针对电化学传感和光电化学优化的银纳米粒子—碳复合电极
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摘要
随着当今社会的发展,能源与健康问题已成为人类要面临的两大挑战。为了解决可能发生的能源危机,世界各国都不遗余力地开发新能源。与此同时,为了解决健康问题而发展起来的痕量分析技术在一些与人类健康密切相关的领域中的应用也日趋广泛。本论文结合纳米尺度银纳米粒子(AgNPs)所具有的独特光学及催化特性,基于团簇束流沉积技术在玻碳或石墨烯表面构建数密度和尺寸可控的AgNPs点阵,并在此基础上围绕AgNPs非酶H202电化学传感以及AgNPs-石墨烯光电复合膜特性调控两方面进行了深入的研究。论文研究结果如下：
1.采用磁控等离子体气体聚集团簇束流源制备AgNPs,并在高真空下同步沉积在衬底表面。研究了冷凝距离、溅射和缓冲气体流量、溅射功率、沉积时间等对Ag团簇束流淀积速率的影响。在固定的磁控溅射条件下改变冷凝距离的长度,有利于获得高的AgNPs淀积速率。在固定的冷凝距离条件下,选择适当的溅射气体流量和缓冲气体流量,可以获得最高的沉积速率。在其他参数相同的条件下,根据团簇淀积速率随溅射功率的变化,可以优化束流源的溅射效率。因此,通过冷凝距离、缓冲和溅射气体流量、溅射功率等制备参数可对AgNPs淀积速率进行精细控制。对沉积于衬底表面的AgNPs的形貌、结构、空间分布参数进行了TEM和AFM显微表征分析。结果表明,在上述优化控制条件下制备的AgNPs,尺寸分布均一具有良好的分散性及洁净的表面,且尺寸分布满足标准的对数正态分布,其平均粒径约为6nm,半峰宽4.6nm,数密度高达1.4×104μm-2。通过HR-TEM及SAED表征显示AgNPs的结晶良好,结构呈规则的球形。采用气相团簇束流沉积制备的AgNPs点阵,能够在保持纯净的纳米粒子表面(无表面活性剂包裹)的同时,获得甚高的纳米粒子面密度,并且具有可调控的纳米粒子面间距,表明团簇束流沉积是可控制备密集排列金属AgNPs点阵的有效方法。
2.首次提出利用团簇束流沉积技术在玻碳电极上牢固而又可控地固定贵金属纳米材料。通过调控束流沉积参数,制备数密度和尺寸可控的AgNPs修饰电极,构建新型H202非酶传感器。该方法克服了传统修饰电极中催化剂聚集和易脱落的难题,并且避免了导电粘结剂的使用,提高了修饰电极的有效催化面积和稳定性,加速了电子在电极与催化剂之间的直接传递。通过循环伏安、线性扫描伏安、计时电流等测试手段分析了AgNPs数密度、尺寸、覆盖率对电极性能的影响。研究表明,AgNPs修饰电极的检测限、灵敏度和线性范围随着纳米粒子沉积量的增加并不是简单的递增,而是存在一个达到最佳电极性能的适当沉积量：使AgNPs的数密度达到最大值。过高的沉积量,会使得新到达表面的AgNPs与表面上原有的AgNPs融合长大,数密度逐渐降低,从而导致电极的有效催化面积变小,性能变差。在当前最佳的制备条件下构建的Ag纳米粒子修饰的玻碳电极在H202非酶生物传感中灵敏度可达63μA/mM、响应速度<1s、检测限达1μM。最后,在实验基础上阐明了AgNPs密集点阵催化H202的电化学传质过程与机理。
3.以膨胀石墨为原料,辅以高温热膨胀,采用高功率超声实现石墨烯的快速液相剥离,克服了当前低功率液相超声剥离法耗时长及难获得大尺寸石墨烯的不足,并通过高分辨透射(HR-TEM)和扫描透射(STEM)两种电子显微镜测量模式的组合,实现对石墨烯层厚的高效率表征与统计。研究了热膨胀温度、超声时间、超声功率对产物石墨烯层数和尺寸的影响。实验表明,热膨胀温度越高越有助于膨胀石墨的快速剥离,而长时间或过高功率的超声则不利于大尺寸薄层石墨烯的形成。在当前最佳的制备条件下,所制备的石墨烯(FLG)典型的厚度约为5层单石墨烯层,平面尺寸为微米级。通过蒸发部分溶剂可获得浓缩的FLG分散液,浓度约5μg mL-1,即每毫升约含5×105片FLG。此外,采用XPS、Raman等手段对所得石墨烯的缺陷和含氧官能团进行表征分析。结果显示,产物中含氧官能团及缺陷获得了良好的控制。通过本方法,可以高效可控制备高质量FLG。
4.采用团簇束流沉积制备AgNPs,并在高真空下可控沉积到FLG修饰电极表面制备出AgNPs-FLG新型光电复合膜修饰电极,避免了当前化学法合成的AgNPs-FLG复合膜被修饰到电极上发生部分堆叠导致AgNPs之间的不可控聚集。在此基础上,系统地研究了AgNPs尺寸、AgNPs覆盖率、入射光波长、入射光功率以及电极偏压等因素对AgNPs-FLG光电复合膜光电化学性能的影响。实验显示,小尺寸AgNPs的密集点阵更有助于增强石墨烯光电流的产生,并且AgNPs-FLG光电流的大小与入射光波长及功率高度相关。据此,阐明了AgNPs的局域表面等离激元(LSP)增强石墨烯光电流产生的可能机制：LSP不仅能提高石墨烯光生电子与空穴的产生效率,也能减小光生电子在FLG内部及电极／电解液界面的淬灭几率,使电子有更加充分的时间在电极偏压的作用下由FLG向玻碳电极方向转移,促进了光生电子与空穴的有效分离,从而增强了石墨烯光电流。
Recently, silver nanoparticles (AgNPs) have attracted much interest due to their unique optical and catalytic properties and found applications in new energy development as well as trace analysis. In this thesis, AgNPs were deposited on glass carbon electrodes and graphene by means of gas phase cluster beam deposition for non-enzymatic hydrogen peroxide detection and high-efficiency photocurrent generation, respectively. The main research results are as follows:
1. The AgNPs fims were fabricated by using gas phase cluster beam deposition. The operation parameters of the source, such as the condensation distance, sputtering power and flow rate of sputtering or buffering gas were systematically investigated to improve the deposition rate of the AgNPs. It was found the deposition rate of the AgNPs can be well controlled by tuning the above parameters and an enhanced deposition rate was realized under a smaller condensation distance and proper sputtering power as well as a special flow rate of sputtering and buffering gas. The morphology, coverage and size distribution of the optimized AgNPs was characterized with transmission electron microscopy (TEM), atomic force microscope (AFM) and selected area electron diffraction (SAED). The results show that the AgNPs fabricated by this method have the merits of well-crystallized, high surface density (1.4×104μm-2), homogeneous size distribution (-6nm), good dispersity and clean surface. Therefore, the technique of gas phase cluster beam deposition is a promising technology for fabricating close-packed AgNPs particles.
2. We demonstrate a novel method to coat AgNPs on glass carbon electrodes(GCE) with high adhesion and good dispersity by performing gas phase cluster beam deposition. A nonenzyme sensing platform for stable detection of H2O2was realized from the silver nanoparticle based electrode with an optimized nanoparticle coverage and number density. AgNPs electrodes fabricated with this method can avoid the problems of catalyst aggregation and shedding that would emerge in sensor applications. To examine the effects of the coverage and size distribution of the AgNPs on the reduction of the H2O2for optimizing the electrode conformation, we fabricated AgNPs-GCE electrodes with different deposition durations. The results show the electrode consists of small nanoparticles which are densely closely-spaced but sufficiently isolated from each other has significantly advantages in electroanalysis. As a result, the fabricated AgNP-GCE shows enhanced electrocatalytic activity toward the reduction of H2O2with a much reduced detection limit (typically1×10-6M) and response time (typically less than1second) as compared with those have been previously reported. Moreover, a possible reaction mechanism is proposed based on the experiments.
3. Few-layer graphene sheets (FLG) were prepared by splitting expanded graphite (EG) using high-power sonication. FLG fabricated with this method can reduce the noise pollution and the FLG breaking that would emerge in long time low-power sonication. Atomic-level calibrated scanning transmission electron microscopy was used to obtain efficient layer statistics, enabling optimization of the experimental conditions. Herein, heating temperature of EG, ultrasonic power and duration were systematically investigated. This resulted in a two-step splitting mechanism in which the mean number of layers was first reduced to less than20by heating to1100℃and then to a few-layer region by a5-minute104W L-1-power-density sonication. Our method can fabricate FLG sheets with about five-layers on micro-lever at a yield of～1wt%, and we show that the FLG sheets concentration could potentially be improved by evaporating the solvent to give the concentration of up to～5μg mL-1, namely about5×105pieces per milliliter. X-Ray Photoelectron Spectrometer (XPS) and Raman spectroscopic (Raman) analysis confirm the above mechanism and demonstrate that the sheets are largely free of defects and functional groups. As a solution-phase method, this approach may be scaled up for high-efficient fabrication of the FLG.
4. Closely spaced Ag nanoparticle arrays (AgNPs) were deposited on graphene sheets attached glassy electrode (FLG-GCE) by means of gas phase cluster beam deposition with controlled coverage and size distribution. This approach fabricated AgNPs-FLG electrode can avoid the overlap of the AgNPs on the electrode emerge during the chemically prepared AgNPs-FLG films were modified on the electrode. The fabricated AgNPs-FLG electrode show enhanced photocurrent generation compared with the FLG electrode. We employ an amperometric technique for high-efficiency photocurrent detection that enables the extensive study of the relationship between the localized surface plasmon (LSP) of AgNPs and the photocurrent enhancement of FLG in detail. The effects of the coverage of the AgNPs, the wavelength and intensity of the incident light, as well as the electrode potential were systematically investigated to improve the photoelectrochemistry performance of the AgNPs/FLG-GCE electrode. Moreover, the possible physical mechanism of the LSP enhanced photoelectrochemistry in the AgNPs-FLG composite film is proposed based on the experiments. Namely, the enhancement of the photocurrent from an illuminated AgNPs-FLG film is determined by the local electromagnetic fields near the AgNPs. On the one hand, they can increase the absorption of the incident light. On the other hand, they can confine the photoexcited electrons within graphene and depress its recombination within graphene and at the graphene/electrolyte interface. Thus, the electron-hole pairs are separated by this field and an enhanced photocurrent is observed.
1.采用磁控等离子体气体聚集团簇束流源制备AgNPs,并在高真空下同步沉积在衬底表面。研究了冷凝距离、溅射和缓冲气体流量、溅射功率、沉积时间等对Ag团簇束流淀积速率的影响。在固定的磁控溅射条件下改变冷凝距离的长度,有利于获得高的AgNPs淀积速率。在固定的冷凝距离条件下,选择适当的溅射气体流量和缓冲气体流量,可以获得最高的沉积速率。在其他参数相同的条件下,根据团簇淀积速率随溅射功率的变化,可以优化束流源的溅射效率。因此,通过冷凝距离、缓冲和溅射气体流量、溅射功率等制备参数可对AgNPs淀积速率进行精细控制。对沉积于衬底表面的AgNPs的形貌、结构、空间分布参数进行了TEM和AFM显微表征分析。结果表明,在上述优化控制条件下制备的AgNPs,尺寸分布均一具有良好的分散性及洁净的表面,且尺寸分布满足标准的对数正态分布,其平均粒径约为6nm,半峰宽4.6nm,数密度高达1.4×104μm-2。通过HR-TEM及SAED表征显示AgNPs的结晶良好,结构呈规则的球形。采用气相团簇束流沉积制备的AgNPs点阵,能够在保持纯净的纳米粒子表面(无表面活性剂包裹)的同时,获得甚高的纳米粒子面密度,并且具有可调控的纳米粒子面间距,表明团簇束流沉积是可控制备密集排列金属AgNPs点阵的有效方法。
2.首次提出利用团簇束流沉积技术在玻碳电极上牢固而又可控地固定贵金属纳米材料。通过调控束流沉积参数,制备数密度和尺寸可控的AgNPs修饰电极,构建新型H202非酶传感器。该方法克服了传统修饰电极中催化剂聚集和易脱落的难题,并且避免了导电粘结剂的使用,提高了修饰电极的有效催化面积和稳定性,加速了电子在电极与催化剂之间的直接传递。通过循环伏安、线性扫描伏安、计时电流等测试手段分析了AgNPs数密度、尺寸、覆盖率对电极性能的影响。研究表明,AgNPs修饰电极的检测限、灵敏度和线性范围随着纳米粒子沉积量的增加并不是简单的递增,而是存在一个达到最佳电极性能的适当沉积量：使AgNPs的数密度达到最大值。过高的沉积量,会使得新到达表面的AgNPs与表面上原有的AgNPs融合长大,数密度逐渐降低,从而导致电极的有效催化面积变小,性能变差。在当前最佳的制备条件下构建的Ag纳米粒子修饰的玻碳电极在H202非酶生物传感中灵敏度可达63μA/mM、响应速度<1s、检测限达1μM。最后,在实验基础上阐明了AgNPs密集点阵催化H202的电化学传质过程与机理。
3.以膨胀石墨为原料,辅以高温热膨胀,采用高功率超声实现石墨烯的快速液相剥离,克服了当前低功率液相超声剥离法耗时长及难获得大尺寸石墨烯的不足,并通过高分辨透射(HR-TEM)和扫描透射(STEM)两种电子显微镜测量模式的组合,实现对石墨烯层厚的高效率表征与统计。研究了热膨胀温度、超声时间、超声功率对产物石墨烯层数和尺寸的影响。实验表明,热膨胀温度越高越有助于膨胀石墨的快速剥离,而长时间或过高功率的超声则不利于大尺寸薄层石墨烯的形成。在当前最佳的制备条件下,所制备的石墨烯(FLG)典型的厚度约为5层单石墨烯层,平面尺寸为微米级。通过蒸发部分溶剂可获得浓缩的FLG分散液,浓度约5μg mL-1,即每毫升约含5×105片FLG。此外,采用XPS、Raman等手段对所得石墨烯的缺陷和含氧官能团进行表征分析。结果显示,产物中含氧官能团及缺陷获得了良好的控制。通过本方法,可以高效可控制备高质量FLG。
4.采用团簇束流沉积制备AgNPs,并在高真空下可控沉积到FLG修饰电极表面制备出AgNPs-FLG新型光电复合膜修饰电极,避免了当前化学法合成的AgNPs-FLG复合膜被修饰到电极上发生部分堆叠导致AgNPs之间的不可控聚集。在此基础上,系统地研究了AgNPs尺寸、AgNPs覆盖率、入射光波长、入射光功率以及电极偏压等因素对AgNPs-FLG光电复合膜光电化学性能的影响。实验显示,小尺寸AgNPs的密集点阵更有助于增强石墨烯光电流的产生,并且AgNPs-FLG光电流的大小与入射光波长及功率高度相关。据此,阐明了AgNPs的局域表面等离激元(LSP)增强石墨烯光电流产生的可能机制：LSP不仅能提高石墨烯光生电子与空穴的产生效率,也能减小光生电子在FLG内部及电极／电解液界面的淬灭几率,使电子有更加充分的时间在电极偏压的作用下由FLG向玻碳电极方向转移,促进了光生电子与空穴的有效分离,从而增强了石墨烯光电流。
Recently, silver nanoparticles (AgNPs) have attracted much interest due to their unique optical and catalytic properties and found applications in new energy development as well as trace analysis. In this thesis, AgNPs were deposited on glass carbon electrodes and graphene by means of gas phase cluster beam deposition for non-enzymatic hydrogen peroxide detection and high-efficiency photocurrent generation, respectively. The main research results are as follows:
1. The AgNPs fims were fabricated by using gas phase cluster beam deposition. The operation parameters of the source, such as the condensation distance, sputtering power and flow rate of sputtering or buffering gas were systematically investigated to improve the deposition rate of the AgNPs. It was found the deposition rate of the AgNPs can be well controlled by tuning the above parameters and an enhanced deposition rate was realized under a smaller condensation distance and proper sputtering power as well as a special flow rate of sputtering and buffering gas. The morphology, coverage and size distribution of the optimized AgNPs was characterized with transmission electron microscopy (TEM), atomic force microscope (AFM) and selected area electron diffraction (SAED). The results show that the AgNPs fabricated by this method have the merits of well-crystallized, high surface density (1.4×104μm-2), homogeneous size distribution (-6nm), good dispersity and clean surface. Therefore, the technique of gas phase cluster beam deposition is a promising technology for fabricating close-packed AgNPs particles.
2. We demonstrate a novel method to coat AgNPs on glass carbon electrodes(GCE) with high adhesion and good dispersity by performing gas phase cluster beam deposition. A nonenzyme sensing platform for stable detection of H2O2was realized from the silver nanoparticle based electrode with an optimized nanoparticle coverage and number density. AgNPs electrodes fabricated with this method can avoid the problems of catalyst aggregation and shedding that would emerge in sensor applications. To examine the effects of the coverage and size distribution of the AgNPs on the reduction of the H2O2for optimizing the electrode conformation, we fabricated AgNPs-GCE electrodes with different deposition durations. The results show the electrode consists of small nanoparticles which are densely closely-spaced but sufficiently isolated from each other has significantly advantages in electroanalysis. As a result, the fabricated AgNP-GCE shows enhanced electrocatalytic activity toward the reduction of H2O2with a much reduced detection limit (typically1×10-6M) and response time (typically less than1second) as compared with those have been previously reported. Moreover, a possible reaction mechanism is proposed based on the experiments.
3. Few-layer graphene sheets (FLG) were prepared by splitting expanded graphite (EG) using high-power sonication. FLG fabricated with this method can reduce the noise pollution and the FLG breaking that would emerge in long time low-power sonication. Atomic-level calibrated scanning transmission electron microscopy was used to obtain efficient layer statistics, enabling optimization of the experimental conditions. Herein, heating temperature of EG, ultrasonic power and duration were systematically investigated. This resulted in a two-step splitting mechanism in which the mean number of layers was first reduced to less than20by heating to1100℃and then to a few-layer region by a5-minute104W L-1-power-density sonication. Our method can fabricate FLG sheets with about five-layers on micro-lever at a yield of～1wt%, and we show that the FLG sheets concentration could potentially be improved by evaporating the solvent to give the concentration of up to～5μg mL-1, namely about5×105pieces per milliliter. X-Ray Photoelectron Spectrometer (XPS) and Raman spectroscopic (Raman) analysis confirm the above mechanism and demonstrate that the sheets are largely free of defects and functional groups. As a solution-phase method, this approach may be scaled up for high-efficient fabrication of the FLG.
4. Closely spaced Ag nanoparticle arrays (AgNPs) were deposited on graphene sheets attached glassy electrode (FLG-GCE) by means of gas phase cluster beam deposition with controlled coverage and size distribution. This approach fabricated AgNPs-FLG electrode can avoid the overlap of the AgNPs on the electrode emerge during the chemically prepared AgNPs-FLG films were modified on the electrode. The fabricated AgNPs-FLG electrode show enhanced photocurrent generation compared with the FLG electrode. We employ an amperometric technique for high-efficiency photocurrent detection that enables the extensive study of the relationship between the localized surface plasmon (LSP) of AgNPs and the photocurrent enhancement of FLG in detail. The effects of the coverage of the AgNPs, the wavelength and intensity of the incident light, as well as the electrode potential were systematically investigated to improve the photoelectrochemistry performance of the AgNPs/FLG-GCE electrode. Moreover, the possible physical mechanism of the LSP enhanced photoelectrochemistry in the AgNPs-FLG composite film is proposed based on the experiments. Namely, the enhancement of the photocurrent from an illuminated AgNPs-FLG film is determined by the local electromagnetic fields near the AgNPs. On the one hand, they can increase the absorption of the incident light. On the other hand, they can confine the photoexcited electrons within graphene and depress its recombination within graphene and at the graphene/electrolyte interface. Thus, the electron-hole pairs are separated by this field and an enhanced photocurrent is observed.
引文
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