Studies on the behaviors of PbSO4/Pb and PbO2/PbSO4 electrodes prepared from lead carbonate by powder microelectrode technique

The behaviors of PbSO₄/Pb and PbO₂/PbSO₄ electrode prepared from PbCO₃ have been examined using powder microelectrode(PME) technique and cyclic voltammetry(CV). Firstly, PMEs packed with PbCO₃ transformed into PbSO₄ PME in 1.0 mol/L H₂SO₄ solution at 30 °C, and then the PbSO₄ in the PMEs were formed to Pb or PbO₂ using an unsymmetrical signal (Q _a/Q _c for PbSO₄/Pb electrode andQ _c/Q _a for PbO₂/PbSO₄ electrode being 0.1–0.3) in 2.5 mol/L H₂SO₄ solution. The results show that the CV characteristic of either PbSO₄/Pb or PbO₂/PhSO₄ PME prepared from PbCO₂ are as good as that of both electrodes made from lead oxide powder produced by ball mill. Foundation item: Supported by the National Natural Science of China(29677013) and Chenguang Foundation of Wuhan Municipal Science and Technology Commission(20005004022) Biography: Dai Zhong-xu(1968-), male, Lecturer, Ph. D. candidate, research direction: electrochemistry.     

Comparative study of oxidation ability between boron-doped diamond (BDD) and lead oxide (PbO<Subscript>2</Subscript>) electrodes

The electrochemical oxidation capabilities of two high-performance electrodes, the boron-doped diamond film on Ti (Ti/BDD) and the lead oxide film on Ti (Ti/PbO₂), were discussed. Hydroxyl radicals (·HO) generated on the electrode surface were detected by using p-nitrosodimethylaniline (RNO) as the trapping reagent. Electrochemical oxidation measurements, including the chemical oxygen demand (COD) removal and the current efficiency (CE), were carried out via the degradation of p-nitrophenol (PNP) under the galvanostatic condition. The results indicate that an indirect reaction, which is attributed to free hydroxyl radicals with high activation, conducts on the Ti/BDD electrode, while the absorbed hydroxyl radicals generated at the Ti/PbO₂ surface results in low degradation efficiency. Due to quick mineralization which combusts PNP to CO₂ and H₂O absolutely by the active hydroxyl radical directly, the CE obtained on the Ti/BDD electrode is much higher than that on the Ti/PbO₂ electrode, notwithstanding the number of hydroxyl radicals produced on PbO₂ is higher than that on the BDD surface.     

Studies on the Behaviors of PbSO4/Pb and PbO2/PbSO4 Electrodes Prepared from Lead Carbonate by Powder Microelectrode Technique

College of Chemistry and Environmental Science, Wuhan University, Wuhan 430072, China Abstract:The behaviors of PbSO4/Pb and PbO2/PbSO4 electrode prepared from PbCOs have been examined using powder microelectrode(PME) technique and cyclic voltammetry(CV). Firstly, PMEs packed with Pb- CO3 transformed into PbSO4 PME in 1.0 mol/L H2SO4 solution at 30 C, and then the PbSO4 in the PMEs were formed to Pb or PbO2 using an unsymmetrical signal (Qa/Qc for PbSO4/Pb electrode and QcQa for PbO2/ PbSO4 electrode being 0. 1-0. 3) in 2. 5 mol/L H2SO4 solution. The results show that the CV characteristic of either PbSO4/Pb or PbO2/PbSO4 PME prepared from PbCO3 are as good as that of both electrodes made from lead oxide powder produced by ball mill.     

基于SnO2/TiO2/Au NPs纳米复合材料发展光电化学方法特异性检测唾液酸

制备了氧化铟锡（ITO）/二氧化锡（SnO₂）/二氧化钛（TiO₂）/金纳米粒子（Au NPs）纳米复合电极（ITO/SnO₂/TiO₂/Au NPs）,并利用它发展了可以选择性检测唾液酸（SA）的光电化学（PEC）法.采用旋涂法制备了ITO/SnO₂电极,并通过静电纺丝和磁控溅射技术在ITO/SnO₂表面原位合成了TiO₂纳米纤维和Au NPs.与单纯SnO₂比,ITO/SnO₂/TiO₂/Au NPs纳米复合电极的光电性能显著提高.这可能与Au NPs的局域表面等离子体共振效应（LSPR）和TiO₂/SnO₂异质结之间的协同作用密切相关.之后,通过金硫键（Au-S）将四巯基苯硼酸（4-MPBA）修饰在ITO/SnO₂/TiO₂/Au NPs电极表面,利用4-MPBA和SA之间的非特异性酯化反应,发展了可以特异性检测SA的PEC传感平台.     

Photoelectrochemical synergetic degradation of Acid Orange II with TiO2 modified β-PbO2 electrode

Electrochemically assisted photocatalysis is an effective approach to improve photocatalytic efficiency. In this paper, modified β-PbO2 electrode was prepared by TiO2 co-deposition and characterized by SEM and XRD. Then 2.0g TiO2 modified β-PbO2 electrode (2.0 g TiO2 involved in the 200 mL co-deposition solution) was used in electrochemically assisted photocatalytic degradation of Acid Orange II and the influence of initial pH values was investigated when the potential applied across the electrodes was 1.5 V. When the potential applied was 2.5 V, the difference of the degradation process and the final products were studied. The results indicated that 2.0 g TiO2 modified β-PbO2 electrode was different from the unmodified one in that the β-PbO2 crystals became finer and the electrode became more compact and more uniform. The synergetic effect in electrochemically assisted photocatalytic degradation of Acid Orange Ⅱ was observed and degradation efficiency and TOC removal were the highest at initial solution pH 2.0. By UV-visible spectral analysis, it was proved that photoelectrochemical synergetic degradation of Acid Orange Ⅱ went through the step of producing main product maleic acid for the solution at the initial pH 2.0 within 2 h, but the degradation was slow for the solution at the initial pH 12.0.     

超级电容器用PbO2电极的电沉积工艺

以钛板为基底,采用电沉积方法制备了Ti-PbO2电极,与活性炭(AC)组成超级电容器.研究了铅盐种类对电沉积PbO2电极放电性能的影响,发现用Pb(CH3COO)2做溶质的氮氧化钠溶液制备的PbO2电极容量最大.利用不同浓度的氢氧化钠溶液配置饱和醋酸铅电解液,制备PbO2电极进行了放电测试,研究了氢氧化钠浓度对电沉积P...     

Ce改性Ti基PbO_2电极的制备及电催化氧化4—氯酚的研究

采用电沉积法制备了Ti基PbO2电极(Ti/PbO2)和Ce改性Ti基PbO2电极(Ti/PbO2—Ce).利用扫描电子显微镜(SEM)和循环伏安法对改性前后的电极进行表征,并考察电极的电催化氧化能力.实验结果表明:Ti/PbO2—Ce电极具有比Ti/PbO2电极更小的晶粒尺寸和更高的电催化氧化降解有机物污染物能力.Ti/PbO2—Ce电极电催化氧化降解4—氯酚(4—CP)2 h后,溶液的BOD5/COD值由0.03升高到0.48,有效地提高了4—CP废水的可生化性.     

Mn_2O_3/CRF复合材料的制备及其在超级电容器中的应用

通过采用沉淀法在碳气凝胶表面负载金属氧化物三氧化二锰,制备得到Mn_2O_3/CRF复合材料。采用X射线衍射及电镜扫描等技术对所制备的复合材料进行结构形貌表征。实验结果发现碳气凝胶具有多重片层结构且孔隙发达。通过调节锰盐的含量考察三氧化二锰负载量对复合材料电化学性能的影响作用。采用循环伏安法及充放电测试对材料的电化学性能进行测试,结果表明Mn_2O_3/CRF复合材料具有良好的电容性及较好的可逆性。当Mn_2O_3含量达15%时复合材料的比电容最大,可达118.5 F/g。通过充放电测试1000次后发现该电极的比电容依然能够保持在一稳定值上,具有较好的稳定性。     

Synthesis of amorphous SeP2/C composite by plasma assisted ball milling for high-performance anode materials of lithium and sodium-ion batteries

To promote substantially the performances of red phosphorous(P) anode for lithium and sodium-ion batteries, a simple plasma assisted milling(P-milling) method was used to in-situ synthesize SeP₂/C composite. The results showed that the amorphous SeP₂/C composite exhibits the excellent lithium and sodium storage performances duo to the small nano-granules size and complete combination of selenium(Se) and phosphorous(P) to generate Se–P alloy phase. It was observed that insid...     

基于Pt-Au-MoS2-ITO传感器对于H2O2的还原检测

实验探究了二硫化钼（MoS₂）作为一种新型材料与贵金属纳米粒子金（Au）、铂（Pt）的复合基底对于过氧化氢（H₂O₂）的还原性检测,采用氧化铟锡导电玻璃（ITO）作为电极,制备出了基于Pt-Au-MoS₂-ITO的生物传感器,为H₂O₂还原性检测的便携性操作打下了基础.实验采用电化学沉积的方法制备材料,同时使用循环伏安（CV）法、计时电流法等传统电化学手段表征了传感器电化学性能,采用场发射扫描电子显微镜（FE-SEM）来表征传感器表面形貌.建立了用于H₂O₂还原检测的、具有高检测限、高灵敏度和宽检测范围的传感器.     

Bi掺杂O3型NaNi0.5Mn0.5O2钠离子电池层状正极材料的制备与储钠性能

O3型NaNi_0.5Mn_0.5O₂拥有高理论比容量且易于制备,是商业钠离子(Na⁺)电池的首选正极材料之一,但其循环稳定性仍面临挑战。利用Bi对NaNi_0.5Mn_0.5O₂进行改性。研究发现,Bi的引入可以在晶粒生长过程中通过调节表面能实现晶粒细化,并且Bi的掺杂增加了层状正极材料的晶胞参数,为Na⁺提供了宽的扩散通道,提高了Na⁺的扩散能力,优化了Na⁺在脱嵌过程中的可逆性。改性后的NaNi_0.495Mn_0.5Bi_0.005O₂实现了在2.0～4.0 V的电势区间内0.2 C倍率下的可逆容量为138.1 mAh/g,在5 C倍率下循环100圈后容量保持率可以达到97%。     

Au_(25)/L-半胱氨酸修饰金电极上CO_2的电化学还原

采用自组装方式制备GNPs/L-Cys/Au和Au_(25)/L-Cys/Au修饰电极,构造不同的CO_2电化学还原界面.利用线性扫描伏安法和红外光谱电化学技术研究修饰电极上CO_2电化学行为.电化学结果表明:与Au电极相比,在GNPs/L-Cys/Au电极上,CO_2还原过电位降低了将近190 mV;而在Au_(25)/L-Cys/Au电极上,过电位降低了将近280mV,Au_(25)/L-Cys/Au电极表现出更好的CO_2电化学催化效果.结合红外光谱电化学结果提出了CO_2在Au_(25)/L-Cys/Au电极上可能的还原机制.     

Enhanced resistive switching properties of HfAlOx/ZrO2- based RRAM devices

Resistive Random-Access Memory (RRAM) devices are recognized as potential candidates for next-generation memory devices, due to their smallest cell size, high write/erase speed, and endurance. Particularly, the resistive switching (RS) characteristics in oxide materials have offered new opportunities for developing CMOS-compatible high-density RRAM devices. In this study, the RS behavior of HfAlO_x/ZrO₂ thin films sandwiched structure between TiN bottom electrode and Au top electrodes were investigated. It was found that Au/HfAlO_x/ZrO₂/TiN stacks were superior in terms of RS performance when compare to Au/HfAlO_x/TiN memory stacks. The devices demonstrated a good resistance ratio of high resistance state and low resistance state ～10³ for Au/HfAlO_x/TiN and ～10⁵ for Au/HfAlO_x/ZrO₂/TiN stacks, respectively. Both stacks showed good retention characteristics (>10⁴ ?s) and endurance (>10³ cycles). The experimental current-voltage characteristics fitted with different conducting mechanisms, the linear lower bias region is dominated by ohmic conductivity, whereas the non-linear higher bias region was dominated by space-charge limited current conduction mechanism.     

基于纳米银-二氧化钛-壳聚糖复合物修饰电极的 芦丁电化学传感器的构建及其应用研究

本实验以Ag-TiO_2-CS纳米复合物修饰电极构建电化学传感器,建立适用于其分析检测的电化学分析新方法。利用Ag-TiO_2-CS修饰电极,以此制备芦丁电化学传感器。用循环伏安法(CV)对电极的电化学特性进行研究,之后用差分脉冲伏安法(DPV)对芦丁进行检测,建立芦丁的电化学检测新方法。CV实验表明Ag-TiO_2-CS纳米复合物具有良好的电化学活性,可以应用于芦丁检测。DPV实验进一步表明,修饰电极峰电流值与芦丁浓度在一定范围内呈线性关系,稳定性、抗干扰性等良好,此电化学传感器可以对芦丁片中的芦丁进行测定,结果良好。该传感器制作方法简单,灵敏度较高,稳定性好,可用于芦丁片中芦丁的分析测定。     

循环伏安法测定Ti/SnO2+Sb2Ox/PbO2阳极的分形维数及电催化性能

采用电沉积法制备了含有SnO2+Sb2Ox中间层的Ti/SnO2+Sb2Ox/PbO2耐酸阳极,用SEM表征了电极表面的形貌,用三电极体系测定了电极在0.5 mol/L H2SO4溶液中不同扫描速度下的循环伏安曲线,同时定量计算出了不同Sb掺杂量的电极表面的分形维数,重点讨论了分形维数和电极在酸性溶液中析氧电催化性能之间的关系。结果表明:Sb摩尔分数为0.02和0.10时电极的分形维数较高,动力学参数a较小,j0较大,且电极表面呈现蘑菇状,催化活性高。因此Ti/SnO2+Sb2Ox/PbO2电极是酸性溶液中较理想的阳极材料。     

Synthesis and characterization of Pt-MoO<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript>-TiO<Subscript>2</Subscript> electrodes for direct ethanol fuel cells

To enhance the CO-tolerance performance of anode catalysts for direct ethanol fuel cells, carbon nanotubes were modified by titanium dioxide (donated as CNTs@TiO₂) and subsequently served as the support for the preparation of Pt/CNTs@TiO₂ and Pt-Mo/CNTs@TiO₂ electrocatalysts via a UV-photoreduction method. The physicochemical characterizations of the catalysts were carried out by using X-ray diffraction (XRD), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), and infrared spectroscopy of adsorbed probe ammonia molecules. The electrocatalytic properties of the catalysts for methanol oxidation were investigated by the cyclic voltammetry technique. The results show that Pt-Mo/CNTs@TiO₂ electrode exhibits the highest performance in all the electrodes. It is explained that, the structure, the oxidation states, and the acid-base properties of the catalysts are influenced due to the strong interaction between Ti and Mo species by adding TiO₂ and MoO _x to the Pt-based catalysts.     

Preparation of transparent TiO2 nanocrystalline film for UV sensor

Nanocrystalline TiO2 is a very important inorganic semiconductor function material with a wild band gap of 3.0-3.2 eV. Owing to its characteristics of selectiveabsorption for UV light, it has been extensively applied in photocatalysts, dye-sensitized sola…     

Alkaline digestion behavior and alumina extraction from sodium aluminosilicate generated in pyrometallurgical process

In pyrometallurgical process, Al-and Si-bearing minerals in iron and aluminum ores are easily transformed into sodium aluminosilicates in the presence of Na₂O constituents, which alters the leaching behaviors of Al₂O₃ and SiO₂. It was confirmed that sodium aluminosilicates with different phase compositions synthesized at various roasting conditions were effectively digested in the alkaline digestion process. Under the optimum conditions at temperature of 100-120℃, liquid-to-solid ratio (L/S) of 10:2 mL/g, caustic ratio of 4, and Na₂O concentration of 240 g/L, the actual and relative digestion ratio of Al₂O₃ from the synthesized sodium aluminosilicates reached maximums of about 65% and 95%, respectively, while SiO₂ was barely leached out. To validate the superior digestion property of sodium aluminosilicate generated via an actual process, the Bayer digestion of an Al₂O₃-rich material derived from reductive roasting of bauxite and comprising Na_1.75Al_1.75Si_0.25O₄ was conducted; the relative digestion ratio of Al₂O₃ attained 90% at 200℃.     

Degradation of the antibiotic sulfamonomethoxine sodium in aqueous solution by photo-Fenton oxidation

In this study, photo-Fenton oxidation was applied to degradation of sulfamonomethoxine sodium (SMMS) in aqueous solution. The operation parameters of pH, temperature, and concentrations of H2O2, Fe2+ and SMMS were investigated. The optimum conditions for the photo-Fenton process were determined as follows: [SMMS]=4.53 mg/L, pH 4.0, [H2O2]=0.49 mmol/L, [Fe2+]= 19.51 μmol/L and T=25°C. Under these conditions 98.5% of the SMMS degraded. The kinetics were also studied, and degradation of SMMS by the photo-Fenton process could be described by first-order kinetics. The apparent activation energy was calculated as 23.95 kJ/mol. Mineralization of the process was investigated by measuring the chemical oxygen demand (COD), and the COD decreased by 99% after 120 min. This process could be used as a pretreatment method for wastewater containing sulfamonomethoxine sodium.     

A study on nano-sized NiO electrodes doping with C and Co prepared by electrochemical deposition-sintering processes and their capacitance performance

In the present work, it was studied that nanoosized NiO electrodes doping with C and Co were prepared by electrochemical deposition in an ethanol solution containing nickel nitrate and cobalt nitrate and sintering processes. The capacitance performance of such electrodes was also studied. The results reveal that samples obtained by electrochemical deposition first on a porous nickel cathode in an ethanol solution contain 0.5 mol/L nitrates, in which Ni(NO3)2 and Co(NO3)2 were mixed in a molar proportion of 8 : 2. After sintering at 300℃ for 2 h, they exhibited the best performance. XRD analysis illustrates that the essential phase of the product is NiO doping with certain content of C and Co. The particles of product imaged a spherical morphology with sizes of 20---30 nm in diameter, and with an average crystal size of 4--5 nm. The capacitance measurement of the simulating C/NiO capacitors indicates that a single electrode can reach as high as 410.0 F/g, and still maintain the value of 323 F/g after 30 recycles showed as a stabilized value with increasing recycles, when it was discharged at a current of 5 mA.