(4)所得的导电高分子薄膜剪裁成长条状样品,用固体石蜡和绝缘胶带将导电薄膜进行固定并对其部分区域进行覆盖;
(6)二硫化钼量子点的制备:将Na2MoO4·2H2O溶解于水中,超声4-6min;用盐酸调节pH至6-7;加入L-半胱氨酸和去离子水,超声4-6min;将溶液转移至反应釜进行水热反应,自然冷却后,离心,收集浅棕色的上清液,得到二硫化钼量子点;
(7)二硫化钼量子点修饰的柔性传感器电极的制备:将步骤(6)所得的二硫化钼量子点加入到全氟磺酸树脂溶液中,超声分散均匀,然后再将其滴加到步骤(5)所得的导电高分子薄膜的未覆盖区域上,于室温下自然干燥,得到二硫化钼量子点修饰的柔性传感器电极。
2.如权利要求1所述的一种二硫化钼量子点修饰的柔性传感器电极的制备方法,其特征在于,步骤(1)中,所述油性成膜溶液中丙烯腈-丁二烯-苯乙烯树脂的质量分数为5%-20%。
3.如权利要求1所述的一种二硫化钼量子点修饰的柔性传感器电极的制备方法,其特征在于,步骤(2)中,石墨烯与聚苯乙烯磺酸、聚3,4-乙烯二氧噻吩、氯化铁的质量比为1-2:1-2:1-3:1-3。
4.如权利要求1所述的一种二硫化钼量子点修饰的柔性传感器电极的制备方法,其特征在于,步骤(3)中,超声分散的时间为25-35min,水性导电溶液中导电复合材料的质量分数为5%-20%。
5.如权利要求1所述的一种二硫化钼量子点修饰的柔性传感器电极的制备方法,其特征在于,步骤(4)中,水性导电溶液和油性成膜溶液的体积比为0.1-1:1;超声处理时间为10-20min,烘干温度为60-70℃,干燥时间为1-2h。
6.如权利要求1所述的一种二硫化钼量子点修饰的柔性传感器电极的制备方法,其特征在于,步骤(4)中,所述导电高分子薄膜剪裁后的尺寸为4*30mm,覆盖后其未覆盖区域的尺寸为4*6mm。
7.如权利要求1所述的一种二硫化钼量子点修饰的柔性传感器电极的制备方法,其特征在于,步骤(6)中,将0.25-0.3g的Na2MoO4·2H2O溶解于25-30毫升的水中,所述盐酸的浓度为0.1M;所述L-半胱氨酸的加入量为0.5-0.55g,所述去离子水的加入量为45-55毫升。
8.如权利要求1或7所述的一种二硫化钼量子点修饰的柔性传感器电极的制备方法,其特征在于,步骤(6)中,水热温度为190-210℃,水热时间为30-40h;离心转速为1800-2200rpm, 离心时间为50-70min。
9.如权利要求1所述的一种二硫化钼量子点修饰的柔性传感器电极的制备方法,其特征在于,步骤(7)中,所述全氟磺酸树脂的浓度为0.4-0.6%,超声分散的时间为50-70min,二硫化钼量子点与全氟磺酸树脂溶液的用量比为0.5-1.5mg/mL。
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