贵金属纳米结构的设计、合成与应用
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摘要
经过近二十年的发展,贵金属纳米材料因其丰富的形貌、独特的物理、化学性质被广泛应用于光学、电学、磁学、催化、生物医学、环境处理及新能源领域。众所周知,贵金属纳米材料的性质往往由包括尺寸、形状、组成及结构(如实心或空心)等一系列物理参数所决定。原则上,这类性质可以通过控制上述参数中的任意一个而得到精确调控,但是其灵活性和变化范围对特定参数来说是高度敏感的。基于以上的特性,经过人为设计、合成的并且具有稳定结构且特殊性能的贵金属纳米结构材料就能够高效、且明确地在众多领域尤其是电化学催化、传感、生化检测及燃料电池等方面得到应用。例如质子交换膜燃料电池(PEMFCs)已经日渐成为解决有关环境污染和能源危机问题的重要途径,而其中贵金属铂及其合金材料是目前PEMFCs中研究、使用最为广泛的一类阳极氧化和阴极还原的电催化剂。然而由于铂催化剂面临着储存量有限,价格高昂,催化剂载量大、易失活,阴极氧气还原反应(ORR)过电位大、动力学活性低且室温操作时容易被CO毒化等问题,严重限制了基于此类催化剂的PEMFCs的商业化应用。而根据理论计算我们已经获得的基本认知是PEMFC阳极氧化及阴极还原过程中铂基催化剂可以通过有效地设计、和控制来制备催化剂,从而避免上述问题的出现。
本文致力于发展一种简单、快速制备贵金属纳米结构的方法,并通过有目的的表面结构设计将其应用于燃料电池阳极催化氧化、阴极催化还原及电化学传感、检测等方面的研究,并探索它们在电催化和燃料电池领域的应用前景。同时考虑到当前已经广泛应用的贵金属纳米材料可能会有的生物安全性问题,我们以最简单的球形纳米金颗粒作为模型考察了其对活体细胞的生物学毒性,并对今后贵金属纳米材料的应用给出一定的指导作用。具体的研究内容如下：
(1)基于经过改进的多元醇法(polyol process)合成得到了一系列具有不同长径比的银纳米线,并以此为模板经过一个化学镀(electroless plating)过程制得金银复合一维纳米线,随后通过浓硝酸的脱合金(dealloyed)腐蚀制备得到了具有双连续孔结构、高孔隙率的一维金银合金多孔纳米管。通过独立调控反应过程中的条件和参数(如纳米线模板的控制生长、化学镀表面修饰过程、热扩散速率以及脱合金过程),我们可以得到一系列的结构可调、功能可预设的一维多孔纳米结构。特别是化学镀过程中,表面金原子层的厚度可以从次原子层到数个原子层内得到精确调控,从而有效控制脱合金后所得纳米管的结构特征。这类管状、多孔纳米结构显示出了独特的光学特性,特别是其特征吸收波长可以从可见光区到近红外光区进行连续调制。因为其独特的开孔结构和特征的高比表面积,金银合金多孔纳米结构显示出了很强的电致化学发光信号的放大增强能力,这就使得其可以作为一类新颖的一维纳米载体用于生物医学、药物缓释及传感应用等领域。
(2)考虑到金银合金多孔纳米管内有一定的银残留,通过银与氯铂酸根离子间的原电池置换反应(galvanic replacement),将极少量的铂修饰于多孔纳米管表面。由于金银合金多孔纳米管中原始银含量较低,且金银可以形成有效的、互溶的合金态,同时与金原子相比铂原子的扩散速率非常低,因此置换出的铂原子在金多孔纳米管表面的分布可以有效地被控制并被表面金原子分割。通过控制金银合金中残留银的含量以及参与置换反应的铂前驱体的浓度,可以得到表面铂修饰量不同的铂金复合多孔纳米管(Pt/Au Porous Nanotubes, PNTs).以铂金复合纳米管为阳极催化剂,利用CV等方法评估了不同Pt载量的Pt/Au PNTs对甲酸的电催化活性。与理论计算所得结果相似的是,实验结果发现铂原子修饰量与甲酸催化性能呈反比,即当铂原子在金表面被分割得足够开,主要以小于两个铂原子相邻的方式出现,因而对甲酸的催化主要选择直接路径或者甲酸盐路径,避免了引发催化剂中毒的CO中间产物的产生。这一简单方法制备的Pt/Au甲酸催化剂不仅在催化氧化中选择了直接路径,而且铂原子的利用率得到大大提升,同时催化剂的稳定性相较于纯铂催化剂也有较大的提升。这一方法有望成为制备其他双元金属催化剂的通用方法。
(3)以一维银纳米线为模板,以化学镀(electroless plating)和选择性腐蚀过程成功制备了铂银复合多孔纳米管(Pt/Ag Porous Nanotubes, PNTs)。考察了不同铂前驱体用量对所得复合多孔纳米管结构的影响。发现复合多孔纳米管的管壁机械强度随铂前驱体盐使用量的增加而增强。随后以铂金复合纳米管为阳极催化剂,在碱性条件下利用CV等方法评估了Pt/Ag PNTs对乙醇的电催化氧化活性。与商业Pt/C催化剂相比,Pt/Ag PNTs有着相似的电化学行为,但是有着更强的催化活性。在酸性条件下的CO扫除实验发现,Pt/Ag PNTs的CO扫除峰电位比商业Pt/C的更负,就说明了纳米管催化剂更不易CO中毒。并用计时电流法进一步探究了催化剂的稳定性。同时在中性条件下用CV研究了Pt/Ag PNTs对双氧水的传感响应,在H2O2浓度为25μmol/L到4mmol/L范围内有着良好的线性关系,对H2O2的响应灵敏度为0.8/μmol/L。催化和传感结果显示铂银复合多孔纳米管可以作为一类出色的碱性燃料电池催化剂和电化学传感电极材料。
(4)发展了一种大量、简便、快速的方法制备了一种可以作为非负载型PEMFC阴极氧气还原反应(ORR)催化剂的Pt/Ag中空多孔纳米球(HPNSs),这一新型催化剂有着比商业Pt/C催化剂更高的催化活性。为了制备HPNSs这一新颖结构,首先通过高温液相还原法制备Ag@Pt核壳纳米颗粒,随后用浓硝酸选择性腐蚀银核即可得到中空的HPNSs。为了得到稳定的外层壳结构,将腐蚀得到的HPNSs置于DMF溶液中在相对温和的温度(-160℃)下对其进行退火即可得到有着稳定壳层的HPNSs(a-HPNSs)。由于其超薄的外壁结构(-3纳米),多孔壳有着超高的比表面积(-65m2/g),而且形成了一种类似合金的结构(近表面合金),a-HPNSs展现出了明显高于商业Pt/C催化剂的ORR催化活性,其ORR极化曲线的半波电位约为0.896V (vs. RHE),比Pt/C的半波电位(～0.828V vs. RHE)要高出接近70mV。催化剂的稳定性测试结果显示这一非负载型铂银复合催化剂有着较好的稳定性,与商业Pt/C相比,其电化学活性面积损失速率明显要低。因此,这一方法提供了一种简单的路径制备了具有高活性的非负载的催化剂,可以作为一种潜在的燃料电池阴极催化剂替代材料。
(5)选用形貌最为简单的球形纳米金颗粒(GNPs,直径约10纳米)和人体肺癌细胞A549作为模型体系来评价贵金属纳米材料对人体细胞的生物学毒性。当单独使用GNPs与细胞孵育时,并未对细胞的增殖产生影响。但是当使用L-丁硫氨酸-亚砜胺(BSO)来抑制A549细胞内的谷胱甘肽(GSH)的表达时,GNPs对细胞的就显现出明显的细胞毒性,一旦向细胞内引入外源性GSH, GNPs毒性立刻发生反转。而GSH在细胞内消除活性氧物种(ROS)起着重要的作用,通过监控细胞内ROS的水平,我们发现在BSO存在下GNPs会产生更多的ROS。因此,GNPs对肺癌细胞的细胞毒性可以部分归因于细胞内ROS水平的上升。这些结果表明在使用GNPs进行体内实验时应当更为小心,由于GNPs当前不仅本身在体内实验中被用作一种治疗试剂同时它也被当作其他药物或者生物大分子的载体在体内实验中使用。
During the last two decades, great attentions have been paid to noble metal nanostructures with abundant morphologies, distinct chemicophysical properties, since they could be applied in various fields, such as, optics, photonics, magnetics, catalysis, biomedicine, environment, and new energy. It was well known that the properties of noble metal nanocrystals usually depends on their physical parameters including szies, shapes, dimensions, compositions and structures (i.e. solid or hollow).In principle, one can tailor and fine-tune the properties of a metal nanocrystal by controlling any one of these parameters, but the flexibility and scope of change are highly sensitive to the specific parameter. Based on these, we could effectively pre-design and controllably synthesize noble metal nanomaterials with specific properties and stable structures, which might be applied in many potential fields with higher efficiency and defined purposes, especially electrocatalysis, sensing, biochemical dectection and fuel cells. Fox example, proton-exchange membrane fuel cells (PEMFCs) have increasingly been an important way to resolve the problems of environmental pollution and energy crisis, and among these platinum and its alloy materials have been extensively investigated and used, since they are one kind of effective electrocatalysts both in the anode and cathode of PEMFCs. However, as an electrocatalyst Pt has to face many problems, such as, low Pt storage on Earth, expensive price, higher loading amount and easily deactive, large overprotential and low kinetic activity of ORR, and readily be poisoned by CO under room temperature, which have been the major obstacles for the commerical application of PEMFCs based on such catalysts. But according to the theoretical calculations for the mechanisms of both anodic and cathodic process, one may have the ability of pre-designing and manufacturing catalysts to avoid these problems.
Herein, we focused on the development of a simple, versatile and rapid route to fabricate noble metal nanostructure with specific properties, and via a targeted way to prepare metallic catalyst with distinctive surface-structural designing, which were used in both the anode catalytic oxidation and the cathode catalytic reduction of fuel cells, as well as electrochemical sensing and detection, especially, we explored their application prospects in both electrocatalysis and fuel cells. Meanwhile, considering the potential biosafety issues due to the extensively using of noble metal nanomaterials, the cytotoxicity investigation has also been done via a simple model of spherical gold nanoparicles (GNPs) and human lung cancer cell A549, which might provide some suggestions for the applications of noble metal nanomaterials.
The results are as follows:
(1) Metallic nanostructures with hollow interiors or tailored porosity represent a special class of attractive materials with intriguing chemicophysical properties. This paper presents the fabrication of a new type of metallic nanoporous nanotube structure based on a facile and effective combination of nanocrystal growth and surface modification. By controlling the individual steps involved in this process, such as nanowire growth, surface modification, thermal diffusion, and dealloying, one-dimensional (1-D) metallic nanostructures can be prepared with tailored structural features and pre-designed functionalities. These tubular and porous nanostructures show distinct optical properties, such as tunable absorption in the near-infrared region, and enhanced capability for electrochemiluminescence signal amplification, which make them particularly desirable as novel1-D nanocarriers for biomedical, drug delivery and sensing applications.
(2) Considering the residual Ag component in the Au/Ag alloy porous nanotubes (APNTs), we fabricated a kind of Pt/Ag composite porous nantubes (PNTs) with enhanced catalytic actvity toward HCOOH electrooxidation via the simple galvanic replacement between the residual and H2PtCl6-Due to the relatively low content of Ag in the Au/Ag APNTs as well as the effective alloy between Au and Ag, we do think the reduced Pt atoms disperesed on the PNTs surface could be effectively controlled and separated by the surface Au atoms, which could be ascribed to the lower diffusion coefficient of Pt than that of Au. By tuning the amount of Pt precursor, Pt/Au PNTs with different Pt-decorated loading could be easily approached. Structural characterizations with scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray powder diffraction (XRD) reveal a novel nanoarchitecture with multimodal open porosity and excellent structural continuity and integrity. Meanwhile, as a kind of anodic catalysts, CV and other techniques demonstrated that the Pt/Au PNTs possess excellent electrocatalytic activity toward HCOOH oxidation and enhanced tolerance to CO poisoning.
(3) Based on the one dimensional Ag nanowires synthesized via a modified polyol process, with a simple electroless plating and selective etching process we sucessfully fabricated Pt/Ag composite porous nanotubes (Pt/Ag PNTs). We have investigated the influence of different amount of Pt precursors toward the final Pt/Ag PNTs structures. It was find that the mechanical strength of the composite PNTs wall sturcture strongly depended on the dosage of H2PtCl6, which presents a positive correlation. Following, the Pt/Ag PNTs were used as an anodic catalyst under alkaline condition and sensing electrode in neutral conditon toward the electrooxidation of ethanol and detection of H2O2, respectively. As for the ethanol oxidation, campared with the commerical Pt/C catalyst, Pt/Ag PNTs possessed the similar electrochemical behaviors, but their intrinsic activity is evidently higher than that of Pt/C. CO stripping in acid sloution showed that Pt/Ag PNTs have much higher tolerance to CO poisoning than Pt/C. During the detection of H2O2, we got find that Pt/Ag PNTs exhibits sensitive respones toward the reduction of H2O2. CV study illustrated that a linear relationship for H2O2determniantion in a concentration range from25μmol/L to4mmol/L, with～0.8μmol/L response sensitivity. These two results revealed that Pt/Ag composite PNTs could be a kind of remarkable alkaline fuel cell catalysts and superior sensing electrode materials.
(4) We developed a large scale, simple and rapid route to fabricate Pt/Ag hollow porous nanospheres (HPNSs) which can be served as a supportless ORR catalyst with higher activity than that of commercial Pt/C catalysts. To prepare the HPNSs, firstly Ag@Pt core-shell nanoparticles were fabricated via a one-pot approach of solvent-thermal process, following a selective etching process by concentrated HNO3was employed to get HPNSs. Thermal annealing under relatively moderate condition (～160℃) was adopted to obtain high quality crystalline and stable shells of HPNSs (a-HPNSs), Owing to their ultra-thin wall structure (～3nm), porous shells with high surface-area-to-volume, and their alloy structures, the α-HPNSs exhibited significant enhancement of the ORR catalytic activity over commercial Pt/C catalyst, and the half-wave potential of α-HPNSs is～0.896V (versus a reversible hydrogen electrode, RHE), which is nearly70mV higher than that of Pt/C (～0.828V vs. RHE). Durability examination adopted the same condition and the α-HPNSs showed surprisingly high activity toward ORR. Although the α-HPNSs are particle-like structure, they displayed superior connectivity and conductivity without any substrates during the electrochemical test. Consequently, this method allows simplification of the experimental procedures by avoiding the tedious mixing and optimization of catalysts with supporting materials.
(5) Gold nanoparticles (GNPs) were used to evaluate their cytotoxicity toward human lung cancer cells A549. No cell proliferation inhibition was found when the cells were treated by GNPs independently. However, when L-buthionine-sulfoximine (BSO) was used to decrease the expression of glutathione (GSH) in A549cells, GNPs showed evident cytotoxicity to cells. Interestingly, the cytotoxicity of GNPs could be reversed after adding outside source GSH into the system. Whereas GSH plays an important role in eliminating reactive oxygen species (ROS), by monitoring the intracellular levels of ROS, GNPs were observed to generate more intracellular ROS in the presence of BSO. The cytotoxicity caused by GNPs toward lung cancer cells could therefore be partially attributed to the increase in intracellular ROS levels. These results suggest that caution should be paid in the use of GNPs for in vivo tests because GNPs can serve as therapeutic agents in their own right as well as carriers for other drugs and biomolecules.
本文致力于发展一种简单、快速制备贵金属纳米结构的方法,并通过有目的的表面结构设计将其应用于燃料电池阳极催化氧化、阴极催化还原及电化学传感、检测等方面的研究,并探索它们在电催化和燃料电池领域的应用前景。同时考虑到当前已经广泛应用的贵金属纳米材料可能会有的生物安全性问题,我们以最简单的球形纳米金颗粒作为模型考察了其对活体细胞的生物学毒性,并对今后贵金属纳米材料的应用给出一定的指导作用。具体的研究内容如下：
(1)基于经过改进的多元醇法(polyol process)合成得到了一系列具有不同长径比的银纳米线,并以此为模板经过一个化学镀(electroless plating)过程制得金银复合一维纳米线,随后通过浓硝酸的脱合金(dealloyed)腐蚀制备得到了具有双连续孔结构、高孔隙率的一维金银合金多孔纳米管。通过独立调控反应过程中的条件和参数(如纳米线模板的控制生长、化学镀表面修饰过程、热扩散速率以及脱合金过程),我们可以得到一系列的结构可调、功能可预设的一维多孔纳米结构。特别是化学镀过程中,表面金原子层的厚度可以从次原子层到数个原子层内得到精确调控,从而有效控制脱合金后所得纳米管的结构特征。这类管状、多孔纳米结构显示出了独特的光学特性,特别是其特征吸收波长可以从可见光区到近红外光区进行连续调制。因为其独特的开孔结构和特征的高比表面积,金银合金多孔纳米结构显示出了很强的电致化学发光信号的放大增强能力,这就使得其可以作为一类新颖的一维纳米载体用于生物医学、药物缓释及传感应用等领域。
(2)考虑到金银合金多孔纳米管内有一定的银残留,通过银与氯铂酸根离子间的原电池置换反应(galvanic replacement),将极少量的铂修饰于多孔纳米管表面。由于金银合金多孔纳米管中原始银含量较低,且金银可以形成有效的、互溶的合金态,同时与金原子相比铂原子的扩散速率非常低,因此置换出的铂原子在金多孔纳米管表面的分布可以有效地被控制并被表面金原子分割。通过控制金银合金中残留银的含量以及参与置换反应的铂前驱体的浓度,可以得到表面铂修饰量不同的铂金复合多孔纳米管(Pt/Au Porous Nanotubes, PNTs).以铂金复合纳米管为阳极催化剂,利用CV等方法评估了不同Pt载量的Pt/Au PNTs对甲酸的电催化活性。与理论计算所得结果相似的是,实验结果发现铂原子修饰量与甲酸催化性能呈反比,即当铂原子在金表面被分割得足够开,主要以小于两个铂原子相邻的方式出现,因而对甲酸的催化主要选择直接路径或者甲酸盐路径,避免了引发催化剂中毒的CO中间产物的产生。这一简单方法制备的Pt/Au甲酸催化剂不仅在催化氧化中选择了直接路径,而且铂原子的利用率得到大大提升,同时催化剂的稳定性相较于纯铂催化剂也有较大的提升。这一方法有望成为制备其他双元金属催化剂的通用方法。
(3)以一维银纳米线为模板,以化学镀(electroless plating)和选择性腐蚀过程成功制备了铂银复合多孔纳米管(Pt/Ag Porous Nanotubes, PNTs)。考察了不同铂前驱体用量对所得复合多孔纳米管结构的影响。发现复合多孔纳米管的管壁机械强度随铂前驱体盐使用量的增加而增强。随后以铂金复合纳米管为阳极催化剂,在碱性条件下利用CV等方法评估了Pt/Ag PNTs对乙醇的电催化氧化活性。与商业Pt/C催化剂相比,Pt/Ag PNTs有着相似的电化学行为,但是有着更强的催化活性。在酸性条件下的CO扫除实验发现,Pt/Ag PNTs的CO扫除峰电位比商业Pt/C的更负,就说明了纳米管催化剂更不易CO中毒。并用计时电流法进一步探究了催化剂的稳定性。同时在中性条件下用CV研究了Pt/Ag PNTs对双氧水的传感响应,在H2O2浓度为25μmol/L到4mmol/L范围内有着良好的线性关系,对H2O2的响应灵敏度为0.8/μmol/L。催化和传感结果显示铂银复合多孔纳米管可以作为一类出色的碱性燃料电池催化剂和电化学传感电极材料。
(4)发展了一种大量、简便、快速的方法制备了一种可以作为非负载型PEMFC阴极氧气还原反应(ORR)催化剂的Pt/Ag中空多孔纳米球(HPNSs),这一新型催化剂有着比商业Pt/C催化剂更高的催化活性。为了制备HPNSs这一新颖结构,首先通过高温液相还原法制备Ag@Pt核壳纳米颗粒,随后用浓硝酸选择性腐蚀银核即可得到中空的HPNSs。为了得到稳定的外层壳结构,将腐蚀得到的HPNSs置于DMF溶液中在相对温和的温度(-160℃)下对其进行退火即可得到有着稳定壳层的HPNSs(a-HPNSs)。由于其超薄的外壁结构(-3纳米),多孔壳有着超高的比表面积(-65m2/g),而且形成了一种类似合金的结构(近表面合金),a-HPNSs展现出了明显高于商业Pt/C催化剂的ORR催化活性,其ORR极化曲线的半波电位约为0.896V (vs. RHE),比Pt/C的半波电位(～0.828V vs. RHE)要高出接近70mV。催化剂的稳定性测试结果显示这一非负载型铂银复合催化剂有着较好的稳定性,与商业Pt/C相比,其电化学活性面积损失速率明显要低。因此,这一方法提供了一种简单的路径制备了具有高活性的非负载的催化剂,可以作为一种潜在的燃料电池阴极催化剂替代材料。
(5)选用形貌最为简单的球形纳米金颗粒(GNPs,直径约10纳米)和人体肺癌细胞A549作为模型体系来评价贵金属纳米材料对人体细胞的生物学毒性。当单独使用GNPs与细胞孵育时,并未对细胞的增殖产生影响。但是当使用L-丁硫氨酸-亚砜胺(BSO)来抑制A549细胞内的谷胱甘肽(GSH)的表达时,GNPs对细胞的就显现出明显的细胞毒性,一旦向细胞内引入外源性GSH, GNPs毒性立刻发生反转。而GSH在细胞内消除活性氧物种(ROS)起着重要的作用,通过监控细胞内ROS的水平,我们发现在BSO存在下GNPs会产生更多的ROS。因此,GNPs对肺癌细胞的细胞毒性可以部分归因于细胞内ROS水平的上升。这些结果表明在使用GNPs进行体内实验时应当更为小心,由于GNPs当前不仅本身在体内实验中被用作一种治疗试剂同时它也被当作其他药物或者生物大分子的载体在体内实验中使用。
During the last two decades, great attentions have been paid to noble metal nanostructures with abundant morphologies, distinct chemicophysical properties, since they could be applied in various fields, such as, optics, photonics, magnetics, catalysis, biomedicine, environment, and new energy. It was well known that the properties of noble metal nanocrystals usually depends on their physical parameters including szies, shapes, dimensions, compositions and structures (i.e. solid or hollow).In principle, one can tailor and fine-tune the properties of a metal nanocrystal by controlling any one of these parameters, but the flexibility and scope of change are highly sensitive to the specific parameter. Based on these, we could effectively pre-design and controllably synthesize noble metal nanomaterials with specific properties and stable structures, which might be applied in many potential fields with higher efficiency and defined purposes, especially electrocatalysis, sensing, biochemical dectection and fuel cells. Fox example, proton-exchange membrane fuel cells (PEMFCs) have increasingly been an important way to resolve the problems of environmental pollution and energy crisis, and among these platinum and its alloy materials have been extensively investigated and used, since they are one kind of effective electrocatalysts both in the anode and cathode of PEMFCs. However, as an electrocatalyst Pt has to face many problems, such as, low Pt storage on Earth, expensive price, higher loading amount and easily deactive, large overprotential and low kinetic activity of ORR, and readily be poisoned by CO under room temperature, which have been the major obstacles for the commerical application of PEMFCs based on such catalysts. But according to the theoretical calculations for the mechanisms of both anodic and cathodic process, one may have the ability of pre-designing and manufacturing catalysts to avoid these problems.
Herein, we focused on the development of a simple, versatile and rapid route to fabricate noble metal nanostructure with specific properties, and via a targeted way to prepare metallic catalyst with distinctive surface-structural designing, which were used in both the anode catalytic oxidation and the cathode catalytic reduction of fuel cells, as well as electrochemical sensing and detection, especially, we explored their application prospects in both electrocatalysis and fuel cells. Meanwhile, considering the potential biosafety issues due to the extensively using of noble metal nanomaterials, the cytotoxicity investigation has also been done via a simple model of spherical gold nanoparicles (GNPs) and human lung cancer cell A549, which might provide some suggestions for the applications of noble metal nanomaterials.
The results are as follows:
(1) Metallic nanostructures with hollow interiors or tailored porosity represent a special class of attractive materials with intriguing chemicophysical properties. This paper presents the fabrication of a new type of metallic nanoporous nanotube structure based on a facile and effective combination of nanocrystal growth and surface modification. By controlling the individual steps involved in this process, such as nanowire growth, surface modification, thermal diffusion, and dealloying, one-dimensional (1-D) metallic nanostructures can be prepared with tailored structural features and pre-designed functionalities. These tubular and porous nanostructures show distinct optical properties, such as tunable absorption in the near-infrared region, and enhanced capability for electrochemiluminescence signal amplification, which make them particularly desirable as novel1-D nanocarriers for biomedical, drug delivery and sensing applications.
(2) Considering the residual Ag component in the Au/Ag alloy porous nanotubes (APNTs), we fabricated a kind of Pt/Ag composite porous nantubes (PNTs) with enhanced catalytic actvity toward HCOOH electrooxidation via the simple galvanic replacement between the residual and H2PtCl6-Due to the relatively low content of Ag in the Au/Ag APNTs as well as the effective alloy between Au and Ag, we do think the reduced Pt atoms disperesed on the PNTs surface could be effectively controlled and separated by the surface Au atoms, which could be ascribed to the lower diffusion coefficient of Pt than that of Au. By tuning the amount of Pt precursor, Pt/Au PNTs with different Pt-decorated loading could be easily approached. Structural characterizations with scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray powder diffraction (XRD) reveal a novel nanoarchitecture with multimodal open porosity and excellent structural continuity and integrity. Meanwhile, as a kind of anodic catalysts, CV and other techniques demonstrated that the Pt/Au PNTs possess excellent electrocatalytic activity toward HCOOH oxidation and enhanced tolerance to CO poisoning.
(3) Based on the one dimensional Ag nanowires synthesized via a modified polyol process, with a simple electroless plating and selective etching process we sucessfully fabricated Pt/Ag composite porous nanotubes (Pt/Ag PNTs). We have investigated the influence of different amount of Pt precursors toward the final Pt/Ag PNTs structures. It was find that the mechanical strength of the composite PNTs wall sturcture strongly depended on the dosage of H2PtCl6, which presents a positive correlation. Following, the Pt/Ag PNTs were used as an anodic catalyst under alkaline condition and sensing electrode in neutral conditon toward the electrooxidation of ethanol and detection of H2O2, respectively. As for the ethanol oxidation, campared with the commerical Pt/C catalyst, Pt/Ag PNTs possessed the similar electrochemical behaviors, but their intrinsic activity is evidently higher than that of Pt/C. CO stripping in acid sloution showed that Pt/Ag PNTs have much higher tolerance to CO poisoning than Pt/C. During the detection of H2O2, we got find that Pt/Ag PNTs exhibits sensitive respones toward the reduction of H2O2. CV study illustrated that a linear relationship for H2O2determniantion in a concentration range from25μmol/L to4mmol/L, with～0.8μmol/L response sensitivity. These two results revealed that Pt/Ag composite PNTs could be a kind of remarkable alkaline fuel cell catalysts and superior sensing electrode materials.
(4) We developed a large scale, simple and rapid route to fabricate Pt/Ag hollow porous nanospheres (HPNSs) which can be served as a supportless ORR catalyst with higher activity than that of commercial Pt/C catalysts. To prepare the HPNSs, firstly Ag@Pt core-shell nanoparticles were fabricated via a one-pot approach of solvent-thermal process, following a selective etching process by concentrated HNO3was employed to get HPNSs. Thermal annealing under relatively moderate condition (～160℃) was adopted to obtain high quality crystalline and stable shells of HPNSs (a-HPNSs), Owing to their ultra-thin wall structure (～3nm), porous shells with high surface-area-to-volume, and their alloy structures, the α-HPNSs exhibited significant enhancement of the ORR catalytic activity over commercial Pt/C catalyst, and the half-wave potential of α-HPNSs is～0.896V (versus a reversible hydrogen electrode, RHE), which is nearly70mV higher than that of Pt/C (～0.828V vs. RHE). Durability examination adopted the same condition and the α-HPNSs showed surprisingly high activity toward ORR. Although the α-HPNSs are particle-like structure, they displayed superior connectivity and conductivity without any substrates during the electrochemical test. Consequently, this method allows simplification of the experimental procedures by avoiding the tedious mixing and optimization of catalysts with supporting materials.
(5) Gold nanoparticles (GNPs) were used to evaluate their cytotoxicity toward human lung cancer cells A549. No cell proliferation inhibition was found when the cells were treated by GNPs independently. However, when L-buthionine-sulfoximine (BSO) was used to decrease the expression of glutathione (GSH) in A549cells, GNPs showed evident cytotoxicity to cells. Interestingly, the cytotoxicity of GNPs could be reversed after adding outside source GSH into the system. Whereas GSH plays an important role in eliminating reactive oxygen species (ROS), by monitoring the intracellular levels of ROS, GNPs were observed to generate more intracellular ROS in the presence of BSO. The cytotoxicity caused by GNPs toward lung cancer cells could therefore be partially attributed to the increase in intracellular ROS levels. These results suggest that caution should be paid in the use of GNPs for in vivo tests because GNPs can serve as therapeutic agents in their own right as well as carriers for other drugs and biomolecules.
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