Materials Chemistry Commons^™

Synthesis Of Novel Alkaline Earth Metal Acetylides, Eva Baker

Renée Crown University Honors Thesis Projects - All

Acetylide complexes of the heavy alkaline-earth metals were first introduced by our group. With our group being interested in how the ligand and donor affect the structural chemistry of the resulting complexes, my project was focused on the detailed analysis of past work and the extension towards new ligand and donor sets. The work required the analysis and development of synthetic procedures towards these highly reactive species.

Past synthetic work in our group had established several synthetic routes towards the target compounds including transamination and toluene elimination. Using toluene elimination, I was able to reproduce the synthesis of M(C≡CSiPh_{3 …}

Synthesis, Structural Studies And Desilylation Reactions Of Some N-2-(Trimethylsilyl)Ethyl-N-Nitrosocarbamates, Arpitha Thakkalapally, Vladimir Benin

Chemistry Faculty Publications

The present report describes the preparation and characterization of several N-2-(trimethylsilyl)ethyl-N-nitrosocarbamates, designed as precursors to thermally unstable secondary N-nitrosocarbamate anions via fluoride-assisted cleavage. X-ray structural studies demonstrate that the core N-nitrosocarbamate moiety has a nearly planar geometry, with an s-E orientation at the N–N bond. DFT calculations (B3LYP/6-31+G(d)) reproduce accurately the structural features of the title compounds and detailed conformational analysis at the same level of theory addresses the long-standing issue of preferred geometries for three classes of related structures: N-nitrosocarbamates, N-nitrosoureas and N-nitrosoamides. Desilylation studies demonstrate that both the …

Anodic Polarization Behaviors Of Carbon Steel In Bicarbonate Solution, Jing-Mao Zhao, Yu Zuo

Journal of Electrochemistry

The anodic polarization curves of mild steel were measured in sodium bicarbonate solution of various concentrations, and the surface products were analyzed by XPS. Two anodic current peaks and two passive zones are observed in all the curves. When HCO₃^- ions concentration is below 0.1mol/L, the two peaks are so close that the first passive zone is difficult to be observed. When HCO₃^- ions concentration is above 0.1 mol/L, the first peak appears clear, while the second becomes smaller. The XPS results indicate that the out layer of film formed at a higher potential is mainly …

Preparation And Characterization Of Lini0.85Co0.10(Timg)0.025O2 As Cathode Materials For Lithium-Ion Batteries, Xian-Jun Zhu, Hong-Hao Chen, Hui Zhan, Dai-Ling Yang, Yun-Hong Zhou

Journal of Electrochemistry

Cathode material of LiNi_0.85Co_0.10(TiMg)_0.025O₂ were prepared by solid state reaction at 725℃ for 24 h from LiOH·H₂O, Ni₂O₃, Co₂O₃, TiO₂ and Mg(OH)₂ under flowing oxygen, and were characterized by TG-DTA, XRD, SEM and electrochemical tests. Effort to simultaneously doped LiNiO₂ with Co-Ti-Mg has been tried to improve the cathode performance. The results show that co-doping definitely has a large beneficial effect in increasing the capacity (182.7mAh/g of the first discharge capacity for  LiNi_0.85Co_0.10(TiMg)_0.025O_{2 …}

Corrosion Resistance For Tio2 Thin Films Coated 316l Stainless Steel In The Nacl Solution, Guang-Xia Shen, Yi-Cong Chen, Chang-Jian Lin

Journal of Electrochemistry

The nano-TiO₂ thin films have been deposited on the 316L stainless steel by sol-gel and the dip-coating methods. Hydrothermal post-treatment leads to crack-free coatings. Meanwhile, the surface structure and properties are optimized. Surface morphology, structure and properties are characterized by XRD, and SEM technologies. The results have shown that the surface of coatings is porous, uniform and orderly, the particle diameters are in the range of 15~18 nm and the pores are about 4~8 nm and TiO₂ is anatase. The results of electrochemical measurements show that in the NaCl solution with pH ≥ 2 and concentration below 1mol/L, …

Calcium Zincate Prepared By Ball Mill Method, Sheng-Xian Li, Shuan-Bao Tian, Shao-Shan Zhu

Journal of Electrochemistry

Calcium zincate was prepared by ball milling method and the factors that influence its synthesis were investigated. The composition of the compound was Ca(OH)₂·2Zn(OH)_2^·2H₂O, which was verified by XRD and TG-DTA methods. The results of powder microelectrode and in simulated batteries showed that the material had excellent cyclic performance.

Influence Of Rare Earth Oxide On The Performance Of Secondary Zinc Electrodes, Xian-Ling Meng, Hua-Bin Yang, Jun-Hong Wang, Zuo-Xiang Zhou

Journal of Electrochemistry

Influence of La(OH)₃ or Ce(OH)₃ in secondary zinc electrode was investigated by the cyclic voltammetry, potentiodynamic polarizationand potentiostatic polarization tests and influence of La₂O₃ or CeO₂ in the charge/discharge performance of Zn/Ni battery was studied by galvanostatic charge/discharge experiment. The results showed that the film of rare earth hydroxide prevented the zincate species from transferring toward solution, enhanced hydrogen overpotential and decreased thecorrosion current density (i_corr), and therefore inhibited zinc corrosion. The potentiostatic polarization results at100mV overpotential showed that La(OH)₃ or Ce(OH)₃ oated on the zinc electrode effectively suppressed the …

The Fabrication And Electrochemical Studies On Carbon Nanotube Array Electrodes, Quan-Yong Gao, Jing Zhang, Yong Yang

Journal of Electrochemistry

An improved technique for fabrication of carbon nanotube array electrodes has been proposed in this work. Firstly, carbon nanotubes (CNs) array electrodes were prepared by combsination of Chemical Vapor Decomposition (CVD) method and sputtering techniques in anodized aluminum oxide (AAO) membrane. The CNs/AAO was immersed into HF solution to remove the barrier layer. Controlling the immersing time, the CNs array electrodes with different length contacted with electrolyte can be prepared. The morphology of CNs array electrodes was observed by SEM. The electrochemical properties of CNs array electrodes were investigated by cyclic voltammetry and electrochemical impedance spectroscopy. Cyclic voltammetric curves of …

Corrosion Behavior Of Mg2-XLaXNi And Mg2-XCeXNi Hydrogen Storage Alloy, Hai-Chang Zhang, Hua-Bin Yang, Jun-Hong Wang, Zuo-Xiang Zhou

Journal of Electrochemistry

The corrosion behavior of Mg-base hydrogen storage alloys has been investigated by potentiodynamic polarization and EIS. The results showed that the corrosion current density (i_corr) and the electrochemical polarized resistance of Mg_2-xCe_xNi alloys decreased with x increase, while i_corr of Mg_2-xLa_xNi alloys increased and the electrochemical polarized resistance of Mg_2-xLa_xNi alloys increased first, then decreased with x increase. SEM results showed that the surface of Mg_1.85Ce_0.15Ni alloy was relatively even while the surface of Mg_2-xLa_xNi alloy had …

A Study Of Metal Borides As High Capacity Anode Materials For Aqueous Primary Batteries, Ya-Dong Wang, Xin-Ping Ai, Han-Xi Yang

Journal of Electrochemistry

The transition metal borides VB₂ and TiB₂ were tested as high capacity anode materials and their electrochemical behaviors were studied by cyclic voltammetry and discharge measurements. The experimental results indicated that transition metal borides VB₂ and TiB₂ electrodes can deliver exceptionally high discharge capacity of over 3100 mAh/g and 1 600 mAh/g respectively, corresponding to 11- and 6-electron oxidation reaction, although their parent elements V, Ti and boron, are almost completely electrochemically inert. The different electrochemical activitis were probably due to the electrochemical activation of boron, which clamp the potential to passivation for Ti and activity …

Study On The New Technique Of Cu Micro-Plating Based On Ceramics, Zhi-Jun Gu, Xiong-Chao Zhao, Qi-Long Guo, Yan-Ping Hong, Qun-Shan Deng, Ren-Huan Chen

Journal of Electrochemistry

By combing the computer processing system (including the design of the line and the pattern, the choice of the scanning area and the treatment of the activation) with the electroless-plating technology, this article provides a new approach for the micro-plating based on the ceramics. The copper film based on ceramics with good properties can be obtained under the mild operating conditions. The line resolution is 35 μm and the wiring speed is 50 mm/s. The results had also showed that the quality of the copper plating is closely related to the roughness of the ceramic substrates.

Electrochemical Performance Of Gel Polymer Electrolyte Prepared By Thermal Initiating Polymerization Of Acrylates, Jin-Dan Piao, Li-Xia Yuan, Xin-Ping Ai, Han-Xi Yang, Yu-Liang Cao

Journal of Electrochemistry

A gel polymer electrolyte was prepared by thermal initiating polymerization of the acrylates in the EC/EMC/DMC electrolyte solution at 100℃. The LiCoO₂/MCMB polymer cells were assembled and their electrochemical properties were evaluated at various charge-discharge rate and temperatures. The ionic conductivity of the polymer electrolyte containing 85wt.% liquid electrolyte is around 3.2×10^-3 S·cm^-1  at 20℃ and 5.6×10^-4 S·cm^-1 at -30℃ respectively. The gel polymer electrolyte has good electrochemical stability up to 4.5V versus Li/Li⁺.The first charge-discharge efficiency of the polymer cell at 0.2C rate is almost 92.1%. The discharge capacity of the …

Application Of Carbon Paste Electrode On The Electrogenerative-Leaching Process Of Sulfide Minerals, Shao-Fen Wang, Zheng Fang, Yun-Yan Wang

Journal of Electrochemistry

The cyclic voltammetry curves of sulfide mineral electrodes or corresponding carbon paste electrodes in NaCl electrolytes have been obtained in this study. The experimental results indicate that acetylene black (revealed) the electro-catalytic propertyin the electrogenerative-leaching process of sulfide minerals. The output currentand potential of carbon paste electrodes were increased to some degrees while the activation energies were lower.

Preparation Of Poly (Bromophenol Blue) Modified Glassy Carbon Electrode And Its Electrocatalytic Activity, Wei Chen, Hong-Bin Luo, Xin-Hua Lin

Journal of Electrochemistry

A film of poly (bromophenol blue) was formed on a glassy carbon electrode by using cyclic voltammetry. A stable film could be obtained with a potential range from -1.0 V to +1.8 V (vs.Ag/AgCl). The experimental results showed that the poly (bromophenol blue) modified glassy carbon electrode could catalyse the oxidation of ascorbic acid. It decreased the oxidation potential by about 270mV but increased the peak current. Meanwhile, this electrode showed a good linear current response for the ascorbic acid range from 2.5 to 250 (g/mL).

Electrochemical Properties Of Polymeric Gel Electrolyte With Gbl/Ec As Plasticizers, Yu-Wen Liu, Yong Zhang, Xiao-Long Li, Qi-Ping Gu, Cui-Fen Zhang, Yu-Dong Huang

Journal of Electrochemistry

Polymeric gel electrolytes (GPE) based on PMMA and PVDF-HFP were prepared using the binary mixtures of γ-butyrolactone (GBL) and ethylene carbonate (EC) as plasticizers. The ionic transport properties and electrochemical stability were studied. The room temperature conductivity reached 1.2 mS·cm^-1, electrochemical stability window exceeded 4.5V. The interfacial stability between GPE and lithium electrode was also investigated. The lithium metal polymer battery (LMPB) prepared with the GPE showed better charge and discharge life cycle when the the lithium metal electrode was treated with 1,4-dioxane.

Research On Phenol Wastewater Treatment By Electrochemical Oxidation, Tian-Cheng Li, Shen-Lin Zhu

Journal of Electrochemistry

Electrochemical oxidation is an effective technology for the phenol wastewater treatment, and the anode properties are important to the electrochemical oxidationefficiency. The over-potentials of oxygen evolution have been measured for thestainless steel, feasible graphite and SnO₂/Ti anode respectively. Moreover, the synthetic phenol wastewater was treated by the electrochemical oxidation with the stainless steel or feasible graphite anodes. The experimental results showed that the order of the over-potential is SnO₂/Ti > graphite > stainless steel; meanwhile, the COD values of purified water were approaching to or less than 100 mg·L^-1, and the phenol concentrations in the purified …

Fabrication And Studies Of A Novel Ag/Agcl Reference Electrode In High Temperature Molten Chloride Salts, Pei Gao, Xian-Bo Jin, Di-Hua Wang, Xiao-Hong Hu, Zheng Chen

Journal of Electrochemistry

A new method for the easy fabrication of a stable and long life silver/silver chloride reference electrode in molten chloride salts is described in this paper. The method is based on the fact that simply placing the silica glass in molten NaCl or its vapour in the presence of oxygen resulted in satisfactory conductivity for sodium ion and possibly calcium ion in the material.The performance of such made electrode has been investigated in a few typical chloride systems at temperatures ranging from 400 to 900℃. Due to the wholly sealed construction, the reference electrode is stable, temperature-reversible, contamination free to …

The Electrophoretic Deposition Of Nano Hydroxyapatite Coating On Titanium Surface, Fei Chen, Chang-Jian Lin, Zhou-Cheng Wang

Journal of Electrochemistry

A hydroxyapatite coating with nano-structure on the roughened titanium surface was prepared by electrophoretic deposition process. To decrease sintering temperature the HAp nanoparticles synthesizedby a wet chemical method was used. It is observed that the coating is uniform without cracks. After sintering the nano-strueture of HAp coating remains unchanged. The surface treatment of Ti is applied to form a distribution of small pits and TiO₂ thin layer that improve the adhesion of coatingto Ti substrate. It is shown that the bonding strength of coating is as high as 18±2.5MPa. The hardness and Young's modulus are 40.6 and 0.42 GPa, …

Planar-To-Tubular Structural Transition In Boron Clusters: B20 As The Embryo Of Single-Walled Boron Nanotubes, Boggavarapu Kiran, Satya S. Bulusu, Hua-Jin Zhai, Soohaeng Yoo, Xiao Cheng Zeng, Lai-Sheng Wang

Xiao Cheng Zeng Publications

Experimental and computational simulations revealed that boron clusters, which favor planar (2D) structures up to 18 atoms, prefer 3D structures beginning at 20 atoms. Using global optimization methods, we found that the B₂₀ neutral cluster has a double-ring tubular structure with a diameter of 5.2 Å. For the B₂₀^- anion, the tubular structure is shown to be isoenergetic to 2D structures, which were observed and confirmed by photoelectron spectroscopy. The 2D-to-3D structural transition observed at B₂₀, reminiscent of the ring-to-fullerene transition at C₂₀ in carbon clusters, suggests it may be considered as the embryo …

Nonlinear Dynamics Of Piezoelectric High Displacement Actuators In Cantilever Mode, Timothy Usher, Alec Sim

Physics Faculty Publications

Experimental results of the nonlinear dynamic response of a piezoelectric high displacement actuator known as thin-layer composite unimorph ferroelectric driver and sensor were compared to a theoretical model, which utilizes the multiple scales method to connect the effective spring constant to higher-order stiffness constants c4 of the piezoelectric layer. This type of actuator has prestress gradients resulting from the manufacturing process that have been reported to play an important role in enhanced actuation. A value of c₄=−4.7x10²⁰ N/m² was obtained for the higher-order lead zirconate titanate (PZT) stiffness coefficient, which is higher than other published results …

Corrosion Of Steel By Lead Bismuth Eutectic, John Farley, Allen L. Johnson, Dale L. Perry

Transmutation Sciences Materials (TRP)

There is an active international interest in lead-bismuth eutectic and similar liquid lead systems because of the relevance to the transmutation of nuclear waste, fast reactors, and spallation neutron sources.

Materials in these systems must be able to tolerate high neutron fluxes, high temperatures, and chemical corrosion. For lead bismuth eutectic (LBE) systems, there is an additional challenge because the corrosive behaviors of materials in LBE are not well understood. Most of the available information on LBE systems has come from the Russians, who have over 80 reactor-years experience with LBE coolant in their Alpha-class submarine reactors. The Russians found …

Environment-Induced Degradation And Crack-Growth Studies Of Candidate Target Materials, Ajit K. Roy

Transmutation Sciences Materials (TRP)

The primary objective of this task was to evaluate the effects of environmental and mechanical parameters on environment induced degradations of candidate target structural materials for applications in spallation-neutron-target systems. The materials selected for evaluation and characterization were martensitic stainless steels including Alloys HT-9, EP-823, and 422.

Accelerator-driven transmutation systems involve bombarding a target material such as molten lead-bismuth-eutectic (LBE) by a proton beam, thereby producing neutrons. The molten LBE target will be contained in a subsystem structural container made of a suitable material such as Alloys HT-9, EP-823, and 422. During the transmutation process, the target structural material may …

Modeling Corrosion In Oxygen Controlled Lbe Systems With Coupling Of Chemical Kinetics And Hydrodynamics, Samir Moujaes, Yitung Chen

Transmutation Sciences Materials (TRP)

The corrosion of structural materials is a major concern for the use of lead-bismuth eutectic (LBE) systems for nuclear applications such as in transmuter targets or fast reactors. Corrosion in liquid metal systems can occur through various processes, including, for example, dissolution, formation of inter-metallic compounds at the interface, and penetration of liquid metal along grain boundaries. Predicting the rate of these processes depends on numerous system operational factors: temperature, system geometry, thermal gradients, solid and liquid compositions, and velocity of the liquid metal, to name a few. Corrosion, along with mechanical and/or hydraulic factors, often contributes to component failure. …

The Electrochemical Performance Of Modified Spinel At Elevated Temperature, Zhen-Ping Cai, Xiao-Hong Chen, Shi-Gang Lu, Ming-Xun Li, Wei-Hua Jin

Journal of Electrochemistry

The modified LiMn₂O₄ cathode materials for lithium ion batteries have been synthesized by solid-state reaction. The crystal structure and electrochemical performance of products have been investigated by SEM, XRD and electrochemical measurements. The XRD analysis indicated that all the synthesized products possess Fd3m spinel LiMn₂O₄ structure. Those modified LiMn₂O₄ materials showed improved cycling capacity over pure spinels at high temperature and room temperature.

Electrochemical Behaviours Of Hemoglobin-Ddab-Modified Powder Microelectrode And The Application Of The Powder Microelectrode In Determination Of Nitric Oxide, Zhi-Mou Guo, Huan Liu, Jian Chen, Wen-Ting Zhang

Journal of Electrochemistry

The electrochemical behaviours of DDAB-Hb-PME were studied in this paper. The (apparent) surface concentration of Hb was enhanced greatly by using the powder microelectrode (technique). NO reacts with Hb and absorbs on the surface of the modified carbon powder. Therefore, the output of the electrode was enhanced greatly by employing PME with higher reaction surface (area). The sensitivity of DDAB-Hb-PME is 3.1 mA/μmol·L^-1·cm², which is much larger than the values obtained with the traditional electrodes. The detection limit is 9 nmol·L^-1 and the linear response range is 9～100 nmol·L^-1.

Improvement And Its Mechanism Of Storage Performance Of Ni-Mh Battery, Xiao-Feng Li, Li-Ping Ma, Yu-Wan Lou, Feng Li, Bao-Jia Xia

Journal of Electrochemistry

The storage performance of nickel-metal-hydride (Ni-MH) battery was studied by using galvanostatic charge-discharge and cyclic voltammetry. The experimental results indicated that CoOOH could not be completely restored after its being thoroughly reduced at lower potential, which might weaken electric conduction network in the positive electrode and result in fading of electrochemical properties of Ni-MH battery. Addition of nickel powder as a conductive agent into the positive electrode was beneficial to the capacity recovery after storage.

Preparation And Electrochemical Magnesium Insertion Behaviors Of Mgv2O6, Hua-Tang Yuan, Li-Fang Jiao, Jian-Sheng Cao, Xiu-Sheng Liu, Ming Zhao, Yong-Mei Wang

Journal of Electrochemistry

MgV₂O₆ was synthesized by conventional solid-state reaction from MgO and V₂O₅ as starting materials. X-Ray diffraction analysis showed that the prepared sample belongs to the monoclinic structure. Electrochemical magnesium insertion from aprotic electrolytes such as organomagnesium halides into this host was found possible and exhibited charge/discharge circulation.

Anodic Dissolution Of Aluminum In Koh-Ethanol Solutions, Hai-Bo Shao, Jian-Ming Wang, Xiao-Yan Wang, Yi Zheng, Jian-Qing Zhang

Journal of Electrochemistry

The feasibility of employing aluminum in KOH ethanol solution as a battery anode system was discussed. Weight loss measurement showed that the corrosion rate of Al is low enough to be used in sealed batteries. Through the measurements done by anodic polarization, EIS and galvanostatic discharge, it was found that Al is electrochemical active in a wide potential range in this system, and its discharge mechanism is similar to that of Al in aqueous solution. The discharge potential increased rapidly after a period of time, which might be caused by the discharge products depositing on the electrode surface.

Study On Mass Transport In Liquid Layer Adjacent To The Electrode Through Transmission Vop-Spectroellipsometry, Wei Zhu, Yu-Ru Yang, Zong-Qing Huang

Journal of Electrochemistry

In electrochemical system, the mass transport process in liquid layer adjacent to electrode is studied through theoretical analysis only.The diffusion process can be analyzed theoretically by Fick's law for homogeneous media. Up to now, none of satisfied experimental method has been reported for studying mass transport of a whole process in liquid media yet. This paper described the experimental approach to explore mass transport in electrochemical system by transmission Vop-spectroellipsometry briefly.

Investigation Of Pulse Potential-Modulated Coulometry For Co2 Detection, Hai-Chuan Wang, Bing-Liang Wu

Journal of Electrochemistry

A pulse potential-modulated technique was applied to measure the concentration of CO₂ in gas samples. In the first step, an anodic pulse and a consequent cathodic pulse were used to remove the organic pollutant and surface oxide on the surface of the platinized Pt gauze electrode before each experiment. As following, a given potential step was used to reduce the CO₂ into adsorbed intermediate on Pt surface, and the adsorbates produced were oxidized by a following anodic potential step. At same time the oxidation current of adsorbates were measured. A certain relation exists between the concentration of CO …