电化学法直接制备纳米金及其应用
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摘要
本论文研究了一种直接在ITO透明导电玻璃上制备纳米金的方法。以ITO玻璃作基底,2.0mmolL~(-1)的亚金氰化钾溶液(pH=8.0)为镀液,采用电化学法在ITO玻璃上直接制备纳米金粒子。通过对镀液温度,循环伏安的扫描圈数、电位范围以及扫描速度等因素的考察,确定最佳试验条件,分别制备了平均粒径约为48nm的纳米金膜和平均粒径约为24nm的纳米金阵列。并借助紫外-可见光度法、扫描电子显微镜、铁氰化钾分子探针、0.05M的硫酸和交流阻抗法对纳米金膜和纳米金阵列进行了表征。
结合自组装法、纳米技术和溶胶-凝胶(SG)法,将本法制备的纳米金膜电极(GFE)和纳米金阵列电极(GAE)用于制备超氧化物歧化酶传感器,对其电化学行为进行了研究,其式量电位分别为100mV和99mV(参比电极为饱和甘汞电极),呈现准可逆的电化学过程。以二甲亚砜/氢氧化钠体系产生超氧阴离子,研究了酶电极对O_2·~-的响应性能。结果证明酶电极对超氧阴离子有明显的响应,且响应信号与O_2·~-/DMSO溶液的注入量呈线性关系。酶电极在4℃下放置90天后,在该期间间歇性使用,SOD-cys-GS/GFE对超氧阴离子的响应仍保持原来的92%以上,SOD-cys-GS/GAE保持原来的85%以上。并实现了SOD-cys-GS/GFE对污泥系统中O_2·~-的检测。
将本法制备的纳米金膜电极(GFE)和纳米金阵列电极(GAE)采用自组装法制备辣根过氧化物酶(HRP)传感器,对其电化学行为进行了研究。实现了HRP酶电极的直接电子传递,并考察了电极的稳定性。检测H_2O_2的线性范围分别为5.0μmolL~(-1)~4.2mmolL~(-1)和8.0μmolL~(-1)~3.0mmolL~(-1),检出限分别为0.57μmolL~(-1)和0.6μmolL~(-1)(信噪比为3),米氏常数分别为1.6mmolL~(-1)和0.40mmolL~(-1)。HRP/cys/GFE在4℃下放置85天后,在此期间间歇性使用,对H_2O_2的响应仍保持原来的90%以上,HRP/cys/GAE保持原来的83%以上。实现了HRP/cys/GFE对实际样品的检测。
An effecttive approach to deposit gold nanoparticles (AuNPs) directly on indium tin oxide (ITO) surface through electrochemical method is reported. Using 2.0mmolL~(-1) KAu(CN)2 (pH=8.0) as electroplating solution, the AuNPs were prepared on the ITO surface by CV. Several electroplate factors were studied through single-factor experiments. These factors are the temperature of the electroplating solution, the sweep segments of CV, the potential range, and the scan rate. Then at the best condition, AuNPs with the average sizes about 48nm of gold-nanoparticle film and 24nm of gold-nanoparticle array were prepared. The AuNPs were characterized by UV-vis, SEM, and electrochemical motheds.
The gold-nanoparticle film electrodes(GFE) and gold-nanoparticle array electrodes(GAE) were applied to fabricate SOD biosensors with self-assembled monolayers, nanothechnology and sol-gel(SG) technology. The electrochemical characteristics of the biosensors were studied. The formal potential were 100mV and 99mV (versus SCE), respectively. The electrode process of SOD is quasi-reversible. The SOD electrodes were used to response to superoxide anion, which was prepared by DMSO/NaOH systems. The biosensors displayed an excellent electrocatalytial response to reduction of O_2·~- without the aid of an electron mediator. The biosensors exhibited high sensitivity, rapid response and long-stability.
The GFE and GAE were also applied to fabricate HRP biosensors with self-assembled monolayers, and the electrochemical characteristics of the biosensors were studied. The biosensors displayed an excellent electrocatalytial response to reduction of H_2O_2. The calibration range of H_2O_2 were 5.0μmolL~(-1)~4.2mmolL~(-1) and 8.0μmolL~(-1)~3.0mmolL~(-1), with detection limits of 0.57μmolL~(-1) and 0.6μmolL~(-1) at a signal-to-noise ratio of 3, respectively. The KMapp value of HRP immobilized on the electrodes surface were found to be 1.6 mmolL~(-1) and 0.40mmolL~(-1), respectively. The biosensors exhibited high sensitivity, rapid response and long-term stability.
结合自组装法、纳米技术和溶胶-凝胶(SG)法,将本法制备的纳米金膜电极(GFE)和纳米金阵列电极(GAE)用于制备超氧化物歧化酶传感器,对其电化学行为进行了研究,其式量电位分别为100mV和99mV(参比电极为饱和甘汞电极),呈现准可逆的电化学过程。以二甲亚砜/氢氧化钠体系产生超氧阴离子,研究了酶电极对O_2·~-的响应性能。结果证明酶电极对超氧阴离子有明显的响应,且响应信号与O_2·~-/DMSO溶液的注入量呈线性关系。酶电极在4℃下放置90天后,在该期间间歇性使用,SOD-cys-GS/GFE对超氧阴离子的响应仍保持原来的92%以上,SOD-cys-GS/GAE保持原来的85%以上。并实现了SOD-cys-GS/GFE对污泥系统中O_2·~-的检测。
将本法制备的纳米金膜电极(GFE)和纳米金阵列电极(GAE)采用自组装法制备辣根过氧化物酶(HRP)传感器,对其电化学行为进行了研究。实现了HRP酶电极的直接电子传递,并考察了电极的稳定性。检测H_2O_2的线性范围分别为5.0μmolL~(-1)~4.2mmolL~(-1)和8.0μmolL~(-1)~3.0mmolL~(-1),检出限分别为0.57μmolL~(-1)和0.6μmolL~(-1)(信噪比为3),米氏常数分别为1.6mmolL~(-1)和0.40mmolL~(-1)。HRP/cys/GFE在4℃下放置85天后,在此期间间歇性使用,对H_2O_2的响应仍保持原来的90%以上,HRP/cys/GAE保持原来的83%以上。实现了HRP/cys/GFE对实际样品的检测。
An effecttive approach to deposit gold nanoparticles (AuNPs) directly on indium tin oxide (ITO) surface through electrochemical method is reported. Using 2.0mmolL~(-1) KAu(CN)2 (pH=8.0) as electroplating solution, the AuNPs were prepared on the ITO surface by CV. Several electroplate factors were studied through single-factor experiments. These factors are the temperature of the electroplating solution, the sweep segments of CV, the potential range, and the scan rate. Then at the best condition, AuNPs with the average sizes about 48nm of gold-nanoparticle film and 24nm of gold-nanoparticle array were prepared. The AuNPs were characterized by UV-vis, SEM, and electrochemical motheds.
The gold-nanoparticle film electrodes(GFE) and gold-nanoparticle array electrodes(GAE) were applied to fabricate SOD biosensors with self-assembled monolayers, nanothechnology and sol-gel(SG) technology. The electrochemical characteristics of the biosensors were studied. The formal potential were 100mV and 99mV (versus SCE), respectively. The electrode process of SOD is quasi-reversible. The SOD electrodes were used to response to superoxide anion, which was prepared by DMSO/NaOH systems. The biosensors displayed an excellent electrocatalytial response to reduction of O_2·~- without the aid of an electron mediator. The biosensors exhibited high sensitivity, rapid response and long-stability.
The GFE and GAE were also applied to fabricate HRP biosensors with self-assembled monolayers, and the electrochemical characteristics of the biosensors were studied. The biosensors displayed an excellent electrocatalytial response to reduction of H_2O_2. The calibration range of H_2O_2 were 5.0μmolL~(-1)~4.2mmolL~(-1) and 8.0μmolL~(-1)~3.0mmolL~(-1), with detection limits of 0.57μmolL~(-1) and 0.6μmolL~(-1) at a signal-to-noise ratio of 3, respectively. The KMapp value of HRP immobilized on the electrodes surface were found to be 1.6 mmolL~(-1) and 0.40mmolL~(-1), respectively. The biosensors exhibited high sensitivity, rapid response and long-term stability.
引文
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