金属修饰硅纳米线的制备及其应用研究
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摘要
近年来,纳米结构材料以其独特的物理化学性质引起了众多研究者的关注。越来越多的纳米材料被应用到各类微纳器件中并扮演着重要角色。其中,以硅为底材的硅纳米线(SiNWs)阵列材料以其独特的性质正逐渐成为纳米材料研究的热点。研究发现,对硅纳米线进行适当修饰后,纳米线会表现出独特的性质。据此,人们制备了不同金属修饰纳米材料,并将其作为开发新一代的微纳传感器件研究的重点。
本文的主要工作围绕着将金属修饰的硅纳米线材料用于电化学葡萄糖传感器以及直接乙醇燃料电池电极展开。首先研究了硅纳米线(SiNWs)材料的制备和修饰方法,制作了基于不同金属修饰的硅纳米线(SiNWs)电极材料,并将其用于电化学葡萄糖传感器以及直接乙醇燃料电池的研究。采用电化学的方法对其敏感性和催化性能进行了探测。初步完成了采用不同金属修饰的硅纳米线作为电极的直接乙醇燃料电池样机的组装。论文的主要研究工作如下：
第一,本文开展了对SiNWs阵列生长机理的探讨,并采用“自上而下”金属诱导化学腐蚀法制备了长度在50-80μm、线径为数百纳米的SiNWs阵列。采用扫描电子显微镜(Scanning Electron Microsocop, SEM)、X-射线衍射(X-Ray Diffraction, XRD)技术对制备的硅纳米线阵列进行了表征。
第二,研究了不同金属修饰SiNWs阵列的制备方法。采用化学溶液浸镀法在制备的SiNWs阵列上分别沉积钯-镍和银金属粒子,形成Pd-Ni/SiNWs和Ag/SiNWs阵列电极。采用扫描电子显微镜(SEM)和X-射线衍射(XRD)等手段对制备的硅纳米线和金属修饰的硅纳米线结构进行了表征。
第三,创新性地提出一种采用钯-镍/硅纳米线(Pd-Ni/SiNWs)阵列结构制作电化学葡萄糖传感器的新方案,较好地克服了当前电化学微纳传感器中普遍存在由于催化剂毒化以及易受温度等外界环境影响等共性问题。采用循环伏安扫描法(Cyclic Voltammetry, CV)、恒电位计时电流法(Fixed Potential Amperometry)等技术实现对Pd-Ni/SiNWs阵列电极材料的催化性能的探测。由于SiNWs阵列结构在纳米量级,具有巨大的比表面积,传感器的灵敏度高达190.7μA·mM-1cm-2,基于三倍信噪比(S/N=3)的探测极限为2.88μM,传感器的响应时间在8s以内,并且可以抵抗抗坏血酸(Ascorbic Acid, AA)、尿酸(Uric Acid, UA)以及四-乙酰氨基酚(4-acetamidophenol,AP)等干扰物的影响。此外,所研制的葡萄糖传感器具有优良的稳定性,耐酸碱腐蚀,随温度变化不敏感,制备工艺简单,同集成电路工艺相兼容,制作成本低等诸多优点。
第四,开展了液态无贵金属催化剂(Pt, Ru)的直接乙醇燃料电池(Direct Ethanol Fuel Cell, DEFC)的研究工作。采用Pd-Ni/SiNWs阵列电极和AgO/SiN Ws阵列电极分别作为直接乙醇燃料电池的阳极和阴极。乙醇作为燃料,空气中的氧气作为氧化剂,氢氧化钾(KOH)碱性溶液作为电解质,构成直接乙醇燃料电池原型样机。对电极材料的催化性能、电池的开路电压(Open Circuit Voltage, OCV)和短路电流(Short Circuit Current, SCC)等参数进行测试。为降低燃料电池催化剂的成本提供了可能性,为非Pt基催化剂的研究提供了一定的理论和实验基础。
Recently, the nanostructured materials have become the research focus due to their unique physical and chemical properties. Nanostructured materials are playing an important role in a variety of niicro-nano devices. Among them, silicon nanowires (SiNWs) has been studied intensively due to their excellent electrical and optical properties. It is also found that the silicon modified nanowires exhibit the special and novel characteristics. Therefore, researchers prepared different metal modified nano materials as a focus study of new generation of micro-nano devices.
In this work, the electrochemical glucose sensors and the direct ethanol fuel cell prototypes based on the metal-modified silicon nanowires is present. First, the silicon nanowire arrays are prepared by wet chemical etching, then the SiNWs were modified by some metals like Pd, Ni and Ag with electroless plating. Finally, the electrochemical detection sensitivity and catalytic properties of SiNWs sensors were studied by electrochemical method. The mainly works are listed as following:
First, the growth and fabrication mechanism of SiNWs arrays is investigated. SiNWs arrays were prepared metal-assisted chemical etching method, which is a also known as a "top-down" technique. The dimension of SiNWs arrays prepared is 80-100μm in length and 200-400nm in diameter. The structural and morphological properties of SiNWs were characterized by SEM (Scanning Electron Microsocop) and XRD (X-Ray Diffraction) technique.
Second, different metal modified SiNWs arrays structures were studied. Chemical solution method was used to deposit Pd-Ni and Ag on SiNWs arrays. The properties of Pd-Ni/SiNWs and Ag/SiNWs were examined by SEM (Scanning Electron Microsocop) and XRD (X-Ray Diffraction) technique.
Thirdly, a novel electrochemical glucose sensor based on Pd-Ni/SiNWs electrode had been constructed. The developed sensors can overcome the catalyst's poisoning and unstablity, which is regarded as the common problems in current electrochemical glucose sensors. The catalytic behavior of Pd-Ni/SiNWs glucose sensor is characterized by cyclic voltammetry (CV) and fixed potential amperometry. The Pd-Ni/SiNWs electrode showed an excellent sensitivity of 190.72μAmM-lcm-2 with the detection limit (S/N ratio=3) of 2.88μM. And it also exhibits superior anti-interference properties to the species including ascorbic acid (AA), uric acid (UA) and 4-acetamidophenol (AP). All results demonstrated that this Pd-Ni/SiNWs electrode is a potential candidate for glucose detection. This sensor has superior stability, and it is easily fabricated and compatible with integrated circuits (ICs) and micro-fabrication process.
At last, a prototype of direct ethanol fuel cell (DEFC) without noble metal catalyst was present in this work. The prototype consisted of Pd-Ni/SiNWs electrode as anode, and AgO/SiNWs electrode as cathode. With ethanol as the fuel, oxygen in the air as the oxidant,1M KOH medium as the electrolyte, the electrodes behaviors are characterized by electrochemical workstation. And the open circuit voltage (OCV) and short circuit current of this prototype were studied. Our work demonstrated that it is possible to develop non-Pt-based catalyst direct ethanol fuel cell.
本文的主要工作围绕着将金属修饰的硅纳米线材料用于电化学葡萄糖传感器以及直接乙醇燃料电池电极展开。首先研究了硅纳米线(SiNWs)材料的制备和修饰方法,制作了基于不同金属修饰的硅纳米线(SiNWs)电极材料,并将其用于电化学葡萄糖传感器以及直接乙醇燃料电池的研究。采用电化学的方法对其敏感性和催化性能进行了探测。初步完成了采用不同金属修饰的硅纳米线作为电极的直接乙醇燃料电池样机的组装。论文的主要研究工作如下：
第一,本文开展了对SiNWs阵列生长机理的探讨,并采用“自上而下”金属诱导化学腐蚀法制备了长度在50-80μm、线径为数百纳米的SiNWs阵列。采用扫描电子显微镜(Scanning Electron Microsocop, SEM)、X-射线衍射(X-Ray Diffraction, XRD)技术对制备的硅纳米线阵列进行了表征。
第二,研究了不同金属修饰SiNWs阵列的制备方法。采用化学溶液浸镀法在制备的SiNWs阵列上分别沉积钯-镍和银金属粒子,形成Pd-Ni/SiNWs和Ag/SiNWs阵列电极。采用扫描电子显微镜(SEM)和X-射线衍射(XRD)等手段对制备的硅纳米线和金属修饰的硅纳米线结构进行了表征。
第三,创新性地提出一种采用钯-镍/硅纳米线(Pd-Ni/SiNWs)阵列结构制作电化学葡萄糖传感器的新方案,较好地克服了当前电化学微纳传感器中普遍存在由于催化剂毒化以及易受温度等外界环境影响等共性问题。采用循环伏安扫描法(Cyclic Voltammetry, CV)、恒电位计时电流法(Fixed Potential Amperometry)等技术实现对Pd-Ni/SiNWs阵列电极材料的催化性能的探测。由于SiNWs阵列结构在纳米量级,具有巨大的比表面积,传感器的灵敏度高达190.7μA·mM-1cm-2,基于三倍信噪比(S/N=3)的探测极限为2.88μM,传感器的响应时间在8s以内,并且可以抵抗抗坏血酸(Ascorbic Acid, AA)、尿酸(Uric Acid, UA)以及四-乙酰氨基酚(4-acetamidophenol,AP)等干扰物的影响。此外,所研制的葡萄糖传感器具有优良的稳定性,耐酸碱腐蚀,随温度变化不敏感,制备工艺简单,同集成电路工艺相兼容,制作成本低等诸多优点。
第四,开展了液态无贵金属催化剂(Pt, Ru)的直接乙醇燃料电池(Direct Ethanol Fuel Cell, DEFC)的研究工作。采用Pd-Ni/SiNWs阵列电极和AgO/SiN Ws阵列电极分别作为直接乙醇燃料电池的阳极和阴极。乙醇作为燃料,空气中的氧气作为氧化剂,氢氧化钾(KOH)碱性溶液作为电解质,构成直接乙醇燃料电池原型样机。对电极材料的催化性能、电池的开路电压(Open Circuit Voltage, OCV)和短路电流(Short Circuit Current, SCC)等参数进行测试。为降低燃料电池催化剂的成本提供了可能性,为非Pt基催化剂的研究提供了一定的理论和实验基础。
Recently, the nanostructured materials have become the research focus due to their unique physical and chemical properties. Nanostructured materials are playing an important role in a variety of niicro-nano devices. Among them, silicon nanowires (SiNWs) has been studied intensively due to their excellent electrical and optical properties. It is also found that the silicon modified nanowires exhibit the special and novel characteristics. Therefore, researchers prepared different metal modified nano materials as a focus study of new generation of micro-nano devices.
In this work, the electrochemical glucose sensors and the direct ethanol fuel cell prototypes based on the metal-modified silicon nanowires is present. First, the silicon nanowire arrays are prepared by wet chemical etching, then the SiNWs were modified by some metals like Pd, Ni and Ag with electroless plating. Finally, the electrochemical detection sensitivity and catalytic properties of SiNWs sensors were studied by electrochemical method. The mainly works are listed as following:
First, the growth and fabrication mechanism of SiNWs arrays is investigated. SiNWs arrays were prepared metal-assisted chemical etching method, which is a also known as a "top-down" technique. The dimension of SiNWs arrays prepared is 80-100μm in length and 200-400nm in diameter. The structural and morphological properties of SiNWs were characterized by SEM (Scanning Electron Microsocop) and XRD (X-Ray Diffraction) technique.
Second, different metal modified SiNWs arrays structures were studied. Chemical solution method was used to deposit Pd-Ni and Ag on SiNWs arrays. The properties of Pd-Ni/SiNWs and Ag/SiNWs were examined by SEM (Scanning Electron Microsocop) and XRD (X-Ray Diffraction) technique.
Thirdly, a novel electrochemical glucose sensor based on Pd-Ni/SiNWs electrode had been constructed. The developed sensors can overcome the catalyst's poisoning and unstablity, which is regarded as the common problems in current electrochemical glucose sensors. The catalytic behavior of Pd-Ni/SiNWs glucose sensor is characterized by cyclic voltammetry (CV) and fixed potential amperometry. The Pd-Ni/SiNWs electrode showed an excellent sensitivity of 190.72μAmM-lcm-2 with the detection limit (S/N ratio=3) of 2.88μM. And it also exhibits superior anti-interference properties to the species including ascorbic acid (AA), uric acid (UA) and 4-acetamidophenol (AP). All results demonstrated that this Pd-Ni/SiNWs electrode is a potential candidate for glucose detection. This sensor has superior stability, and it is easily fabricated and compatible with integrated circuits (ICs) and micro-fabrication process.
At last, a prototype of direct ethanol fuel cell (DEFC) without noble metal catalyst was present in this work. The prototype consisted of Pd-Ni/SiNWs electrode as anode, and AgO/SiNWs electrode as cathode. With ethanol as the fuel, oxygen in the air as the oxidant,1M KOH medium as the electrolyte, the electrodes behaviors are characterized by electrochemical workstation. And the open circuit voltage (OCV) and short circuit current of this prototype were studied. Our work demonstrated that it is possible to develop non-Pt-based catalyst direct ethanol fuel cell.
引文
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