纳米银形状控制合成与聚合物纳米银复合材料

纳米银(Ag NPs)由于其独特的物理、化学和生物学特性备受研究人员的关注.纳米银应用性能除了受到粒子尺寸、分布、纯度等因素影响,还与纳米银的形状密切相关.纳米银的形状对纳米银的抗菌性能、光学性能以及聚合物纳米银复合材料的综合性能都会产生重要影响.纳米银的形状控制合成可以进一步发挥聚合物纳米银复合材料的性能潜力.因此,不断发展纳米银新的合成方法,研究纳米银形状控制的机理就显得尤为重要.本文综述了纳米银合成方法和不同形状纳米银的最新研究进展,合成方法重点介绍了辐射法、激光烧蚀法、电化学法、光化学法和生物合成法,评述了这些方法的优缺点;同时从模板法、动力学、热力学以及氧化刻蚀4个方面介绍了纳米银形状控制的机理.介绍了聚合物纳米银复合材料的研究进展.     

硫化亚铁电极的电化学合成及性能测试

采用循环伏安法确定了合成硫化亚铁的电极电位,在ＬｉＣｌ－ＫＣｌ－Ｌｉ２和Ｌｉ（ＦＣｌＩ）－Ｌｉ２Ｓ两种熔体中,控制铁电极的电位为－１．０Ｖ合成了硫化亚铁电极,测试了电极的充电性能,在Ｌｉ（ＦＣｌＩ）－Ｌｉ２Ｓ熔盐２体系中电化学合成硫化亚铁电极的性能最好。     

纳米银修饰电极差分脉冲伏安法测定盐酸金霉素

建立了快速测定盐酸金霉素(CTC)的方法。通过NaBH4还原法制备纳米银(AgNPs)溶胶,并利用X射线衍射和紫外-可见光谱进行表征。将制备好的AgNPs滴涂到玻碳电极表面制备修饰电极(AgNPs/GCE),研究了CTC在AgNPs/GCE上的电化学行为及伏安法测定,优化了缓冲溶液和pH等检测条件。结果表明,CTC在pH 3.3的柠檬酸-NaOH-HCl缓冲溶液中检测效果最佳。CTC在AgNPs/GCE上发生2个电子和2个质子的不可逆电化学氧化反应,且反应受吸附控制。最佳条件下,CTC的氧化峰电流与其浓度呈现良好的线性关系,线性范围为0.5~100μmol/L,检出限为0.14μmol/L。该修饰电极可用于河水样品检测。     

抗坏血酸在纳米银DNA修饰电极上的电化学行为研究

利用电化学生长法制备了纳米银DNA修饰电极.在pH 4.1的磷酸盐(PBS)缓冲溶液中研究了抗坏血酸(AA)在该电极上的电化学行为,实验得到电荷传递系数α=0.41、扩散系数D=1.22×10-5 cm2 /s.建立了利用修饰电极催化作用快速测定抗坏血酸的方法,修饰电极对抗坏血酸的催化氧化峰与抗坏血酸的浓度分别在1.0×10-2～5.0×10-5 mol/L、5.0×10-6～5.0×10-8 mol/L范围内呈线性关系,检出限为1.0×10-9 mol/L.该方法快速、灵敏.     

纳米银、金溶胶的电化学合成及其基本胶体性质——物理化学综合实验设计

电化学和胶体体系基础理论是大学本科物理化学学习的重要内容。通过综合化学实验设计,以直接电化学还原方法制备纳米银、金溶胶,利用紫外-可见光谱分析溶胶粒子的特征吸收光谱,并运用循环伏安法探讨表面活性剂的稳定作用和纳米金属溶胶的形成机理,从而提高学生的基础知识综合运用能力与综合实验技能,适合在大学化学及其相关专业的综合化学实验中推广。     

纳米银粒子修饰电极法测定血红蛋白

报道了一种利用纳米材料修饰电极检测血红蛋白的新方法。制作了以纳米银粒子修饰的银电极,并研究了血红蛋白在该修饰电极上的直接电化学行为。实验结果表明,血红蛋白在该修饰电极上具有良好的电流响应。在2.0×10-7~1.0×10-5mol/L浓度范围内,血红蛋白的氧化峰电流与其浓度呈良好线性关系;检出限为7.4×10-8mol/L。研究了该修饰电极对血红蛋白的催化机理,利用该电极所建立的方法实现了对血红蛋白的分析测定。     

树枝状纳米银颗粒的制备与电活性

在Ag(NH3)2+溶液中,在钛基体上电沉积出树枝状纳米银颗粒,研究了沉积电位对树枝状纳米银颗粒形成的影响,探讨了这种树枝状纳米银颗粒形成的机理,并研究了这种钛基树枝状纳米银电极(Ag/Ti)在碱性溶液中对甲醛氧化的电催化活性。结果表明,在30 mmol/LAg(NH3)2+以及沉积电位在-1.8～-1.2 V(vsAg)时,形成了形态为树枝状的纳米银颗粒。在沉积电位为-1.6 V(vs Ag),Ag(NH3)2+浓度为30 mmol/L的溶液中,电沉积制备的这种树枝状纳米银电极(Ag/Ti)对甲醛氧化具有强的电催化活性。循环伏安曲线表明,在0.1 mol/LNaOH溶液中以及甲醛的浓度范围在0～40 mmol/L,甲醛浓度和它的氧化峰电流密度呈现良好的线性关系,检测下限达到0.662 mmol/L,这种新型的树枝状纳米银电极有望作为甲醛检测的传感器。     

有机氟化物的电化学合成

有机氟化物在很多领域(尤其是药物方面)有着广泛的应用,但鉴于氟的特殊反应性,氟原子的引入一直是有机化学中的难题.而有机电化学合成作为近年来新兴的合成手段,大大拓宽了有机反应的界限,使得更多绿色简易的氟化方法被开发了出来.本文就将集中列举这些有机电化学方法氟化的实例,并探讨电化学方法对于氟化学这一领域可能的推动作用.     

高分散纳米银/蒙脱土复合材料的制备及表征

In this paper, the nanosized silver particles with a narrow size distribution and high dispersivity located in both interior and exterior layers of montmorillonite as a confinement reactor by a chemical reduction method were prepared. It was found that the obvious changes of the particle size and dispersivity of the nanosilver located in both interior and exterior layers of montmorillonite did not occur after being treated by supercritical ethanol dried at the temperature of 270 ℃ and proven that the nanosilver/montmorillonite composites had a good thermal stability, which will have some potential applications as a high activity catalyst, antibacterial agents etc.     

纳米NiAl_2O_4前驱体的电化学合成

在乙醇溶液中,按Ni/Al电量比为1∶3依次电解铝片和镍片,制得复合氧化物纳米粉体NiO Al2O3的前驱体NiAl2(OCH2CH3)(8-y)(acac)y[acac为乙酰丙酮基].产物通过红外光谱、X射线衍射、电子透射显微镜进行了表征,同时研究了镍电极在铝醇盐溶液中的电化学行为,讨论了影响电合成镍、铝醇盐配合物的关键因素.实验表明,电解温度控制在54～60℃、导电盐Bu4NBr浓度为0.040～0.045mol/L时,电流效率约为93%.水解后的干凝胶粒径在10nm左右,为纳米NiAl2O4粉体的制备创造了条件.     

银纳米粒子的合成及其在喷墨打印电路中的应用

银纳米粒子在光学、电磁学和生物相容性等方面所具有的独特优点,使其在一系列领域得到了广泛的应用。本文综述了银纳米粒子的合成方法,以及其作为喷墨打印材料在电路制备中的应用,并展望了其发展前景。     

甲烷氧化菌素介导一步法合成合成纳米银

以硝酸银为前体物,甲烷氧化菌素(Mb)将Ag(Ⅰ)还原Ag(0),并形成纳米银粒子(AgNPs),同时Mb吸附在形成的AgNPs表面,起到保护剂作用避免AgNPs聚集沉淀.采用紫外-可见光谱、荧光光谱、红外光谱、透射电镜和X射线电子能谱等对合成的AgNPs粒子过程、Mb合成AgNPs官能团、AgNPs形貌和AgNPs结构及价态等进行了分析.结果表明Mb可以一步法合成AgNPs离子.     

油酸囊泡层状液晶作为模板电化学合成银纳米颗粒

在油酸囊泡的层状液晶中利用电化学沉积法成功地制备了银纳米颗粒。并用扫描隧道显微镜(STM)和透射电子显微镜(TEM)对银纳米颗粒进行了表征，发现银纳米颗粒能够均匀地分散在油酸囊泡中，并且油酸囊泡能够有效地阻止产生的银纳米颗粒发生聚集反应。此外，我们还提出了银纳米颗粒形成的机理。     

Electrochemical Dissolution of Silver Nanoparticles and Its Application in Metalloimmunoassay

This work demonstrates the use of silver nanoparticles as a simple electrochemical biolabel to induce 10⁶ signal enhancement. We propose a mechanism of measuring the silver nanoparticles on a specific screen‐printed planar carbon electrode, without the requirement for the harsh oxidant or toxic reagents described in prior‐art for gold sol methods. The possible measurement process was validated with orthogonal techniques such as UV/Vis spectroscopy, dynamic light scattering and by anodic stripping voltammetry (ASV). The findings were utilized to develop a novel electrochemical sandwich immunoassay where the analyte concentration is directly proportional to ASV oxidation peak of silver. This technique in the future is envisaged to form the foundation of a generic Point of Care platform. The assay was applied to cardiac marker: myoglobin with detection limit of 3 ng/mL.     

银纳米粒子修饰银电极法测定酪氨酸

通过NaBH₄还原AgNO₃得到胶体银纳米粒子,制作了以该纳米粒子修饰的银电极。研究了银纳米粒子修饰银电极在电催化中的应用,并对相关机理进行了探讨。该修饰电极对醋酸具有电催化活性,但酪氨酸却对该催化信号有明显的抑制作用,因此建立了用胶体银纳米粒子修饰银电极在NaAc-HAc缓冲溶液中检测酪氨酸的方法,并讨论了最佳工作条件。结果表明：在pH = 5.5时,峰电流与酪氨酸的浓度在1.0×10_-8～1.0×10_-3mol L_-1 范围内呈良好的线性关系,检出限为4.2×10_-9 mol L_-1,线性回归方程为Ip (μA) = 7.64 pC – 15.69 ( R = 99.73% )。用该方法检测氨基酸注射液中酪氨酸的含量,加标回收率在95.2%~107.8%之间。     

Interference‐Free Electrochemical Detection of Nanomolar Dopamine Using Doped Polypyrrole and Silver Nanoparticles

This paper presents a new approach to detect dopamine in nanomolar range using an electrochemical sensor utilizing a composite made of chitosan‐stabilized silver nanoparticles and p‐toluene sulfonic acid‐doped ultrathin polypyrrole film. Studies included cyclic voltammogram, amperometry, differential pulse voltammetry and also investigation by electrochemical impedance spectroscopy. A detection limit of 0.58 nM was achieved in the linear range 1×10^?9 M to 1.2×10^?7 M. High sensitivity towards DA, good reproducibility and long‐term stability have been demonstrated without interference from ascorbic acid, uric acid, epinephrine, L ‐dopa, glucose. The sensing system was successfully applied for quantitative determination of dopamine in commercially available human blood serum.     

Synthesis of Silver and Gold Nanoparticles by a Novel Electrochemical Method

Spherical silver and gold nanoparticles with narrow size distributions were conveniently synthesized in aqueous solution by a novel electrochemical method. The technological keys to the electrochemical synthesis of monodispersed metallic nanoparticles lie in the choice of an ideal stabilizer for the metallic nanoclusters and the use of a rotating platinum cathode. Poly(N‐vinylpyrrolidone) (PVP) was chosen as the stabilizer for the silver and gold clusters. PVP not only protects metallic particles from agglomeration, but also promotes metal nucleation, which tends to produce small metal particles. Using a rotating platinum cathode effectively solves the technological difficulty of rapidly transferring the (electrochemically synthesized) metallic nanoparticles from the cathode vicinity to the bulk solution, avoiding the occurrence of flocculates in the vicinity of the cathode, and ensuring the monodispersity of the particles. The particle size and particle size distribution of the silver and gold nanoparticles were improved by adding sodium dodecyl benzene sulfonate (SDBS) to the electrolyte. The electrochemically synthesized nanoparticles were characterized by TEM and UV/Vis spectroscopy.     

Synthesis of Silver Nanoparticle‐Graphene Composites for Electroanalysis Applications using Chemical and Electrochemical Methods

An electrochemical device was developed for the simultaneous determination of sulfamethoxazole (SMX) and trimethoprim (TMP) using differential pulse voltammetry and glassy carbon (GC) electrodes modified with reduced graphene oxide (rGO) and silver nanoparticle (AgNP) composites, synthesised using both chemical and electrochemical methods. The morphology and electrochemical behaviour of the GC electrodes modified with the rGO/AgNP (chemical method) and rGO‐AgNP (electrochemical method) composites were characterised by scanning electron microscopy and cyclic voltammetry. These techniques demonstrated that, in both methods, the graphene oxide was modified by the AgNPs, and the composite synthesised by the electrochemical method showed a better dispersion of the nanoparticles, resulting in an increase in the surface area compared to the rGO/AgNP composite. The GC/rGO‐AgNP electrode was evaluated and optimised for the simultaneous determination of SMX and TMP, achieving detection limits of 0.6 μmol L⁻¹ for the SMX and 0.4 μmol L⁻¹ for the TMP. The proposed GC/rGO‐AgNP electrochemical device was successfully applied to the simultaneous determination of SMX and TMP in wastewaters samples.     

化学还原法制备多形貌银纳米材料

银纳米材料因具有导热导电性能好、光电性能优良及抗菌能力强等优点而引起广泛关注,近年来其制备方法得到广泛研究。已报道的制备方法可分为化学法、物理法和生物法等,其中化学还原法可以通过使用不同的还原剂、包裹试剂及助剂,实现不同形貌及粒径的银纳米材料的快速制备。本文综述了化学还原法制备颗粒状、线形、片状、立方体及其它形貌的银纳米材料的原理及应用,并展望了银纳米材料工业化制备及应用研究的发展趋势。可控制备多形貌银纳米材料对于电子行业、医药生物以及传感器等相关领域的发展具有重要意义。