MnO2/碳纳米球电化学超级电容器电极材料的制备与性能研究

利用水热法合成了纳米棒状的MnO_2/碳纳米球(CNPs)作为电化学超级电容器的电极材料.利用场发射扫描电镜(FESEM)、X射线衍射光谱分析(XRD)对样品的微观形貌、物相进行分析;利用循环伏安法和恒电流充放电测试材料的电化学性能.结果表明:纳米棒状MnO_2/CNPs复合材料具有良好的电化学性能.在0.1 A/g的电流密度,1 mol/L Na_2SO_4电解液中,电极材料的比电容高达305.6 F/g,远高于纯碳球的比电容(49.3 F/g),当电流密度增至5 A/g时,材料的比电容为235 F/g,比电容仍能保持76.9%.     

Preparation and application of electrochemical barbital sensor based on molecularly imprinting technique

A molecularly imprinted electrochemical sensor was prepared based on poly folic acid(PFA) for rapid detection of barbital(BAR). The PFA membrane was obtained via directly electropolymerization technique on the surface of chemically modified Au electrode(Au/CME) by means of cyclic voltammetry(CV) in the potential range between-0.4 and 1.0 V in phosphate buffer solution(PBS) pH 7.04. The molecularly imprinted polymers(MIP) membrane was synthesized with BAR as template molecules and folic acid(FA) as the functional monomer. The performance and surface feature of the proposed imprinted sensor were investigated using CV, differential pulse voltammetry(DPV), electrochemical impedance spectroscopy(EIS) and scanning electron microscope(SEM). Under the optimized conditions, the peak current decrease(ΔI_p) was proportional to the BAR concentration in the range of 1.00×10~(–7)-1.00×10~(–4) mol/L(R~2=0.998 2) with a detection limit(S/N=3) of 4.65×10~(–8) mol/L. The results indicated that the imprinted sensor exhibited an excellent selectivity for BAR and it was successfully used to determine BAR in real samples with recoveries of 94.7%-106.2% by using the standard addition method.     

Luminol在GO（GN）/Nafion/GCE上的电聚合

基于石墨烯良好的导电性和luminol较好的电化学发光性能,利用循环伏安法研究了luminol在GO/Nafion,GN/Nafion修饰电极上的电化学聚合行为.考察了修饰剂组成成分、初始电位对电化学聚合的影响,并以铁氰化钾为探针考察了luminol电聚合前后的导电性.结果显示,在较负的起始电位下,luminol在GO/Nafion/GCE上更容易发生电化学聚合过程,且聚合后对[Fe(CN)6]3-显示了更强的电催化能力.     

MPA包覆的银纳米粒子修饰电极制备和电化学表征

运用自组装和电化学组装法,将MPA包裹的银纳米粒子修饰到金电极表面,制备成银纳米粒子单层和多层膜修饰电极. 循环电压-电流和电化学阻抗谱测定结果表明:以MPA包覆的银纳米粒子修饰电极的氧化电位明显负移,显示出银纳米粒子具有更高的活性. 以0.5mmol/L的K3[Fe(CN)6]溶液为检测体系,电化学阻抗谱测试得出电极表面对探针分子的阻碍作用有所增加. 循环电压-电流结果表明:与单层膜修饰电极相比,多层膜修饰电极的峰电流显著增加.     

基于二硫化钼-碳纳米颗粒复合物的电化学传感器

采用L-半胱氨酸辅助溶液相方法合成二硫化钼-碳纳米颗粒复合物,并利用扫描电子电镜对复合物的形貌进行表征.基于二硫化钼-碳纳米颗粒复合物修饰玻碳电极构建电化学传感器,用于扑热息痛的灵敏检测,利用循环伏安法和微分脉冲伏安法考察了电化学传感器的电化学行为.结果表明,扑热息痛的线性检测范围为0.1~100μmol/L,检出限为0.01μmol/L.而且,该方法成功地用于实际药品中扑热息痛的检测.该传感器具有选择性高、抗干扰能力强、重现性和稳定性好的优点.     

One-step and high-density protein immobilization on epoxysilane-modified silica nanoparticles

Silica nanoparticles are most commonly modified with amino-silanes, followed by post-modification activation for protein immobilization. In this work, epoxy-functionalized silica nanoparticles were prepared by modification with glycidyloxypropyl trimethoxysilane （GPTMS） for direct protein immobilization. Silica nanoparticles possessed an average size of 46 nm, but increased to 63 nm after GPTMS modification. Reaction time, reaction temperature and GPTMS content had no significant effect on par- ticle size. Zeta potential of SiO2 changed from -26mV to ＋38mV after modification. Fourier-transformed infrared spectroscopy revealed alkyl C--H bending and stretching bands at 2944 cm-1, 1343 cm-1 and 1465 cm-1, respectively, for the modified nanoparticles. Fluorescein cadaverine was found to bind to GPTMS-modified SiO2, but not to bare SiO2, indicating the chemical reactivity of epoxy groups on the modified nanoparticle with amines. Finally, fluorescenUy labeled bovine serum albumin （BSA） was used as a model protein to investigate the capacity of epoxy-SiO2 nanoparticles for protein immobilization. The results showed that more proteins were immobilized on the particle with longer reaction time, higher NaCI concentration, lower pH, and less GPTMS content. More importantly, proteins bound to epoxy-SiO2 nanoparticle were highly stable. Under optimized reaction conditions, as much as 25 mg BSA/g nanoparticle was covalentiy attached to the nanoparticle. The epoxy silane modification of silica nanoparticles offers a reactive surface for one-step and high-density protein immobilization.     

The Escherichia coli O157:H7 DNA detection on a gold nanoparticle-enhanced piezoelectric biosensor

This paper presents development of a quartz crystal microbalance （QCM） biosensor for real-time detection of E. coil O157：H7 DNA based on nanogold particles amplification. Many inner Au nanoparticles were immobilized onto the thioled surface of the Au electrode, then more specific thiolated sin- gle-stranded DNA （ssDNA） probes could be fixed through Au-SH bonding. The hybridization was induced by exposing the ssDNA probe to the complementary target DNA of E. coli O157：H7 gene eaeA, then resulted in a mass change and corresponding frequency shifts （ △f ） of the QCM. The outer avidin-coated Au nanoparticles could combine with the target DNA to increase the mass. The electrochemical techniques, cyclic voltammetry （CV） and electrochemical impedance spectroscopy （EIS） were adopted to manifest and character each step. The target DNA corresponding to 2.0×10^3 colony forming unit （CFU）/mL E. coil O157：H7 cells can be detected by this biosensor, so it is practical to develop a sensitive and effective QCM biosensor for pathogenic bacteria detection based on specific DNA analysis. The piezoelectric biosensing system has potential for further applications, such as food safety and environment monitoring, and this approach lays the groundwork for incorporating the method into an integrated system for in-field bacteria detection.     

金纳米粒子与电化学还原氧化石墨烯复合材料修饰电极的制备及其电化学应用

利用金纳米粒子(Au NPs)和电化学还原氧化石墨烯(ERGO)制备了以玻碳电极(GCE)为基底电极的复合材料修饰电极Au NPs-ERGO/GCE.采用场发射扫描电子显微镜(FESEM)、拉曼光谱、循环伏安(CV)法、计时电流法等方法对复合材料修饰电极进行了系统表征与分析.将所制备的复合材料修饰电极应用于葡萄糖的电化学分析研究.研究数据表明:所制备的Au NPs-ERGO/GCE电极对葡萄糖具有良好的电催化性能,有较宽的检测范围和较好的灵敏度,同时,对抗坏血酸(AA)、尿酸(UA)和氯离子(Cl~-)等共存的干扰物均有良好的抗干扰性能.     

电流型DNA传感器检测Pb~(2+)对DNA的损伤

在玻碳电极(GCE)表面依次电聚合硫堇(PTh)膜、电沉积普鲁士蓝包金纳米粒子(PB@Au)、电沉积纳米金粒子(Au NPs),利用Au NPs大的比表面积和良好的生物相容性,进而固定双链DNA(dsDNA),制备一种电流型DNA传感器(GCE/PTh/PB@Au/Au NPs/dsDNA).利用电化学交流阻抗技术(EIS)和循环伏安法(CV)对dsDNA修饰电极进行表征,以亚甲基蓝(MB)为杂交指示剂,利用微分脉冲伏安法(DPV)对Pb2+对DNA的损伤进行了检测.结果表明,利用所制备的GCE/PTh/PB@Au/Au NPs/dsDNA可以高灵敏地测定铅金属离子对dsDNA损伤的程度,在25⁴5℃温度范围内,Pb2+对DNA的损伤速度随着温度升高而加快,Pb2+浓度越大对DNA的损伤越严重,即使微量的Pb2+对DNA也有明显的损伤.所制备的传感器灵敏准确,可用于其他重金属离子的检测以及基因损伤的研究.     

分级纳米多孔铋电化学传感器用于镉离子的检测

采用电化学方法实现对水溶液中重金属离子的超灵敏检测是分子生物学、环境学和医学等领域长期研究的课题,而如何制备具有高比表面积和快速响应特性的电极则是电化学痕量检测的关键。以双相合金Mg₇₉Bi₂₁条带为前驱体,通过一步脱合金法制备了分级纳米多孔铋（hierarchical nanoporous bismuth, HNBi）电极,结合方波阳极溶出伏安法,实现了对水溶液中Cd²⁺的快速检测,检测极限低于10⁻⁹ mol/L,线性动态响应范围介于10⁻⁸ mol/L和10⁻⁶ mol/L之间。HNBi电极绿色环保,在电化学检测领域显示出巨大的应用潜力。     

Electrochemical Behavior and Determination of Trifluoperazine at Decanethiol Self-Assembled Monolayer Modified Gold Electrodes

0　IntroductionTrifluoperazine is a derivative of phenothiazine. It hasneuroleptic and antidepressive actions, hence has beenwidely used in the treatment of psychotic patients[1]. As it hassuch function and application, trifluoperazine’s characteristicsand detection methods were studied by means of spectropho tometry[2], capillary zone electrophoresis[3], titrimetry[4],fluorometry[5], high performance liquid chromatographyetc[6]. Because of the electroactivity of trifluoperaz…     

纳米金增强DNA修饰金电极电化学性能的研究

采用小牛胸腺DNA修饰金电极并用纳米金增强了DNA在电极上的吸附量.Co(bpy)3 3被用作电子媒介体来表征通过恒电位法吸附在电极表面的DNA的变化过程,并通过循环伏安法测定Co(bpy)3 3在电极上的富集量;同时,考察了DNA修饰金电极在不同pH值及不同温度下的稳定性,发现纳米金使DNA修饰电极稳定性增加.     

An ultra-sensitive non-enzymatic hydrogen peroxide sensor based on SiO2-APTES supported Au nanoparticles modified glassy carbon electrode

A novel electrochemical sensor based on (3-aminopropyl)triethoxysilane (APTES) functionalized SiO₂ supported Au nanoparticles and Nafion (Nf) as the protective membrane was fabricated for the electrochemical determination of H₂O₂ in contact lens-cleaning solution. The modification steps of glassy carbon working electrode (GCE) were evaluated by electrochemical impedance spectroscopy (EIS) and cyclic voltammetry (CV). The amperometric results showed that Nf/[email protected]₂-APTES/GCE sensor can be used to determine H₂O₂ in contact lens solutions with the linear ranges of 14–180 μM and 0.18–7.15 mM, excellent sensitivities of 2514.6 and 894.2 μA mM cm^?2, and a low limit of detection (LOD) of 4.25 μM depending upon signal-to-noise ratio of 3. Nf/[email protected]₂-APTES/GCE exhibited excellent repeatability with relative standard deviation (RDS) of 2.66% and acceptable reproducibility with RSD of 3.35%. The sensor displayed reasonable selectivity in the presence of uric acid, dopamine, ascorbic acid, glucose, mannose, glycine, fructose, histidine, and arginine with RSD less than 2.5%. The fabricated Nf/[email protected]₂-APTES/GCE sensor has been successfully applied to detect H₂O₂ in contact lens cleaning solutions.     

一种检测电芬顿体系下DNA损伤的电化学生物传感器的研制

为了检测电芬顿体系下DNA的损伤,先采用石墨烯制备了一种致密的rGO/Fe₃O₄复合材料;再将复合材料和DNA修饰到玻碳电极上,利用电化学还原作用释放游离态Fe²⁺,并加入H₂O₂形成电芬顿体系;最后构建了一种检测电芬顿体系下DNA损伤的新型电化学生物传感器。检测结果表明,检测DNA损伤的最佳时间为30 min,最佳pH值为7.0。     

Thermodynamic functions and growth constants of web-like ZnO nanostructures

Web-like ZnO nanostructures have been successfully synthesized using the potassium nitrate route at various temperatures to simplify conventional preparation methods. The structures and morphologies of the as-prepared products were characterized by X-ray powder diffraction (XRD) and field-emission scanning electron microscopy (FE-SEM). The results showed that the reaction temperature was an important parameter, and that there was a feedback effect between nano-structure and growth parameters, combined with in situ micro-calorimetry, the reaction rate constants of the three systems were found to have been: 2.43×10-6, 2.70×10-8 and 3.12×10-7s-1 respectively. Furthermore, based on the relationship governing the potential differences between nanoand bulk ZnO, thermodynamic functions of nano-ZnO such as standard molar entropy (Sm,ZnO(nano)), standard molar Gibbs free energy of formation (△rGm,ZnO(nano)), and standard molar enthalpy of formation (△rHm,ZnO(nano)) have been calculated by the electrochemical method.     

Cyclic voltammetry,convolutive voltammetry,chronopotentiometry and disital simulation studies of [Pt（C≡C tol）2（dppm）2lr（CO）2]^＋PF^-6 complex

The electrochemical behaviour of the heterobimetallic complex [Pt（C≡C tol）2（dppm）2lr（CO）2]^＋PF^-6 was studied via cyclic voltammetry, convolutive voltammetry and chronopotentiometry at glassy carbon electrode in dichloromethane solution. The electrochemical parameters calculated from experimental data were tested and confirmed by matching the experimental cyclic voltammograms with the simulated data. It was found that convolutive voltammetry provided higher sensitivity, better resolution and more accurate method for determination of the electrochemical parameters than ordinary cyclic voltammetry.     

Electrodeposition of aluminium and aluminium-copper alloys from a room temperature ionic liquid electrolyte containing aluminium chloride and triethylamine hydrochloride

The electrodeposition of Al and Al-Cu binary alloys on to gold substrates from a room temperature ionic liquid electrolyte containing AlCl₃-Et₃NHCl was studied. The electrochemical behavior of the electrolyte and the mechanism of deposition were investigated through cyclic voltammetry (CV), and the properties of deposits obtained were assessed by scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM-EDS) and X-ray diffraction (XRD). Al of 70 μm in thickness and an Al-Cu alloy of 30 μm in thickness with 8at% copper were deposited from the electrolyte. SEM images of the deposits indicate that the Al deposit was smooth and uniform, whereas the Al-Cu deposit was nodular. The average crystalline size, as determined by XRD patterns, was found to be (30 ± 5) and (29 ± 5) nm, respectively, for Al and Al-Cu alloys. Potentiodynamic polarization (Tafel plots) and electrochemical impedance spectroscopic (EIS) measurements showed that Al-Cu alloys are more corrosion resistant than Al.     

Synthesis, structure, and optical properties of manganese phthalocyanine thin films and nanostructures

Manganese phthalocyanine(MnPc) nanostructures with different morphologies were prepared on porous anodic alumina oxide(AAO) at different substrate temperature(T_S=50 ℃,80 ℃,120 ℃,180 ℃,240 ℃) in an organic molecular beam deposition(OMBD) system.The nanostructures morphologies were studied using scanning electron microscopy(SEM) and the results showed that the nanostructures morphologies could be modulated by the control of T_S,as a result,the continuous film was obtained at 50 ℃,whereas the nanorods(NRs),nanoribbons(NBs),nanowires(NWs),nanosheets(NSs) and nanoparticles(NPs) were facilely generated as T_S increased.At the same time,the density and the uniformity of the nanostructures decreased.The results of X-ray diffraction(XRD) indicated that only the(3-phase polymorph formed throughout the growth process irrelevant to the T_S.Additionally,the ultraviolet visible(UV-Vis) absorption spectra demonstrated that the main absorption bands of MnPc nanostructures showed a remarkable band broadening as the T_S was increased.     

Electrochemical performance of a nickel-rich LiNi<Subscript>0.6</Subscript>Co<Subscript>0.2</Subscript>Mn<Subscript>0.2</Subscript>O<Subscript>2</Subscript> cathode material for lithium-ion batteries under different cut-off voltages

A spherical-like Ni_0.6Co_0.2Mn_0.2(OH)₂ precursor was tuned homogeneously to synthesize LiNi_0.6Co_0.2Mn_0.2O₂ as a cathode material for lithium-ion batteries. The effects of calcination temperature on the crystal structure, morphology, and the electrochemical performance of the as-prepared LiNi_0.6Co_0.2Mn_0.2O₂ were investigated in detail. The as-prepared material was characterized by X-ray diffraction, scanning electron microscopy, laser particle size analysis, charge-discharge tests, and cyclic voltammetry measurements. The results show that the spherical-like LiNi_0.6Co_0.2Mn_0.2O₂ material obtained by calcination at 900℃ displayed the most significant layered structure among samples calcined at various temperatures, with a particle size of approximately 10 μm. It delivered an initial discharge capacity of 189.2 mAh·g-1 at 0.2C with a capacity retention of 94.0% after 100 cycles between 2.7 and 4.3 V. The as-prepared cathode material also exhibited good rate performance, with a discharge capacity of 119.6 mAh·g-1 at 5C. Furthermore, within the cut-off voltage ranges from 2.7 to 4.3, 4.4, and 4.5 V, the initial discharge capacities of the calcined samples were 170.7, 180.9, and 192.8 mAh·g-1, respectively, at a rate of 1C. The corresponding retentions were 86.8%, 80.3%, and 74.4% after 200 cycles, respectively.     

Synthesis, characterization and magnetic properties of near monodisperse Fe3O4 sub-microspheres

Near monodisperse Fe3O4 sub-microspheres with an average diameter of 170 nm have been synthesized by a solvothermal reduction method, using K3[Fe（CN）6] as the raw material in the absence of any surfactants at 200~C℃ for 24 h. The products were detected by XRD, FESEM, TEM, and XPS. The investigation of the reaction parameters indicates that ethylene glycol plays a key role both as reducing agent and solvent. In addition, the reaction time and temperature also have important influences on the final product. The hysteresis loop of the near monodisperse Fe3O4 sub-microspheres shows a ferromagnetic behavior with saturation magnetization of 60.8 emu/g and coercivity of 124.7Oe.