CN108467029A - 一种柔性、自支撑的Pd/还原氧化石墨烯纸、制备方法及其应用 - Google Patents
一种柔性、自支撑的Pd/还原氧化石墨烯纸、制备方法及其应用 Download PDFInfo
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Abstract
本发明公开了一种柔性、自支撑的Pd/还原氧化石墨烯纸、制备方法及其应用。本发明中采用简单的一锅法共还原,在聚乙烯吡咯烷酮的参与下,使用水浴加热法利用水合肼共还原PdCl2与氧化石墨烯,而后利用简单的真空抽滤方法制备柔性、自支撑的Pd/还原氧化石墨烯纸。本发明的有益效果在于:合成工艺简单,可大批量制备,适用于规模化生产和应用。将发明得到的柔性、自支撑材料制备成葡萄糖电化学传感器,该葡萄糖传感器对葡萄糖表现出快速的响应、较宽的线性响应范围,以及具有较高的灵敏度。
Description
技术领域
本发明涉及柔性材料设计与传感器技术领域,具体地说,涉及一种柔性、自支撑的Pd/还原氧化石墨烯纸、制备方法及其应用。
背景技术
近年来,便携式和可穿戴设备的发展给人们的生活带来了极大的便利。然而,为便携式和可穿戴设备寻找一种低成本、质量轻的理想化功能材料仍然是一项挑战。由于柔性的、自支撑导电纸基材料在传感器、锂离子电池、超级电容器、燃料电池与储氢器件等领域的都具有潜在的应用,其可能成为便携式和可穿戴设备的功能化材料选项之一。
石墨烯是一种具有sp2杂化的碳二维(2D)原子薄片,由于其独特的热学、机械、化学和电学性质,其已然成为一种明星材料。氧化石墨烯(graphene oxide, GO)的基面与边缘上包含氧官能团,使其易于在水中分散。另一方面,由于含氧官能团破坏了sp2成键的网络,使得氧化石墨烯的导电性较差。然而,较差的电导率可能会限制GO在电学上或者电化学领域方面的应用,如超级电容器、燃料电池、锂离子电池和传感器。为了恢复GO的电导率,应除去其大部分含氧官能团,因此应实现GO的还原。而获得的还原氧化石墨烯(reducedgraphene oxide, rGO)由于其在水中的聚集趋势,难以在水中很好地分散。
现今,包括电、光、质敏、热等各类传感器已经被广泛地投入到环境分析、工业生产与医疗诊断等领域的基础研究和实际应用当中。其中,电化学传感器具有设备简单、廉价、响应快和易于微型化等优点,被广泛应用于葡萄糖传感器的制备。随着便携式与可穿戴设备的发展,制备一种新型的、柔性的、可自支撑的葡萄糖电化学传感器具有重要意义。糖尿病是与血糖浓度失调相关的最显著疾病,是继恶性肿瘤、心脑血管后致死率排名第3的非传染性疾病。持续性高血糖可对人体健康造成长期损害并伴随着多器官的功能衰竭(眼睛、肾脏、神经、心脏与血管)。糖尿病是世界性的公共健康问题,根据国际糖尿病联盟(IDF)统计,2017年,全球范围内,20-79岁成年人中有4.25亿患有糖尿病。因此,实现葡萄糖的检测,尤其是基于柔性的、可自支撑材料的葡萄糖检测具有重要意义。
发明内容
为了克服现有技术的不足,本发明的目的在于提供一种柔性、自支撑的Pd/还原氧化石墨烯纸、制备方法及其应用。本发明基于一锅法共还原制备Pd/还原氧化石墨烯纸,工艺简单;获得的Pd/还原氧化石墨烯纸可用作葡萄糖电化学传感器,其对葡萄糖表现出快速的响应、较宽的线性响应范围,以及具有较高的灵敏度。
本发明的目的是通过以下技术方案来实现的。
本发明提供一种柔性、自支撑的Pd/还原氧化石墨烯纸的制备方法,具体步骤如下:
(1)分别取2-20mL 1mg/mL GO,0.1-1mmol 可溶性含钯前驱体与5-2000mg聚乙烯吡咯烷酮PVP,而后使用去离子水稀释至70mL,搅拌、超声混合均匀,得到棕色溶液;
(2)将混合均匀后的溶液水浴加热至80-100℃后,逐滴加入2-30mL 85wt%的水合肼溶液,继续反应0.5-3 h;
(3)反应结束后,冷却至室温,再继续超声分散0.5-3h;
(4)将超声分散后的溶液倒入抽滤器中,使用孔径0.22-0.45μm的水系滤膜真空抽滤;
(5)溶液抽滤完全后,将滤膜从抽滤器上取下,于室温环境下放置10-15h,最后将获得的Pd/还原氧化石墨烯纸从滤膜上剥离。
本发明中,步骤(2)中,可溶性含钯前驱体选自PdCl2,H2PdCl4,Na2PdCl4或K2PdCl4中的一种或几种。
本发明中,步骤(2)中,5-10mL 1mg/mL GO,0.1-0.5mmol 可溶性含钯前驱体,50-100mg聚乙烯吡咯烷酮PVP。
本发明中,步骤(2)中,水浴加热至80-90℃,85wt%的水合肼溶液的体积为8~15mL。
本发明还提供一种上述的制备方法制得的柔性、自支撑的Pd/还原氧化石墨烯纸。
本发明进一步提供一种上述的柔性、自支撑的Pd/还原氧化石墨烯纸在制备葡萄糖传感器中的应用。
与现有技术相比,本发明的有益效果在于:
本发明采用简单的水浴加热合成法,一锅反应共还原得到Pd与rGO的混合物,而后通过简单的真空抽滤法得到柔性、自支撑的Pd/还原氧化石墨烯纸。该方法简化了真空抽滤法制备金属粒子修饰的还原氧化石墨烯纸(rGO paper, rGOP)步骤,并且可获得rGO层间掺杂Pd粒子的材料结构。将该材料裁剪直接使用,或者将材料贴附于电极表面,制备出一种葡萄糖电化学传感器,构建的电化学传感器对葡萄糖检测具有快速的响应(<5s)、较宽的线性响应范围(0.5-8 mM),以及具有较高的灵敏度(0.4176 µA mM-1)等优点。
附图说明
图1为实施例1制得的Pd/还原氧化石墨烯纸的数码照片。
图2为实施例1制得的Pd/还原氧化石墨烯纸的400倍的扫描电镜(SEM)照片。
图3为实施例1制得的Pd/还原氧化石墨烯纸的扫描电镜(SEM)照片。
图4为实施例2制得的Pd/还原氧化石墨烯纸的XRD图谱。
图5为实施例5制得的Pd/还原氧化石墨烯纸的扫描电镜(SEM)照片。
图6为实施例10制得的Pd/还原氧化石墨烯纸电极对葡萄糖的电化学循环伏安测试图。
图7为实施例11制得的Pd/还原氧化石墨烯纸电极对葡萄糖的在不同电位下的响应电流曲线图。
图8为实施例11制得的Pd/还原氧化石墨烯纸电极在电位0.4V下对不同浓度葡萄糖的计时电流响应图。
具体实施方式
以下提供本发明柔性、自支撑的Pd/还原氧化石墨烯纸葡萄糖电化学传感器的制备实施例。
实施例1:Pd/还原氧化石墨烯纸的制备
(1) 分别取5mL 1mg/mL GO,50mg PdCl2与50mg PVP,而后使用去离子水稀释至70mL,搅拌、超声混合均匀,得到棕色溶液;
(2)将混合均匀后的溶液转移至烧瓶中,水浴加热至90 ℃;
(3)向烧瓶中逐滴加入10mL 85%的水合肼溶液,继续反应1 h;
(4)冷却至室温后,将反应混合物转移至烧杯中,超声分散0.5h;
(5)将超声分散后的溶液倒入抽滤器中,使用孔径0.22μm的水系滤膜真空抽滤;
(6)溶液抽滤完全后,将滤膜从抽滤器上取下,于室温环境下放置过夜。使用前可将获得的Pd/还原氧化石墨烯纸从滤膜上剥离,其数码照片见图1,扫描电镜图见图2,图3。图2所示,所获得的Pd/还原氧化石墨烯纸表面褶皱较为明显,Pd粒子均匀点缀于还原石墨烯纸上,且隐约可见部分Pd粒子嵌于还原石墨烯层间。图3所示,a方框区域为位于还原石墨烯纸较靠近表面的Pd粒子;b方框区域为位于还原石墨烯纸表面以下若干层的Pd粒子。由此可见,所获得的Pd/还原氧化石墨烯纸为rGO层间掺杂Pd粒子的材料结构。
实施例2:Pd/还原氧化石墨烯纸的制备
将实施例1的步骤(1)中的PVP的质量为50mg,改为PVP的质量为100mg,其他步骤和条件都与实施例1相同,得到Pd/还原氧化石墨烯纸,其XRD图谱见图4。其中,22.6°的衍射峰应归因于还原石墨烯片中的C(200)短程有序排列。根据布拉格定律,碳(200)在22.6°的衍射峰对应于0.40nm的晶格间距。 除了C(200)的衍射峰之外,Pd/还原氧化石墨烯纸在40.2°,46.7°和68.3°处的衍射峰则分别对应Pd晶体的(111),(200)和(220) 晶面,表明晶体Pd的存在。
实施例3:Pd/还原氧化石墨烯纸的制备
将实施例1的步骤(1)中的PdCl2的质量为50mg,改为PdCl2的质量为20mg,其他步骤和条件都与实施例1相同,得到Pd/还原氧化石墨烯纸。
实施例4:Pd/还原氧化石墨烯纸的制备
将实施例1的步骤(2)中的90℃的水浴温度用80 ℃的水浴温度替换,其他步骤和条件都与实施例1相同,得到Pd/还原氧化石墨烯纸。
实施例5:Pd/还原氧化石墨烯纸的制备
将实施例1的步骤(1)中的PVP的质量为50mg改为PVP的质量为5mg,其他步骤和条件都与实施例1相同,得到Pd/还原氧化石墨烯纸,其扫描电镜图见图5。PVP的量减少后,所获得的还原石墨烯纸表面褶皱明显减少,Pd粒子的分布没有较大改变。
实施例6:Pd/还原氧化石墨烯纸的制备
将实施例1的步骤(1)中,5mL 1mg/mL GO改为10mL 1mg/mL GO,其他步骤和条件都与实施例1相同,得到Pd/还原氧化石墨烯纸。
实施例7:电极的制备
将Pd/还原氧化石墨烯纸裁切成0.5cm*1cm方条状,使用鳄鱼夹夹持电极后,测试其葡萄糖传感性能。
实施例8:电极的制备
使用打孔器将Pd/还原氧化石墨烯纸冲打出直径5mm圆片,贴附于电极上后使用孔径3mm聚四氟乙烯板夹持,测试其葡萄糖传感性能。
实施例9:电极的制备
使用打孔器将Pd/还原氧化石墨烯纸冲打出直径3mm圆片,贴附于电极上后,在电极表面滴加5μL 0.5% Nafion溶液将其固定,测试其葡萄糖传感性能。
实施例10:所制备电极对葡萄糖的电化学行为测试
使用CHI760e电化学工作站对实施例1方法获得的Pd/还原氧化石墨烯纸,使用实施例9方法所制备电极对葡萄糖的电化学行为测试。使用0.1M NaOH作为底液,测试加入30mM葡萄糖前后的电化学循环伏安曲线,扫描范围-0.8V-0.8V(vs.SCE),扫速50mVs-1。所制备电极在加入30mM葡萄糖前,在电位-0.46V处有Pd的氧吸附物种还原峰;加入30mM葡萄糖后,在电位-0.07V与-0.46V处分别有一个葡萄糖的氧化峰。表明所制备电极对葡萄糖有良好的电催化氧化性能,所得电化学循环伏安图如图6所示。
实施例11:所制备电极对葡萄糖的传感测试
使用CHI760e电化学工作站对实施例1方法获得的Pd/还原氧化石墨烯纸,使用实施例9方法所制备电极进行葡萄糖的电化学传感测试。分别在0.1M NaOH溶液中磁力搅拌情况下,控制不同电位,向溶液中加入2mM葡萄糖,测试所制备电极在不同电位下对葡萄糖的响应电流,测试结果如图7所示。在电位0.4V(vs.SCE)时,对2mM葡萄糖响应最大,约为1.21 µA。而后,在电位0.4V时,在磁力搅拌情况下,向20mL 0.1M NaOH溶液每隔50s滴加不同浓度葡萄糖,所得到的计时电流曲线图如图8所示。所制备电极对葡萄糖的响应时间在5s以内,线性范围为0.5-8 mM,其对应的电流灵敏度为0.4176 µA mM-1。说明Pd/还原氧化石墨烯纸电极对葡萄糖有良好的电化学传感性能。
以上实施例的说明仅是本发明的优选实施方式,应当指出,对于所述技术领域的普通技术人员来说,在不脱离本发明构思的前提下,还可以对本发明进行若有改进和修饰,这些改进和修饰也应视为本发明权利要求的保护范围内。
Claims (6)
1.一种柔性、自支撑的Pd/还原氧化石墨烯纸的制备方法,其特征在于,具体步骤如下:
(1)分别取2-20mL 1mg/mL GO,0.1-1mmol 可溶性含钯前驱体与5-2000mg聚乙烯吡咯烷酮PVP,而后使用去离子水稀释至70mL,搅拌、超声混合均匀,得到棕色溶液;
(2)将混合均匀后的溶液水浴加热至80-100℃后,逐滴加入2-30mL 85wt%的水合肼溶液,继续反应0.5-3 h;
(3)反应结束后,冷却至室温,再继续超声分散0.5-3h;
(4)将超声分散后的溶液倒入抽滤器中,使用孔径0.22-0.45μm的水系滤膜真空抽滤;
(5)溶液抽滤完全后,将滤膜从抽滤器上取下,于室温环境下放置10-15h,最后将获得
的Pd/还原氧化石墨烯纸从滤膜上剥离。
2.根据权利要求1所述的制备方法,其特征在于,步骤(2)中,可溶性含钯前驱体选自PdCl2,H2PdCl4,Na2PdCl4或K2PdCl4中的一种或几种。
3.根据权利要求1所述的制备方法,其特征在于,步骤(2)中,5-10mL 1mg/mL GO,0.1-0.5mmol 可溶性含钯前驱体,50-100mg聚乙烯吡咯烷酮PVP。
4.根据权利要求1所述的制备方法,其特征在于,步骤(2)中,水浴加热至80-90℃,85wt%的水合肼溶液的体积为8~15mL。
5.一种根据权利要求1~4之一所述的制备方法制得的柔性、自支撑的Pd/还原氧化石墨烯纸。
6.一种根据权利要求5所述的柔性、自支撑的Pd/还原氧化石墨烯纸在制备葡萄糖传感器中的应用。
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