电化学法合成荧光碳纳米粒子及性能表征

介绍了一种通过电化学氧化-还原循环的方法的制备碳纳米粒子并对其相关性质进行了表征.透射电镜结果表明,制备的纳米粒子粒径大小分布在(2.5±0.3)nm区间,而且其晶格间距为0.33nm左右,完全符合石墨的晶体特征.荧光光谱显示,该粒子在456nm具有稳定的可见光发射,其荧光量子效率达到了0.11.此外还考察了纳米碳颗粒的电化学发光性质,结果表明,该粒子在电化学发光检测方面具有潜在的应用价值.     

金属纳米电极的制备、表征及其在电化学测量中的应用

本文简要介绍了各种金属纳米电极的制备及表征方法。结合我们自己的工作,重点介绍了纳米电极在电化学反应动力学参数测量及扫描电化学显微镜(SECM)中的应用,并对其发展前景进行了展望。引用文献78篇。     

沉淀法制备CeO2纳米晶与表征

采用乙醇为分散剂和保护剂,用反向沉淀法制备了不同粒径的CeO2纳米晶。XRD分析表明,当焙烧温度为250－800℃时,所合成的CeO2纳米粒子属于立方晶系,空间群为OH^5-FM3M。TEM分析表明,CeO2纳米粒子呈球形,粒度随焙烧温度的增加而增大。热失重分析表明样品的热失重主要受温度的影响,而焙烧时间的影响不大。相对密度分析表明,随CeO2纳米晶粒度的增大,粉末的密度增加。     

电化学电容器电极材料超细MnO2的制备及表征

高性能的电化学电容器具有极其重要和广阔的应用前景(1)。以RuO2等贵重金属氧化物为电极材料的电化学电容器已应用于多个领域(2),但昂贵的价格限制了它们更加广泛的应用。有些廉价金属氧化物也具有一定的氧化还原准电容,如Co3O4、NiO和MnO2等(1,3 6)。二氧化锰价格低廉,资源丰富,电化学性能好,其作为电化学电容器的活性材料具有更大的应用前景和价值。本文采用K2S2O8氧化MnSO4·H2O制得超细MnO2,并通过XRD、TEM和SEM测试对其进行表征,并研究了其在0 5mol/LNa2SO4水溶液中的循环伏安性能、恒流充放性能以及电容稳定性能。1…     

纳米结构Ce掺杂PbO2膜电极的电化学沉积和性质

The effect of Ce(Ⅲ) on the morphology and structure of deposited film of lead dioxide was studied by cyclic voltammetry (CV), X-ray diffractometry (XRD) and scanning tunneling microscopy (STM). The results indicated that the Ce-doped PbO2 film consisted of a mixture of α- and β-phase of PbO2. Ce doping changed the size of PbO2 crystal grains and made the crystallite size on the electrode surface in the nanometer range. Owing to the formation of nanometer-structured grains, the specific surface areas and activity sites of the electrode surface were increased, hence the catalytic activity of Ce-doped PbO2 electrode was evidently higher than that of undoped PbO2 electrode.     

CeO2—TiO2复合纳米晶多孔膜的光电化学行为

用溶胶凝胶法制备了CeO2－TiO2复合纳米晶多孔膜电极，并用XRD及原子力显微镜（AFM）进行表征．通过光电化学研究，发现了CeO2-TiO2复合纳米晶电极光响应的p型和n型转换现象．结果表明，随着CeO2含量的不同及外电场的变化，CeO2－TiO2复合纳米晶电极可以呈现不同的光响应．     

纳米碳管电极的制备与电化学检测性能研究

纳米碳管由于其独特的物理和化学性能及广阔的应用前景而备受关注,其相关研究涉及到众多领域[1￣3]。在电化学分析领域,与其它碳电极材料相比,纳米碳管电极具有较大的电极表面积和较高的电子传递速率,其使用能增大响应电流、降低检出限,是目前电化学分析电极中一个十分引人注目     

Ru(bpy)2(NCS)2染料敏化CdS/Zn2+TiO2复合半导体纳米多孔膜的光电化学

采用水热法合成了Zn²⁺离子掺杂的TiO₂纳米粒子[Zn²⁺掺杂量0.5%(物质的量的比)],并用光电化学方法研究了经Ru(bpy)₂(NCS)₂(bpy=2,2′bipyridine₄,4′dicarboxylicacid)分别敏化的掺杂Zn²⁺的TiO₂电极(简写为Zn²⁺-TiO₂)和CdS/Zn²⁺-TiO₂复合半导体纳米多孔膜电极的光电化学行为.实验证明Ru(bpy)₂(NCS)₂敏化CdS/Zn²⁺-TiO₂复合半导体纳米多孔膜电极比单独敏化Zn²⁺-TiO₂电极的光电转换效率高,且敏化Zn²⁺TiO₂电极和敏化CdS/Zn²⁺TiO₂复合半导体纳米多孔膜电极比Zn²⁺-TiO₂电极的光电流产生的起始波长都向长波方向移动.在360600nm范围内,Ru(bpy)₂(NCS)₂敏化CdS/Zn²⁺-TiO₂复合半导体纳米多孔膜电极光电转换效率最好.     

形貌可控的钯纳米粒子的电化学制备及电催化性质

以NaPdCl4为前驱体, 以柠檬酸钠为包裹剂, 通过两步恒电势法在氧化铟锡(ITO)导电玻璃基底上沉积得到不同形貌的钯纳米粒子(PdNPs). 通过调节晶种沉积电势和粒子生长电势、柠檬酸根和溴离子的浓度及反应温度等因素, 可以控制PdNPs的形貌、尺寸及在ITO基底上的生长密度; 制备出了钯纳米锥阵列及球形、花状和多面体形的PdNPs. 研究结果表明, 钯纳米锥阵列与其它形状的PdNPs相比, 在单位面积ITO基底上具有更大的表面积, 表现出对甲醇更强的电化学氧化能力.     

聚磷腈荧光纳米粒子的制备及表征

以六氯环三磷腈(HCCP)和荧光素(FL)为单体、乙腈为溶剂、三乙胺(TEA)为缚酸剂,在室温超声作用下,通过沉淀聚合,成功制备了具有良好荧光性能的聚磷腈纳米粒子(PZF)。通过红外光谱、X射线能谱分析(EDS)、扫描电子显微镜(SEM)和透射电子显微镜(TEM)对PZF的化学结构和组成元素进行了分析。结果表明:制备的PZF是实心结构且粒径均一,具有良好的荧光性能;在365nm紫外光下照射不同时间后PZF的荧光强度几乎没有发生变化,说明制备得到的PZF具有强耐光漂白性。     

Effects of Na2SiF6 on Preparing Mullite Material with Sludge from the Aluminum Profile Factory and Pyrophyllite

In this research,the mullite material with sludge from aluminum profile factory and pyrophyllite as primary raw materials was prepared. Based on the optimal formula,optimal calcining temperature and holding time determined in the research,effects of Na2SiF6 mineralizer on crystal structure,microstructure and properties of mullite were discussed to determine the optimal addition of Na2SiF6 mineralizer. With XRD and SEM methods,crystal structure and microstructure of the test samples were characterized; with Rietveld Quantification method,contents of various crystal phases in the test samples were determined; properties of the test samples were tested. In combination with the structural and property analysis results,the optimal Na2SiF6 addition was determined to be 2%. Correspondingly,the content of solid solution of mullite-Al4.59Si1.41O9.7 was 96.9wt%,the bulk density was 2.10 g/cm3,the degree of porosity was 27.0%,the water absorption rate was 12.8%,the rupture strength was 24.30 MPa and primary thermal-shock rupture strength retention rate was 87.4%.     

电化学沉积技术制备LiNiO2薄膜及表征

Well-crystallized LiNiO₂ thin films were prepared directly on nickel substrates in LiOH solution by constant current electrochemical deposition technique at 95 ℃. The as-prepared LiNiO₂ thin films were characterized by using XRD, SEM and XPS, and the results reveal that the as-prepared LiNiO₂ thin films are dense and uniform in surface and show hexagonal structure. The influence of processing parameters such as reaction temperature, duration, electrical current density as well as the concentration of LiOH solution on the structure and morphologies of as-prepared LiNiO₂ thin films were studied，and the preferable electrochemical processing conditions for preparing LiNiO₂ thin films were suggested.     

Synthesis and Electrochemical Properties of Highly Crystallized CuV2O6 Nanowires

CuV₂O₆ nanowires were prepared via a simple hydrothermal route using NH₄VO₃ and Cu(NO₃)₂ as starting materials. The structures and electrochemical properties of CuV₂O₆ nanowires were characterized by means of X-ray diffraction(XRD), scanning electron microscopy(SEM) and transmission electron microscopy(TEM). The results show that the CuV₂O₆ nanowires are about 100 nm in width and single crystalline grown along [001] direction. CuV₂O₆ nanowires delivered a high initial discharge capacity of 435 and 351 mA·h/g at current densities of 50 and 100 mA·h/g, respectively. The electrochemical kinetics of the CuV₂O₆ nanowires was also investigated by means of electrochemical impedance spectroscopy(EIS) and the poor rate performance was observed, which may be attributed to the low ion diffusion coefficient of the CuV₂O₆ nanowires.     

几种对称镍卟啉配合物的合成、表征和电化学性质

卟啉试剂是一类重要的离子配位显色剂,在生物体中具有重要作用．作为自然界存在的金属卟啉之一,镍卟啉的电化学研究具有化学和生物学意义．四对羟基苯基卟啉合成已有不少报道［１,２］,但产率较低,只有１０％左右．Ｌｉｎｄｓｅｙ等发现用ＢＦ３作催化剂,在ＣＨ２Ｃ...     

微波辅助合成双1,2,4-三嗪化合物及其荧光特性研究

以联苯甲酰、二甲酰肼为原料, 采用微波技术合成了5个双1,2,4-三嗪化合物3, 产率72%～85%, 利用元素分析、MS, IR, ¹H NMR和荧光光谱对其结构进行了表征, 并研究了金属离子对化合物3a的荧光性质的影响. 结果表明, 微波合成具有缩短反应时间、提高产率的优点; Cu^2＋, Ni^2＋等金属离子对化合物3a产生明显的荧光猝灭作用.     

[Co(mim)_6]Br_2·2H_2O的离子热合成、晶体结构及电化学性质

以N-甲基咪唑(min)为配体,采用离子热方法在离子液体(1-乙基-3-甲基咪唑溴盐)中合成了Co(Ⅱ)配合物{[Co(mim)6]Br2·2H2O, 1},其结构经IR和元素分析表征.X-射线单晶衍射分析表明:1属单斜晶系,P21/c空间群,晶胞参数:a＝0.818 2(2) nm, b＝1.357 3(2) nm, c＝1.623 4(19) nm, β＝111.12(4)°, V＝1.682(5) nm3, Dc＝1.476 g·cm-3, F(000)＝762, Z＝2, μ(MoKα)＝2.927 mm-1, R1＝0.036 8, R2＝0.098 9.在1的晶体结构中,钴(Ⅱ)与配位原子形成畸变的八面体结构.采用循环伏安法研究了1在水溶液中的电化学性质,结果表明1中存在一对可逆的氧化还原峰,其峰值分别为0.51 V和0.25 V,为Co(Ⅱ)/Co(Ⅲ)间的相互转化.     

硅烷基取代苯并二硫杂环戊烯的合成及电化学性质

以苯并-1,3-二硫杂环戊烯为原料,通过金属化反应以及锂化二硫杂环戊烯与氯代硅烷反应合成了系列2-硅烷基取代苯并-1,3-二硫杂环戊烯化合物.测定了化合物的氧化电位,发现硅的引入导致苯并-1,3-二硫杂环戊烯的氧化电位明显降低,给体的给电子能力增强.     

新型卟啉衍生物的合成、结构表征和电化学性质的研究

以合成的[5-(4-溴苯基)-10,15,20-三苯基卟啉]锌为底物,通Stille偶联的方法合成5-(4’-氨基-4-联苯基)-10,15,20-三苯基卟啉,[5-(4’-氨基-4-联苯基)-10,15,20-三苯基卟啉]锌配合物以及[5- (4’-甲硫基-4-联苯基)-10,15,20-三苯基卟啉]锌配合物。并用Uv,‘H NMR, IR, Ms, Fs等表征确证了该系列配合物的结构,并用循环伏安法对以上部分产物进行了电化学性质的研究.     

十八硫醇自组装膜对TiO2光电氧化甲醇的敏化作用

纳米电极;甲醇光电氧化;十八硫醇自组装膜对TiO2光电氧化甲醇的敏化作用