CN110216295A - 一种银纳米花的室温水相制备方法及其葡萄糖电催化氧化 - Google Patents
一种银纳米花的室温水相制备方法及其葡萄糖电催化氧化 Download PDFInfo
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Abstract
本专利涉及一种银纳米花的室温水相制备方法,属于金属纳米材料制备方法的技术领域。制备过程包括:配置前驱物硝酸银(AgNO3)溶液,加入络合剂柠檬酸钠(Na3Cit),室温磁力搅拌1小时,加入维生素C粉末,室温磁力搅拌一定时间(1‑6小时)即可得到银纳米花。制备过程中通过调节还原剂维生素C与硝酸银的摩尔比为(0.25‑1):1,可制备出不同尺寸(100‑1000纳米)的银纳米花。本发明方法简单、绿色环保,所制备的银纳米化尺寸形貌分布均一,且形貌及尺寸可控,利于批量制备银纳米花催化剂。并且此制备方法所制备出的银纳米花在葡萄糖电催化氧化应用中表现优异,在能源催化应用领域展现出潜力。
Description
技术领域
本发明涉及一种银纳米花的室温水相制备方法,利用该方法能够高效、绿色、快捷、大规模地制备出银纳米花,属于贵金属纳米催化剂制备的技术领域。
背景技术
银相比较其他的贵金属材料,价格相对便宜,且在催化,表面拉曼增强(SERS),荧光增强,抗菌性等方面表现优异,并且银纳米材料具有优良的生物相容性,在免疫标记、细胞染色、DNA检测、药物和基因载体、生物传感器等领域均有重要应用价值。随着纳米科技的逐步发展,人们发现纳米材料的功能性与其形貌紧密相连。数十年来,大量的研究工作围绕银纳米材料的形貌设计、尺寸调控、生长机制及相关应用而展开。目前,对于银纳米结构的形貌设计方面往往采取加入表面活性剂的方案,如PVP、CTAB等表面活性剂稳定银纳米晶的某一特定晶面降低该晶面表面能获得相应形貌,但是表面活性剂的引入却破坏了生物相容性的优势。因此,发展一种不借助表面活性剂的绿色水相制备方法,例如直接利用对身体无害的弱还原剂批量获取形貌尺寸可控的银纳米材料,将有利于银纳米材料的工业化应用。
发明内容
本发明的目的在于开发一种简单绿色、便捷规模的合成方案制备银纳米花,利用柠檬酸钠作为络合剂控制反应溶液中的银离子浓度,弱还原剂维生素C还原银离子获得银纳米花,通过控制维生素C与硝酸银的质量比获得不同尺寸的银纳米花。
具体技术方案如下:
首先,称量1.156克硝酸银溶于10毫升去离子水为溶液①;随后,称量0.217克柠檬酸钠溶于17毫升去离子水中,置于磁力搅拌器上搅拌至完全溶解,为溶液②;取3毫升溶液①加入到溶液②中为溶液③,继续磁力搅拌溶液③,溶液③由无色转变为白色悬浊液,持续搅拌1小时待络合均匀;最后称量0.1克维生素C粉末加入溶液③中为溶液④,磁力搅拌一定时间(1-6小时),溶液④由白色悬浊液逐渐变澄清、随后转为浅蓝又逐渐变灰,将灰色溶液④离心洗样干燥即可获得银纳米花粉末样品。此外,通过调节还原剂维生素C与硝酸银的摩尔比为(0.25-1):1,实现尺寸可控(100到1000纳米)的银纳米花的制备。
综上所述,本发明一种银纳米花的室温水相制备方法及其葡萄糖电催化氧化有以下有益效果:
可以制备出尺寸均一的银纳米花。这种形貌的银纳米花具有高的比表面积、丰富的高指数晶面等结构优势,可以暴露出更多的活性位点,大大增加其理化性质。
实现银纳米花尺寸由100纳米到1000纳米可调。
此制备方法简单、绿色,可实现大规模制备,有利于能源催化的工业化利用。
此方案所制备的银纳米花在葡萄糖电催化氧化中表现优异,其葡萄糖电催化氧化电流密度可达2.86 mA cm-2。
附图说明
图1是实施例1制备的100纳米银纳米花的扫描电镜照片。
图2是实施例1制备的100纳米银纳米花的放大的扫描电镜照片.
图3是实施例2制备的300纳米银纳米花的扫描电镜照片。
图4是实施例3制备的500纳米银纳米花的扫描电镜照片。
图5是实施例4制备的800纳米银纳米花的扫描电镜照片。
图6是实施例5制备的1000纳米银纳米花的扫描电镜照片。
图7是实施例1产物的XRD衍射图。
图8是实施例1产物在0.1摩尔每升的NaOH溶液中的氧化还原电位测试。
图9是实施例1产物在含有浓度为10毫摩尔每升的葡萄糖/NaOH溶液中葡萄糖电催化氧化测试。
具体实施方式
实施例1:
首先,称量1.156克硝酸银溶于10毫升去离子水为溶液①;随后,称量0.217克柠檬酸钠溶于17毫升去离子水中,置于磁力搅拌器上搅拌至完全溶解,为溶液②;取3毫升溶液①加入到溶液②中为溶液③,继续磁力搅拌溶液③,溶液③由无色转变为白色悬浊液,持续搅拌1小时待络合均匀;最后称量0.1克维生素C粉末加入溶液③中为溶液④,磁力搅拌一定时间(1-6小时),溶液④由白色悬浊液逐渐变澄清、随后转为浅蓝又逐渐变灰,白色悬浊液逐渐变澄清、随后由浅蓝变灰色,利用离心机将以上混合溶液离心洗样,依次分散于去离子水和无水乙醇中多次反复洗样,经烘箱干燥后制得100纳米银纳米花粉末。 如图1、图2、图7所示,分别为100纳米银纳米花的扫描电镜照片及XRD图谱。
实施例2:
制备过程同实施例1类似,只是将所加入的维生素C粉末的质量增加为0.15克,其余过程均与一致实施例1。最终经离心洗样干燥获得300纳米银纳米花,如图3所示为其扫描电镜照片。
实施例3:
制备过程同实施例1类似,只是将所加入的维生素C粉末的质量增加为0.2克,其余过程均与一致实施例1。最终经离心洗样干燥获得500纳米银纳米花,如图4所示为其扫描电镜照片。
实施例4:
制备过程同实施例1类似,只是将所加入的维生素C粉末的质量增加为0.25克,其余过程均与一致实施例1。最终经离心洗样干燥获得800纳米银纳米花,如图5所示为其扫描电镜照片。
实施例5:
制备过程同实施例1类似,只是将所加入的维生素C粉末的质量增加为0.3克,其余过程均与一致实施例1。最终经离心洗样干燥获得1000纳米银纳米花,如图6所示为其扫描电镜照片。
实施例6:
将实施例1中所获得的产物银配置成纳米花墨汁,取4微升置于干净的玻碳工作电极上,待自然晾干后,利用电化学工作站,电解液为0.1摩尔每升的NaOH,首先设置测试量程为0v到1.8v(vs.RHE)测试其特征氧化还原峰,如图8所示为银纳米花在碱性条件下的特征氧化还原峰。然后,向以上电解液中加入葡萄糖,配置成10毫摩尔每升的葡萄糖/NaOH溶液,设置测试电位量程为0-1.6v(vs.RHE),以扫速为0.1v/s进行测试。如图9为银纳米花的葡萄糖电催化氧化情况。从图中我们可以观测到葡萄糖的特征氧化峰,三个特征氧化峰位为1.04V(vs.RHE)、1.41V(vs.RHE)、1.06 V(vs.RHE),在1.41V处的电流密度为2.86 mA cm-2,催化性能表现出色。
显然,本发明的上述实施例仅仅是为清楚地说明本发明所作的举例,而并非是对本发明的实施方式的限定。凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等,均应包含在本发明权利要求的保护范围之内。
Claims (2)
1.一种银纳米花的室温水相制备方法,其特征在于,包含以下实验步骤:以去离子水为溶剂,硝酸银为前驱物溶质,首先,称量1.156克硝酸银溶于10毫升去离子水为溶液①;随后,称量0.217克柠檬酸钠溶于17毫升去离子水中,置于磁力搅拌器上搅拌至完全溶解,为溶液②;取3毫升溶液①加入到溶液②中为溶液③,继续磁力搅拌溶液③,溶液③由无色转变为白色悬浊液,持续搅拌1小时待络合均匀;最后称量0.1克维生素C粉末加入溶液③中为溶液④,磁力搅拌一定时间(1-6小时),溶液④由白色悬浊液逐渐变澄清、随后转为浅蓝又逐渐变灰,将灰色溶液④离心洗样干燥即可获得银纳米花粉末样品。
2.根据权利要求1中所述的一种银纳米花的室温水相制备方法,其特征在于,通过调节还原剂维生素C与硝酸银的摩尔比为(0.25-1):1,可实现尺寸由100到1000纳米银花的可控制备;且此类银纳米花在葡萄糖电催化氧化应用中表现优异,其葡萄糖电催化氧化电流密度可达2.86 mA cm-2。
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