聚中性红/铁氰化镍/碳纳米管修饰电极的制备及其电催化过氧化氢的特性

采用循环伏安法在碳纳米管(CNTs)修饰的玻碳电极上合成聚中性红(PNR)/铁氰化镍(NiHCF)颗粒,并分别采用扫描电镜(SEM)、傅里叶红外(FTIR)、循环伏安法(CV)和计时安培电流法(CA)等方法考察了复合膜的微观形貌、结构和电化学催化性能。结果表明,复合膜为三维多孔有序的网络状结构,PNR和NiHCF以纳米颗粒形式存在并沿CNTs均匀分布。PNR/NiHCF/CNTs复合膜对过氧化氢(H2O2)表现出了优异的电催化性能并显示出了良好的协同效应。该复合膜电极对H2O2的催化还原电流与其浓度在6.25×10-6~3×10-3之间呈良好的线性关系,线性相关系数R=0.9989,检出限为1×10-7mol/L,同时具有较高的灵敏度1 455.9 mA·L/(mol·cm2),并且复合膜有良好的稳定性和重现性,可实际应用于H2O2传感器。     

对硝基酚在β-环糊精/碳纳米管修饰电极上的电催化行为研究

以酸化处理的多壁碳纳米管与β环糊精为原料,采用静电自组装法制备了β环糊精/多壁碳纳米管复合材料。用循环伏安法研究了pH值、扫描速率、催化时间、原料比例、待测液浓度等因素对β环糊精/多壁碳纳米管修饰电极在对硝基酚溶液中电化学催化效果的影响。实验结果表明,β环糊精/多壁碳纳米管复合材料对对硝基酚电催化效果明显,且该催化过程为吸附控制过程。确定了最佳催化条件为选取邻苯二甲酸氢钾作为缓冲溶液,极化时间40s,碳纳米管与环糊精质量比为1∶3。对硝基酚浓度在1.3×10-6~3.5×10-4 mol/L时,对硝基酚的浓度与差分脉冲峰电流呈线性关系,相关系数为0.9985,检出限为1.223×10-7 mol/L。     

叶酸在聚苯胺修饰铂电极上的电催化氧化行为

采用电化学聚合法制备了聚苯胺修饰的铂电极(PAN/Pt),并用循环伏安法(CV)研究了该电极对叶酸(FA)的电催化氧化性能。结果显示:FA在裸铂电极上的直接电化学氧化十分迟缓,无氧化峰出现,而在PAN/Pt修饰电极上0.561V处出现氧化峰,表明此电极对FA有很良好的电催化作用。另外,氧化峰电流与叶酸浓度在1×10-12 mol/L~1×10-6 mol/L范围内呈线性关系,检测限为1×10-11 mol/L。利用该电极测定市售叶酸片中的叶酸,获得令人满意的结果。     

多孔的修饰电极对抗坏血酸的电催化氧化

通过循环伏安(CV)法制备了聚苯胺/聚砜(PAN/PSF)复合膜修饰电极,考察了电极对抗坏血酸(AA)的电催化性能。结果显示,PAN/PSF复合膜修饰电极对AA有很好的电催化氧化作用和高的稳定性。氧化峰电流与AA浓度在一定浓度范围内呈良好的线性关系,检测限为6×10-6 mol/L。该电极制备简单、灵敏度高、检测限低,对水果中AA具有很好的检测效果。     

桑色素功能化碳纳米管修饰电极对多巴胺与抗坏血酸的电化学行为研究

通过电聚合的方法构置了桑色素功能化碳纳米管修饰电极(morin/MWNTs/GCE),以多巴胺(DA)和抗坏血酸(AA)为模型化合物,考察了该修饰电极的电催化作用与机理.结果表明:DA与AA在Morin/MWNTs/GCE上的峰电流比裸电极、碳纳米管修饰电极明显增大,氧化峰电位差达210 mV,可实现多巴胺的灵敏测定.AA存在下,DA在1.0×10-7～5.0×10-4mol/L浓度范围内与峰电流有良好的线性关系,方法检出限2.0×10-8mol/L.     

新型CMCS/WMCNTs修饰电极对槲皮素的电化学检测及应用

研究了一种黄酮类物质槲皮素在新颖的多壁碳纳米管(WMCNTs)/羧甲基壳聚糖(CMCS)复合物修饰电极上的循环伏安行为。实验采用直接滴涂方法制备CMCS/WMCNTs修饰电极,在不同的pH、扫描速度、底液浓度、修饰材料等条件下通过循环伏安法来研究槲皮素在修饰电极上电化学行为。修饰电极与裸电极相比,峰电流有明显提升,表明修饰材料对槲皮素的电化学氧化还原行为有一定的催化增敏作用。槲皮素在pH=5.0的醋酸-醋酸钠(NaAc-HAc)缓冲溶液中有一对明显的氧化还原峰,电极过程为等量质子和电子参与的吸附控制过程,且还原峰电流与槲皮素浓度在(1.0×10~(-4)~1.0×10~(-3))mol/L范围内呈良好的线性关系。     

PDDA/MWNT自组装膜修饰碳纤维微电极选择性测定多巴胺的研究

结合了碳纳米管和微电极两者的优越性,通过静电自组装方法有序地将混酸切割多壁碳纳米管修饰到碳纤维微电极上,并表征了自组装膜PDDA/MWNT修饰到碳纤维微电极上的均匀程度和稳定性,进一步采用循环伏安法研究了多巴胺和抗坏血酸在该修饰电极上的电化学行为。结果表明,该修饰微电极成功实现在抗坏血酸共存下选择性测定多巴胺,峰电流与多巴胺浓度在4μM/L到52μM/L之间呈现良好的线性关系,最低检测限是0.1μmol/L,该工作为多巴胺的活体、实时的电化学选择性测定奠定了基础。     

基于Pt-Pb纳米花的无酶葡萄糖传感器性能研究

利用超声恒电流沉积法在金电极表面制备了Pt-Pb纳米花,并将其用于构建无酶葡萄糖传感器,采用阻抗谱、循环伏安和差分脉冲伏安法研究了其电化学性能。SEM结果表明,当沉积电流为10mA时,电极表面形成Pt-Pb纳米花结构。电化学测试结果表明,该电极对葡萄糖具有很好的电催化性能,在含有氯离子的溶液中不会失活。Pt-Pb纳米花电极构建的无酶传感器对葡萄糖的线性响应范围为0.5×10-3～22×10-3 mol/L,灵敏度为3.68mA·cm-2·(mol/L)-1,检测限为24×10-6 mol/L。此外,传感器具有良好的选择性、重复性和稳定性。     

电化学法制备铁氰化铜/Nafion及其对卡托普利的检测

为对药片中卡托普利的含量进行精确测定,采用电聚合的方法,在玻碳电极表面沉积均匀分布的铁氰化铜/Nafion复合物。用扫描电镜(SEM)和X射线能量色散光谱(EDX)分别对样品的形貌和成分进行表征。利用循环伏安法(CV)研究药物分子卡托普利在该修饰电极上的电化学行为。研究结果显示,该修饰电极对卡托普利具有非常好的电催化性能。一定条件下,卡托普利在6.62×10-5~3.80×10-3mol/L范围内,其氧化峰电流与物质量浓度呈现很好的线性关系,其相关系数是0.996,检出限为5.0×10-6mol/L。该修饰电极具有快速、灵敏和高效的特点,并且可用于卡托普利实际样品的检测。     

电沉积制备铁氰化镍/Nafion纳米粒子及其对葡萄糖的电化学检测

采用电沉积的方法,在玻碳电极表面快速电沉积均匀分布的铁氰化镍/Naion纳米粒子。用X射线能量色散光谱图(EDX)和扫描电镜(SEM)对样品进行了表征,然后采用循环伏安法对该修饰电极进行电化学研究。结果表明:该电极对葡萄糖具有良好的电催化氧化性能,对葡萄糖响应的线性范围为1.560×10~(-6)~10.32×10~(-3)mol/L(R~2=0.999),检出限为1.2μmol/L(S/N=3)。制得的修饰电极对葡萄糖的电催化具有灵敏度高、重现性好和选择性强的优点。     

Structural and optical properties of AlxOy/Pt/AlxOy multilayer absorber

We report on the microstructure and optical properties of Al_xO_y–Pt–Al_xO_y interference-type multilayer films, deposited by electron beam (e-beam) deposition onto corning 1737 glass, silicon (1 1 1) and copper substrates. The structural properties were investigated by Rutherford backscattering spectrometry, X-ray diffraction, scanning electron microscopy, energy dispersive X-ray spectroscopy and atomic force microscopy. The optical properties were extracted from specular reflection/transmission, diffuse reflectance and emissometer measurements. The stratification of the coatings consists of a semi-transparent middle Pt layer sandwiched between two layers of Al_xO_y. The top and bottom Al_xO_y layers were non-stoichiometric with no crystalline phases present. The Pt layer is in the fcc crystalline phase with a broad size distribution and spheroidal shape in and between the rims of Al_xO_y. The surface roughness of the stack was found to be comparable to the inter-particle distance. The optical calculations confirm a high solar absorptance of ∼0.94 and a low thermal emittance of ∼0.06 for the multilayer stack, which is attributed not only to the optimized nature of the multilayer interference stacks, but also to the specific surface morphology and texture of the coatings. These optical characteristics validate the spectral selectivity of the Al_xO_y–Pt–Al_xO_y interference-type multilayer stack for use in high temperature solar-thermal applications.     

Synthesis of a new perovskite Pb(Li14Nb34)O3

A high-pressure technique was adopted to obtain perovskite-type $\text{Pb(Li}{}_{\mathrm{<mtext>1</mtext><mtext>4</mtext>}}\text{Nb}{}_{\mathrm{<mtext>3</mtext><mtext>4</mtext>}}\text{)}\text{O}{}_3$. A new perovskite $\text{Pb(Li}{}_{\mathrm{<mtext>1</mtext><mtext>4</mtext>}}\text{Nb}{}_{\mathrm{<mtext>3</mtext><mtext>4</mtext>}}\text{)}\text{O}{}_3$ was characterized to have a cubic symmetry with $\text{a}{}_{\mathrm{<mtext>o</mtext>}}\text{= 4.069}\text{A}\text{?}$; Li and Nb ions in the B-site of perovskite lattice may be in a random arrangement.     

Optimization of AlxOy/Pt/AlxOy multilayer spectrally selective coatings for solar-thermal applications

Spectrally selective Al_xO_y/Pt/Al_xO_y multilayer absorber coatings were deposited onto corning 1737 glass, Si (111) and copper substrates using electron beam (e-beam) vacuum evaporator at room temperature. The employment of ellipsometric measurements and optical simulation was proposed as an effective method to optimize and deposit multilayer solar absorber coatings. The optical constants (n and k) measured using spectroscopic ellipsometry, showed that both Al_xO_y layers, which used in the coatings, were dielectric in nature and the Pt layer was semi-transparent. The optimized multilayer coatings exhibited high solar absorptance α ∼ 0.94 ± 0.01 and low thermal emittance ? ∼ 0.06 ± 0.01 at 82 °C. The Rutherford backscattering spectroscopy (RBS) data of Al_xO_y/Pt/Al_xO_y multilayer absorber indicated the Al_xO_y layers present in the coating were nearly stoichiometry. The scanning electron microscope analysis (SEM) result indicated that the average diameter and inter-particles distance of Pt grains were statistically about 146 ± 0.17 nm and 6-10 ± 0.2 nm respectively.     

Bulk crystalline BaPb34Bi14O3: A ceramic superconductor

The preparation conditions of the high T_C ceramic superconductor Ba(Pb,Bi)O₃ is correlated with the superconducting transition. Transition onsets of all materials are similar, but transition widths and transition completeness is strongly dependent on firing temperature. Only materials prepared over a narrow temperature range, resulting in a nearly ideal weight loss, have a complete and narrow transition.     

Electrostriction in Pb (Zn13Nb23)O3

The electrostriction in $\text{Pb (Zn}{}_{\mathrm{<mtext>1</mtext><mtext>3</mtext>}}\text{Nb}{}_{\mathrm{<mtext>2</mtext><mtext>3</mtext>}}\text{)}\text{O}{}_3$ crystals has been investigated using a strain gauge method. In the ferroelectric phase below 140 C, the strain vs the electric field shows a hysteresis, which is ascribed to the effect of ferroelectric domains. A quadratic relation holds between the strain x and the electric polarization P as x = QP² above about 170 C in the paraelectric phase. Values of the electrostrictive Q coefficients are determined from the measurements near 190 C, as Q₁₁ = 1.6·10^?2m⁴/C², Q₁₂ = ?0.86·10^?2m⁴/C², and Q₄₄ = 0.85·10^?2m⁴/C².     

Magnetic,electrical and thermal studies on the V1−xMox02

The monoclinic-to-tetragonal structure transition of oxides V_1?xMo_x0₂ with $\text{0≤}\text{x}\text{≤0.20}$ has been studied by means of DTA, X-ray diffraction, magnetic susceptibility (powder samples) and electrical conductivity (single crystals) measurements within the temperature region 80 K to 400 K. A linear decrease of the transition temperature of 11 K per atom % Mo was observed. The magnetic susceptibility of the low temperature phase was found to be temperature independent paramagnetic for all preparations. Electrical conductivity measurements on the same phase showed crystals with $\text{x}\text{? 0.04}$ to be semiconducting, while a metallic behavior was observed in the region $\text{0.10 ?}\text{x}\text{? 0.14}$.     

n-PbTep+−Pb1−xSnxTe heterojunctions prepared by a modified hot wall technique

$\text{n-PbTe}\text{p}{}^{\mathrm{+}}\text{?}\text{Pb}{}_{\mathrm{1?x}}\text{Sn}{}_{\mathrm{x}}\text{Te}$ heterojunctions with a long wavelength spectral cutoff (λ_c ≈ 6 μm) were prepared using the double-channel hot wall technique. The electrical and photoelectrical properties of the heterojunctions at 77, 197 and 300 K were investigated. Detectors with R_oA equal to 170 Ω cm² and a quantum efficiency of 25–40% were obtained. Reasons for the shift of the long wavelength spectral cutoff of the heterojunctions towards shorter wavelengths are given.     

Core-current-enhanced domain-wall pinning in nanocrystalline Fe/sub 73.5/Cu/sub 1/Nb/sub 3/Si/sub 15.5/B/sub 7/ ribbon

We have studied the influence of surface fields H/sub p/ (generated by either direct or alternating core current) on soft magnetic properties of amorphous and nanocrystalline Fe/sub 73.5/Cu/sub 1/Nb/sub 3/Si/sub 15.5/B/sub 7/ ribbon. While in an amorphous ribbon the coercive field H/sub c/ decreases with H/sub p/, in the same optimally annealed ribbon (H/sub c/=1.3 A/m, M/sub m//spl ap/M/sub s/) H/sub c/ increases with H/sub p/ for all the explored types of H/sub p/ (static and dynamic with different phases with respect to that of the magnetizing field H). The unexpected increase of H/sub c/ in nanocrystalline ribbon is associated with the influence of H/sub p/ on the surface and main (inner) domain structure. Here, we develop a model that takes into account this influence and explains the experimental results.     

Interfacial microstructure of NiSix/HfO2/SiOx/Si gate stacks

Integration of NiSi_x based fully silicided metal gates with HfO₂ high-k gate dielectrics offers promise for further scaling of complementary metal-oxide- semiconductor devices. A combination of high resolution transmission electron microscopy and small probe electron energy loss spectroscopy (EELS) and energy dispersive X-ray analysis has been applied to study interfacial reactions in the undoped gate stack. NiSi was found to be polycrystalline with the grain size decreasing from top to bottom of NiSi_x film. Ni content varies near the NiSi/HfO_x interface whereby both Ni-rich and monosilicide phases were observed. Spatially non-uniform distribution of oxygen along NiSi_x/HfO₂ interface was observed by dark field Scanning Transmission Electron Microscopy and EELS. Interfacial roughness of NiSi_x/HfO_x was found higher than that of poly-Si/HfO₂, likely due to compositional non-uniformity of NiSi_x. No intermixing between Hf, Ni and Si beyond interfacial roughness was observed.     

Reactive plasma deposited SixCyHz films

Si_xC_yH_z films have been prepared at 200°C by reactive plasma deposition from SiH₄ and CH₄ diluted in helium in a tubular reactor. These films have a ratio s (equal to $\text{Si}\text{(}\text{Si+C}\text{))}$ ranging from 0.2 to 0.8, a refractive index ranging from 1.96 to 2.6 and an optical energy band gap in the range 2.7-2.2 eV. The total quantity of hydrogen in the film is 40% when s=0.5. Infrared analysis shows that these films have large fractions of homonuclear bonds and that this material is best described as a polymer. Mass spectrometric measurements of the gaseous products formed in the SiH₄-CH₄-He plasma have been performed and the results are related to the composition of the deposited layers.