Effect of the microstructure of Ti-5Mo on the anodic dissolution in H/sub 2/SO/sub 4/

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kim, Y.J.; Oriani, R.A.

1987-04-01

The effect of microstructure of the Ti-5Mo alloy on its anodic dissolution rate in sulfuric acid solution at various temperatures has been investigated. TiMo alloys exhibit a region of increased dissolution rate in the vicinity of +0.20 V (saturated calomel electrode (SCE)) in 10% H/sub 2/SO/sub 4/, the same potential region in which pure Mo exhibits a large anodic dissolution rate. Aging of Ti-5Mo at 350 C was found to lead to the formation of ..omega.. phase. Heat treatment caused larger passive currents in 10% H/sub 2/SO/sub 4/, but the critical passivation potentials and corrosion potentials were not significantly affected.more » Molybdenum was enriched in the oxide formed on aged Ti-5Mo at +0.23 V (SCE), in comparison with the Mo concentration found in the oxide on as-received Ti-5Mo.« less

Lanthanum Nitrate As Electrolyte Additive To Stabilize the Surface Morphology of Lithium Anode for Lithium-Sulfur Battery.

PubMed

Liu, Sheng; Li, Guo-Ran; Gao, Xue-Ping

2016-03-01

Lithium-sulfur (Li-S) battery is regarded as one of the most promising candidates beyond conventional lithium ion batteries. However, the instability of the metallic lithium anode during lithium electrochemical dissolution/deposition is still a major barrier for the practical application of Li-S battery. In this work, lanthanum nitrate, as electrolyte additive, is introduced into Li-S battery to stabilize the surface of lithium anode. By introducing lanthanum nitrate into electrolyte, a composite passivation film of lanthanum/lithium sulfides can be formed on metallic lithium anode, which is beneficial to decrease the reducibility of metallic lithium and slow down the electrochemical dissolution/deposition reaction on lithium anode for stabilizing the surface morphology of metallic Li anode in lithium-sulfur battery. Meanwhile, the cycle stability of the fabricated Li-S cell is improved by introducing lanthanum nitrate into electrolyte. Apparently, lanthanum nitrate is an effective additive for the protection of lithium anode and the cycling stability of Li-S battery.

Effects of pretreatment processes for Zr electrorefining of oxidized Zircaloy-4 cladding tubes

NASA Astrophysics Data System (ADS)

Hwa Lee, Chang; Lee, Yoo Lee; Jeon, Min Ku; Choi, Yong Taek; Kang, Kweon Ho; Park, Geun Il

2014-06-01

The effect of pretreatment processes for the Zr electrorefining of oxidized Zircaloy-4 cladding tubes is examined in LiCl-KCl-ZrCl4 molten salts at 500 °C. The cyclic voltammetries reveal that the Zr dissolution kinetics is highly dependent on the thickness of a Zr oxide layer formed at 500 °C under air atmosphere. For the Zircaloy-4 tube covered with a 1 μm thick oxide layer, the Zr dissolution process is initiated from a non-stoichiometric Zr oxide surface through salt treatment at an open circuit potential in the molten salt electrolyte. The Zr dissolution of the samples in the middle range of oxide layer thickness appears to be more effectively derived by the salt treatment coupled with an anodic potential application at an oxidation potential of Zr. A modification of the process scheme offers an applicability of Zr electrorefining for the treatment of oxidized cladding hull wastes.

Preventing the dissolution of lithium polysulfides in lithium-sulfur cells by using Nafion-coated cathodes.

PubMed

Oh, Soo Jung; Lee, Jun Kyu; Yoon, Woo Young

2014-09-01

The principal drawback of lithium-sulfur batteries is the dissolution of long-chain lithium polysulfides into the electrolyte, which limits cycling performance. To overcome this problem, we focused on the development of a novel cathode as well as anode material and designed Nafion-coated NiCrAl/S as a cathode and lithium powder as an anode. Nafion-coated NiCrAl/S cathode was synthesized using a two-step dip-coating technique. The lithium-powder anode was used instead of a lithium-foil anode to prohibit dendrite growth and to improve on the electrochemical behaviors. The cells showed an initial discharge capacity of about 900 mA g(-1) and a final discharge capacity of 772 mA g(-1) after 100 cycles at 0.1 C-rate. Scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS) demonstrate that using the Nafion-coated NiCrAl/S cathode can suppress the dissolution of long-chain lithium polysulfides. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Zirconium behaviour during electrorefining of actinide-zirconium alloy in molten LiCl-KCl on aluminium cathodes

NASA Astrophysics Data System (ADS)

Meier, R.; Souček, P.; Malmbeck, R.; Krachler, M.; Rodrigues, A.; Claux, B.; Glatz, J.-P.; Fanghänel, Th.

2016-04-01

A pyrochemical electrorefining process for the recovery of actinides from metallic nuclear fuel based on actinide-zirconium alloys (An-Zr) in a molten salt is being investigated. In this process actinides are group-selectively recovered on solid aluminium cathodes as An-Al alloys using a LiCl-KCl eutectic melt at a temperature of 450 °C. In the present study the electrochemical behaviour of zirconium during electrorefining was investigated. The maximum amount of actinides that can be oxidised without anodic co-dissolution of zirconium was determined at a selected constant cathodic current density. The experiment consisted of three steps to assess the different stages of the electrorefining process, each of which employing a fresh aluminium cathode. The results indicate that almost a complete dissolution of the actinides without co-dissolution of zirconium is possible under the applied experimental conditions.

Ellipsometry of anodic film growth

DOE Office of Scientific and Technical Information (OSTI.GOV)

Smith, C.G.

1978-08-01

An automated computer interpretation of ellisometer measurements of anodic film growth was developed. Continuous mass and charge balances were used to utilize more fully the time dependence of the ellipsometer data and the current and potential measurements. A multiple-film model was used to characterize the growth of films which proceeds via a dissolution--precipitation mechanism; the model also applies to film growth by adsorption and nucleation mechanisms. The characteristic parameters for film growth describe homogeneous and heterogeneous crystallization rates, film porosities and degree of hydration, and the supersaturation of ionic species in the electrolyte. Additional descriptions which may be chosen aremore » patchwise film formation, nonstoichiometry of the anodic film, and statistical variations in the size and orientation of secondary crystals. Theories were developed to describe the optical effects of these processes. An automatic, self-compensating ellipsometer was used to study the growth in alkaline solution of anodic films on silver, cadmium, and zinc. Mass-transport conditions included stagnant electrolyte and forced convection in a flow channel. Multiple films were needed to characterize the optical properties of these films. Anodic films grew from an electrolyte supersatuated in the solution-phase dissolution product. The degree of supersaturation depended on transport conditions and had a major effect on the structure of the film. Anodic reaction rates were limited by the transport of charge carriers through a primary surface layer. The primary layers on silver, zinc, and cadmium all appeared to be nonstoichiometric, containing excess metal. Diffusion coefficients, transference numbers, and the free energy of adsorption of zinc oxide were derived from ellipsometer measurements. 97 figures, 13 tables, 198 references.« less

The application of electrolytic photoetching and photopolishing to AISI 304 stainless steel and the electrolytic photoetching of amorphous cobalt alloy

NASA Astrophysics Data System (ADS)

Thomaz, Marita Duarte Canhao da Silva Pereira Fernandes

The results presented cover broad aspects of a quantitative investigation into the elecrolytic etching and polishing of metals and alloys through photographically produced dielectric stencils (Photoresists). A study of the potential field generated between a cathode and relatively smaller anode sites as those defined by a dielectric stencil was carried out. Numerical, analytical and graphical methods yielded answers to the factors determining lateral dissolution (undercut) at the anode/stencil interface. A quasi steady state numerical model simulating the transient behavior of the partially masked electrodes undergoing dissolution was obtained. AISI 304 stainless steel was electrolytically photoetched in 10% w/w HCl electrolyte. The optimised process parameters were utilised for quantifying the effects of galvanostatic etching of the anode as that defined by a relatively narrow adherent resist stencil. Stainless steel was also utilised in investigating electrolytic photopolishing. A polishing electrolyte (orthophosphoric acid-glycerol) was modified by the addition of a surfactant which yielded surface texture values of 70nm (Ra) and high levels of specular reflectance. These results were used in the production of features upon the metal surface through photographically produced precision stencils. The process was applied to the production of edge filters requiring high quality surface textures in precision recesses. Some of the new amorphous material exhibited high resistance to dissolution in commercially used spray etching formulations. One of these materials is a cobalt based alloy produced by chill block spinning. This material was also investigated and electro etched in 10% w/w HCl solution. Although passivity was not overcome, by selecting suitable operating parameters the successful electro photoetching of precision magnetic recording head laminations was achieved. Similarly, a polycrystalline nickel based alloy also exhibiting passivity in commercially used etchants was successfully etched in the above electrolyte.

Passivation dynamics in the anisotropic deposition and stripping of bulk magnesium electrodes during electrochemical cycling

DOE PAGES

Wetzel, David J.; Malone, Marvin A.; Haasch, Richard T.; ...

2015-08-10

Rechargeable magnesium (Mg) batteries show promise for use as a next generation technology for high-density energy storage, though little is known about the Mg anode solid electrolyte interphase and its implications for the performance and durability of a Mg-based battery. We explore in this report passivation effects engendered during the electrochemical cycling of a bulk Mg anode, characterizing their influences during metal deposition and dissolution in a simple, nonaqueous, Grignard electrolyte solution (ethylmagnesium bromide, EtMgBr, in tetrahydrofuran). Scanning electron microscopy images of Mg foil working electrodes after electrochemical polarization to dissolution potentials show the formation of corrosion pits. The pitmore » densities so evidenced are markedly potential-dependent. When the Mg working electrode is cycled both potentiostatically and galvanostatically in EtMgBr these pits, formed due to passive layer breakdown, act as the foci for subsequent electrochemical activity. Detailed microscopy, diffraction, and spectroscopic data show that further passivation and corrosion results in the anisotropic stripping of the Mg {0001} plane, leaving thin oxide-comprising passivated side wall structures that demark the {0001} fiber texture of the etched Mg grains. Upon long-term cycling, oxide side walls formed due to the pronounced crystallographic anisotropy of the anodic stripping processes, leading to complex overlay anisotropic, columnar structures, exceeding 50 μm in height. Finally, the passive responses mediating the growth of these structures appear to be an intrinsic feature of the electrochemical growth and dissolution of Mg using this electrolyte.« less

Passivation dynamics in the anisotropic deposition and stripping of bulk magnesium electrodes during electrochemical cycling

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wetzel, David J.; Malone, Marvin A.; Haasch, Richard T.

Rechargeable magnesium (Mg) batteries show promise for use as a next generation technology for high-density energy storage, though little is known about the Mg anode solid electrolyte interphase and its implications for the performance and durability of a Mg-based battery. We explore in this report passivation effects engendered during the electrochemical cycling of a bulk Mg anode, characterizing their influences during metal deposition and dissolution in a simple, nonaqueous, Grignard electrolyte solution (ethylmagnesium bromide, EtMgBr, in tetrahydrofuran). Scanning electron microscopy images of Mg foil working electrodes after electrochemical polarization to dissolution potentials show the formation of corrosion pits. The pitmore » densities so evidenced are markedly potential-dependent. When the Mg working electrode is cycled both potentiostatically and galvanostatically in EtMgBr these pits, formed due to passive layer breakdown, act as the foci for subsequent electrochemical activity. Detailed microscopy, diffraction, and spectroscopic data show that further passivation and corrosion results in the anisotropic stripping of the Mg {0001} plane, leaving thin oxide-comprising passivated side wall structures that demark the {0001} fiber texture of the etched Mg grains. Upon long-term cycling, oxide side walls formed due to the pronounced crystallographic anisotropy of the anodic stripping processes, leading to complex overlay anisotropic, columnar structures, exceeding 50 μm in height. Finally, the passive responses mediating the growth of these structures appear to be an intrinsic feature of the electrochemical growth and dissolution of Mg using this electrolyte.« less

Passivation Dynamics in the Anisotropic Deposition and Stripping of Bulk Magnesium Electrodes During Electrochemical Cycling.

PubMed

Wetzel, David J; Malone, Marvin A; Haasch, Richard T; Meng, Yifei; Vieker, Henning; Hahn, Nathan T; Gölzhäuser, Armin; Zuo, Jian-Min; Zavadil, Kevin R; Gewirth, Andrew A; Nuzzo, Ralph G

2015-08-26

Although rechargeable magnesium (Mg) batteries show promise for use as a next generation technology for high-density energy storage, little is known about the Mg anode solid electrolyte interphase and its implications for the performance and durability of a Mg-based battery. We explore in this report passivation effects engendered during the electrochemical cycling of a bulk Mg anode, characterizing their influences during metal deposition and dissolution in a simple, nonaqueous, Grignard electrolyte solution (ethylmagnesium bromide, EtMgBr, in tetrahydrofuran). Scanning electron microscopy images of Mg foil working electrodes after electrochemical polarization to dissolution potentials show the formation of corrosion pits. The pit densities so evidenced are markedly potential-dependent. When the Mg working electrode is cycled both potentiostatically and galvanostatically in EtMgBr these pits, formed due to passive layer breakdown, act as the foci for subsequent electrochemical activity. Detailed microscopy, diffraction, and spectroscopic data show that further passivation and corrosion results in the anisotropic stripping of the Mg {0001} plane, leaving thin oxide-comprising passivated side wall structures that demark the {0001} fiber texture of the etched Mg grains. Upon long-term cycling, oxide side walls formed due to the pronounced crystallographic anisotropy of the anodic stripping processes, leading to complex overlay anisotropic, columnar structures, exceeding 50 μm in height. The passive responses mediating the growth of these structures appear to be an intrinsic feature of the electrochemical growth and dissolution of Mg using this electrolyte.

Double layer, diluent and anode effects upon the electrodeposition of aluminium from chloroaluminate based ionic liquids.

PubMed

Abbott, Andrew P; Qiu, Fulian; Abood, Hadi M A; Ali, M Rostom; Ryder, Karl S

2010-02-28

The deposition of aluminium from a chloroaluminate based ionic liquid was studied to elucidate the effect of a diluent (toluene) and electrolyte (LiCl) on the deposit morphology. A wide variety of analytical techniques was applied to this system to determine the speciation and mechanism of material growth. These included: (27)Al NMR, FAB-MS, cyclic voltammetry, chronocoulometry, chronopotentiometry, scanning electron microscopy and atomic force microscopy. It was found that under-potential deposition (upd) causes a change in the way in which metal grows on the electrode surface. Metal grows in two regimes which are believed to be nano-material and bulk material. The addition of toluene causes a change in speciation and a decrease in upd which in turn changes the morphology of the deposit obtained and can lead to mirror finish aluminium. The addition of LiCl has the opposite effect encouraging upd and leading to larger crystallites and a dark grey deposit. It is also shown for the first time that under many conditions the rate of the anodic dissolution process is overall rate controlling and one effect of the addition of toluene is to increase the rate of anodic dissolution.

Effect of Low-Temperature Environment on Stress Corrosion Cracking Behavior of X80 Pipeline Steel in Simulated Alkaline Soil Solution

NASA Astrophysics Data System (ADS)

Xie, Fei; Wang, Dan; Wu, Ming; Yu, Chengxiang; Sun, Dongxu; Yang, Xu; Xu, Changhao

2018-04-01

The stress corrosion cracking (SCC) of X80 pipeline steel in simulated alkaline soil solution under different temperatures was investigated by slow-strain-rate testing, scanning electron microscopy and energy-dispersive spectroscopy. Results showed that the fracture was transgranular and brittle at 273 K to 278 K (0 °C to 5 °C), and the metal surface was dissolved by a large number of chloride ions. Furthermore, hydrogen embrittlement was caused by the hydrogen atom extended to the high-stress region. The fracture process was controlled by hydrogen-induced cracking, and SCC was highly sensitive at this stage. At 288 K to 298 K (15 °C to 25 °C), the fracture morphology was attributed to the mixed mode of ductile and brittle fractures, the fracture process was controlled by the mechanism of hydrogen-induced cracking and anodic dissolution, and the susceptibility to SCC decreased. When the temperature reached 308 K to 318 K (35 °C to 45 °C), the fracture was mainly intergranular and ductile, the fracture process was controlled by anodic dissolution, and SCC sensitivity was the smallest in this temperature range.

A novel rotating electrochemically anodizing process to fabricate titanium oxide surface nanostructures enhancing the bioactivity of osteoblastic cells.

PubMed

Chang, Chih-Hung; Lee, Hsin-Chun; Chen, Chia-Chun; Wu, Yi-Hau; Hsu, Yuan-Ming; Chang, Yin-Pen; Yang, Ta-I; Fang, Hsu-Wei

2012-07-01

Titanium oxide (TiO(2) ) surface layers with various surface nanostructures (nanotubes and nanowires) have been developed using an anodizing technique. The pore size and length of TiO(2) nanotubes can be tailored by changing the anodizing time and applied voltage. We developed a novel method to transform the upper part of the formed TiO(2) nanotubes into a nanowire-like structure by rotating the titanium anode during anodizing process. The transformation of nanotubes contributed to the preferential chemical dissolution of TiO(2) on the areas with intense interface tension stress. Furthermore, we further compared the effect of various TiO(2) surface nanostructures including flat, nanotubes, and nanowires on bioactive applications. The MG-63 osteoblastic cells cultured on the TiO(2) nanowires exhibited a polygonal shape with extending filopodia and showed highest levels of cell viability and alkaline phosphatase activity (ALP). The TiO(2) nanowire structure formed by our novel method can provide beneficial effects for MG-63 osteoblastic cells in attachment, proliferation, and secretion of ALP on the TiO(2) surface layer. Copyright © 2012 Wiley Periodicals, Inc.

Electrical power production from low-grade waste heat using a thermally regenerative ethylenediamine battery

NASA Astrophysics Data System (ADS)

Rahimi, Mohammad; D'Angelo, Adriana; Gorski, Christopher A.; Scialdone, Onofrio; Logan, Bruce E.

2017-05-01

Thermally regenerative ammonia-based batteries (TRABs) have been developed to harvest low-grade waste heat as electricity. To improve the power production and anodic coulombic efficiency, the use of ethylenediamine as an alternative ligand to ammonia was explored here. The power density of the ethylenediamine-based battery (TRENB) was 85 ± 3 W m-2-electrode area with 2 M ethylenediamine, and 119 ± 4 W m-2 with 3 M ethylenediamine. This power density was 68% higher than that of TRAB. The energy density was 478 Wh m-3-anolyte, which was ∼50% higher than that produced by TRAB. The anodic coulombic efficiency of the TRENB was 77 ± 2%, which was more than twice that obtained using ammonia in a TRAB (35%). The higher anodic efficiency reduced the difference between the anode dissolution and cathode deposition rates, resulting in a process more suitable for closed loop operation. The thermal-electric efficiency based on ethylenediamine separation using waste heat was estimated to be 0.52%, which was lower than that of TRAB (0.86%), mainly due to the more complex separation process. However, this energy recovery could likely be improved through optimization of the ethylenediamine separation process.

2D MoS2 as an efficient protective layer for lithium metal anodes in high-performance Li-S batteries.

PubMed

Cha, Eunho; Patel, Mumukshu D; Park, Juhong; Hwang, Jeongwoon; Prasad, Vish; Cho, Kyeongjae; Choi, Wonbong

2018-04-01

Among the candidates to replace Li-ion batteries, Li-S cells are an attractive option as their energy density is about five times higher (~2,600 Wh kg -1 ). The success of Li-S cells depends in large part on the utilization of metallic Li as anode material. Metallic lithium, however, is prone to grow parasitic dendrites and is highly reactive to several electrolytes; moreover, Li-S cells with metallic Li are also susceptible to polysulfides dissolution. Here, we show that ~10-nm-thick two-dimensional (2D) MoS 2 can act as a protective layer for Li-metal anodes, greatly improving the performances of Li-S batteries. In particular, we observe stable Li electrodeposition and the suppression of dendrite nucleation sites. The deposition and dissolution process of a symmetric MoS 2 -coated Li-metal cell operates at a current density of 10 mA cm -2 with low voltage hysteresis and a threefold improvement in cycle life compared with using bare Li-metal. In a Li-S full-cell configuration, using the MoS 2 -coated Li as anode and a 3D carbon nanotube-sulfur cathode, we obtain a specific energy density of ~589 Wh kg -1 and a Coulombic efficiency of ~98% for over 1,200 cycles at 0.5 C. Our approach could lead to the realization of high energy density and safe Li-metal-based batteries.

The rapid growth of 3 µm long titania nanotubes by anodization of titanium in a neutral electrochemical bath

NASA Astrophysics Data System (ADS)

Lockman, Zainovia; Ismail, Syahriza; Sreekantan, Srimala; Schmidt-Mende, L.; MacManus-Driscoll, J. L.

2010-02-01

The length of titania nanotubes formed by anodization of 0.1 mm thick titanium foil was found to be a strong function of the pH of the electrolyte. The longest nanotubes were formed by using an electrolyte consisting of 1 M Na2SO4 plus 5 wt% NH4F with pH 7. At this pH, after 30 min of anodization, 3 µm length nanotubular titania arrays with top diameters of ~50 nm and bottom diameters of 100 nm were produced. No acid was added to this electrolyte. The formation of titania nanotubes in neutral pH systems was therefore successful due to the excess NH4F in the electrolyte which increases the chemical dissolution process at the metal/oxide interface. Since the pH of the electrolyte at the top part of the nanotubes is kept very high, the dissolution of the nanotubes at the surface is minimal. However, the amount is adequate to remove the initial barrier layer, forming a rather well-defined nanoporous structure. All anodized foils were weakly crystalline and the transformation to anatase phase was achieved by heat treatment at temperatures from 200 to 500 °C for 1 h in air. Annealing at temperatures above 500 °C induce rutile phase formation and annealing at higher temperatures accelerates the diffusion of Ti4+ leading to excessive growth and the nanotubular structure diminishes.

2D MoS2 as an efficient protective layer for lithium metal anodes in high-performance Li-S batteries

NASA Astrophysics Data System (ADS)

Cha, Eunho; Patel, Mumukshu D.; Park, Juhong; Hwang, Jeongwoon; Prasad, Vish; Cho, Kyeongjae; Choi, Wonbong

2018-04-01

Among the candidates to replace Li-ion batteries, Li-S cells are an attractive option as their energy density is about five times higher ( 2,600 Wh kg-1). The success of Li-S cells depends in large part on the utilization of metallic Li as anode material. Metallic lithium, however, is prone to grow parasitic dendrites and is highly reactive to several electrolytes; moreover, Li-S cells with metallic Li are also susceptible to polysulfides dissolution. Here, we show that 10-nm-thick two-dimensional (2D) MoS2 can act as a protective layer for Li-metal anodes, greatly improving the performances of Li-S batteries. In particular, we observe stable Li electrodeposition and the suppression of dendrite nucleation sites. The deposition and dissolution process of a symmetric MoS2-coated Li-metal cell operates at a current density of 10 mA cm-2 with low voltage hysteresis and a threefold improvement in cycle life compared with using bare Li-metal. In a Li-S full-cell configuration, using the MoS2-coated Li as anode and a 3D carbon nanotube-sulfur cathode, we obtain a specific energy density of 589 Wh kg-1 and a Coulombic efficiency of 98% for over 1,200 cycles at 0.5 C. Our approach could lead to the realization of high energy density and safe Li-metal-based batteries.

Fabrication of porous anodic alumina using normal anodization and pulse anodization

NASA Astrophysics Data System (ADS)

Chin, I. K.; Yam, F. K.; Hassan, Z.

2015-05-01

This article reports on the fabrication of porous anodic alumina (PAA) by two-step anodizing the low purity commercial aluminum sheets at room temperature. Different variations of the second-step anodization were conducted: normal anodization (NA) with direct current potential difference; pulse anodization (PA) alternate between potential differences of 10 V and 0 V; hybrid pulse anodization (HPA) alternate between potential differences of 10 V and -2 V. The method influenced the film homogeneity of the PAA and the most homogeneous structure was obtained via PA. The morphological properties are further elucidated using measured current-transient profiles. The absent of current rise profile in PA indicates the anodization temperature and dissolution of the PAA structure were greatly reduced by alternating potential differences.

High-capacity aqueous zinc batteries using sustainable quinone electrodes

PubMed Central

Zhao, Qing; Huang, Weiwei; Luo, Zhiqiang; Liu, Luojia; Lu, Yong; Li, Yixin; Li, Lin; Hu, Jinyan; Ma, Hua; Chen, Jun

2018-01-01

Quinones, which are ubiquitous in nature, can act as sustainable and green electrode materials but face dissolution in organic electrolytes, resulting in fast fading of capacity and short cycle life. We report that quinone electrodes, especially calix[4]quinone (C4Q) in rechargeable metal zinc batteries coupled with a cation-selective membrane using an aqueous electrolyte, exhibit a high capacity of 335 mA h g−1 with an energy efficiency of 93% at 20 mA g−1 and a long life of 1000 cycles with a capacity retention of 87% at 500 mA g−1. The pouch zinc batteries with a respective depth of discharge of 89% (C4Q) and 49% (zinc anode) can deliver an energy density of 220 Wh kg−1 by mass of both a C4Q cathode and a theoretical Zn anode. We also develop an electrostatic potential computing method to demonstrate that carbonyl groups are active centers of electrochemistry. Moreover, the structural evolution and dissolution behavior of active materials during discharge and charge processes are investigated by operando spectral techniques such as IR, Raman, and ultraviolet-visible spectroscopies. Our results show that batteries using quinone cathodes and metal anodes in aqueous electrolyte are reliable approaches for mass energy storage. PMID:29511734

High-capacity aqueous zinc batteries using sustainable quinone electrodes.

PubMed

Zhao, Qing; Huang, Weiwei; Luo, Zhiqiang; Liu, Luojia; Lu, Yong; Li, Yixin; Li, Lin; Hu, Jinyan; Ma, Hua; Chen, Jun

2018-03-01

Quinones, which are ubiquitous in nature, can act as sustainable and green electrode materials but face dissolution in organic electrolytes, resulting in fast fading of capacity and short cycle life. We report that quinone electrodes, especially calix[4]quinone (C4Q) in rechargeable metal zinc batteries coupled with a cation-selective membrane using an aqueous electrolyte, exhibit a high capacity of 335 mA h g -1 with an energy efficiency of 93% at 20 mA g -1 and a long life of 1000 cycles with a capacity retention of 87% at 500 mA g -1 . The pouch zinc batteries with a respective depth of discharge of 89% (C4Q) and 49% (zinc anode) can deliver an energy density of 220 Wh kg -1 by mass of both a C4Q cathode and a theoretical Zn anode. We also develop an electrostatic potential computing method to demonstrate that carbonyl groups are active centers of electrochemistry. Moreover, the structural evolution and dissolution behavior of active materials during discharge and charge processes are investigated by operando spectral techniques such as IR, Raman, and ultraviolet-visible spectroscopies. Our results show that batteries using quinone cathodes and metal anodes in aqueous electrolyte are reliable approaches for mass energy storage.

High resolution electrolyte for thinning InP by anodic dissolution and its applications to EC-V profiling, defect revealing and surface passivation

NASA Technical Reports Server (NTRS)

Faur, Maria; Faur, Mircea; Weinberg, Irving; Goradia, Manju; Vargas, Carlos

1991-01-01

An extensive experimental study was conducted using various electrolytes in an effort to find an appropriate electrolyte for anodic dissolution of InP. From the analysis of electrochemical characteristics in the dark and under different illumination levels, x ray photoelectron spectroscopy and SEM/Nomarski inspection of the surfaces, it was determined that the anodic dissolution of InP front surface layers by FAP electrolyte is a very good choice for rendering smooth surfaces, free of oxides and contaminants and with good electrical characteristics. The FAP electrolyte, based on HF, CH3COOH, and H2O2 appears to be inherently superior to previously reported electrolytes for performing accurate EC-V profiling of InP at current densities of up to 0.3 mA/sq cm. It can also be used for accurate electrochemical revealing of either precipitates or dislocation density with application to EPD mapping as a function of depth, and for defect revealing of multilayer InP structures at any depth and/or at the interfaces.

Corrosion of Cu-xZn alloys in slightly alkaline chloride solutions studied by stripping voltammetry and microanalysis.

PubMed

Milosev, I; Minović, A

2001-01-01

The mechanism of corrosion of Cu-xZn alloys (x = 10-40 wt %) in slightly alkaline chloride solutions was investigated by analysing solid reaction products by energy dispersive X-ray analysis (EDS) and dissolved reaction products by differential anodic pulse stripping (DAPS) voltammetry. The corrosion process was studied under open circuit and under potentiostatic conditions at selected potentials. Pure metals were studied comparatively so that an interacting effect of particular metal components in the alloy could be determined. All four Cu-xZn alloys show an improved behaviour compared to pure metals. Under open-circuit condition both components dissolve simultaneously in the solution. With increasing immersion time the preferential, dissolution of zinc in the solution becomes pronounced. It is the highest for Cu-10Zn and the lowest for Cu-30Zn alloy. Under potentiostatic control the dissolution mechanism depends on the electrode potential and changes from exclusive dissolution of zinc to simultaneous dissolution of both components with preferential dissolution of zinc. The latter decreases, as the electrode potential becomes more positive.

Accelerated corrosion of stainless steel in thiocyanate-containing solutions

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pistorius, P Chris; Li, Wen

2012-09-19

It is known that reduced sulfur compounds (such as thiocyanate and thiosulfate) can accelerate active corrosion of austenitic stainless steel in acid solutions, but before we started this project the mechanism of acceleration was largely unclear. This work combined electrochemical measurements and analysis using scanning electron microscopy (SEM) and X-ray photo-electron spectroscopy (XPS), which provided a comprehensive understanding of the catalytic effect of reduced sulfur species on the active corrosion of stainless steel. Both the behavior of the pure elements and the steel were studied and the work focused on the interaction between the pure elements of the steel, whichmore » is the least understood area. Upon completion of this work, several aspects are now much clearer. The main results from this work can be summarized as follows: The presence of low concentrations (around 0.1 mM) of thiocyanate or tetrathionate in dilute sulfuric acid greatly accelerates the anodic dissolution of chromium and nickel, but has an even stronger effect on stainless steels (iron-chromium-nickel alloys). Electrochemical measurements and surface analyses are in agreement with the suggestion that accelerated dissolution really results from suppressed passivation. Even well below the passivation potential, the electrochemical signature of passivation is evident in the electrode impedance; the electrode impedance shows clearly that this pre-passivation is suppressed in the presence of thiocyanate. For the stainless steels, remarkable changes in the morphology of the corroded metal surface and in the surface concentration of chromium support the suggestion that pre-passivation of stainless steels is suppressed because dissolution of chromium is accelerated. Surface analysis confirmed that adsorbed sulfur / sulfide forms on the metal surfaces upon exposure to solutions containing thiocyanate or thiosulfate. For pure nickel, and steels containing nickel (and residual copper), bulk sulfide (visible as a black corrosion product) forms during anodic dissolution. The sulfide is electronically conductive, and gives an increase of several orders of magnitude in the electrode capacitance; the sulfide also causes anodic activation to persist after the pure metals and steels were removed from the thiocyanate-containing electrolyte and transferred to a thiocyanate-free electrolyte. The main practical implications of this work are that low concentrations of reduced sulfur compounds strongly affect anodic dissolution of stainless steels, and that selecting steels with elevated concentrations of chromium, nickel or molybdenum would serve to limit the anodic dissolution rate in the presence of reduced sulfur compounds.« less

Recovery of critical and value metals from mobile electronics enabled by electrochemical processing

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tedd E. Lister; Peiming Wang; Andre Anderko

2014-10-01

Electrochemistry-based schemes were investigated as a means to recover critical and value metals from scrap mobile electronics. Mobile electronics offer a growing feedstock for replenishing value and critical metals and reducing need to exhaust primary sources. The electrorecycling process generates oxidizing agents at an anode to dissolve metals from the scrap matrix while reducing dissolved metals at the cathode. The process uses a single cell to maximize energy efficiency. E vs pH diagrams and metals dissolution experiments were used to assess effectiveness of various solution chemistries. Following this work, a flow chart was developed where two stages of electrorecycling weremore » proposed: 1) initial dissolution of Cu, Sn, Ag and magnet materials using Fe+3 generated in acidic sulfate and 2) final dissolution of Pd and Au using Cl2 generated in an HCl solution. Experiments were performed using a simulated metal mixture equivalent to 5 cell phones. Both Cu and Ag were recovered at ~ 97% using Fe+3 while leaving Au and Pd intact. Strategy for extraction of rare earth elements (REE) from dissolved streams is discussed as well as future directions in process development.« less

X-ray reflectivity study of formation of multilayer porous anodic oxides of silicon.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chu, Y.; Fenollosa, R.; Parkhutik, V.

1999-07-21

The paper reports data on the kinetics of anodic oxide films growth on silicon in aqueous solutions of phosphoric acids as well as a study of the morphology of the oxides grown in a special regime of the oscillating anodic potential. X-ray reflectivity measurements were performed on the samples of anodic oxides using an intense synchrotron radiation source. They have a multilayer structure as revealed by theoretical fitting of the reflectivity data. The oscillations of the anodic potential are explained in terms of synchronized oxidation/dissolution reactions at the silicon surface and accumulation of mechanic stress in the oxide film.

Superhydrophilicity of novel anodic alumina nanofibers films and their formation mechanism

NASA Astrophysics Data System (ADS)

Peng, Rong; Yang, Wulin; Fu, Licai; Zhu, Jiajun; Li, Deyi; Zhou, Lingping

2017-06-01

A novel anodic alumina nanofibers structure, which is different from the traditional porous anodic structure, has been quickly fabricated via anodizing in a new electrolyte, pyrophosphoric acid. The effects of the solution concentration and the anodizing time on the formation of the anodic alumina nanofibers were analyzed. The results show that the nanostructure of anodic alumina can change to the nanofiber oxide from the porous oxide by increasing the solution concentration. Prolonging the anodizing time is beneficial to obtain alumina nanofibers at high solution concentration. Growth behavior of the alumina nanofibers was also discussed by scanning electron microscopy observations. Owing to the unique hexagonal structure of anodic alumina as well as the preferential chemical dissolution between the porous anodic alumina and the anodic alumina nanotips, the slightly soluble anodic alumina nanotips could form novel alumina nanofibers during anodizing. The results show that the nanofibers-covered aluminum surface exhibits superhydrophilic property, with a near-zero water contact angle. Such alumina nanofibers with superhydrophilic property could be used for various potential applications.

The influence of surface roughness and high pressure torsion on the growth of anodic titania nanotubes on pure titanium

NASA Astrophysics Data System (ADS)

Hu, Nan; Gao, Nong; Starink, Marco J.

2016-11-01

Anodic titanium dioxide nanotube (TNT) arrays have wide applications in photocatalytic, catalysis, electronics, solar cells and biomedical implants. When TNT coatings are combined with severe plastic deformation (SPD), metal processing techniques which efficiently improve the strength of metals, a new generation of biomedical implant is made possible with both improved bulk and surface properties. This work investigated the effect of processing by high pressure torsion (HPT) and different mechanical preparations on the substrate and subsequently on the morphology of TNT layers. HPT processing was applied to refine the grain size of commercially pure titanium samples and substantially improved their strength and hardness. Subsequent anodization at 30 V in 0.25 wt.% NH4F for 2 h to form TNT layers on sample surfaces prepared with different mechanical preparation methods was carried out. It appeared that the local roughness of the titanium surface on a microscopic level affected the TNT morphology more than the macroscopic surface roughness. For HPT-processed sample, the substrate has to be pre-treated by a mechanical preparation finer than 4000 grit for HPT to have a significant influence on TNTs. During the formation of TNT layers the oxide dissolution rate was increased for the ultrafine-grained microstructure formed due to HPT processing.

Direct electrochemical reduction of metal-oxides

DOEpatents

Redey, Laszlo I.; Gourishankar, Karthick

2003-01-01

A method of controlling the direct electrolytic reduction of a metal oxide or mixtures of metal oxides to the corresponding metal or metals. A non-consumable anode and a cathode and a salt electrolyte with a first reference electrode near the non-consumable anode and a second reference electrode near the cathode are used. Oxygen gas is produced and removed from the cell. The anode potential is compared to the first reference electrode to prevent anode dissolution and gas evolution other than oxygen, and the cathode potential is compared to the second reference electrode to prevent production of reductant metal from ions in the electrolyte.

Sequential pretreatment for cell disintegration of municipal sludge in a neutral Bio-electro-Fenton system.

PubMed

Yu, Qilin; Jin, Xiaochen; Zhang, Yaobin

2018-05-15

Sludge cell disruption was generally considered as the rate-limiting step for the anaerobic digestion of waste activated sludge (WAS). Advanced oxidation processes and bio-electro-chemical systems were recently reported to enhance the hydrolysis of WAS and sludge cell disruption, while the cell-breaking processes of these systems remain unclear yet. In this study, an innovative Bio-electro-Fenton system was developed to pretreat the WAS sequentially with cathode Fenton process and anode anaerobic digestion. Significant cell disruption and dissolution intracellular organics were founded after the treatment. X-ray photoelectron spectroscopy (XPS) analysis and fourier transform infrared spectroscopy (FT-IR) spectra indicated that Gram-negative bacteria were more sensitive to free radicals yielded in cathode to induce a chain reaction that destroyed the lipid-contained outer membrane, while Gram-positive bacteria with thick peptidoglycan layer were liable to be biologically decomposed in the anode. Compared with the oxidation of organic matters in the cathode Fenton, the secretion of enzyme increased in the anode which was beneficial to break down the complex matters (peptidoglycans) into simples that were available for anode oxidation by exoelectrogens. The results also showed a possible prospect for the application of this sequential pretreatment in bio-electro-Fenton systems to disrupt sludge cells and enhance the anaerobic digestion. Copyright © 2018 Elsevier Ltd. All rights reserved.

Electrolysis of plutonium nitride in LiCl-KCl eutectic melts

NASA Astrophysics Data System (ADS)

Shirai, O.; Iwai, T.; Shiozawa, K.; Suzuki, Y.; Sakamura, Y.; Inoue, T.

2000-01-01

The electrolysis of plutonium nitride, PuN, was investigated in the LiCl-KCl eutectic salt with 0.54 wt% PuCl 3 at 773 K in order to understand the dissolution of PuN at the anode and the deposition of metal at the cathode from the viewpoint of the application of a pyrochemical process to nitride fuel cycle. It was found from cyclic voltammetry that the electrochemical dissolution of PuN began nearly at the theoretically evaluated potential and this reaction was irreversible. Several grams of plutonium metal were successfully recovered at the molybdenum electrode as a deposit with a current efficiency of about 90%, although some fractions of the deposited plutonium often fell from the molybdenum electrode.

New insights into pre-lithiation kinetics of graphite anodes via nuclear magnetic resonance spectroscopy

NASA Astrophysics Data System (ADS)

Holtstiege, Florian; Schmuch, Richard; Winter, Martin; Brunklaus, Gunther; Placke, Tobias

2018-02-01

Pre-lithiation of anode materials can be an effective method to compensate active lithium loss which mainly occurs in the first few cycles of a lithium ion battery (LIB), due to electrolyte decomposition and solid electrolyte interphase (SEI) formation at the surface of the anode. There are many different pre-lithiation methods, whereas pre-lithiation using metallic lithium constitutes the most convenient and widely utilized lab procedure in literature. In this work, for the first time, solid state nuclear magnetic resonance spectroscopy (NMR) is applied to monitor the reaction kinetics of the pre-lithiation process of graphite with lithium. Based on static 7Li NMR, we can directly observe both the dissolution of lithium metal and parallel formation of LiCx species in the obtained NMR spectra with time. It is also shown that the degree of pre-lithiation as well as distribution of lithium metal on the electrode surface have a strong impact on the reaction kinetics of the pre-lithiation process and on the remaining amount of lithium metal. Overall, our findings are highly important for further optimization of pre-lithiation methods for LIB anode materials, both in terms of optimized pre-lithiation time and appropriate amounts of lithium metal.

Engineering of highly ordered TiO2 nanopore arrays by anodization

NASA Astrophysics Data System (ADS)

Wang, Huijie; Huang, Zhennan; Zhang, Li; Ding, Jie; Ma, Zhaoxia; Liu, Yong; Kou, Shengzhong; Yang, Hangsheng

2016-07-01

Finite element analysis was used to simulate the current density distributions in the TiO2 barrier layer formed at the initial stage of Ti anodization. The morphology modification of the barrier layer was found to induce current density distribution change. By starting the anodization with proper TiO2 barrier layer morphology, the current density distribution can be adjusted to favor the formation of either nanotube arrays or nanopore arrays of anodic TiO2. We also found that the addition of sodium acetate into the electrolyte suppressed both the field-assisted chemical dissolution of TiO2 and the TiF62- hydrolysis induced TiO2 deposition during anodization, and thus further favored the nanopore formation. Accordingly, highly ordered anodic TiO2 nanopore arrays, similar to anodic aluminum oxide nanopore arrays, were successfully prepared.

First-Principles Modeling of Mn(II) Migration above and Dissolution from Li x Mn 2 O 4 (001) Surfaces

DOE PAGES

Leung, Kevin

2016-12-10

The density functional theory and ab initio molecular dynamics simulations are applied to investigate the migration of Mn(II) ions to above-surface sites on spinel Li xMn 2O 4 (001) surfaces, the subsequent Mn dissolution into the organic liquid electrolyte, and the detrimental effects on graphite anode solid electrolyte interphase (SEI) passivating films after Mn(II) ions diffuse through the separator. The dissolution mechanism proves complex; the much-quoted Hunter disproportionation of Mn(III) to form Mn(II) is far from sufficient. Key steps that facilitate Mn(II) loss include concerted liquid/solid-state motions; proton-induced weakening of Mn–O bonds forming mobile OH – surface groups; and chemicalmore » reactions of adsorbed decomposed organic fragments. Mn(II) lodged between the inorganic Li 2CO 3 and organic lithium ethylene dicarbonate (LEDC) anode SEI components facilitate electrochemical reduction and decomposition of LEDC. Our findings help inform future design of protective coatings, electrolytes, additives, and interfaces.« less

ANODIC TREATMENT OF URANIUM

DOEpatents

Kolodney, M.

1959-02-01

A method is presented for effecting eloctrolytic dissolution of a metallic uranium article at a uniform rate. The uranium is made the anode in an aqueous phosphoric acid solution containing nitrate ions furnished by either ammonium nitrate, lithium nitrate, sodium nitrate, or potassium nitrate. A stainless steel cathode is employed and electrolysls carried out at a current density of about 0.1 to 1 ampere per square inch.

Electrochemical polishing of thread fastener test specimens of nickel-chromium iron alloys

DOEpatents

Kephart, Alan R.

1991-01-01

An electrochemical polishing device and method for selective anodic dissolution of the surface of test specimens comprised, for example, of nickel-chromium-iron alloys, which provides for uniform dissolution at the localized sites to remove metal through the use of a coiled wire electrode (cathode) placed in the immediate proximity of the working, surface resulting in a polished and uniform grain boundary.

Electrolyte with Low Polysulfide Solubility for Li-S Batteries

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sun, Ke; Wu, Qin; Tong, Xiao

Here, Li-S battery is one of the most promising next generation rechargeable battery technologies due to its high theoretical energy density and low material cost. While its success is impeded by the low energy efficiency and fast capacity fade primarily caused by the discharge intermediates, Li-polysulfides (PS), dissolution in the electrolyte. Mitigation of PS dissolution in electrolyte involves the search of new electrolyte solvent system that exhibits poor solvation to the PS while still have good solvation ability to the electrolyte salt for high ionic conductivity. Applying co-solvents with reduced solvating power but compatible with the state of art Li-Smore » battery’s ether-based electrolyte is one of the most promising concepts. This route is also advantageous of having a low scale-up cost. With the aids of Quantum Chemical Calculation, we have identified high carbon-to-oxygen (C/O) ratio ethers as co-solvent in the new electrolytes that effectively impede PS dissolution while still maintaining high ionic conductivity. Significantly improved cycle life and cycling Coulombic efficiency are observed for Li-S cells using the new composite electrolytes. Anode analysis with different methods also demonstrate that reducing electrolyte’s PS solubility results in less sulfur total amount on the lithium anode surface and lower ratio of the longer-chain PS, which is probably a sign of suppressed side reactions between the anode and PS in the electrolyte.« less

Electrolyte with Low Polysulfide Solubility for Li-S Batteries

DOE PAGES

Sun, Ke; Wu, Qin; Tong, Xiao; ...

2018-05-23

Here, Li-S battery is one of the most promising next generation rechargeable battery technologies due to its high theoretical energy density and low material cost. While its success is impeded by the low energy efficiency and fast capacity fade primarily caused by the discharge intermediates, Li-polysulfides (PS), dissolution in the electrolyte. Mitigation of PS dissolution in electrolyte involves the search of new electrolyte solvent system that exhibits poor solvation to the PS while still have good solvation ability to the electrolyte salt for high ionic conductivity. Applying co-solvents with reduced solvating power but compatible with the state of art Li-Smore » battery’s ether-based electrolyte is one of the most promising concepts. This route is also advantageous of having a low scale-up cost. With the aids of Quantum Chemical Calculation, we have identified high carbon-to-oxygen (C/O) ratio ethers as co-solvent in the new electrolytes that effectively impede PS dissolution while still maintaining high ionic conductivity. Significantly improved cycle life and cycling Coulombic efficiency are observed for Li-S cells using the new composite electrolytes. Anode analysis with different methods also demonstrate that reducing electrolyte’s PS solubility results in less sulfur total amount on the lithium anode surface and lower ratio of the longer-chain PS, which is probably a sign of suppressed side reactions between the anode and PS in the electrolyte.« less

Application of Electro Chemical Machining for materials used in extreme conditions

NASA Astrophysics Data System (ADS)

Pandilov, Z.

2018-03-01

Electro-Chemical Machining (ECM) is the generic term for a variety of electrochemical processes. ECM is used to machine work pieces from metal and metal alloys irrespective of their hardness, strength or thermal properties, through the anodic dissolution, in aerospace, automotive, construction, medical equipment, micro-systems and power supply industries. The Electro Chemical Machining is extremely suitable for machining of materials used in extreme conditions. General overview of the Electro-Chemical Machining and its application for different materials used in extreme conditions is presented.

Characterization of Localized Filament Corrosion Products at the Anodic Head on a Model Mg-Zn-Zr Alloy Surface

DOE PAGES

Rossouw, David; Fu, Dong; Leonard, Donovan N.; ...

2017-02-15

In this study, localized filament corrosion products at the anodic head on a model Mg-1%Zn-0.4%Zr alloy surface were characterized by electron microscopy techniques of site-specific lamella prepared by focused ion beam milling. It is revealed that the anodic head propagates underneath a largely intact thin and dense MgO surface film and comprises dense aggregates of nano-crystalline MgO within a nano-porous Mg(OH) 2 network. In conclusion, the findings contribute new supportive direct imaging insight into the source of the enhanced H 2 evolution that accompanies anodic dissolution of Mg and its alloys.

Characterization of Localized Filament Corrosion Products at the Anodic Head on a Model Mg-Zn-Zr Alloy Surface

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rossouw, David; Fu, Dong; Leonard, Donovan N.

In this study, localized filament corrosion products at the anodic head on a model Mg-1%Zn-0.4%Zr alloy surface were characterized by electron microscopy techniques of site-specific lamella prepared by focused ion beam milling. It is revealed that the anodic head propagates underneath a largely intact thin and dense MgO surface film and comprises dense aggregates of nano-crystalline MgO within a nano-porous Mg(OH) 2 network. In conclusion, the findings contribute new supportive direct imaging insight into the source of the enhanced H 2 evolution that accompanies anodic dissolution of Mg and its alloys.

Combined Effect of Alternating Current Interference and Cathodic Protection on Pitting Corrosion and Stress Corrosion Cracking Behavior of X70 Pipeline Steel in Near-Neutral pH Environment.

PubMed

Wang, Liwei; Cheng, Lianjun; Li, Junru; Zhu, Zhifu; Bai, Shuowei; Cui, Zhongyu

2018-03-22

Influence of alternating current (AC) on pitting corrosion and stress corrosion cracking (SCC) behavior of X70 pipeline steel in the near-neutral pH environment under cathodic protection (CP) was investigated. Both corrosion and SCC are inhibited by -0.775 V SCE CP without AC interference. With the superimposition of AC current (1-10 mA/cm²), the direct current (DC) potential shifts negatively under the CP of -0.775 V SCE and the cathodic DC current decreases and shifts to the anodic direction. Under the CP potential of -0.95 V SCE and -1.2 V SCE , the applied AC current promotes the cathodic reaction and leads to the positive shift of DC potential and increase of cathodic current. Local anodic dissolution occurs attributing to the generated anodic current transients in the positive half-cycle of the AC current, resulting in the initiation of corrosion pits (0.6-2 μm in diameter). AC enhances the SCC susceptibility of X70 steel under -0.775 V SCE CP, attributing to the promotion of anodic dissolution and hydrogen evolution. Even an AC current as low as 1 mA/cm² can enhance the SCC susceptibility.

A Kinetics and Equilibrium Study of Vanadium Dissolution from Vanadium Oxides and Phosphates in Battery Electrolytes: Possible Impacts on ICD Battery Performance.

PubMed

Bock, David C; Marschilok, Amy C; Takeuchi, Kenneth J; Takeuchi, Esther S

2013-06-01

Silver vanadium oxide (Ag 2 V 4 O 11 , SVO) has enjoyed widespread commercial success over the past 30 years as a cathode material for implantable cardiac defibrillator (ICD) batteries. Recently, silver vanadium phosphorous oxide (Ag 2 VO 2 PO 4 , SVPO) has been studied as possibly combining the desirable thermal stability aspects of LiFePO 4 with the electrical conductivity of SVO. Further, due to the noted insoluble nature of most phosphate salts, a lower material solubility of SVPO relative to SVO is anticipated. Thus, the first vanadium dissolution studies of SVPO in battery electrolyte solutions are described herein. The equilibrium solubility of SVPO was ~5 times less than SVO, with a rate constant of dissolution ~3.5 times less than that of SVO. The vanadium dissolution in SVO and SVPO can be adequately described with a diffusion layer model, as supported by the Noyes-Whitney equation. Cells prepared with vanadium-treated anodes displayed higher AC impedance and DC resistance relative to control anodes. These data support the premise that SVPO cells are likely to exhibit reduced cathode solubility and thus less affected by increased cell resistance due to cathode solubility compared to SVO based cells.

The study of aluminium anodes for high power density Al/air batteries with brine electrolytes

NASA Astrophysics Data System (ADS)

Nestoridi, Maria; Pletcher, Derek; Wood, Robert J. K.; Wang, Shuncai; Jones, Richard L.; Stokes, Keith R.; Wilcock, Ian

Aluminium alloys containing small additions of both tin (∼0.1 wt%) and gallium (∼0.05 wt%) are shown to dissolve anodically at high rates in sodium chloride media at room temperatures; current densities >0.2 A cm -2 can be obtained at potentials close to the open circuit potential, ∼-1500 mV versus SCE. The tin exists in the alloys as a second phase, typically as ∼1 μm inclusions (precipitates) distributed throughout the aluminium structure, and anodic dissolution occurs to form pits around the tin inclusions. Although the distribution of the gallium in the alloy could not be established, it is also shown to be critical in the formation of these pits as well as maintaining their activity. The stability of the alloys to open circuit corrosion and the overpotential for high rate dissolution, both critical to battery performance, are shown to depend on factors in addition to elemental composition; both heat treatment and mechanical working influence the performance of the alloy. The correlation between alloy performance and their microstructure has been investigated.

Effect of the Crevice Former on the Corrosion Behavior of 316L Stainless Steel in Chloride-Containing Synthetic Tap Water

NASA Astrophysics Data System (ADS)

Kim, Seon-Hong; Lee, Ji-Hoon; Kim, Jung-Gu; Kim, Woo-Cheol

2018-05-01

To restrain the failure of the plate heat exchanger (PHE) in customer boiler working fluid, the effect of crevice former type on the corrosion behavior of the 316L stainless steel plate was investigated using electrochemical methods and surface analyses in chloride-containing synthetic tap water (60 °C). The localized corrosion under metal-metal crevice condition was initiated more easily than that under the metal-gasket crevice condition due to the restricted mass transport at the gasket crevice mouth. However, the anodic current under the metal-metal crevice condition was lower than that under metal-gasket crevice condition at a higher anodic potential, indicating that that the metal dissolution under EPDM crevice would be higher than that under metal crevice under the accelerated corrosion condition. Because narrow crevice gap that was formed under gasket accelerated the anodic dissolution at the crevice mouth, the perforation tendency under metal-gasket crevice condition is much higher than that under metal-metal crevice condition. As a result, the crevice geometry, especially the crevice gap, mainly affected the corrosion behavior of PHE material.

Effect of the Crevice Former on the Corrosion Behavior of 316L Stainless Steel in Chloride-Containing Synthetic Tap Water

NASA Astrophysics Data System (ADS)

Kim, Seon-Hong; Lee, Ji-Hoon; Kim, Jung-Gu; Kim, Woo-Cheol

2018-03-01

To restrain the failure of the plate heat exchanger (PHE) in customer boiler working fluid, the effect of crevice former type on the corrosion behavior of the 316L stainless steel plate was investigated using electrochemical methods and surface analyses in chloride-containing synthetic tap water (60 °C). The localized corrosion under metal-metal crevice condition was initiated more easily than that under the metal-gasket crevice condition due to the restricted mass transport at the gasket crevice mouth. However, the anodic current under the metal-metal crevice condition was lower than that under metal-gasket crevice condition at a higher anodic potential, indicating that that the metal dissolution under EPDM crevice would be higher than that under metal crevice under the accelerated corrosion condition. Because narrow crevice gap that was formed under gasket accelerated the anodic dissolution at the crevice mouth, the perforation tendency under metal-gasket crevice condition is much higher than that under metal-metal crevice condition. As a result, the crevice geometry, especially the crevice gap, mainly affected the corrosion behavior of PHE material.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ulin, V. P.; Ulin, N. V.; Soldatenkov, F. Yu., E-mail: f.soldatenkov@mail.ioffe.ru

The interaction of heavily doped p- and n-type Si crystals with hydrofluoric acid in the dark with and without contact with metals having greatly differing work functions (Ag and Pd) is studied. The dependences of the dissolution rates of Si crystals in HF solutions that contain oxidizing agents with different redox potentials (FeCl{sub 3}, V{sub 2}O{sub 5} and CrO{sub 3}) on the type and level of silicon doping are determined. Analysis of the experimental data suggests that valence-band holes in silicon are not directly involved in the anodic reactions of silicon oxidation and dissolution and their generation in crystals doesmore » not limit the rate of these processes. It is also shown that the character and rate of the chemical process leading to silicon dissolution in HF-containing electrolytes are determined by the interfacial potential attained at the semiconductor–electrolyte interface. The mechanism of electrochemical pore formation in silicon crystals is discussed in terms of selfconsistent cooperative reactions of nucleophilic substitution between chemisorbed fluorine anions and coordination- saturated silicon atoms in the crystal subsurface layer. A specific feature of these reactions for silicon crystals is that vacant nonbonding d{sup 2}sp{sup 3} orbitals of Si atoms, associated with sixfold degenerate states corresponding to the Δ valley of the conduction band, are involved in the formation of intermediate complexes. According to the suggested model, the pore-formation process spontaneously develops in local regions of the interface under the action of the interfacial potential in the adsorption layer and occurs as a result of the detachment of (SiF{sub 2}){sub n} polymer chains from the crystal. Just this process leads to the preferential propagation of pores along the <100> crystallographic directions. The thermodynamic aspects of pore nucleation and the effect of the potential drop across the interface, conduction type, and free-carrier concentration in the crystal on the pore size and structure are discussed. The concepts developed in the study can consistently account for experimental facts characterizing the etching of silicon crystals with various electrical parameters under various conditions providing the anodic polarization of crystals in HF-containing solutions.« less

Humidity Effect on Nanoscale Electrochemistry in Solid Silver Ion Conductors and the Dual Nature of Its Locality

DOE PAGES

Yang, Sangmo; Strelcov, Evgheni; Paranthaman, Mariappan Parans; ...

2015-01-07

Scanning probe microscopy (SPM) is a powerful tool to investigate electrochemistry in nanoscale volumes. While most SPM-based studies have focused on reactions at the tip-surface junction, charge and mass conservation requires coupled and intrinsically non-local cathodic and anodic processes that can be significantly affected by ambient humidity. Here, we explore the role of water in both cathodic and anodic processes, associated charge transport, and topographic volume changes depending on the polarity of tip bias. The first-order reversal curve current-voltage technique combined with simultaneous detection of the sample topography, referred to as FORC-IVz, was applied to a silver solid ion conductor.more » We found that the protons generated from water affect silver ionic conduction, silver particle formation and dissolution, and mechanical integrity of the material. This work highlights the dual nature (simultaneously local and non-local) of electrochemical SPM studies, which should be considered for comprehensive understanding of nanoscale electrochemistry.« less

Controllable construction of flower-like FeS/Fe2O3 composite for lithium storage

NASA Astrophysics Data System (ADS)

Wang, Jie; He, Huan; Wu, Zexing; Liang, Jianing; Han, Lili; Xin, Huolin L.; Guo, Xuyun; Zhu, Ye; Wang, Deli

2018-07-01

Transitions metal sulfides/oxides have been considered as promising anode candidates for next generation lithium-ion batteries (LIBs) due to high theoretical capacities. However, the large volume change during lithiation/delithiation process and poor electronic conductivity often result in a poor charging/discharging performance. Herein, we design a flower-like FeS/Fe2O3 composite via a simple "solvothermal-oxidation" method, in which the Fe2O3 is most distributed on the surface of the flower. The unique porous structure and synergistic effect between FeS and Fe2O3 not only accommodate the large volume expansion, but also facilitate Li ion and electron transport. The Fe2O3 shell effectively reduce the dissolution of Li2Sx during discharge/charge process. When serving as the anode material in lithium ion battery, FeS/Fe2O3 exhibits superior specific capacity, rate capacity and cycling stability compared with pure FeS and Fe2O3.

Humidity effect on nanoscale electrochemistry in solid silver ion conductors and the dual nature of its locality.

PubMed

Yang, Sang Mo; Strelcov, Evgheni; Paranthaman, M Parans; Tselev, Alexander; Noh, Tae Won; Kalinin, Sergei V

2015-02-11

Scanning probe microscopy (SPM) is a powerful tool to investigate electrochemistry in nanoscale volumes. While most SPM-based studies have focused on reactions at the tip-surface junction, charge and mass conservation requires coupled and intrinsically nonlocal cathodic and anodic processes that can be significantly affected by ambient humidity. Here, we explore the role of water in both cathodic and anodic processes, associated charge transport, and topographic volume changes depending on the polarity of tip bias. The first-order reversal curve current-voltage technique combined with simultaneous detection of the sample topography, referred to as FORC-IVz, was applied to a silver solid ion conductor. We found that the protons generated from water affect silver ionic conduction, silver particle formation and dissolution, and mechanical integrity of the material. This work highlights the dual nature (simultaneously local and nonlocal) of electrochemical SPM studies, which should be considered for comprehensive understanding of nanoscale electrochemistry.

Tandem dissolution of UO 3 in amide-based acidic ionic liquid and in situ electrodeposition of UO 2 with regeneration of the ionic liquid: a closed cycle

DOE PAGES

Wanigasekara, Eranda; Freiderich, John W.; Sun, Xiao-Guang; ...

2016-05-19

A closed cycle is demonstrated for the tandem dissolution and electroreduction of UO 3 to UO 2 with regeneration of the acidic ionic liquid. The dissolution is achieved by use of the acidic ionic liquid N,N-dimethylacetimidium bis(trifluoromethanesulfonimide) in 1-ethyl-3-methylimidazolium bis(trifluoromethanesulfonimide) serving as the diluent. Bulk electrolysis performed at 1.0 V vs. Ag reference yields a dark brown-black uranium deposit (UO 2) on the cathode. Anodic oxidation of water in the presence of dimethylacetamide regenerates the acidic ionic liquid. We have demonstrated the individual steps in the cycle together with a sequential dissolution, electroreduction, and regeneration cycle.

Tandem dissolution of UO 3 in amide-based acidic ionic liquid and in situ electrodeposition of UO 2 with regeneration of the ionic liquid: a closed cycle

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wanigasekara, Eranda; Freiderich, John W.; Sun, Xiao-Guang

A closed cycle is demonstrated for the tandem dissolution and electroreduction of UO 3 to UO 2 with regeneration of the acidic ionic liquid. The dissolution is achieved by use of the acidic ionic liquid N,N-dimethylacetimidium bis(trifluoromethanesulfonimide) in 1-ethyl-3-methylimidazolium bis(trifluoromethanesulfonimide) serving as the diluent. Bulk electrolysis performed at 1.0 V vs. Ag reference yields a dark brown-black uranium deposit (UO 2) on the cathode. Anodic oxidation of water in the presence of dimethylacetamide regenerates the acidic ionic liquid. We have demonstrated the individual steps in the cycle together with a sequential dissolution, electroreduction, and regeneration cycle.

Anodic Behavior of the Aluminum Current Collector in Imide-Based Electrolytes: Influence of Solvent, Operating Temperature, and Native Oxide-Layer Thickness.

PubMed

Meister, Paul; Qi, Xin; Kloepsch, Richard; Krämer, Elisabeth; Streipert, Benjamin; Winter, Martin; Placke, Tobias

2017-02-22

The inability of imide salts to form a sufficiently effective passivation layer on aluminum current collectors is one of the main obstacles that limit their broad application in electrochemical energy-storage systems. However, under certain circumstances, the use of electrolytes with imide electrolyte salts in combination with the aluminum current collector is possible. In this contribution, the stability of the aluminum current collector in electrolytes containing either lithium bis(trifluoromethanesulfonyl) imide (LiTFSI) or lithium fluorosulfonyl-(trifluoromethanesulfonyl) imide (LiFTFSI) as conductive salt was investigated by electrochemical techniques, that is, cyclic voltammetry (CV) and chronocoulometry (CC) in either room-temperature ionic liquids or in ethyl methyl sulfone. In particular, the influence of the solvent, operating temperature, and thickness of the native oxide layer of aluminum on the pit formation at the aluminum current collector surface was studied by means of scanning electron microscopy. In general, a more pronounced aluminum dissolution and pit formation was found at elevated temperatures as well as in solvents with a high dielectric constant. An enhanced thickness of the native aluminum oxide layer increases the oxidative stability versus dissolution. Furthermore, we found a different reaction rate depending on dwell time at the upper cut-off potential for aluminum dissolution in TFSI- and FTFSI-based electrolytes during the CC measurements; the use of LiFTFSI facilitated the dissolution of aluminum compared to LiTFSI. Overall, the mechanism of anodic aluminum dissolution is based on: i) the attack of the Al 2 O 3 surface by acidic species and ii) the dissolution of bare aluminum into the electrolyte, which, in turn, is influenced by the electrolyte's dielectric constant. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Hybrid pulse anodization for the fabrication of porous anodic alumina films from commercial purity (99%) aluminum at room temperature.

PubMed

Chung, C K; Zhou, R X; Liu, T Y; Chang, W T

2009-02-04

Most porous anodic alumina (PAA) or anodic aluminum oxide (AAO) films are fabricated using the potentiostatic method from high-purity (99.999%) aluminum films at a low temperature of approximately 0-10 degrees C to avoid dissolution effects at room temperature (RT). In this study, we have demonstrated the fabrication of PAA film from commercial purity (99%) aluminum at RT using a hybrid pulse technique which combines pulse reverse and pulse voltages for the two-step anodization. The reaction mechanism is investigated by the real-time monitoring of current. A possible mechanism of hybrid pulse anodization is proposed for the formation of pronounced nanoporous film at RT. The structure and morphology of the anodic films were greatly influenced by the duration of anodization and the type of voltage. The best result was obtained by first applying pulse reverse voltage and then pulse voltage. The first pulse reverse anodization step was used to form new small cells and pre-texture concave aluminum as a self-assembled mask while the second pulse anodization step was for the resulting PAA film. The diameter of the nanopores in the arrays could reach 30-60 nm.

[Study on electrochemical mechanism of coronary stent used austenitic stainless steel in flowing artificial body fluid].

PubMed

Liang, Chenghao; Guo, Liang; Chen, Wan; Wang, Hua

2005-08-01

The electrochemical mechanism of austenitic stainless steel (SUS316L and SUS317L) coronary stents in flowing artificial body fluid has been investigated with electrochemical technologies. The results indicated that the flowing medium coursed the samples' pitting potential Eb shift negatively, increased the pitting corrosion sensitivity, accelerated its anodic dissolution, but had little effects on repassivated potential. The flowing environment had great effects on cathodic process. The oxygen reaction on the samples' surface became faster as the cathodic process was not controlled by oxygen diffusion but by mixed diffusion and electrochemical process. With the increase of velocity of solution, the pitting corrosion becomes liable to occur under this circumstance.

Performance Enhancement and Side Reactions in Rechargeable Nickel-Iron Batteries with Nanostructured Electrodes.

PubMed

Lei, Danni; Lee, Dong-Chan; Magasinski, Alexandre; Zhao, Enbo; Steingart, Daniel; Yushin, Gleb

2016-01-27

We report for the first time a solution-based synthesis of strongly coupled nanoFe/multiwalled carbon nanotube (MWCNT) and nanoNiO/MWCNT nanocomposite materials for use as anodes and cathodes in rechargeable alkaline Ni-Fe batteries. The produced aqueous batteries demonstrate very high discharge capacities (800 mAh gFe(-1) at 200 mA g(-1) current density), which exceed that of commercial Ni-Fe cells by nearly 1 order of magnitude at comparable current densities. These cells also showed the lack of any "activation", typical in commercial batteries, where low initial capacity slowly increases during the initial 20-50 cycles. The use of a highly conductive MWCNT network allows for high-capacity utilization because of rapid and efficient electron transport to active metal nanoparticles in oxidized [such as Fe(OH)2 or Fe3O4] states. The flexible nature of MWCNTs accommodates significant volume changes taking place during phase transformation accompanying reduction-oxidation reactions in metal electrodes. At the same time, we report and discuss that high surface areas of active nanoparticles lead to multiple side reactions. Dissolution of Fe anodes leads to reprecipitation of significantly larger anode particles. Dissolution of Ni cathodes leads to precipitation of Ni metal on the anode, thus blocking transport of OH(-) anions. The electrolyte molarity and composition have a significant impact on the capacity utilization and cycling stability.

Trends in reactivity of electrodeposited 3d transition metals on gold revealed by operando soft x-ray absorption spectroscopy during water splitting

NASA Astrophysics Data System (ADS)

Velasco-Vélez, J. J.; Jones, Travis E.; Pfeifer, Verena; Dong, Chung-Li; Chen, Yu-Xun; Chen, Chieh-Ming; Chen, Hsin-Yu; Lu, Ying-Rui; Chen, Jin-Ming; Schlögl, R.; Knop-Gericke, A.; Chuang, C.-H.

2017-01-01

We activated gold electrodes for their use as electrocatalyst for water splitting by electrodepositing Cu, Ni and Co. A combination of operando x-ray absorption spectroscopy and potentiometric control under aqueous conditions revealed the trends in reactivity yielded by these electrodes, which are directly associated with the cross- and overpotentials as well as the occupancy of the 3d orbitals. It was found that under anodic polarization the materials electrodeposited on gold suffer from a lack of stability, while under cathodic polarization they exhibit stable behavior. The observed activity is strongly related to the lack of stability shown by these composites under anodic polarization revealing a dynamic process ruled by corrosion. By operando x-ray absorption, we established that the overall enhancement of the activity for the oxygen evolution reaction is directly attributable to the cross-potential and corrosion process of the electrodeposited materials. It is associated with the high potential deposition, which is the origin of the incipient oxidation-corrosion resistance of the lattice. We conclude that the observed trends in the total current are directly associated with the loss of oxygen in the metal-oxide lattice and the subsequent dissolution of metallic ions in the electrolyte under anodic polarization.

Synthesis and characterization of nanoporous anodic oxide film on aluminum in H3PO4 + KMnO4 electrolyte mixture at different anodization conditions

NASA Astrophysics Data System (ADS)

Verma, Naveen; Jindal, Jitender; Singh, Krishan Chander; Mari, Bernabe

2016-04-01

The micro structural properties of nanoporous anodic oxide film formed in H3PO4 were highly influenced by addition of a low concentration of KMnO4 (0.0005 M) in 1 M H3PO4 solution. The KMnO4 as additive enhanced the growth rate of oxide film formation as well as thickness of pore walls. Furthermore the growth rate was found increased with increase in applied current density. The increase in temperature and lack of stirring during anodization causes the thinness of pore wall which leads to increase in pore volume. With the decrease in concentration of H3PO4 in anodizing electrolyte from 1M to 0.3 M, keeping all other conditions constant, the decrease in porosity was observed. This might be due to the dissolution of aluminium oxide film in highly concentrated acidic solution.

Passive films on magnesium anodes in primary batteries

NASA Technical Reports Server (NTRS)

Ratnakumar, B. V.

1988-01-01

The characteristics of the passive films over Mg anodes, which essentially govern the voltage delay of the latter, have been determined nondestructively from an analysis of the transient and steady-state response of the electrode potential to low amplitude galvanostatic polarization under various experimental conditions viz., with different corrosion inhibitor coatings on Mg, after various periods of ageing of anode in solutions containing corrosion inhibitors, at various low temperatures etc. Using these parameters, the kinetics of film build-up or dissolution under these conditions have been monitored. The morphology of the anode film has been verified with scanning electron microscopy. Similar transients at low temperatures point out a steep rise in the film resistivity which is essentially responsible for the severe voltage delay. Finally, possible application of this technique in secondary Li batteries to improve cycling characteristics of the Li anode has been pointed out.

An Insoluble Titanium-Lead Anode for Sulfate Electrolytes

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ferdman, Alla

2005-05-11

The project is devoted to the development of novel insoluble anodes for copper electrowinning and electrolytic manganese dioxide (EMD) production. The anodes are made of titanium-lead composite material produced by techniques of powder metallurgy, compaction of titanium powder, sintering and subsequent lead infiltration. The titanium-lead anode combines beneficial electrochemical behavior of a lead anode with high mechanical properties and corrosion resistance of a titanium anode. In the titanium-lead anode, the titanium stabilizes the lead, preventing it from spalling, and the lead sheathes the titanium, protecting it from passivation. Interconnections between manufacturing process, structure, composition and properties of the titanium-lead compositemore » material were investigated. The material containing 20-30 vol.% of lead had optimal combination of mechanical and electrochemical properties. Optimal process parameters to manufacture the anodes were identified. Prototypes having optimized composition and structure were produced for testing in operating conditions of copper electrowinning and EMD production. Bench-scale, mini-pilot scale and pilot scale tests were performed. The test anodes were of both a plate design and a flow-through cylindrical design. The cylindrical anodes were composed of cylinders containing titanium inner rods and fitting over titanium-lead bushings. The cylindrical design allows the electrolyte to flow through the anode, which enhances diffusion of the electrolyte reactants. The cylindrical anodes demonstrate higher mass transport capabilities and increased electrical efficiency compared to the plate anodes. Copper electrowinning represents the primary target market for the titanium-lead anode. A full-size cylindrical anode performance in copper electrowinning conditions was monitored over a year. The test anode to cathode voltage was stable in the 1.8 to 2.0 volt range. Copper cathode morphology was very smooth and uniform. There was no measurable anode weight loss during this time period. Quantitative chemical analysis of the anode surface showed that the lead content after testing remained at its initial level. No lead dissolution or transfer from the anode to the product occurred.A key benefit of the titanium-lead anode design is that cobalt additions to copper electrolyte should be eliminated. Cobalt is added to the electrolyte to help stabilize the lead oxide surface of conventional lead anodes. The presence of the titanium intimately mixed with the lead should eliminate the need for cobalt stabilization of the lead surface. The anode should last twice as long as the conventional lead anode. Energy savings should be achieved due to minimizing and stabilizing the anode-cathode distance in the electrowinning cells. The anode is easily substitutable into existing tankhouses without a rectifier change.The copper electrowinning test data indicate that the titanium-lead anode is a good candidate for further testing as a possible replacement for a conventional lead anode. A key consideration is the cost. Titanium costs have increased. One of the ways to get the anode cost down is manufacturing the anodes with fewer cylinders. Additional prototypes having different number of cylinders were constructed for a long-term commercial testing in a circuit without cobalt. The objective of the testing is to evaluate the need for cobalt, investigate the effect of decreasing the number of cylinders on the anode performance, and to optimize further the anode design in order to meet the operating requirements, minimize the voltage, maximize the life of the anode, and to balance this against a reasonable cost for the anode. It is anticipated that after testing of the additional prototypes, a whole cell commercial test will be conducted to complete evaluation of the titanium-lead anode costs/benefits.« less

Evaluating the Passivation of Corrosion of API-X100 Steel with Cyclic Voltammetry

NASA Astrophysics Data System (ADS)

Eliyan, Faysal Fayez; Alfantazi, Akram

2017-10-01

In this research, cyclic voltammetry, in oxygen-free low bicarbonate-carbonate solutions, was used to study the corrosion reactions of a high-strength steel, API-X100. With cycles of different scan ranges, the effects of cycling, transpassivation, and cathodic reduction on the electrochemistry of the passive films were analyzed. It was found that carbonate in higher concentrations reduces the anodic activity and the cathodic reactions of the surface. Bicarbonate in small concentrations in solutions that contained low carbonate concentrations catalyzed dissolution and disrupted the formation of the passive films, in reference to the measured anodic currents. From the experiments, there was electrochemical evidence that with more cycles, the passive films were growing thicker, the transpassivation deteriorated the passive films, and during the cathodic reduction, the dissolution was occurring at lower potentials to facilitate later the passivation at higher potentials.

Effect of Hydrogen Charging on the Stress Corrosion Behavior of 2205 Duplex Stainless Steel Under 3.5 wt.% NaCl Thin Electrolyte Layer

NASA Astrophysics Data System (ADS)

Zhao, Tianliang; Liu, Zhiyong; Hu, Shanshan; Du, Cuiwei; Li, Xiaogang

2017-05-01

The effect of hydrogen charging on the stress corrosion cracking (SCC) behavior of 2205 duplex stainless steel (DSS) under 3.5 wt.% NaCl thin electrolyte layer was investigated on precharged samples through hydrogen determination, electrochemical measurement, and slow strain rate tensile test. Results show that hydrogen charging weakens the passive film without inducing any obvious trace of localized anodic dissolution. Therefore, hydrogen charging increases the SCC susceptibility of 2205 DSS mainly through mechanism of hydrogen embrittlement rather than mechanism of localized anodic dissolution. 2205 DSS shows a more susceptibility to hydrogen under the TEL when hydrogen charging current density (HCCD) is between 20 and 50 mA cm-2. The increasing trend is remarkable when hydrogen charging current density increases from 20 to 50 mA cm-2 and fades after 50 mA cm-2.

Analyzing the anodic reactions for iron surface with a porous Al2O3 cluster with the scanning vibrating electrode

NASA Astrophysics Data System (ADS)

Eliyan, Faysal Fayez

2017-09-01

The Scanning Vibrating Electrode Technique (SVET) was used to analyze the anodic reactions inside and around a porous Al2O3 cluster embedded onto an iron foil. The tests were carried out at -0.7 V vs. Saturated Calomel Electrode, in naturally aerated solutions of 0.1, 0.2, 0.35, and 0.5 M bicarbonate concentration. During 10 h of testing, the SVET showed evidence for a formation of a passive film in and around the cluster, in the scanning area shown in the graphical abstract. In the dilute 0.1 and 0.2 M solutions, the passive films formed slower than those in 0.35 and 0.5 M solutions. In the SVET maps, the passive films showed that they could suppress dissolution to currents comparable to those of slower dissolution under the porous Al2O3 cluster.

Fabrication of complete titania nanoporous structures via electrochemical anodization of Ti

PubMed Central

2011-01-01

We present a novel method to fabricate complete and highly oriented anodic titanium oxide (ATO) nano-porous structures with uniform and parallel nanochannels. ATO nano-porous structures are fabricated by anodizing a Ti-foil in two different organic viscous electrolytes at room temperature using a two-step anodizing method. TiO2 nanotubes covered with a few nanometer thin nano-porous layer is produced when the first and the second anodization are carried out in the same electrolyte. However, a complete titania nano-porous (TNP) structures are obtained when the second anodization is conducted in a viscous electrolyte when compared to the first one. TNP structure was attributed to the suppression of F-rich layer dissolution between the cell boundaries in the viscous electrolyte. The structural morphologies were examined by field emission scanning electron microscope. The average pore diameter is approximately 70 nm, while the average inter-pore distance is approximately 130 nm. These TNP structures are useful to fabricate other nanostructure materials and nanodevices. PMID:21711844

First-Principles Modeling of the Initial Stages of Organic Solvent Decomposition on Li xMn 2O 4 (100) Surfaces [First principles modeling of Mn(II) migration to and dissolution from Li xMn 2O 4 (100) surfaces

DOE PAGES

Leung, Kevin

2012-04-13

Density functional theory and ab initio molecular dynamics simulations are applied to investigate the migration of Mn(II) ions to above-surface sites on spinel Li xMn 2O 4 (100) surfaces, the subsequent Mn dissolution into the organic liquid electrolyte, and the detrimental effects on anode solid electrolyte interphase (SEI) passivating films after Mn(II) ions diffuse through the separator. The dissolution mechanism proves complex; the much-quoted Hunter disproportionation of Mn(III) to form Mn(II) is necessary but far from sufficient. Key steps that facilitate Mn(II) ion migration include concerted liquid/solid-state motions, proton-induced weakening of Mn-O bonds forming mobile OH - surface groups; andmore » chemical reactions of adsorbed decomposed organic fragments. Mn(II) lodged between the inorganic Li 2CO 3 and organic lithium ethylene dicarbonate (LEDC) anode SEI component facilitates electrochemical reduction and decomposition of LEDC. These findings help inform future design of protective coatings, electrolytes, additives, and interfaces.« less

Electron transfer processes occurring on platinum neural stimulating electrodes: pulsing experiments for cathodic-first/charge-balanced/biphasic pulses for 0.566 ≤ k ≤ 2.3 in oxygenated and deoxygenated sulfuric acid.

PubMed

Kumsa, Doe W; Montague, Fred W; Hudak, Eric M; Mortimer, J Thomas

2016-10-01

The application of a train of cathodic-first/charge-balanced/biphasic pulses applied to a platinum electrode resulted in a positive creep of the anodic phase potential that increases with increasing charge injection but reaches a steady-state value before 1000 pulses have been delivered. The increase follows from the fact that charge going into irreversible reactions occurring during the anodic phase must equal the charge going into irreversible reactions during the cathodic phase for charge-balanced pulses. In an oxygenated electrolyte the drift of the measured positive potential moved into the platinum oxidation region of the i(V e) profile when the charge injection level exceeds k = 1.75. Platinum dissolution may occur in this region and k = 1.75 defines a boundary between damaging and non-damaging levels on the Shannon Plot. In a very low oxygen environment, the positive potential remained below the platinum oxidation region for the highest charge injection values studied, k = 2.3. The results support the hypothesis that platinum dissolution is the defining factor for the Shannon limit, k = 1.75. Numerous instrumentation issues were encountered in the course of making measurements. The solutions to these issues are provided.

A multiphase interfacial model for the dissolution of spent nuclear fuel

NASA Astrophysics Data System (ADS)

Jerden, James L.; Frey, Kurt; Ebert, William

2015-07-01

The Fuel Matrix Dissolution Model (FMDM) is an electrochemical reaction/diffusion model for the dissolution of spent uranium oxide fuel. The model was developed to provide radionuclide source terms for use in performance assessment calculations for various types of geologic repositories. It is based on mixed potential theory and consists of a two-phase fuel surface made up of UO2 and a noble metal bearing fission product phase in contact with groundwater. The corrosion potential at the surface of the dissolving fuel is calculated by balancing cathodic and anodic reactions occurring at the solution interfaces with UO2 and NMP surfaces. Dissolved oxygen and hydrogen peroxide generated by radiolysis of the groundwater are the major oxidizing agents that promote fuel dissolution. Several reactions occurring on noble metal alloy surfaces are electrically coupled to the UO2 and can catalyze or inhibit oxidative dissolution of the fuel. The most important of these is the oxidation of hydrogen, which counteracts the effects of oxidants (primarily H2O2 and O2). Inclusion of this reaction greatly decreases the oxidation of U(IV) and slows fuel dissolution significantly. In addition to radiolytic hydrogen, large quantities of hydrogen can be produced by the anoxic corrosion of steel structures within and near the fuel waste package. The model accurately predicts key experimental trends seen in literature data, the most important being the dramatic depression of the fuel dissolution rate by the presence of dissolved hydrogen at even relatively low concentrations (e.g., less than 1 mM). This hydrogen effect counteracts oxidation reactions and can limit fuel degradation to chemical dissolution, which results in radionuclide source term values that are four or five orders of magnitude lower than when oxidative dissolution processes are operative. This paper presents the scientific basis of the model, the approach for modeling used fuel in a disposal system, and preliminary calculations to demonstrate the application and value of the model.

The effect of current reversal on coated titanium electrodes

NASA Astrophysics Data System (ADS)

Elnathan, Francis

Coated titanium electrodes have applications in the electrochemical industry, including water treatment and swimming pool chlorination. Current/polarity reverse electrolysis is a technique used for "self-cleaning" of the coated titanium anodes employed in water disinfection and treatment. However, the literature holds very little information about the effects of polarity reversal on these anodes. The present work appears to be the first to investigate coated titanium anodes in polarity reversal in a systematic method. Two commercial titanium electrodes (RuTi and IrTa) were studied. Polarity reversal was the main electrochemical technique employing a current density of 1200 A/m 2, except when current density was studied. The effects of NO 3-, SO42-, ClO4 -, HPO42-, CO32-, Mg2+ and Ca2+ on electrode lifetime were examined. Analysis of the electrochemical results showed that plateau time (tau p), for gas evolution, is highly important to the lifetime of the coated titanium anodes. The effects of three electrolysis variables on the coated titanium anode life were examined. Current density was observed to have an inverse relationship with anode life while reversal cycle time had a direct relation with lifetime. NaCl concentration had no discernible effect. In general, the RuTi electrode exhibited longer lifetimes than IrTa except for a few specific conditions. The influence of the concentration of five anions (NO3-, SO42-, ClO 4-, HPO42-, and CO3 2-) was determined. Changing the composition and concentration of anions affected the lifetimes of the two electrodes, especially nitrate, hydrogen phosphate and carbonate. The lifetime of IrTa was highest in nitrate, and increased as a function of nitrate concentration. The service life of RuTi was highest in hydrogen phosphate, and increased with increasing hydrogen phosphate concentration. Lifetime of both anodes decreased with increasing carbonate ions. The effects of Mg2+ and Ca2+ on electrode lifetime were examined with three anions (NO3-, HPO42-, ClO4-) electrolytes. While there were numerous effects and interactions between Mg2+ or Ca2+ and anions on lifetime, these effects were found to mainly affect the amount of time the electrodes spent in the charging and discharging reactions. The times related to gas evolution (which is the plateau time, tau p) were found to be strikingly similar. The charging times (tau C) which are related to adsorption and desorption of species were not also any significantly different. Coating dissolution, substrate and/or coating passivation mechanisms were identified as being responsible for coated titanium anode failure in current reverse and hard water electrolysis. IrTa is believed to have failed predominantly by the dissolution mechanism in nitrate, hydrogen phosphate and perchlorate. RuTi failed predominantly by substrate and/or coating passivation in hydrogen phosphate, nitrate and carbonate. Anode failure is believed to be the result of plateau (taup) and charging (tauC)reactions occurring at the coating/electrolyte and/or substrate/coating interface. The tau p and tauC are useful determinants for the process of anode failure.

Method for providing uranium articles with a corrosion resistant anodized coating

DOEpatents

Waldrop, Forrest B.; Washington, Charles A.

1982-01-01

Uranium articles are provided with anodized oxide coatings in an aqueous solution of an electrolyte selected from the group consisting of potassium phosphate, potassium hydroxide, ammonium hydroxide, and a mixture of potassium tetraborate and boric acid. The uranium articles are anodized at a temperature greater than about 75.degree. C. with a current flow of less than about 0.036 A/cm.sup.2 of surface area while the pH of the solution is maintained in a range of about 2 to 11.5. The pH values of the aqueous solution and the low current density utilized during the electrolysis prevent excessive dissolution of the uranium and porosity in the film or watering. The relatively high temperature of the electrolyte bath inhibits hydration and the attendant deleterious pitting so as to enhance corrosion resistance of the anodized coating.

Alumina-coated and manganese monoxide embedded 3D carbon derived from avocado as high-performance anode for lithium-ion batteries

NASA Astrophysics Data System (ADS)

rehman, Wasif ur; Xu, Youlong; Du, Xianfeng; Sun, Xiaofei; Ullah, Inam; Zhang, Yuan; Jin, Yanling; Zhang, Baofeng; Li, Xifei

2018-07-01

Derived from avocado fruit, a three dimension (3D) carbon is prepared via a hydrothermal/pyrolysis process followed by embedding with MnO nanoparticles by a wet chemical method and coating with Al2O3 through an atomic layer deposition technique. The obtained material presents a hierarchical structure that MnO nanocrystals wrapped in 3D carbon and then encapsulated in a uniform Al2O3 layer with a thickness of about 5 nm. Benefiting from this hierarchical structure in which 3D carbon offers numerous electronic pathways to enhance the conductivity and Al2O3 nanolayer provide a shelter to keep away from dissolution of Mn4+ and volume changes during charge/discharge process. This material (marked as C/MnO@Al2O3) has exhibited high rate performance and excellent cyclability as an anode for lithium ion batteries. A high specific capacity of about 600 mA h g-1 is achieved at a current density of 1000 mA g-1 and the electrode can still deliver a high specific capacity of about 1165 mA h g-1 at 150 mA g-1 after 100 cycles. These results facilitate a green and high potential of anode materials towards promising devices for advance performance of lithium-ion batteries.

Self-Formed Hybrid Interphase Layer on Lithium Metal for High-Performance Lithium-Sulfur Batteries.

PubMed

Li, Guoxing; Huang, Qingquan; He, Xin; Gao, Yue; Wang, Daiwei; Kim, Seong H; Wang, Donghai

2018-02-27

Lithium-sulfur (Li-S) batteries are promising candidates for high-energy storage devices due to high theoretical capacities of both the sulfur cathode and lithium (Li) metal anode. Considerable efforts have been devoted to improving sulfur cathodes. However, issues associated with Li anodes, such as low Coulombic efficiency (CE) and growth of Li dendrites, remain unsolved due to unstable solid-electrolyte interphase (SEI) and lead to poor capacity retention and a short cycling life of Li-S batteries. In this work, we demonstrate a facile and effective approach to fabricate a flexible and robust hybrid SEI layer through co-deposition of aromatic-based organosulfides and inorganic Li salts using poly(sulfur-random-1,3-diisopropenylbenzene) as an additive in an electrolyte. The aromatic-based organic components with planar backbone conformation and π-π interaction in the SEI layers can improve the toughness and flexibility to promote stable and high efficient Li deposition/dissolution. The as-formed durable SEI layer can inhibit dendritic Li growth, enhance Li deposition/dissolution CE (99.1% over 420 cycles), and in turn enable Li-S batteries with good cycling stability (1000 cycles) and slow capacity decay. This work demonstrates a route to address the issues associated with Li metal anodes and promote the development of high-energy rechargeable Li metal batteries.

The anodizing behavior of aluminum in malonic acid solution and morphology of the anodic films

NASA Astrophysics Data System (ADS)

Ren, Jianjun; Zuo, Yu

2012-11-01

The anodizing behavior of aluminum in malonic acid solution and morphology of the anodic films were studied. The voltage-time response for galvanostatic anodization of aluminum in malonic acid solution exhibits a conventional three-stage feature but the formation voltage is much higher. With the increase of electrolyte concentration, the electrolyte viscosity increases simultaneously and the high viscosity decreases the film growth rate. With the concentration increase of the malonic acid electrolyte, the critical current density that initiates local "burning" on the sample surface decreases. For malonic acid anodization, the field-assisted dissolution on the oxide surface is relatively weak and the nucleation of pores is more difficult, which results in greater barrier layer thickness and larger cell dimension. The embryo of the porous structure of anodic film has been created within the linear region of the first transient stage, and the definite porous structure has been established before the end of the first transient stage. The self-ordering behavior of the porous film is influenced by the electrolyte concentration, film thickness and the applied current density. Great current density not only improves the cell arrangement order but also brings about larger cell dimension.

Method for providing uranium articles with a corrosion-resistant anodized coating

DOEpatents

Waldrop, F.B.; Washington, C.A.

1981-01-07

Uranium articles are provided with anodized oxide coatings in an aqueous solution of an electrolyte selected from the group consisting of potassium phosphate, potassium hydroxide, ammonium hydroxide, and a mixture of potassium tetraborate and boric acid. The uranium articles are anodized at a temperature greater than about 75/sup 0/C with a current flow of less than about 0.036 A/cm/sup 2/ of surface area while the pH of the solution is maintained in a range of about 2 to 11.5. The pH values of the aqueous solution and the low current density utilized during the electrolysis prevent excessive dissolution of the uranium and porosity in the film or watering. The relatively high temperature of the electrolyte bath inhibits hydration and the attendant deleterious pitting so as to enhance corrosion resistance of the anodized coating.

Double-walled structure of anodic TiO2 nanotubes in H3PO4/NH4F mixed electrolyte

NASA Astrophysics Data System (ADS)

Chen, Siyu; Chen, Ying; Li, Chengyuan; Ouyang, Huijun; Qin, Shuai; Song, Ye

2018-04-01

Normally, the well-ordered anodic TiO2 nanotubes (ATNTs) are obtained in NH4F electrolyte, after annealing, the double-walled structure of nanotubes will appear. Here, after adding H3PO4 into NHF4 electrolyte, we got the double-walled structure of nanotubes by anodizing without annealing, which means the direct existence of anion-contaminated layer in ATNTs. Influence of H3PO4 content on anodizing voltage and morphology of ATNTs were compared in detail. The XRD pattern illustrated that the crystallinity decreases with increasing H3PO4 concentration, and the anion-contaminated layer thickens with the increase of H3PO4 concentration. Meanwhile, the existence of the anion-contaminated layer also proved the limitations of the filed-assisted dissolution theory, while the double-walled structure can be explained by oxygen bubble model and plastic flow model.

Phenomenological Transition of an Aluminum Surface in an Ionic Liquid and Its Beneficial Implementation in Batteries.

PubMed

Shvartsev, B; Gelman, D; Amram, D; Ein-Eli, Y

2015-12-29

Aluminum (Al) electrochemical dissolution in organic nonaqueous media and room temperature ionic liquids (RTILs) is partially hampered by the presence of a native oxide. In this work, Al activation in EMIm(HF)2.3F RTIL is reported. It was confirmed that as a result of the interaction of Al with the RTIL, a new film is formed instead of the pristine oxide layer. Aluminum surface modifications result in a transformation from a passive state to the active behavior of the metal. This was confirmed via the employment of electrochemical methods and characterization by XPS, AFM, and TEM. It was shown that the pristine oxide surface film dissolves in EMIm(HF)2.3F, allowing an Al-O-F layer to be formed instead. This newly built up layer dramatically restricts Al corrosion while enabling high rates of Al anodic dissolution. These beneficial features allow the implementation of Al as an anode in advanced portable power sources, such as aluminum-air batteries.

Effects of natural organic matter properties on the dissolution kinetics of zinc oxide nanoparticles

USGS Publications Warehouse

Jiang, Chuanjia; Aiken, George R.; Hsu-Kim, Heileen

2015-01-01

The dissolution of zinc oxide (ZnO) nanoparticles (NPs) is a key step of controlling their environmental fate, bioavailability, and toxicity. Rates of dissolution often depend upon factors such as interactions of NPs with natural organic matter (NOM). We examined the effects of 16 different NOM isolates on the dissolution kinetics of ZnO NPs in buffered potassium chloride solution using anodic stripping voltammetry to directly measure dissolved zinc concentrations. The observed dissolution rate constants (kobs) and dissolved zinc concentrations at equilibrium increased linearly with NOM concentration (from 0 to 40 mg C L–1) for Suwannee River humic and fulvic acids and Pony Lake fulvic acid. When dissolution rates were compared for the 16 NOM isolates, kobs was positively correlated with certain properties of NOM, including specific ultraviolet absorbance (SUVA), aromatic and carbonyl carbon contents, and molecular weight. Dissolution rate constants were negatively correlated to hydrogen/carbon ratio and aliphatic carbon content. The observed correlations indicate that aromatic carbon content is a key factor in determining the rate of NOM-promoted dissolution of ZnO NPs. The findings of this study facilitate a better understanding of the fate of ZnO NPs in organic-rich aquatic environments and highlight SUVA as a facile and useful indicator of NOM interactions with metal-based nanoparticles.

Visualizing elemental deposition patterns on carbonaceous anodes from lithium ion batteries: A laser ablation-inductively coupled plasma-mass spectrometry study on factors influencing the deposition of lithium, nickel, manganese and cobalt after dissolution and migration from the Li1[Ni1/3Mn1/3Co1/3]O2 and LiMn1.5 Ni0.5O4 cathode

NASA Astrophysics Data System (ADS)

Schwieters, Timo; Evertz, Marco; Fengler, Alexander; Börner, Markus; Dagger, Tim; Stenzel, Yannick; Harte, Patrick; Winter, Martin; Nowak, Sascha

2018-03-01

In this study, laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) is applied to previously aged carbonaceous anodes from lithium ion batteries (LIBs). These electrodes are treated by cyclic aging in a lithium ion cell set-up against Li1[Ni1/3Mn 1/3Co1/3]O2 = NMC111 to elucidate factors that influence transition metal dissolution (TMD) of the cathode and subsequent deposition on the anode. The investigations are carried out by qualitatively visualizing the 7Li and TM patterns (60Ni, 55Mn and 59Co) of whole coin and pouch-bag electrodes. The lithium, as well as the TM amount, found on the anode, is directly correlated to the applied upper cut-off voltage (4.6, 4.7, 4.8 and 4.9 V) showing more deposition of Li and TMs at elevated voltages. While 7Li shows a more homogeneous pattern, the TM distribution is inhomogeneous but showing a similar pattern for all TMs of the same sample. An unequal pressure distribution, resulting in a nonparallel electrode alignment, on the electrode stack is identified to be responsible for the inhomogeneous TM deposition pattern. This uneven electrode orientation results in different diffusion pathways for the TM migration with regard to the spatial distances.

Molten salt bath circulation design for an electrolytic cell

DOEpatents

Dawless, Robert K.; LaCamera, Alfred F.; Troup, R. Lee; Ray, Siba P.; Hosler, Robert B.

1999-01-01

An electrolytic cell for reduction of a metal oxide to a metal and oxygen has an inert anode and an upwardly angled roof covering the inert mode. The angled roof diverts oxygen bubbles into an upcomer channel, thereby agitating a molten salt bath in the upcomer channel and improving dissolution of a metal oxide in the molten salt bath. The molten salt bath has a lower velocity adjacent the inert anode in order to minimize corrosion by substances in the bath. A particularly preferred cell produces aluminum by electrolysis of alumina in a molten salt bath containing aluminum fluoride and sodium fluoride.

Hydrogen-facilitated corrosion and stress corrosion cracking of austenitic stainless steel of type 310

DOE Office of Scientific and Technical Information (OSTI.GOV)

Qiao Lijie; Chu Wuyang; Miao Huijun

1993-04-01

The effects of hydrogen precharge and stress on anodic dissolution for Type 310 austenitic stainless steel (ASS) have been investigated. An experiment determining the effect of hydrogen on stress corrosion cracking (SCC) was carried out in a boiling 42% MgCl[sub 2] solution and in a 2.5 mol/l H[sub 2]SO[sub 4] + 1 mol/l HCl solution. The results showed that both hydrogen and stress would increase the dissolution rate, and the effects of hydrogen and stress on the dissolution rate were synergistic rather than simply additive. Hydrogen lowered the threshold stress and the shortened fracture time of SCC in a boilingmore » MgCl[sub 2] solution by a factor of 1/5 and 10, respectively.« less

Asymmetrical interfacial reactions of Ni/SAC101(NiIn)/Ni solder joint induced by current stressing

NASA Astrophysics Data System (ADS)

Lin, Chen-Yi; Chiu, Tsung-Chieh; Lin, Kwang-Lung

2018-03-01

An electric current can asymmetrically trigger either atomic migration or interfacial reactions between a cathode and an anode. The present study investigated the dissolution of metallization and formation of an interfacial intermetallic compound (IMC) in the Cu/Ni/Sn1.0Ag0.1Cu0.02Ni0.05In/Ni/Cu solder joint at various current densities in the order of 103 A/cm2 at temperatures ranging from 100 °C to 150 °C. The polarization behavior of Ni dissolution and IMC formation under current stressing were systematically investigated. The asymmetrical interfacial reactions of the solder joint were found to be greatly influenced by ambient temperature. The dissolution of Ni and its effect on interfacial IMC formation were also discussed.

Anodized titanium and stainless steel in contact with CFRP: an electrochemical approach considering galvanic corrosion.

PubMed

Mueller, Yves; Tognini, Roger; Mayer, Joerg; Virtanen, Sannakaisa

2007-09-15

The combination of different materials in an implant gives the opportunity to better fulfill the requirements that are needed to improve the healing process. However, using different materials increases the risk of galvanic coupling corrosion. In this study, coupling effects of gold-anodized titanium, stainless steel for biomedical applications, carbon fiber reinforced polyetheretherketone (CFRP), and CFRP containing tantalum fibers are investigated electrochemically and by long-term immersion experiments in simulated body fluid (SBF). Potentiodynamic polarization experiments (i/E curves) and electrochemical impedance spectroscopy (EIS) of the separated materials showed a passive behavior of the metallic samples. Anodized titanium showed no corrosion attacks, whereas stainless steel is highly susceptibility for localized corrosion. On the other side, an active dissolution behavior of both of the CFRPs in the given environment could be determined, leading to delaminating of the carbon fibers from the matrix. Long-term immersion experiments were carried out using a set-up especially developed to simulate coupling conditions of a point contact fixator system (PC-Fix) in a biological environment. Electrochemical data were acquired in situ during the whole immersion time. The results of the immersion experiments correlate with the findings of the electrochemical investigation. Localized corrosion attacks were found on stainless steel, whereas anodized titanium showed no corrosion attacks. No significant differences between the two CFRP types could be found. Galvanic coupling corrosion in combination with crevice conditions and possible corrosion mechanisms are discussed. Copyright 2007 Wiley Periodicals, Inc.

Self-Formed Hybrid Interphase Layer on Lithium Metal for High-Performance Lithium–Sulfur Batteries

DOE Office of Scientific and Technical Information (OSTI.GOV)

Li, Guoxing; Huang, Qingquan; He, Xin

Lithium–sulfur (Li–S) batteries are promising candidates for high-energy storage devices due to high theoretical capacities of both the sulfur cathode and lithium (Li) metal anode. Considerable efforts have been devoted to improving sulfur cathodes. However, issues associated with Li anodes, such as low Coulombic efficiency (CE) and growth of Li dendrites, remain unsolved due to unstable solid-electrolyte interphase (SEI) and lead to poor capacity retention and a short cycling life of Li–S batteries. In this paper, we demonstrate a facile and effective approach to fabricate a flexible and robust hybrid SEI layer through co-deposition of aromatic-based organosulfides and inorganic Limore » salts using poly(sulfur-random-1,3-diisopropenylbenzene) as an additive in an electrolyte. The aromatic-based organic components with planar backbone conformation and π–π interaction in the SEI layers can improve the toughness and flexibility to promote stable and high efficient Li deposition/dissolution. The as-formed durable SEI layer can inhibit dendritic Li growth, enhance Li deposition/dissolution CE (99.1% over 420 cycles), and in turn enable Li–S batteries with good cycling stability (1000 cycles) and slow capacity decay. Finally, this work demonstrates a route to address the issues associated with Li metal anodes and promote the development of high-energy rechargeable Li metal batteries.« less

Self-Formed Hybrid Interphase Layer on Lithium Metal for High-Performance Lithium–Sulfur Batteries

DOE PAGES

Li, Guoxing; Huang, Qingquan; He, Xin; ...

2018-01-29

Lithium–sulfur (Li–S) batteries are promising candidates for high-energy storage devices due to high theoretical capacities of both the sulfur cathode and lithium (Li) metal anode. Considerable efforts have been devoted to improving sulfur cathodes. However, issues associated with Li anodes, such as low Coulombic efficiency (CE) and growth of Li dendrites, remain unsolved due to unstable solid-electrolyte interphase (SEI) and lead to poor capacity retention and a short cycling life of Li–S batteries. In this paper, we demonstrate a facile and effective approach to fabricate a flexible and robust hybrid SEI layer through co-deposition of aromatic-based organosulfides and inorganic Limore » salts using poly(sulfur-random-1,3-diisopropenylbenzene) as an additive in an electrolyte. The aromatic-based organic components with planar backbone conformation and π–π interaction in the SEI layers can improve the toughness and flexibility to promote stable and high efficient Li deposition/dissolution. The as-formed durable SEI layer can inhibit dendritic Li growth, enhance Li deposition/dissolution CE (99.1% over 420 cycles), and in turn enable Li–S batteries with good cycling stability (1000 cycles) and slow capacity decay. Finally, this work demonstrates a route to address the issues associated with Li metal anodes and promote the development of high-energy rechargeable Li metal batteries.« less

Dissolution and characterization of HEV NiMH batteries.

PubMed

Larsson, Kristian; Ekberg, Christian; Ødegaard-Jensen, Arvid

2013-03-01

Metal recovery is an essential part of the recycling of hybrid electric vehicle battery waste and the first step in a hydrometallurgical treatment is dissolution of the solid material. The properties of separated battery electrode materials were investigated. Focus was put on both the solid waste and then the dissolution behaviour. The cathode contains metallic nickel that remains undissolved when utilizing non-oxidizing conditions such as hydrochloric or sulphuric acid in combination with a low oxygen atmosphere. In these conditions the cathode active electrode material is fully dissolved. Not dissolving the nickel metal saves up to 37% of the acid consumption for the cathode electrode material. In the commonly used case of oxidizing conditions the nickel metal dissolves and a cobalt-rich phase remains undissolved from the cathode active material. For the anode material a complete and rapid dissolution can be achieved at mild conditions with hydrochloric, nitric or sulphuric acid. Optimal parameters for all cases of dissolution was pH 1 with a reaction time of approximately ≥ 20,000 s. Copyright © 2012 Elsevier Ltd. All rights reserved.

Corrosion fatigue studies on a bulk glassy Zr-based alloy under three-point bending

NASA Astrophysics Data System (ADS)

Grell, Daniel; Wilkin, Yannic; Gostin, Petre F.; Gebert, Annett; Kerscher, Eberhard

2016-12-01

Corrosion fatigue (CF) tests were carried out on bulk glassy Zr52.5Cu17.9Al10Ni14.6Ti5 (Vitreloy 105) samples under load-controlled three-point bending conditions with a load ratio of R = 0.1 in 0.01 M Na2SO4 + 0.01 M NaCl electrolyte. During cyclic testing, the bar-shaped specimens were polarized in situ at constant potentials and the current was monitored. Three different anodic potentials within the interval between the pitting potential EP and the repassivation potential ER, and three different load amplitudes were applied. In some cases, in situ microscopic observations revealed the formation of black corrosion products in the vicinity of the crack tip during anodic polarization. Fractographic analysis revealed a clear distinction between two modes of crack growth characterized by smooth dissolution induced regions on the one hand and slim fast fracture areas on the other hand. Both alternating features contributed to a broad striated corrosion fatigue fracture surface. Moreover, further fatigue tests were carried out under free corrosion conditions yielding additional information on crack initiation and crack propagation period by means of the open circuit potential (OCP) changes. Thereby, a slight increase in OCP was detected after rupture of the passive layer due to bare metal exposed to the electrolyte. The electrochemical response increased continuously according to stable crack propagation until fracture occurred. Finally, the fracture surfaces of the corrosion fatigue samples were investigated by energy dispersive X-ray with the objective of analyzing the elemental distribution after anodic dissolution. Interestingly, anodic polarization at a near repassivation potential of -50 mV vs. SCE (Saturated Calomel Electrode, E = 0.241 V vs. SHE, Standard Hydrogen Electrode) led to favorable effects on the fatigue lifetime. In conclusion, all results are conflated to a corrosion fatigue model for bulk glassy Vitreloy 105 under anodic polarization in chloride-containing electrolyte and compared to the previously proposed stress corrosion mechanisms under similar conditions.

Enhancing long-term photostability of BiVO4 photoanodes for solar water splitting by tuning electrolyte composition

NASA Astrophysics Data System (ADS)

Lee, Dong Ki; Choi, Kyoung-Shin

2018-01-01

As the performance of photoelectrodes used for solar water splitting continues to improve, enhancing the long-term stability of the photoelectrodes becomes an increasingly crucial issue. In this study, we report that tuning the composition of the electrolyte can be used as a strategy to suppress photocorrosion during solar water splitting. Anodic photocorrosion of BiVO4 photoanodes involves the loss of V5+ from the BiVO4 lattice by dissolution. We demonstrate that the use of a V5+-saturated electrolyte, which inhibits the photooxidation-coupled dissolution of BiVO4, can serve as a simple yet effective method to suppress anodic photocorrosion of BiVO4. The V5+ species in the solution can also incorporate into the FeOOH/NiOOH oxygen-evolution catalyst layer present on the BiVO4 surface during water oxidation, further enhancing water-oxidation kinetics. The effect of the V5+ species in the electrolyte on both the long-term photostability of BiVO4 and the performance of the FeOOH/NiOOH oxygen-evolution catalyst layer is systematically elucidated.

Molten salt bath circulation design for an electrolytic cell

DOEpatents

Dawless, R.K.; LaCamera, A.F.; Troup, R.L.; Ray, S.P.; Hosler, R.B.

1999-08-17

An electrolytic cell for reduction of a metal oxide to a metal and oxygen has an inert anode and an upwardly angled roof covering the inert mode. The angled roof diverts oxygen bubbles into an upcomer channel, thereby agitating a molten salt bath in the upcomer channel and improving dissolution of a metal oxide in the molten salt bath. The molten salt bath has a lower velocity adjacent the inert anode in order to minimize corrosion by substances in the bath. A particularly preferred cell produces aluminum by electrolysis of alumina in a molten salt bath containing aluminum fluoride and sodium fluoride. 4 figs.

[Complex technology for water and wastewater disinfection and its industrial realization in prototype unit].

PubMed

Arakcheev, E N; Brunman, V E; Brunman, M V; Konyashin, A V; Dyachenko, V A; Petkova, A P

Usage of complex automated electrolysis unit for drinking water disinfection and wastewater oxidation and coagulation is scoped, its ecological and energy efficiency is shown. Properties of technological process of anolyte production using membrane electrolysis of brine for water disinfection in municipal pipelines and potassium ferrate production using electrochemical dissolution of iron anode in NaOH solution for usage in purification plants are listed. Construction of modules of industrial prototype for anolyte and ferrate production and applied aspects of automation of complex electrolysis unit are proved. Results of approbation of electrolytic potassium ferrate for drinking water disinfection and wastewater, rain water and environmental water oxidation and coagulation are shown.

Al-Air Batteries: Fundamental Thermodynamic Limitations from First-Principles Theory.

PubMed

Chen, Leanne D; Nørskov, Jens K; Luntz, Alan C

2015-01-02

The Al-air battery possesses high theoretical specific energy (4140 W h/kg) and is therefore an attractive candidate for vehicle propulsion. However, the experimentally observed open-circuit potential is much lower than what bulk thermodynamics predicts, and this potential loss is typically attributed to corrosion. Similarly, large Tafel slopes associated with the battery are assumed to be due to film formation. We present a detailed thermodynamic study of the Al-air battery using density functional theory. The results suggest that the maximum open-circuit potential of the Al anode is only -1.87 V versus the standard hydrogen electrode at pH 14.6 instead of the traditionally assumed -2.34 V and that large Tafel slopes are inherent in the electrochemistry. These deviations from the bulk thermodynamics are intrinsic to the electrochemical surface processes that define Al anodic dissolution. This has contributions from both asymmetry in multielectron transfers and, more importantly, a large chemical stabilization inherent to the formation of bulk Al(OH)3 from surface intermediates. These are fundamental limitations that cannot be improved even if corrosion and film effects are completely suppressed.

Long-term behaviour of solid oxide fuel cell interconnect materials in contact with Ni-mesh during exposure in simulated anode gas at 700 and 800 °C

NASA Astrophysics Data System (ADS)

Garcia-Fresnillo, L.; Shemet, V.; Chyrkin, A.; de Haart, L. G. J.; Quadakkers, W. J.

2014-12-01

In the present study the long-term behaviour of two ferritic steels, Crofer 22 APU and Crofer 22H, in contact with a Ni-mesh during exposure in simulated anode gas, Ar-4%H2-2%H2O, at 700 and 800 °C for exposure times up to 3000 h was investigated. Ni diffusion from the Ni-mesh into the steel resulted in the formation of an austenitic zone whereas diffusion of iron and chromium from the steel into the Ni-mesh resulted in the formation of chromia base oxides in the Ni-mesh. Depending on the chemical composition of the steel, the temperature and the exposure time, interdiffusion processes between ferritic steel and Ni-mesh also resulted in σ-phase formation at the austenite-ferrite interface and in Laves-phase dissolution in the austenitic zone. The extent and morphology of the σ-phase formation are discussed on the basis of thermodynamic considerations, including reaction paths in the ternary alloy system Fe-Ni-Cr.

Enhancing Near Zero Volt Storage Tolerance of Lithium-ion Batteries

NASA Astrophysics Data System (ADS)

Crompton, Kyle R.

There are inherent safety risks associated with inactive lithium ion batteries leading to greater restrictions and regulations on shipping and storage. Maintaining all cells of a lithium ion battery at near zero voltage with an applied fixed resistive load is one promising approach which can lessen (and potentially eliminate) the risk of a lithium ion battery entering thermal runaway when in an inactive state. However, in a conventional lithium ion cell, a near zero cell voltage can be damaging if the anode electrochemical potential increases to greater than the potential where dissolution of the standard copper current collector occurs (i.e. 3.1 V vs. Li/Li+ at room temperature). Past approaches to yield lithium ion cells that are resilient to a near zero volt state of charge involve use of secondary active materials or alternative current collectors which have anticipated tradeoffs in terms of cell performance and cost. In the the present dissertation work the approach of managing the amount of reversible lithium in a cell during construction to prevent the anode potential from increasing to greater than 3.1 V vs. Li/Li+ during near zero volt storage is introduced. Anode pre-lithiation was used in LiCoO 2/MCMB pouch cells to appropriately manage the amount of reversible lithium so that there is excess reversible lithium compared to the cathodes intercalation capacity (reversible lithium excess cell or RLE cell). RLE LiCoO 2/MCMB cells maintained 99% of their original capacity after three, 3-day and three, 7-day storage periods at near zero volts under fixed load. A LiCoO2/MCMB pouch cell fabricated with a pre-lithiated anode also maintained its original discharge performance after three, 3-day storage periods under fixed load at 45°C. The strong recharge performance after near zero volt storage is attributed to the anode potential remaining below the copper dissolution potential during near zero volt storage as informed by reference electrode measurements. Pulse discharge measurements were performed and show that double layer capacitance likely plays a major role in determining the behavior of electrode potentials during near zero volt storage. To further the viability of the anode pre-lithiation method in LiCoO2/MCMB cells, stabilization coatings on the cathode materials are being investigated to increase the tolerance of the cathode to the low potentials it may experience during near zero volt storage of an RLE lithium ion cell. Results show that an AlPO4 coating prevents cation exhange in the cathode crystal structure and substantially increases the cathode's resilience to low electrochemical potentials. Investigations into applying anode pre-lithiation to cells utilizing LiNiCoAlO2 (NCA) cathodes have also been initiated and found to maintain the anode potential below the copper dissolution potential during near zero volt storage. RLE NCA/MCMB cells showed strong recharge performance and improved rate capability retention over a conventional NCA/MCMB cell after ten, 3-day near zero volt storage periods. Scale up of reversible lithium management to NCA/MCMB x3450 pouch cells was achieved using bath lithium addition and rendered a cell that retained 100% of its discharge performance after a 14 day period at near zero volts under fixed load. The near zero volt storage tolerance of lithium ion cells utilizing an advanced, high energy density lithium rich cathode material (0.49Li2MnO3˙0.51LiNi 0.37Co0.24Mn0.39O2 or HE5050) has also been studied and found to be high at room temperature without the need for anode pre-lithiation. HE5050/MCMB cells maintained 100% of their discharge capacity after five, 3-day and five, 7-day near zero volt storage periods at room temperature. HE5050/MCMB also maintained 99% of their discharge capacity after two, 3-day near zero volt storage periods at 40°C. The high first cycle loss and lower intercalation potential of the HE5050 cathode lead to the anode potential remaining <2.8 V vs. Li/Li+ during near zero volt storage and as such, no copper dissolution is expected to be occurring. Finally, Carbon Nanotube (CNT) papers have been shown to be stable up to high potentials vs. Li/Li+ and thus, using them as an anode current collector in place of standard copper can generate lithium ion cells that can tolerate near zero volt storage. However, CNT papers suffer from significant irreversible loss due to their high surface area. An Al2O3 coating deposited by atomic layer deposition is investigated for its effect in reducing the irreversible losses of a CNT paper. The Al2O3 coating was found to reduce irreversible loss by 55% over 50 cycles and still serve as an effective current collector for a graphitic anode composite.

Transpassive Dissolution of Copper and Rapid Formation of Brilliant Colored Copper Oxide Films

NASA Astrophysics Data System (ADS)

Fredj, Narjes; Burleigh, T. David; New Mexico Tech Team

2014-03-01

This investigation describes an electrochemical technique for growing adhesive copper oxide films on copper with attractive colors ranging from gold-brown to pearl with intermediate colors from red violet to gold green. The technique consists of anodically dissolving copper at transpassive potentials in hot sodium hydroxide, and then depositing brilliant color films of Cu2O onto the surface of copper after the anodic potential has been turned off. The color of the copper oxide film depends on the temperature, the anodic potential, the time t1 of polarization, and the time t2, which is the time of immersion after potential has been turned off. The brilliant colored films were characterized using glancing angle x-ray diffraction, and the film was found to be primarily Cu2O. Cyclic voltammetry, chronopotentiometry, scanning electron microscopy, and x-ray photoelectron spectroscopy were also used to characterize these films.

Comparative studies of thin film growth on aluminium by AFM, TEM and GDOES characterization

NASA Astrophysics Data System (ADS)

Qi, Jiantao; Thompson, George E.

2016-07-01

In this present study, comparative studies of trivalent chromium conversion coating formation, associated with aluminium dissolution process, have been investigated using atomic force microscopy (AFM), transmission electron microscopy (TEM) and glow-discharge optical emission spectroscopy (GDOES). High-resolution electron micrographs revealed the evident and uniform coating initiation on the whole surface after conversion treatment for only 30 s, although a network of metal ridges was created by HF etching pre-treatment. In terms of conversion treatment process on electropolished aluminium, constant kinetics of coating growth, ∼0.30 ± 0.2 nm/s, were found after the prolonged conversion treatment for 600 s. The availability of electrolyte anions for coating deposition determined the growth process. Simultaneously, a proceeding process of aluminium dissolution during conversion treatment, of ∼0.11 ± 0.02 nm/s, was found for the first time, indicating constant kinetics of anodic reactions. The distinct process of aluminium consumption was assigned with loss of corrosion protection of the deposited coating material as evidenced in the electrochemical impedance spectroscopy. Based on the present data, a new mechanism of coating growth on aluminium was proposed, and it consisted of an activation period (0-30 s), a linear growth period (0.30 nm/s, up for 600 s) and limited growth period (0.17 nm/s, 600-1200 s). In addition, the air-drying post-treatment and a high-vacuum environment in the microscope revealed a coating shrinkage, especially in the coatings after conversion treatments for longer time.

Electrical neurostimulation with imbalanced waveform mitigates dissolution of platinum electrodes

PubMed Central

Kumsa, Doe; Hudak, Eric M; Montague, Fred W; Kelley, Shawn C; Untereker, Darrel F; Hahn, Benjamin P; Condit, Chris; Cholette, Martin; Lee, Hyowon; Bardot, Dawn; Takmakov, Pavel

2017-01-01

Objective Electrical neurostimulation has traditionally been limited to the use of charge-balanced waveforms. Charge-imbalanced and monophasic waveforms are not used to deliver clinical therapy, because it is believed that these stimulation paradigms may generate noxious electrochemical species that cause tissue damage. Approach In this study, we investigated the dissolution of platinum as one of such irreversible reactions over a range of charge densities up to 160 µC cm−2 with current-controlled first phase, capacitive discharge second phase waveforms of both cathodic-first and anodic-first polarity. We monitored the concentration of platinum in solution under different stimulation delivery conditions including charge-balanced, charge-imbalanced, and monophasic pulses. Main results We observed that platinum dissolution decreased during charge-imbalanced and monophasic stimulation when compared to charge-balanced waveforms. Significance This observation provides an opportunity to re-evaluate the charge-balanced waveform as the primary option for sustainable neural stimulation. PMID:27650936

Recovery of Metal Values from Spent Zinc-Carbon Dry Cell Batteries

NASA Astrophysics Data System (ADS)

Khan, Majharul Haque; Gulshan, Fahmida; Kurny, A. S. W.

2013-04-01

Spent zinc-carbon dry cell batteries were characterized in the process of recovery of metal values. Zinc, manganese and steel were the major metallic materials constituting 63 % of the weight of spent batteries. Different components of the spent batteries were separately processed to extract the metallic values. A maximum of 92 % of total amount of zinc contained in the anodes could be extracted with a purity of over 99.0 % from the anodes by heating at 600 °C for 10 min in presence of 12 % NH4Cl flux. Spent electrolyte paste containing manganese and zinc as major metallic elements, was leached in sulfuric acid solution in presence of hydrogen peroxide as a reducing agent. The optimum condition for leaching was found to be concentration of sulfuric acid: 2.5 M, concentration of hydrogen peroxide: 10 %, temperature: 60 °C, stirring speed: 600 rpm and solid/liquid ratio 1:12. A maximum of 88 % manganese contained in the paste could be dissolved within 27 min of leaching under the optimized conditions. Dissolution of zinc under the same conditions was 97 %. A maximum of 69.89 % of manganese and 83.29 % of zinc contained in the leach liquor could be precipitated in the form of manganese carbonate and zinc oxalate.

Polymer nanoimprinting using an anodized aluminum mold for structural coloration

NASA Astrophysics Data System (ADS)

Kikuchi, Tatsuya; Nishinaga, Osamu; Natsui, Shungo; Suzuki, Ryosuke O.

2015-06-01

Polymer nanoimprinting of submicrometer-scale dimple arrays with structural coloration was demonstrated. Highly ordered aluminum dimple arrays measuring 530-670 nm in diameter were formed on an aluminum substrate via etidronic acid anodizing at 210-270 V and subsequent anodic oxide dissolution. The nanostructured aluminum surface led to bright structural coloration with a rainbow spectrum, and the reflected wavelength strongly depends on the angle of the specimen and the period of the dimple array. The reflection peak shifts gradually with the dimple diameter toward longer wavelength, reaching 800 nm in wavelength at 670 nm in diameter. The shape of the aluminum dimple arrays were successfully transferred to a mercapto-ester ultra-violet curable polymer via self-assembled monolayer coating and polymer replications using a nanoimprinting technique. The nanostructured polymer surfaces with positively and negatively shaped dimple arrays also exhibited structural coloration based on the periodic nanostructure, and reflected light mostly in the visible region, 400-800 nm. This nanostructuring with structural coloration can be easily realized by simple techniques such as anodizing, SAM coating, and nanoimprinting.

Innovative approach for the valorization of useful metals from waste electric and electronic equipment (WEEE)

NASA Astrophysics Data System (ADS)

Soare, V.; Burada, M.; Dumitrescu, D. V.; Constantin, I.; Soare, V.; Popescu, A.-M. J.; Carcea, I.

2016-08-01

Waste electric and electronic equipment are an important secondary source of rare and precious metals and their processing through ecological technologies constitutes a major concern in the European Union and significantly contributes to the reduction of environmental pollution and to the preservation of valuable resources of nonferrous metals. The paper presents an innovative approach for the complex valorization of useful metals contained in WEEE. The method consists in the melting of WEEE in a furnace in a microwave field at temperatures of 1000 ÷1200°C, for the complete separation of the metallic fraction from the organic components. The gases resulting from the melting process were also treated/neutralized in a microwave environment and the obtained metallic bulk (multi-component alloy) was processed through combined hydrometallurgical and electrochemical methods. The major elements in the metallic bulk (Cu, Sn, Zn, Pb) were separated/recovered by anodic dissolution, respectively by leaching in nitric acid followed by cementation using various agents, or by electrodeposition. Depending on the electrochemical parameters, cathodic deposits consisting of Cu, with a purity higher than 99.9%, or of Cu-Sn and Cu-Sn-Zn alloys were obtained. Silver was valorized by leaching/precipitation with NaCl and the gold concentrated in the anodic slime will be recovered by thiourea extraction. The experiments performed demonstrate the possibility of ecological and efficient processing of WEEE in a microwave field and the recovery of nonferrous and precious metals through combined hydrometallurgical and electrochemical methods.

Formation and Entrapment of Tris(8-hydroxyquinoline)aluminum from 8-Hydroxyquinoline in Anodic Porous Alumina

PubMed Central

Yamaguchi, Shohei; Matsui, Kazunori

2016-01-01

The formation and entrapment of tris(8-hydroxyquinoline)aluminum (Alq3) molecules on the surface of anodic porous alumina (APA) immersed in an ethanol solution of 8-hydroxyquinoline (HQ) were investigated by absorption, fluorescence, and Raman spectroscopies. The effects of the selected APA preparation conditions (galvanostatic or potentiostatic anodization method, anodizing current and voltage values, one- or two-step anodizing process, and sulfuric acid electrolyte concentration) on the adsorption and desorption of Alq3 species were examined. Among the listed parameters, sulfuric acid concentration was the most important factor in determining the Alq3 adsorption characteristics. The Alq3 content measured after desorption under galvanostatic conditions was 2.5 times larger than that obtained under potentiostatic ones, regardless of the adsorbed quantities. The obtained results suggest the existence of at least two types of adsorption sites on the APA surface characterized by different magnitudes of the Alq3 bonding strength. The related fluorescence spectra contained two peaks at wavelengths of 480 and 505 nm, which could be attributed to isolated Alq3 species inside nanovoids and aggregated Alq3 clusters in the pores of APA, respectively. The former species were attached to the adsorption sites with higher binding energies, whereas the latter ones were bound to the APA surface more weakly. Similar results were obtained for the Alq3 species formed from the HQ solution, which quantitatively exceeded the number of the Alq3 species adsorbed from the Alq3 solution. Alq3 molecules were formed in the HQ solution during the reaction of HQ molecules with the Al3+ ions in the oxide dissolution zone near the oxide/electrolyte interface through the cracks and the Al3+ ions adsorbed on surface of pore and cracks. In addition, it was suggested that HQ molecules could penetrate the nanovoids more easily than Alq3 species because of their smaller sizes, which resulted in higher magnitudes of the adsorption. PMID:28773840

Electrolysis of a molten semiconductor

PubMed Central

Yin, Huayi; Chung, Brice; Sadoway, Donald R.

2016-01-01

Metals cannot be extracted by electrolysis of transition-metal sulfides because as liquids they are semiconductors, which exhibit high levels of electronic conduction and metal dissolution. Herein by introduction of a distinct secondary electrolyte, we reveal a high-throughput electro-desulfurization process that directly converts semiconducting molten stibnite (Sb2S3) into pure (99.9%) liquid antimony and sulfur vapour. At the bottom of the cell liquid antimony pools beneath cathodically polarized molten stibnite. At the top of the cell sulfur issues from a carbon anode immersed in an immiscible secondary molten salt electrolyte disposed above molten stibnite, thereby blocking electronic shorting across the cell. As opposed to conventional extraction practices, direct sulfide electrolysis completely avoids generation of problematic fugitive emissions (CO2, CO and SO2), significantly reduces energy consumption, increases productivity in a single-step process (lower capital and operating costs) and is broadly applicable to a host of electronically conductive transition-metal chalcogenides. PMID:27553525

Electricity generation from bio-treatment of sewage sludge with microbial fuel cell.

PubMed

Jiang, Junqiu; Zhao, Qingliang; Zhang, Jinna; Zhang, Guodong; Lee, Duu-Jong

2009-12-01

A two-chambered microbial fuel cell (MFC) with potassium ferricyanide as its electron acceptor was utilized to degrade excess sewage sludge and to generate electricity. Stable electrical power was produced continuously during operation for 250 h. Total chemical oxygen demand (TCOD) of sludge was reduced by 46.4% when an initial TCOD was 10,850 mg/l. The MFC power output did not significantly depend on process parameters such as substrate concentration, cathode catholyte concentration, and anodic pH. However, the MFC produced power was in close correlation with the soluble chemical oxygen demand (SCOD) of sludge. Furthermore, ultrasonic pretreatment of sludge accelerated organic matter dissolution and, hence, TCOD removal rate in the MFC was increased, but power output was insignificantly enhanced. This study demonstrates that this MFC can generate electricity from sewage sludge over a wide range of process parameters.

Electrolysis of a molten semiconductor.

PubMed

Yin, Huayi; Chung, Brice; Sadoway, Donald R

2016-08-24

Metals cannot be extracted by electrolysis of transition-metal sulfides because as liquids they are semiconductors, which exhibit high levels of electronic conduction and metal dissolution. Herein by introduction of a distinct secondary electrolyte, we reveal a high-throughput electro-desulfurization process that directly converts semiconducting molten stibnite (Sb2S3) into pure (99.9%) liquid antimony and sulfur vapour. At the bottom of the cell liquid antimony pools beneath cathodically polarized molten stibnite. At the top of the cell sulfur issues from a carbon anode immersed in an immiscible secondary molten salt electrolyte disposed above molten stibnite, thereby blocking electronic shorting across the cell. As opposed to conventional extraction practices, direct sulfide electrolysis completely avoids generation of problematic fugitive emissions (CO2, CO and SO2), significantly reduces energy consumption, increases productivity in a single-step process (lower capital and operating costs) and is broadly applicable to a host of electronically conductive transition-metal chalcogenides.

Electrolysis of a molten semiconductor

NASA Astrophysics Data System (ADS)

Yin, Huayi; Chung, Brice; Sadoway, Donald R.

2016-08-01

Metals cannot be extracted by electrolysis of transition-metal sulfides because as liquids they are semiconductors, which exhibit high levels of electronic conduction and metal dissolution. Herein by introduction of a distinct secondary electrolyte, we reveal a high-throughput electro-desulfurization process that directly converts semiconducting molten stibnite (Sb2S3) into pure (99.9%) liquid antimony and sulfur vapour. At the bottom of the cell liquid antimony pools beneath cathodically polarized molten stibnite. At the top of the cell sulfur issues from a carbon anode immersed in an immiscible secondary molten salt electrolyte disposed above molten stibnite, thereby blocking electronic shorting across the cell. As opposed to conventional extraction practices, direct sulfide electrolysis completely avoids generation of problematic fugitive emissions (CO2, CO and SO2), significantly reduces energy consumption, increases productivity in a single-step process (lower capital and operating costs) and is broadly applicable to a host of electronically conductive transition-metal chalcogenides.

Assessment of capacitor electrodes for intracortical neural stimulation.

PubMed

Rose, T L; Kelliher, E M; Robblee, L S

1985-01-01

Capacitor electrodes offer the potential for the safest method of stimulation of neural tissue because they operate without any faradaic process occurring at the electrode-electrolyte interface. Their use eliminates problems associated with metal dissolution or water electrolysis which may occur with electrodes of noble metals. This paper reviews recent work aimed at increasing the charge storage density of capacitor electrodes to allow their application with the small areas of 10(-4) mm2 required for intracortical stimulation of single neurons. Increased charge storage with electrodes using anodic films such as TiO2 and Ta2O5 has been obtained by increasing the real surface area of microelectrodes. Experiments have also been done with BaTiO3 films which have a much higher dielectric constant than the anodic film dielectrics. State-of-the-art electrodes made with these materials, however, have a charge storage density which at best is comparable to that obtained with Pt and is considerably lower than electrochemically safe charge densities that have been reported for activated Ir. It is concluded that for very small intracortical electrodes, capacitor electrodes will not be competitive with electrodes which operate using surface localized faradaic reactions.

Research progress in formation mechanism of anodizing aluminum oxide

NASA Astrophysics Data System (ADS)

Lv, Yudong

2017-12-01

The self-ordering porous anodizing aluminum oxide (AAO) has attracted much attention because of its potential value of application. Valve metals (Al, Ti, Zr etc.) anodic studies have been conducted for more than 80 years, but the mechanism of the formation of hexagonal prismatic cell structure has so far been different. In this paper, the research results of AAO film formation mechanism are reviewed, and the growth models of several AAO films are summarized, including the field-assisted dissolution (FAD), the viscous flow model, the critical current density effect model, the bulk expansion stress model and the steady-state pore growth model and so on. It analyzed the principle of each model and its rationality. This paper will be of great help to reveal the nature of pore formation and self-ordering, and with the hope that through the study of AAO film formation mechanism, the specific effects of various oxidation parameters on AAO film morphology can be obtained.

Formation of TiO2 nanotube arrays in KOH added fluoride-ethylene glycol (EG) electrolyte and its photoelectrochemical response

NASA Astrophysics Data System (ADS)

Nyein, Nyein; Lockman, Zainovia; Matsuda, Astunori; Kawamura, Go; Tan, Wai Kian; Oo, Than Zaw

2016-07-01

In this study, highly ordered TiO2 nanotube arrays were prepared by anodic oxidation of titanium foil in fluoride -EG electrolyte containing a small amount of potassium hydroxide, KOH at 60 V for 30 min. This electrolyte resulted in the formation of long nanotubes with an average length of 10 µm and diameter of 170 nm. For comparison, TiO2 nanotubes anodized in H2O added EG electrolyte which produces short nanotubes with an average tube length of 5 µm and diameter of 170 nm. It appears that the addition of KOH into the fluoride EG electrolyte accelerated the formation of the TiO2 nanotubes as it is believed that the chemical dissolution at the tips of the nanotubes is suppressed. Highly ordered TiO2 nanotubes anodized in KOH added EG electrolyte exhibited the photocurrent density of 2 mA/cm2, which is significantly higher than H2O added sample (1.5 mA/cm2).

Visible light to electrical energy conversion using photoelectrochemical cells

NASA Technical Reports Server (NTRS)

Wrighton, Mark S. (Inventor); Ellis, Arthur B. (Inventor); Kaiser, Steven W. (Inventor)

1983-01-01

Sustained conversion of low energy visible or near i.r. light (>1.25 eV) to electrical energy has been obtained using wet photoelectrochemical cells where there are no net chemical changes in the system. Stabilization of n-type semi-conductor anodes of CdS, CdSe, CdTe, GaP, GaAs and InP to photoanodic dissolution is achieved by employing selected alkaline solutions of Na.sub.2 S, Na.sub.2 S/S, Na.sub.2 Se, Na.sub.2 Se/Se, Na.sub.2 Te and Na.sub.2 Te/Te as the electrolyte. The oxidation of (poly) sulfide, (poly)selenide or (poly)telluride species occurs at the irradiated anode, and reduction of polysulfide, polyselenide or polytelluride species occurs at the dark Pt cathode of the photoelectrochemical cell. Optical to electrical energy conversion efficiencies approaching 15% at selected frequencies have been observed in some cells. The wavelength for the onset of photocurrent corresponds to the band gap of the particular anode material used in the cell.

Length-dependent corrosion behavior, Ni2+ release, cytocompatibility, and antibacterial ability of Ni-Ti-O nanopores anodically grown on biomedical NiTi alloy.

PubMed

Hang, Ruiqiang; Liu, Yanlian; Bai, Long; Zhang, Xiangyu; Huang, Xiaobo; Jia, Husheng; Tang, Bin

2018-08-01

In the present work, nickel-titanium-oxygen nanopores with different length (0.55-114 μm) were anodically grown on nearly equiatomic nickel-titanium (NiTi) alloy. Length-dependent corrosion behavior, nickel ion (Ni 2+ ) release, cytocompatibility, and antibacterial ability were investigated by electrochemical, analytical chemistry, and biological methods. The results show constructing nanoporous structure on the NiTi alloy improve its corrosion resistance. However, the anodized samples release more Ni 2+ than that of the bare NiTi alloy, suggesting chemical dissolution of the nanopores rather than electrochemical corrosion governs the Ni 2+ release. In addition, the Ni 2+ release amount increases with nanopore length. The anodized samples show good cytocompatibility when the nanopore length is <11 μm. Encouragingly, the length scale covers the one (1-11 μm) that the nanopores showing favorable antibacterial ability. Consequently, the nanopores with length in the range of 1-11 μm are promising as coatings of biomedical NiTi alloy for anti-infection, drug delivery, and other desirable applications. Copyright © 2018 Elsevier B.V. All rights reserved.

Heterogeneous WS x/WO 3 thorn-bush nanofiber electrodes for sodium-ion batteries

DOE PAGES

Ryu, Won -Hee; Wilson, Hope; Sohn, Sungwoo; ...

2016-01-25

Heterogeneous electrode materials with hierarchical architectures promise to enable considerable improvement in future energy storage devices. In this study, we report on a tailored synthetic strategy used to create heterogeneous tungsten sulfide/oxide core–shell nanofiber materials with vertically and randomly aligned thorn-bush features, and we evaluate them as potential anode materials for high-performance Na-ion batteries. The WS x (2 ≤ x ≤ 3, amorphous WS 3 and crystalline WS 2) nanofiber is successfully prepared by electrospinning and subsequent calcination in a reducing atmosphere. To prevent capacity degradation of the WS x anodes originating from sulfur dissolution, a facile post-thermal treatment inmore » air is applied to form an oxide passivation surface. Interestingly, WO 3 thorn bundles are randomly grown on the nanofiber stem, resulting from the surface conversion. We elucidate the evolving morphological and structural features of the nanofibers during post-thermal treatment. The heterogeneous thorn-bush nanofiber electrodes deliver a high second discharge capacity of 791 mAh g –1 and improved cycle performance for 100 cycles compared to the pristine WS x nanofiber. Lastly, we show that this hierarchical design is effective in reducing sulfur dissolution, as shown by cycling analysis with counter Na electrodes.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shkrob, Ilya A.; Pupek, Krzysztof Z.; Gilbert, James A.

Lithium hexafluorophosphate (LiPF 6) is ubiquitous in commercial lithium-ion batteries, but it is hydrolytically unstable and corrosive on electrode surfaces. Using a more stable salt would confer multiple benefits for high-voltage operation, but many such electrolyte systems facilitate anodic dissolution and pitting corrosion of aluminum current collectors that negate their advantages. Lithium 2-trifluoromethyl-4,5-dicyanoimidazolide (LiTDI) is a new salt that was designed specifically for high-voltage cells. In this study we demonstrate that in carbonate electrolytes, LiTDI prevents anodic dissolution of Al current collectors, which places it into a select group of corrosion inhibitors. However, we also demonstrate that LiTDI becomes reducedmore » on lithiated graphite, undergoing sequential defluorination and yielding a thick and resistive solid-electrolyte interphase (SEI), which increases impedance and lowers electrode capacity. The mechanistic causes for this behavior are examined using computational chemistry methods in the light of recent spectroscopic studies. Here, we demonstrate that LiTDI reduction can be prevented by certain electrolyte additives, which include fluoroethylene carbonate, vinylene carbonate and lithium bis(oxalato)borate. This beneficial action is due to preferential reduction of these additives over LiTDI at a higher potential vs. Li/Li +, so the resulting SEI can prevent the direct reduction of LiTDI at lower potentials on the graphite electrode.« less

Preparation and characterization of ultraflat Pt facets by atom-height-resolved differential optical microscopy

NASA Astrophysics Data System (ADS)

Azhagurajan, M.; Wen, R.; Kim, Y. G.; Itoh, T.; Sashikata, K.; Itaya, K.

2015-01-01

We recently demonstrated that improvements to our technique, laser confocal microscopy with differential interference microscopy (LCM-DIM), has rendered it fully capable of resolving monatomic steps with heights of ca. 0.25 nm on Au(111) and Pd(111) surfaces, even as low as 0.14 nm on Si(100), in aqueous solution. In this paper, we describe in detail a method to prepare and characterize, via atomic-layer-resolved LCM-DIM, ultraflat Pt(111) and Pt(100) facets over a wide surface area. The preparation of ultraflat surfaces is important in the characterization at the atomic scale of electrochemical processes under reaction conditions. To showcase the elegance of LCM-DIM, the anodic dissolution of Pt in aqueous HCl is briefly recounted.

Experience with soluble neutron poisons for criticality control at ICPP

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wilson, R.E.; Mortimer, S.R.

1978-01-01

Soluble neutron poisons assure criticality control in two of the headend fuel reprocessing systems at the Idaho Chemical Processing Plant. Soluble poisons have been used successfully since 1964 and will be employed in the projected new headend processes. The use of soluble poisons (1) greatly increases the process output (2) allows versatility in the size of fuel assemblies processed and (3) allows the practical reprocessing of some fuels. The safety limit for all fluids entering the U-Zr alloy dissolver is 3.6 g/liter boron. To allow for possible deviations in the measurement systems and drift between analytical sampling periods, the standardmore » practice is to use 3.85 g/liter boron as the lower limit. This dissolver has had 4000 successful hours of operation using soluble poisons. The electrolytic dissolution process depends on soluble gadolinium for criticality safety. This system is used to process high enriched uranium clad in stainless steel. Electrolytic dissolution takes advantage of the anodic corrosion that occurs when a large electrical current is passed through the fuel elements in a corrosive environment. Three control methods are used on each headend system. First, the poison is mixed according to standard operating procedures and the measurements are affirmed by the operator's supervisor. Second, the poisoned solution is stirred, sampled, analyzed, and the analysis reported while still in the mix tank. Finally, a Nuclear Poison Detection System (NPDS) must show an acceptable poison concentration before the solution can be transferred. The major disadvantage of using soluble poisons is the need for very sophisticated control systems and procedures, which require extensive checkout. The need for a poisoned primary heating and cooling system means a secondary system is needed as well. Experience has shown, however, that production enhancement more than makes up for the problems.« less

Carbon Disulfide Cosolvent Electrolytes for High-Performance Lithium Sulfur Batteries.

PubMed

Gu, Sui; Wen, Zhaoyin; Qian, Rong; Jin, Jun; Wang, Qingsong; Wu, Meifen; Zhuo, Shangjun

2016-12-21

Development of lithium sulfur (Li-S) batteries with high Coulombic efficiency and long cycle stability remains challenging due to the dissolution and shuttle of polysulfides in electrolyte. Here, a novel additive, carbon disulfide (CS 2 ), to the organic electrolyte is reported to improve the cycling performance of Li-S batteries. The cells with the CS 2 -additive electrolyte exhibit high Coulombic efficiency and long cycle stability, showing average Coulombic efficiency >99% and a capacity retention of 88% over the entire 300 cycles. The function of the CS 2 additive is 2-fold: (1) it inhibits the migration of long-chain polysulfides to the anode by forming complexes with polysulfides and (2) it passivates electrode surfaces by inducing the protective coatings on both the anode and the cathode.

Nuclear fuel electrorefiner

DOEpatents

Ahluwalia, Rajesh K.; Hua, Thanh Q.

2004-02-10

The present invention relates to a nuclear fuel electrorefiner having a vessel containing a molten electrolyte pool floating on top of a cadmium pool. An anodic fuel dissolution basket and a high-efficiency cathode are suspended in the molten electrolyte pool. A shroud surrounds the fuel dissolution basket and the shroud is positioned so as to separate the electrolyte pool into an isolated electrolyte pool within the shroud and a bulk electrolyte pool outside the shroud. In operation, unwanted noble-metal fission products migrate downward into the cadmium pool and form precipitates where they are removed by a filter and separator assembly. Uranium values are transported by the cadmium pool from the isolated electrolyte pool to the bulk electrolyte pool, and then pass to the high-efficiency cathode where they are electrolytically deposited thereto.

Research on rechargeable oxygen electrodes

NASA Technical Reports Server (NTRS)

Giner, J.; Malachesky, P. A.; Holleck, G.

1971-01-01

Studies were carried out on a number of factors which may influence the behavior of the platinum electrocatalyst of oxygen electrodes for use in rechargeable metal-oxygen batteries or hydrogen-oxygen fuel cells. The effects of pretreatments for various potentials and added ionic species, which could be present in such systems, were studied with reguard to: (1) the state of surface oxidation, (2) platinum dissolution, (3) the kinetics of oxygen evolution and reduction (including the role of hydrogen peroxide), and (4) changes in porous electrode structure. These studies were carried out on smooth platinum, platinized platinum, and Teflon-bonded platinum black electrodes in carefully purified electrolyte solutions. The main factors which appear to affect rechargeable oxygen electrode performance and life are: (1) the buildup of a refractory anodic layer on extended cycling, and (2) the dissolution of platinum.

Very Large Arrays of Bipolar Electrodes

DTIC Science & Technology

2013-01-01

two driving electrodes and a simple power supply. The system was designed to have faradic reactions occurring at the cathode end of each electrode...related to sensing chemistry present at the cathode end. Accordingly, a series of experiments was designed to determine the amount of current passing...reduction reaction occurs at the cathodic end of the BPE, it triggers the oxidation and dissolution of Ag metal present at the anodic pole. The loss of Ag

Electro-kinetic remediation coupled with phytoremediation to remove lead, arsenic and cesium from contaminated paddy soil

PubMed Central

Mao, Xinyu; Han, Fengxiang X.; Shao, Xiaohou; Guo, Kai; McComb, Jacqueline; Arslan, Zikri; Zhang, Zhanyu

2017-01-01

The objectives of this study were to investigate distribution and solubility of Pb, Cs and As in soils under electrokinetic field and examine the processes of coupled electrokinetic phytoremediation of polluted soils. The elevated bioavailability and bioaccumulation of Pb, As and Cs in paddy soil under an electrokinetic field (EKF) were studied. The results show that the EKF treatment is effective on lowering soil pH to around 1.5 near the anode which is beneficial for the dissolution of metal(loid)s, thus increasing their overall solubility. The acidification in the anode soil efficiently increased the water soluble (SOL) and exchangeable (EXC) Pb, As and Cs, implying enhanced solubility and elevated overall potential bioavailability in the anode region while lower solubility in the cathode areas. Bioaccumulations of Pb, As and Cs were largely determined by the nature of elements, loading levels and EKF treatment. The native Pb in soil usually is not bioavailable. However, EKF treatment tends to transfer Pb to the SOL and EXC fractions improving the phytoextraction efficiency. Similarly, EKF transferred more EXC As and Cs to the SOL fraction significantly increasing their bioaccumulation in plant roots and shoots. Pb and As were accumulated more in plant roots than in shoots while Cs was accumulated more in shoots due to its similarity of chemical properties to potassium. Indian mustard, spinach and cabbage are good accumulators for Cs. Translocation of Pb, As and Cs from plant roots to shoots were enhanced by EKF. However, this study indicated the overall low phytoextraction efficiency of these plants. PMID:26650421

Water oxidation by size selected Co 27 clusters supported on Fe 2O 3

DOE PAGES

Pellin, Michael J.; Riha, Shannon C.; Tyo, Eric C.; ...

2016-09-22

The complexity of the water oxidation reaction makes understanding the role of individual catalytic sites critical to improving the process. Here, size-selected 27-atom cobalt clusters (Co 27) deposited on hematite (Fe 2O 3) anodes were tested for water oxidation activity. The uniformity of these anodes allows measurement of the activity of catalytic sites of well-defined nuclearity and known density. Grazing incidence X-ray absorption near-edge spectroscopy (GIXANES) characterization of the anodes before and after electrochemical cycling demonstrates that these Co 27 clusters are stable to dissolution even in the harsh water oxidation electrochemical environment. They are also stable under illumination atmore » the equivalent of 0.4suns irradiation. The clusters show turnover rates for water oxidation that are comparable or higher than those reported for Pd- and Co-based materials or for hematite. The support for the Co 27 clusters is Fe 2O 3 grown by atomic layer deposition on a Si chip. We have chosen to deposit a Fe2O3 layer that is only a few unit cells thick (2nm), to remove complications related to exciton diffusion. We find that the electrocatalytic and the photoelectrocatalytic activity of the Co 27/Fe 2O 3 material is significantly improved when the samples are annealed (with the clusters already deposited). Lastly, given that the support is thin and that the cluster deposition density is equivalent to approximately 5% of an atomic monolayer, we suggest that annealing may significantly improve the exciton diffusion from the support to the catalytic moiety.« less

Antibacterial activity of microstructured sacrificial anode thin films by combination of silver with platinum group elements (platinum, palladium, iridium).

PubMed

Köller, Manfred; Bellova, Petri; Javid, Siyamak Memar; Motemani, Yahya; Khare, Chinmay; Sengstock, Christina; Tschulik, Kristina; Schildhauer, Thomas A; Ludwig, Alfred

2017-05-01

Five different Ag dots arrays (16 to 400dots/mm 2 ) were fabricated on a continuous platinum, palladium, or iridium thin film and for comparison also on titanium film by sputter deposition and photolithographic patterning. To analyze the antibacterial activity of these microstructured films Staphylococcus aureus (S. aureus) were placed onto the array surfaces and cultivated overnight. To analyze the viability of planktonic as well as surface adherent bacteria, the applied bacterial fluid was subsequently aspirated, plated on blood agar plates and adherent bacteria were detected by fluorescence microscopy. A particular antibacterial effect towards S. aureus was induced by Ag dot arrays on each of the platinum group thin film (sacrificial anode system for Ag) in contrast to Ag dot arrays fabricated on the Ti thin films (non-sacrificial anode system for Ag). Among platinum group elements the Ir-Ag system exerted the highest antibacterial activity which was accompanied by most advanced dissolution of the Ag dots and Ag ion release compared to Ag dots on Pt or Pd. Copyright © 2016 Elsevier B.V. All rights reserved.

Can CO-tolerant Anodes be Economically Viable for PEMFC Applications with Reformates?

DOE PAGES

He, P.; Zhang, Y.; Ye., S.; ...

2014-10-05

Several years ago, the answer to this question was negative based on the criteria for an anode with <0.1 mg cm-2 of platinum group metals to perform similarly without and with 50 ppm CO in hydrogen proton exchange membrane fuel cells (PEMFCs). Now, with the amount of CO impurities reduced to 10 ppm in reformates, a <1% performance loss with a 1.5% air-bleed has become a reasonable target. The CO-tolerant catalyst also needs to be dissolution resistant up to 0.93 V, viz., the potential experienced at the anode during startup and shutdown of the fuel cells. We recently demonstrated ourmore » ability to simultaneously enhance activity and stability by using single crystalline Ru@Pt core-shell nanocatalysts. Here, we report that the performance target with reformates was met using bilayer-thick Ru@Pt core-shell nanocatalysts with 0.047 mg cm-2 Pt and 0.024 mg cm-2 Ru loading, supporting a positive prognosis for the economically viable use of reformates in PEMFC applications.« less

Investigation of Ruthenium Dissolution in Advanced Membrane Electrode Assemblies for Direct Methanol Based Fuel Cell Stacks

NASA Technical Reports Server (NTRS)

Valdez, Thomas I.; Firdosy, S.; Koel, B. E.; Narayanan, S. R.

2005-01-01

Dissolution of ruthenium was observed in the 80-cell stack. Duration testing was performed in single cell MEAs to determine the pathway of cell degradation. EDAX analysis on each of the single cell MEAs has shown that the Johnson Matthey commercial catalyst is stable in DMFC operation for 250 hours, no ruthenium dissolution was observed. Changes in the hydrophobicity of the cathode backing papers was minimum. Electrode polarization analysis revealed that the MEA performance loss is attributed to changes in the cathode catalyst layer. Ruthenium migration does not seem to occur during cell operation but can occur when methanol is absent from the anode compartment, the cathode compartment has access to air, and the cells in the stack are electrically connected to a load (Shunt Currents). The open-to-air cathode stack design allowed for: a) The MEAs to have continual access to oxygen; and b) The stack to sustain shunt currents. Ruthenium dissolution in a DMFC stack can be prevented by: a) Developing an internally manifolded stacks that seal reactant compartments when not in operation; b) Bringing the cell voltages to zero quickly when not in operation; and c) Limiting the total number of cells to 25 in an effort to limit shunt currents.

Mechanical Properties of TRIP Steel Microalloyed with Ti

NASA Astrophysics Data System (ADS)

Krizan, Daniel; De Cooman, Bruno C.

2014-07-01

The precipitation state, microstructure, retained austenite stability, and mechanical properties of cold-rolled Ti-microalloyed CMnAlSiP TRIP steel were investigated. The precipitation state was analyzed in each processing step by means of transmission electron microscopy, chemical analysis using the anodic dissolution method, and by model calculations. Ti additions refined the microstructure mainly by the pinning of austenite and ferrite grain boundaries by various Ti-containing precipitates. Ti additions also resulted in a refinement of the size of the retained austenite islands and caused a slight decrease of the volume fraction and carbon content of the retained austenite. The morphology of the retained austenite was also changed and the stability of the retained austenite decreased, but Ti addition still resulted in an adequate strength-ductility balance and a tensile strength close to 1 GPa.

Electrochemical characterization of p(+)n and n(+)p diffused InP structures

NASA Technical Reports Server (NTRS)

Wilt, David M.; Faur, Maria; Faur, Mircea; Goradia, M.; Vargas-Aburto, Carlos

1993-01-01

The relatively well documented and widely used electrolytes for characterization and processing of Si and GaAs-related materials and structures by electrochemical methods are of little or no use with InP because the electrolytes presently used either dissolve the surface preferentially at the defect areas or form residual oxides and introduce a large density of surface states. Using an electrolyte which was newly developed for anodic dissolution of InP, and was named the 'FAP' electrolyte, accurate characterization of InP related structures including nature and density of surface states, defect density, and net majority carrier concentration, all as functions of depth was performed. A step-by-step optimization of n(+)p and p(+)n InP structures made by thermal diffusion was done using the electrochemical techniques, and resulted in high performance homojunction InP structures.

Effects of substrate microstructure on the formation of oriented oxide nanotube arrays on Ti and Ti alloys

NASA Astrophysics Data System (ADS)

Ferreira, C. P.; Gonçalves, M. C.; Caram, R.; Bertazzoli, R.; Rodrigues, C. A.

2013-11-01

The formation of nanotubular oxide layers on Ti and Ti alloys has been widely investigated for the photocatalytic degradation of organic compounds due to their excellent catalytic efficiency, chemical stability, and low cost and toxicity. Aiming to improve the photocatalytic efficiency of this nanostructured oxide, this work investigated the influence of substrate grain size on the growth of nanotubular oxide layers. Ti and Ti alloys (Ti-6Al, Ti-6Al-7Nb) were produced by arc melting with non-consumable tungsten electrode and water-cooled copper hearth under argon atmosphere. Some of the ingots were heat-treated at 1000 °C for 12 and 24 h in argon atmosphere, followed by slow cooling rates to reduce crystalline defects and increase the grain size of their microstructures. Three types of samples were anodized: commercial substrate, as-prepared and heat-treated samples. The anodization was performed using fluoride solution and a cell potential of 20 V. The samples were characterized by optical microscopy, field-emission scanning electron microscopy and X-ray diffraction. The heat treatment preceding the anodization process increased the grain size of pure Ti and Ti alloys and promoted the formation of Widmanstätten structures in Ti6Al7Nb. The nanotubes layers grown on smaller grain and thermally untreated samples were more regular and homogeneous. In the case of Ti-6Al-7Nb alloy, which presents a α + β phase microstructure, the morphology of nanotubes nucleated on α matrix was more regular than those of nanotubes nucleated on β phase. After the annealing process, the Ti-6Al-7Nb alloy presented full diffusion process and the growth of equilibrium phases resulting in the appearance of regions containing higher concentrations of Nb, i.e. beta phase. In those regions the dissolution rate of Nb2O5 is lower than that of TiO2, resulting in a nanoporous layer. In general, heat treating reduces crystalline defects and promotes the increasing of the grain sizes, not favoring the process of nanotube nucleation and growth on the metallic surface.

Fabrication and characterization of conductive anodic aluminum oxide substrates

NASA Astrophysics Data System (ADS)

Altuntas, Sevde; Buyukserin, Fatih

2014-11-01

Biomaterials that allow the utilization of electrical, chemical and topographic cues for improved neuron-material interaction and neural regeneration hold great promise for nerve tissue engineering applications. The nature of anodic aluminum oxide (AAO) membranes intrinsically provides delicate control over topographic and chemical cues for enhanced cell interaction; however their use in nerve regeneration is still very limited. Herein, we report the fabrication and characterization of conductive AAO (CAAO) surfaces for the ultimate goal of integrating electrical cues for improved nerve tissue behavior on the nanoporous substrate material. Parafilm was used as a protecting polymer film, for the first time, in order to obtain large area (50 cm2) free-standing AAO membranes. Carbon (C) was then deposited on the AAO surface via sputtering. Morphological characterization of the CAAO surfaces revealed that the pores remain open after the deposition process. The presence of C on the material surface and inside the nanopores was confirmed by XPS and EDX studies. Furthermore, I-V curves of the surface were used to extract surface resistance values and conductive AFM demonstrated that current signals can only be achieved where conductive C layer is present. Finally, novel nanoporous C films with controllable pore diameters and one dimensional (1-D) C nanostructures were obtained by the dissolution of the template AAO substrate.

Uranium Anodic Dissolution under Slightly Alkaline Conditions Progress Report Full-Scale Demonstration with DU Foil

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gelis, A.; Brown, M. A.; Wiedmeyer, S.

2014-02-18

Argonne National Laboratory (Argonne) is developing an alternative method for digesting irradiated low enriched uranium (LEU) foil targets to produce 99Mo in neutral/alkaline media. This method consists of the electrolytic dissolution of irradiated uranium foil in sodium bicarbonate solution, followed by precipitation of base-insoluble fission and activation products, and uranyl-carbonate species with CaO. The addition of CaO is vital for the effective anion exchange separation of 99MoO 4 2- from the fission products, since most of the interfering anions (e.g., CO 3 2-) are removed from the solution, while molybdate remains in solution. An anion exchange is used to retainmore » and to purify the 99Mo from the filtrate. The electrochemical dissolver has been designed and fabricated in 304 stainless-steel (SS), and tested for the dissolution of a full-size depleted uranium (DU) target, wrapped in Al foil. Future work will include testing with low-burn-up DU foil at Argonne and later with high-burn-up LEU foils at Oak Ridge National Laboratory.« less

Manufacturing of Dysprosium-Iron Alloys by Electrolysis in Fluoride-Based Electrolytes. Electrolysis in a Laboratory-Scale Cell

NASA Astrophysics Data System (ADS)

Martinez, Ana Maria; Osen, Karen Sende; Støre, Anne; Gudbrandsen, Henrik; Kjos, Ole Sigmund; Solheim, Asbjørn; Wang, Zhaohui; Oury, Alexandre; Namy, Patrick

2018-04-01

Electrolytic production of light rare earth elements and rare earth alloys with transition elements takes place in a fluoride-based electrolyte using rare earth oxides as raw material. The optimization of this method, mainly in terms of the energy efficiency and environmental impact control, is rather challenging. Anode effects, evolution of fluorine-containing compounds and side cathode reactions could largely be minimized by good control of the amount of rare earth oxide species dissolved in the fluoride-based electrolyte and their dissolution rate. The Dy2O3 feed rate needed for stable cell operation was studied by following up the anode voltage and gas analysis. On-line analysis of the cell off-gases by FTIR showed that the electrochemical reaction for the formation of Dy-Fe alloy gives mainly CO gas and that CF4 is starting to evolve gradually at anode voltages of ca. 3.25 V. The limiting current density for the discharge of the oxide ions at the graphite anode was in the range of 0.1 to 0.18 A cm-2 at dissolved Dy2O3 contents of ca. 1 wt pct. Modeling of the laboratory cell reactor was also carried out by implementing two models, i.e., an electrical model simulating the current density distribution at the electrodes and a laminal bubbly flow model that explains the electrolyte velocity induced by gas bubble production at the anode.

Effects of Anion Mobility on Electrochemical Behaviors of Lithium–Sulfur Batteries

DOE Office of Scientific and Technical Information (OSTI.GOV)

Han, Kee Sung; Chen, Junzheng; Cao, Ruiguo

The electrolyte is a crucial component of lithium-sulfur (Li-S) batteries, as it controls polysulfide dissolution, charge shuttling processes, and solid-electrolyte interphase (SEI) layer formation. Experimentally, the overall performance of Li-S batteries varies with choice of solvent system and Li-salt used in the electrolyte, and a lack of predictive understanding about the effects of individual electrolyte components inhibits the rational design of electrolytes for Li-S batteries. Here we analyze the role of the counter anions of common Li salts (such as TfO-, FSI-, TFSI-, and TDI-) when dissolved in DOL/DME (1:1 vol.) for use in Li-S batteries. The evolution of ion-ionmore » and ion-solvent interactions due to vari-ous anions was analyzed using 17O NMR and pulsed-field gradient (PFG) NMR and then correlated with electrochemi-cal performance in Li-S cells. These data reveal that the for-mation of the passivation layer on the anode and the loss of active materials from the cathode (evidenced by polysulfide dissolution) are related to anion mobility and affinity with lithium polysulfide, respectively. For future electrolyte de-sign, anions with lower mobility and weaker interactions with lithium polysulfides may be superior candidates for increasing the long-term stability of Li-S batteries.« less

Al-Air Batteries: Fundamental Thermodynamic Limitations from First Principles Theory

NASA Astrophysics Data System (ADS)

Chen, Leanne D.; Noerskov, Jens K.; Luntz, Alan C.

2015-03-01

The Al-air battery possesses high theoretical specific energy (4140 Wh/kg) and is therefore an attractive candidate for vehicle propulsion applications. However, the experimentally observed open-circuit potential is much lower than what thermodynamics predicts, and this potential loss is widely believed to be an effect of corrosion. We present a detailed study of the Al-air battery using density functional theory. The results suggest that the difference between bulk thermodynamic and surface potentials is due to both the effects of asymmetry in multi-electron transfer reactions that define the anodic dissolution of Al and, more importantly, a large chemical step inherent to the formation of bulk Al(OH)3 from surface intermediates. The former results in an energy loss of 3%, while the latter accounts for 14 -29% of the total thermodynamic energy depending on the surface site where dissolution occurs. Therefore, the maximum open-circuit potential of the Al anode is only -1.87 V vs. SHE in the absence of thermal excitations, contrary to -2.34 V predicted by bulk thermodynamics at pH 14.6. This is a fundamental limitation of the system and governs the maximum output potential, which cannot be improved even if corrosion effects were completely suppressed. Supported by the Natural Sciences and Engineering Research Council of Canada and the ReLiable Project (#11-116792) funded by the Danish Council for Strategic Research.

Chemical stability of Lithium 2-trifluoromethyl-4,5-dicyanoimidazolide, an electrolyte salt for Li-ion cells

DOE PAGES

Shkrob, Ilya A.; Pupek, Krzysztof Z.; Gilbert, James A.; ...

2016-12-01

Lithium hexafluorophosphate (LiPF 6) is ubiquitous in commercial lithium-ion batteries, but it is hydrolytically unstable and corrosive on electrode surfaces. Using a more stable salt would confer multiple benefits for high-voltage operation, but many such electrolyte systems facilitate anodic dissolution and pitting corrosion of aluminum current collectors that negate their advantages. Lithium 2-trifluoromethyl-4,5-dicyanoimidazolide (LiTDI) is a new salt that was designed specifically for high-voltage cells. In this study we demonstrate that in carbonate electrolytes, LiTDI prevents anodic dissolution of Al current collectors, which places it into a select group of corrosion inhibitors. However, we also demonstrate that LiTDI becomes reducedmore » on lithiated graphite, undergoing sequential defluorination and yielding a thick and resistive solid-electrolyte interphase (SEI), which increases impedance and lowers electrode capacity. The mechanistic causes for this behavior are examined using computational chemistry methods in the light of recent spectroscopic studies. Here, we demonstrate that LiTDI reduction can be prevented by certain electrolyte additives, which include fluoroethylene carbonate, vinylene carbonate and lithium bis(oxalato)borate. This beneficial action is due to preferential reduction of these additives over LiTDI at a higher potential vs. Li/Li +, so the resulting SEI can prevent the direct reduction of LiTDI at lower potentials on the graphite electrode.« less

Lithium-sulfur batteries: electrochemistry, materials, and prospects.

PubMed

Yin, Ya-Xia; Xin, Sen; Guo, Yu-Guo; Wan, Li-Jun

2013-12-09

With the increasing demand for efficient and economic energy storage, Li-S batteries have become attractive candidates for the next-generation high-energy rechargeable Li batteries because of their high theoretical energy density and cost effectiveness. Starting from a brief history of Li-S batteries, this Review introduces the electrochemistry of Li-S batteries, and discusses issues resulting from the electrochemistry, such as the electroactivity and the polysulfide dissolution. To address these critical issues, recent advances in Li-S batteries are summarized, including the S cathode, Li anode, electrolyte, and new designs of Li-S batteries with a metallic Li-free anode. Constructing S molecules confined in the conductive microporous carbon materials to improve the cyclability of Li-S batteries serves as a prospective strategy for the industry in the future. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Electrolysis of a molten semiconductor

DOE PAGES

Yin, Huayi; Chung, Brice; Sadoway, Donald R.

2016-08-24

Metals cannot be extracted by electrolysis of transition-metal sulfides because as liquids they are semiconductors, which exhibit high levels of electronic conduction and metal dissolution. Herein by introduction of a distinct secondary electrolyte, we reveal a high-throughput electro-desulfurization process that directly converts semiconducting molten stibnite (Sb 2S 3) into pure (99.9%) liquid antimony and sulfur vapour. At the bottom of the cell liquid antimony pools beneath cathodically polarized molten stibnite. At the top of the cell sulfur issues from a carbon anode immersed in an immiscible secondary molten salt electrolyte disposed above molten stibnite, thereby blocking electronic shorting across themore » cell. In conclusion, as opposed to conventional extraction practices, direct sulfide electrolysis completely avoids generation of problematic fugitive emissions (CO 2, CO and SO 2), significantly reduces energy consumption, increases productivity in a single-step process (lower capital and operating costs) and is broadly applicable to a host of electronically conductive transition-metal chalcogenides.« less

Effect of hydrogen on cathodic corrosion of titanium aluminide

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gao, K.W.; Jin, J.W.; Qiao, L.J.

1996-01-01

Cathodic corrosion of titanium aluminide (TiAl) during hydrogen charging in various acidic aqueous solutions and in molten salt at 160 C was studied. At constant potential, the rate of cathodic corrosion (V) was much higher than during anodic dissolution, and V increased linearly with increasing current. V was 10 times higher in the acid solution than in the salt solution under the same current. Disruption of the surface film by local hydride formation during cathodic polarization was shown to be the key step.

Electro-kinetic remediation coupled with phytoremediation to remove lead, arsenic and cesium from contaminated paddy soil.

PubMed

Mao, Xinyu; Han, Fengxiang X; Shao, Xiaohou; Guo, Kai; McComb, Jacqueline; Arslan, Zikri; Zhang, Zhanyu

2016-03-01

The objectives of this study were to investigate distribution and solubility of Pb, Cs and As in soils under electrokinetic field and examine the processes of coupled electrokinetic phytoremediation of polluted soils. The elevated bioavailability and bioaccumulation of Pb, As and Cs in paddy soil under an electro-kinetic field (EKF) were studied. The results show that the EKF treatment is effective on lowering soil pH to around 1.5 near the anode which is beneficial for the dissolution of metal(loid)s, thus increasing their overall solubility. The acidification in the anode soil efficiently increased the water soluble (SOL) and exchangeable (EXC) Pb, As and Cs, implying enhanced solubility and elevated overall potential bioavailability in the anode region while lower solubility in the cathode areas. Bioaccumulations of Pb, As and Cs were largely determined by the nature of elements, loading levels and EKF treatment. The native Pb in soil usually is not bioavailable. However, EKF treatment tends to transfer Pb to the SOL and EXC fractions improving the phytoextraction efficiency. Similarly, EKF transferred more EXC As and Cs to the SOL fraction significantly increasing their bioaccumulation in plant roots and shoots. Pb and As were accumulated more in plant roots than in shoots while Cs was accumulated more in shoots due to its similarity of chemical properties to potassium. Indian mustard, spinach and cabbage are good accumulators for Cs. Translocation of Pb, As and Cs from plant roots to shoots were enhanced by EKF. However, this study indicated the overall low phytoextraction efficiency of these plants. Copyright © 2015 Elsevier Inc. All rights reserved.

Interfacial Chemistry Regulation via a Skin-Grafting Strategy Enables High-Performance Lithium-Metal Batteries

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gao, Yue; Zhao, Yuming; Li, Yuguang C.

The lithium (Li) metal anode suffers severe interfacial instability from its high reactivity toward liquid electrolytes, especially carbonate-based electrolytes, resulting in poor electrochemical performance of batteries that use 4 V high-capacity cathodes. In this paper, we report a new skin-grafting strategy that stabilizes the Li metal–liquid electrolyte interface by coating the Li metal surface with poly((N-2,2-dimethyl-1,3-dioxolane-4-methyl)-5-norbornene-exo-2,3-dicarboximide), a chemically and electrochemically active polymer layer. This layer, composed of cyclic ether groups with a stiff polycyclic main chain, serves as a grafted polymer skin on the Li metal anode not only to incorporate ether-based polymeric components into the solid-electrolyte interphase (SEI) butmore » also to accommodate Li deposition/dissolution under the skin in a dendrite/moss-free manner. Consequently, a Li-metal battery employing a Li metal anode with the grafted skin paired with LiNi 0.5Co 0.2Mn 0.3O 2 cathode has a 90.0% capacity retention after 400 charge/discharge cycles and a capacity of 1.2 mAh/cm 2 in a carbonate-based electrolyte. Finally, this proof-of-concept study provides a new direction for regulating the interfacial chemistry of Li metal anodes and for enabling high-performance Li-metal batteries.« less

Interfacial Chemistry Regulation via a Skin-Grafting Strategy Enables High-Performance Lithium-Metal Batteries

DOE PAGES

Gao, Yue; Zhao, Yuming; Li, Yuguang C.; ...

2017-10-06

The lithium (Li) metal anode suffers severe interfacial instability from its high reactivity toward liquid electrolytes, especially carbonate-based electrolytes, resulting in poor electrochemical performance of batteries that use 4 V high-capacity cathodes. In this paper, we report a new skin-grafting strategy that stabilizes the Li metal–liquid electrolyte interface by coating the Li metal surface with poly((N-2,2-dimethyl-1,3-dioxolane-4-methyl)-5-norbornene-exo-2,3-dicarboximide), a chemically and electrochemically active polymer layer. This layer, composed of cyclic ether groups with a stiff polycyclic main chain, serves as a grafted polymer skin on the Li metal anode not only to incorporate ether-based polymeric components into the solid-electrolyte interphase (SEI) butmore » also to accommodate Li deposition/dissolution under the skin in a dendrite/moss-free manner. Consequently, a Li-metal battery employing a Li metal anode with the grafted skin paired with LiNi 0.5Co 0.2Mn 0.3O 2 cathode has a 90.0% capacity retention after 400 charge/discharge cycles and a capacity of 1.2 mAh/cm 2 in a carbonate-based electrolyte. Finally, this proof-of-concept study provides a new direction for regulating the interfacial chemistry of Li metal anodes and for enabling high-performance Li-metal batteries.« less

Electrically conductive anodized aluminum coatings

NASA Technical Reports Server (NTRS)

Alwitt, Robert S. (Inventor); Liu, Yanming (Inventor)

2001-01-01

A process for producing anodized aluminum with enhanced electrical conductivity, comprising anodic oxidation of aluminum alloy substrate, electrolytic deposition of a small amount of metal into the pores of the anodized aluminum, and electrolytic anodic deposition of an electrically conductive oxide, including manganese dioxide, into the pores containing the metal deposit; and the product produced by the process.

Internal passivation of Al-based microchannel devices by electrochemical anodization

NASA Astrophysics Data System (ADS)

Hymel, Paul J.; Guan, D. S.; Mu, Yang; Meng, W. J.; Meng, Andrew C.

2015-02-01

Metal-based microchannel devices have wide-ranging applications. We report here a method to electrochemically anodize the internal surfaces of Al microchannels, with the purpose of forming a uniform and dense anodic aluminum oxide (AAO) layer on microchannel internal surfaces for chemical passivation and corrosion resistance. A pulsed electrolyte flow was utilized to emulate conventional anodization processes while replenishing depleted ionic species within Al microtubes and microchannels. After anodization, the AAO film was sealed in hot water to close the nanopores. Focused ion beam (FIB) sectioning, scanning electron microscopy (SEM), and energy dispersive spectroscopy (EDS) were utilized to characterize the AAO morphology and composition. Potentiodynamic polarization corrosion testing of anodized Al microtube half-sections in a NaCl solution showed an order of magnitude decrease in anodic corrosion current when compared to an unanodized tube. The surface passivation process was repeated for Al-based microchannel heat exchangers. A corrosion testing method based on the anodization process showed higher resistance to ion transport through the anodized specimens than unanodized specimens, thus verifying the internal anodization and sealing process as a viable method for surface passivation of Al microchannel devices.

Molten Salt Electrolysis of MgCl2 in a Cell with Rapid Chlorine Removal Feature

NASA Astrophysics Data System (ADS)

Demirci, Gökhan; Karakaya, İshak

An experimental electrolytic magnesium production cell was designed to remove chlorine gas from the electrolyte rapidly and demonstrate the beneficial effects of reduced chlorine dissolution into the molten salt electrolyte. The back reaction that is the main cause of current losses in electrolytic magnesium production was reduced as a result of effective separation of electrode products and decreased contact time of chlorine gas with the electrolyte. Moreover, smaller inter electrode distances employed and lower chlorine gas present on the anode surface made it possible to work at low cell voltages. Electrolytic cell was tested at different current densities. Energy consumption of 7.0 kWh kg-1 Mg that is slightly above the theoretical minimum, 6.2 kWh kg-1 Mg, at 0.68 Acm-2 anodic current density was achieved for a MgCl2/NaCl/KCl electrolyte.

Autonomous colloidal crystallization in a galvanic microreactor

NASA Astrophysics Data System (ADS)

Punckt, Christian; Jan, Linda; Jiang, Peng; Frewen, Thomas A.; Saville, Dudley A.; Kevrekidis, Ioannis G.; Aksay, Ilhan A.

2012-10-01

We report on a technique that utilizes an array of galvanic microreactors to guide the assembly of two-dimensional colloidal crystals with spatial and orientational order. Our system is comprised of an array of copper and gold electrodes in a coplanar arrangement, immersed in a dilute hydrochloric acid solution in which colloidal micro-spheres of polystyrene and silica are suspended. Under optimized conditions, two-dimensional colloidal crystals form at the anodic copper with patterns and crystal orientation governed by the electrode geometry. After the aggregation process, the colloidal particles are cemented to the substrate by co-deposition of reaction products. As we vary the electrode geometry, the dissolution rate of the copper electrodes is altered. This way, we control the colloidal motion as well as the degree of reaction product formation. We show that particle motion is governed by a combination of electrokinetic effects acting directly on the colloidal particles and bulk electrolyte flow generated at the copper-gold interface.

Corrosion behavior and microstructures of experimental Ti-Au alloys.

PubMed

Takahashi, Masatoshi; Kikuchi, Masafumi; Takada, Yukyo; Okuno, Osamu; Okabe, Toru

2004-06-01

Anodic polarization was performed in 0.9% NaCl and 1% lactic acid solutions to characterize the relationship between the corrosion behavior and microstructures of cast Ti-Au (5-40%) alloys. An abrupt increase in the current density occurred at approximately 0.6 V vs. SCE for the 30% and 40% Au alloys in the 0.9% NaCl solution. The microstructures after corrosion testing indicated that this breakdown may have been caused by the preferential dissolution of the Ti3Au. However, the potential for preferential dissolution was higher than the breakdown potential of stainless steel or Co-Cr alloy, which meant that the corrosion resistance of the Ti-Au alloys was superior. In 1% lactic acid solution, the corrosion resistance of the Ti-Au alloys was excellent, with no breakdown at any composition. In the present test solutions, the Ti-Au alloys up to 20% Au had good corrosion resistance comparable to that for pure titanium.

Electrorecycling of Critical and Value Metals from Mobile Electronics

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tedd E. Lister; Peming Wang; Andre Anderko

2014-09-01

Mobile electronic devices such as smart phones and tablets are a significant source of valuable metals that should be recycled. Each year over a billion devices are sold world-wide and the average life is only a couple years. Value metals in phones are gold, palladium, silver, copper, cobalt and nickel. Devices now contain increasing amounts of rare earth elements (REE). In recent years the supply chain for REE has moved almost exclusively to China. They are contained in displays, speakers and vibrators within the devices. By US Department of Energy (DOE) classification, specific REEs (Nd, Dy, Eu, Tb and Y)more » are considered critical while others (Ce, La and Pr) are deemed near critical. Effective recycling schemes should include the recovery of these critical materials. By including more value materials in a recovery scheme, more value can be obtained by product diversification and less waste metals remains to be disposed of. REEs are mined as a group such that when specific elements become critical significantly more ore must be processed to capture the dilute but valuable critical elements. Targeted recycling of items containing the more of the less available critical materials could address their future criticality. This presentation will describe work in developing aqueous electrochemistry-based schemes for recycling metals from scrap mobile electronics. The electrorecycling process generates oxidizing agents at an anode while reducing dissolved metals at the cathode. E vs pH diagrams and metals dissolution experiments are used to assess effectiveness of various solution chemistries. Although several schemes were envisioned, a two stages process has been the focus of work: 1) initial dissolution of Cu, Sn, Ag and magnet materials using Fe+3 generated in acidic sulfate and 2) final dissolution of Pd and Au using Cl2 generated in an HCl solution. Experiments were performed using simulated metal mixtures. Both Cu and Ag were recovered at ~ 97% using Fe+3 while leaving Au and Ag intact. REE were extracted from the dissolved mixture using conventional methods. A discussion of future research directions will be discussed.« less

Anodization process produces opaque, reflective coatings on aluminum

NASA Technical Reports Server (NTRS)

1965-01-01

Opaque, reflective coatings are produced on aluminum articles by an anodizing process wherein the anodizing bath contains an aqueous dispersion of finely divided insoluble inorganic compounds. These particles appear as uniformly distributed occlusions in the anodic deposit on the aluminum.

Stabilizing the Performance of High-Capacity Sulfur Composite Electrodes by a New Gel Polymer Electrolyte Configuration.

PubMed

Agostini, Marco; Lim, Du Hyun; Sadd, Matthew; Fasciani, Chiara; Navarra, Maria Assunta; Panero, Stefania; Brutti, Sergio; Matic, Aleksandar; Scrosati, Bruno

2017-09-11

Increased pollution and the resulting increase in global warming are drawing attention to boosting the use of renewable energy sources such as solar or wind. However, the production of energy from most renewable sources is intermittent and thus relies on the availability of electrical energy-storage systems with high capacity and at competitive cost. Lithium-sulfur batteries are among the most promising technologies in this respect due to a very high theoretical energy density (1675 mAh g -1 ) and that the active material, sulfur, is abundant and inexpensive. However, a so far limited practical energy density, life time, and the scaleup of materials and production processes prevent their introduction into commercial applications. In this work, we report on a simple strategy to address these issues by using a new gel polymer electrolyte (GPE) that enables stable performance close to the theoretical capacity of a low cost sulfur-carbon composite with high loading of active material, that is, 70 % sulfur. We show that the GPE prevents sulfur dissolution and reduces migration of polysulfide species to the anode. This functional mechanism of the GPE membranes is revealed by investigating both its morphology and the Li-anode/GPE interface at various states of discharge/charge using Raman spectroscopy. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Temporal patterning of the potential induced by localized corrosion of iron passivity in acid media. Growth and breakdown of the oxide film described in terms of a point defect model.

PubMed

Sazou, Dimitra; Pavlidou, Maria; Pagitsas, Michael

2009-10-21

This work analyses the nature of temporal patterning of the anodic potential induced by chlorides during polarization of iron under current-controlled conditions in acid solutions. It is shown that potential oscillations emerged as a result of the local chloride attack of a thin oxide layer, which covers the iron surface in its passive state. The mechanism by which both the local oxide breakdown and the subsequent localized active dissolution (pitting) occur is explained by considering a point defect model (PDM) developed to describe the oxide growth and breakdown. According to the PDM, chlorides occupy oxygen vacancies resulting in the inhibition of oxide growth and autocatalytic generation of cation vacancies that destabilize the oxide layer. Simultaneous transformation of the outer surface of the inner oxide layer to non-adherent ferrous chloride or oxo-chloride species leads to a further thinning of the oxide layer and its lifting-on from the iron surface. The process repeats again yielding sustained oscillations of the anodic potential. Analysis of the oscillatory response obtained under current-controlled conditions as a function of either the current or the time allows the suggestion of a set of alternate diagnostic criteria, which might be used to characterize localized corrosion of iron in acid solutions.

Characterization of Pulse Reverses Electroforming on Hard Gold Coating.

PubMed

Byoun, Young-Min; Noh, Young-Tai; Kim, Young-Geun; Ma, Seung-Hwan; Kim, Gwan-Hoon

2018-03-01

Effect of pulse reverse current (PRC) method on brass coatings electroplated from gold solution was investigated by various plating parameters such as plating duration, the anodic duty cycle, the anodic current density and the cathodic current density. The reversed current results in a significant change in the morphology of electrodeposits, improvement of the overall current efficiency and reduction of deposit porosity. With longer pulses, hemispherical surface features are generated, while larger grains result from shorter pulse widths. The porosity of the plated samples is found to decrease compared with results at the same time-average plating rate obtained from DC or Pulse plating. A major impediment to reducing gold later thickness is the corrosion of the underlying substrate, which is affected by the porosity of the gold layer. Both the morphology and the hydrogen evolution reaction have significant impact on porosity. PRC plating affect hydrogen gold and may oxidize hydrogen produced during the cathodic portion of the waveform. Whether the dissolution of gold and oxidation of hydrogen occur depends on the type of plating bath and the plating conditions adapted. In reversed pulse plating, the amount of excess near-surface cyanide is changed after the cathodic current is applied, and the oxidation of gold under these conditions has not been fully addressed. The effects of the current density, pulse-reverse ratio and brightener concentration of the electroplating process were investigated and optimized for suitable performance.

Electrochemical characteristics of bioresorbable binary MgCa alloys in Ringer's solution: Revealing the impact of local pH distributions during in-vitro dissolution.

PubMed

Mareci, D; Bolat, G; Izquierdo, J; Crimu, C; Munteanu, C; Antoniac, I; Souto, R M

2016-03-01

Biodegradable magnesium-calcium (MgCa) alloy is a very attractive biomaterial. Two MgCa alloys below the solid solubility of Ca were considered, as to solely investigate the effect of Ca content on the behavior of magnesium and the pH changes associated to metal dissolution. X-ray diffraction analysis and optical microscopy showed that both Mg-0.63Ca and Mg-0.89Ca alloys were solely composed of α(Mg) phase. Degradation characteristics and electrochemical characterization of MgCa alloys were investigated during exposure to Ringer's solution at 37 °C by electrochemical impedance spectroscopy and scanning electrochemical microscopy. The impedance behavior showed both capacitive and inductive features that are related to the alloy charge transfer reaction and the relaxation of the absorbed corrosion compounds, and can be described in terms of an equivalent circuit. Scanning electron microscopy (SEM) was employed to view the surface morphology of the MgCa samples after 1 week immersion in Ringer's solution showing extensive precipitation of corrosion products, whereas the substrate shows evidence of a non-uniform corrosion process. Energy dispersive analysis showed that the precipitates contained oxygen, calcium, magnesium and chlorine, and the Mg:Ca ratios were smaller than in the alloys. Scanning electrochemical microscopy (SECM) was used to visualize local pH changes associated to these physicochemical processes with high spatial resolution. The occurrence of pH variations in excess of 3 units between anodic and cathodic half-cell reactions was monitored in situ. Copyright © 2015 Elsevier B.V. All rights reserved.

Clustered Single Cellulosic Fiber Dissolution Kinetics and Mechanisms through Optical Microscopy under Limited Dissolving Conditions.

PubMed

Mäkelä, Valtteri; Wahlström, Ronny; Holopainen-Mantila, Ulla; Kilpeläinen, Ilkka; King, Alistair W T

2018-05-14

Herein, we describe a new method of assessing the kinetics of dissolution of single fibers by dissolution under limited dissolving conditions. The dissolution is followed by optical microscopy under limited dissolving conditions. Videos of the dissolution were processed in ImageJ to yield kinetics for dissolution, based on the disappearance of pixels associated with intact fibers. Data processing was performed using the Python language, utilizing available scientific libraries. The methods of processing the data include clustering of the single fiber data, identifying clusters associated with different fiber types, producing average dissolution traces and also extraction of practical parameters, such as, time taken to dissolve 25, 50, 75, 95, and 99.5% of the clustered fibers. In addition to these simple parameters, exponential fitting was also performed yielding rate constants for fiber dissolution. Fits for sample and cluster averages were variable, although demonstrating first-order kinetics for dissolution overall. To illustrate this process, two reference pulps (a bleached softwood kraft pulp and a bleached hardwood pre-hydrolysis kraft pulp) and their cellulase-treated versions were analyzed. As expected, differences in the kinetics and dissolution mechanisms between these samples were observed. Our initial interpretations are presented, based on the combined mechanistic observations and single fiber dissolution kinetics for these different samples. While the dissolution mechanisms observed were similar to those published previously, the more direct link of mechanistic information with the kinetics improve our understanding of cell wall structure and pre-treatments, toward improved processability.

The improved dissolution performance of a post processing treated spray-dried crystalline solid dispersion of poorly soluble drugs.

PubMed

Chan, Siok-Yee; Toh, Seok-Ming; Khan, Nasir Hayat; Chung, Yin-Ying; Cheah, Xin-Zi

2016-11-01

Solution-mediated transformation has been cited as one of the main problems that deteriorate dissolution performances of solid dispersion (SD). This is mainly attributed by the recrystallization tendency of poorly soluble drug. Eventually, it will lead to extensive agglomeration which is a key process in reducing the dissolution performance of SD and offsets the true benefit of SD system. Here, a post-processing treatment is suggested in order to reduce the recrystallization tendency and hence bring forth the dissolution advantage of SD system. The current study investigates the effect of a post processing treatment on dissolution performance of SD in comparison to their performances upon production. Two poorly soluble drugs were spray dried into SD using polyvinyl alcohol (PVA) as hydrophilic carrier. The obtained samples were post processing treated by exposure to high humidity, i.e. 75% RH at room temperature. The physical properties and release rate of the SD system were characterized upon production and after the post-processing treatment. XRPD, Infrared and DSC results showed partial crystallinity of the fresh SD systems. Crystallinity of these products was further increased after the post-processing treatment at 75% RH. This may be attributed to the high moisture absorption of the SD system that promotes recrystallization process of the drug. However, dissolution efficiencies of the post-treated systems were higher and more consistent than the fresh SD. The unexpected dissolution trend was further supported by the results intrinsic dissolution and solubility studies. An increase of crystallinity in a post humidity treated SD did not exert detrimental effect to their dissolution profiles. A more stabilized system with a preferable enhanced dissolution rate was obtained by exposing the SD to a post processing humidity treatment.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mehdi, Beata L.; Qian, Jiangfeng; Nasybulin, Eduard

Lithium (Li)-ion batteries are currently used for a wide variety of portable electronic devices, electric vehicles and renewable energy applications. In addition, extensive worldwide research efforts are now being devoted to more advanced “beyond Li-ion” battery chemistries - such as lithium-sulfur (Li-S) and lithium-air (Li-O2) - in which the carbon anode is replaced with Li metal. However, the practical application of Li metal anode systems has been highly problematic. The main challenges involve controlling the formation of a solid-electrolyte interphase (SEI) layer and the suppression of Li dendrite growth during the charge/discharge process (achieving “dendrite-free” cycling). The SEI layer formationmore » continuously consumes the electrolyte components creating highly resistive layer, which leads to the rapid decrease of cycling performance and degradation of the Li anode. The growth of Li metal dendrites at the anode contributes to rapid capacity fading (the presence of “dead Li” created during the discharge leads to an increased overpotential) and, in the case of continuous growth, leads to internal short circuits and extreme safety issues. Here we demonstrate the application of an operando electrochemical scanning transmission electron microscopy (ec-(S)TEM) cell to study the SEI layer formation and the initial stages of Li dendrite growth - the goal is to develop a mechanism for mitigating the degradation processes and increasing safety. Bright field (BF) STEM images in Figure 1 A-C show Li metal deposition and dissolution processes at the interface between the Pt working electrode and the lithium hexafluorophosphate (LiPF6) in propylene carbonate (PC) electrolyte during three charge/discharge cycles. A contrast reversal caused by Li metal being lighter/less dense than surrounding electrolyte (Li appears brighter than the background in BF STEM images) allows Li to be uniquely identified from the other components in the system - the only solid material that is less dense than the electrolyte is Li metal. Using these images, we can precisely quantify the total volume of Li deposition, the thickness of the SEI layer (observed as a ring of positive contrast around the electrode) and alloy formation due to Li+ ion insertion during each cycle. Furthermore, at the end of each discharge cycle we can quantify the presence of “dead Li” detached from the Pt electrode, thereby demonstrating the degree of irreversibility (and degradation of Pt electrode) associated with insertion/removal of Li+during this process with direct correlation to electrochemical performance. Such analyses provide significant insights into Li metal dendrite growth, which is critical to understand the complex interfacial reactions needed to be controlled for future Li-based and next generation energy storage systems.« less

Environmental resistance of oxide tags fabricated on 304L stainless steel via nanosecond pulsed laser irradiation

DOE PAGES

Lawrence, Samantha Kay; Adams, David P.; Bahr, David F.; ...

2015-11-14

Nanosecond pulsed laser irradiation was used to fabricate colored, mechanically robust oxide “tags” on 304L stainless steel. Immersion in simulated seawater solution, salt fog exposure, and anodic polarization in a 3.5% NaCl solution were employed to evaluate the environmental resistance of these oxide tags. Single layer oxides outside a narrow thickness range (~ 100–150 nm) are susceptible to dissolution in chloride containing environments. The 304L substrates immediately beneath the oxides corrode severely—attributed to Cr-depletion in the melt zone during laser processing. For the first time, multilayered oxides were fabricated with pulsed laser irradiation in an effort to expand the protectivemore » thickness range while also increasing the variety of film colors attainable in this range. Layered films grown using a laser scan rate of 475 mm/s are more resistant to both localized and general corrosion than oxides fabricated at 550 mm/s. Furthermore, in the absence of pre-processing to mitigate Cr-depletion, layered films can enhance environmental stability of the system.« less

Influence of Pb 2+ ions in the H 2 oxidation on Pt catalyzed hydrogen diffusion anodes in sulfuric acid: presence of oscillatory phenomena

NASA Astrophysics Data System (ADS)

Expósito, E.; Sánchez-Sánchez, C. M.; Solla-Gullón, J.; Montiel, V.

The influence of Pb 2+ ions in sulfuric acid medium on the behavior of a platinum catalyzed hydrogen diffusion electrode (HDE) in a filter press reactor has been studied. A voltammetric study of the H 2 oxidation reaction on a polyoriented platinum electrode and a platinum rotating disk electrode (RDE) in presence of lead ions in solution has also been carried out. Potential oscillations were found in galvanostatic experiments of H 2 oxidation using a HDE catalyzed with platinum when Pb 2+ ions are present in solution. This oscillatory phenomenon was also observed when hydrogen oxidation was carried out in presence of Pb 2+ ions using a platinum RDE. The oscillatory behavior observed has been attributed to an adsorption-oxidation-desorption process of lead on the platinum surface. Due to the low solubility of Pb 2+ in sulfuric acid, at high values of coverage, lead is oxidised to insoluble lead sulfate that blocks the Pt surface. The coupling of the dissolution of lead sulfate and the Pb electrochemical adsorption-oxidation processes cause the oscillatory phenomenon.

Regenerable Cu-intercalated MnO2 layered cathode for highly cyclable energy dense batteries

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yadav, Gautam G.; Gallaway, Joshua W.; Turney, Damon E.

2017-03-06

Manganese dioxide cathodes are inexpensive and have high theoretical capacity (based on two electrons) of 617 mAh g-1, making them attractive for low-cost, energy-dense batteries. They are used in non-rechargeable batteries with anodes like zinc. Only ~10% of the theoretical capacity is currently accessible in rechargeable alkaline systems. Attempts to access the full capacity using additives have been unsuccessful. We report a class of Bi-birnessite (a layered manganese oxide polymorph mixed with bismuth oxide (Bi2O3)) cathodes intercalated with Cu2+ that deliver near-full two-electron capacity reversibly for >6,000 cycles. The key to rechargeability lies in exploiting the redox potentials of Cumore » to reversibly intercalate into the Bi-birnessite-layered structure during its dissolution and precipitation process for stabilizing and enhancing its charge transfer characteristics. This process holds promise for other applications like catalysis and intercalation of metal ions into layered structures. A large prismatic rechargeable Zn-birnessite cell delivering ~140 Wh l-1 is shown.« less

A Highly Controllable Electrochemical Anodization Process to Fabricate Porous Anodic Aluminum Oxide Membranes

NASA Astrophysics Data System (ADS)

Lin, Yuanjing; Lin, Qingfeng; Liu, Xue; Gao, Yuan; He, Jin; Wang, Wenli; Fan, Zhiyong

2015-12-01

Due to the broad applications of porous alumina nanostructures, research on fabrication of anodized aluminum oxide (AAO) with nanoporous structure has triggered enormous attention. While fabrication of highly ordered nanoporous AAO with tunable geometric features has been widely reported, it is known that its growth rate can be easily affected by the fluctuation of process conditions such as acid concentration and temperature during electrochemical anodization process. To fabricate AAO with various geometric parameters, particularly, to realize precise control over pore depth for scientific research and commercial applications, a controllable fabrication process is essential. In this work, we revealed a linear correlation between the integrated electric charge flow throughout the circuit in the stable anodization process and the growth thickness of AAO membranes. With this understanding, we developed a facile approach to precisely control the growth process of the membranes. It was found that this approach is applicable in a large voltage range, and it may be extended to anodization of other metal materials such as Ti as well.

A Highly Controllable Electrochemical Anodization Process to Fabricate Porous Anodic Aluminum Oxide Membranes.

PubMed

Lin, Yuanjing; Lin, Qingfeng; Liu, Xue; Gao, Yuan; He, Jin; Wang, Wenli; Fan, Zhiyong

2015-12-01

Due to the broad applications of porous alumina nanostructures, research on fabrication of anodized aluminum oxide (AAO) with nanoporous structure has triggered enormous attention. While fabrication of highly ordered nanoporous AAO with tunable geometric features has been widely reported, it is known that its growth rate can be easily affected by the fluctuation of process conditions such as acid concentration and temperature during electrochemical anodization process. To fabricate AAO with various geometric parameters, particularly, to realize precise control over pore depth for scientific research and commercial applications, a controllable fabrication process is essential. In this work, we revealed a linear correlation between the integrated electric charge flow throughout the circuit in the stable anodization process and the growth thickness of AAO membranes. With this understanding, we developed a facile approach to precisely control the growth process of the membranes. It was found that this approach is applicable in a large voltage range, and it may be extended to anodization of other metal materials such as Ti as well.

Manufacturing High-Quality Carbon Nanotubes at Lower Cost

NASA Technical Reports Server (NTRS)

Benavides, Jeanette M.; Lidecker, Henning

2004-01-01

A modified electric-arc welding process has been developed for manufacturing high-quality batches of carbon nanotubes at relatively low cost. Unlike in some other processes for making carbon nanotubes, metal catalysts are not used and, consequently, it is not necessary to perform extensive cleaning and purification. Also, unlike some other processes, this process is carried out at atmospheric pressure under a hood instead of in a closed, pressurized chamber; as a result, the present process can be implemented more easily. Although the present welding-based process includes an electric arc, it differs from a prior electric-arc nanotube-production process. The welding equipment used in this process includes an AC/DC welding power source with an integral helium-gas delivery system and circulating water for cooling an assembly that holds one of the welding electrodes (in this case, the anode). The cathode is a hollow carbon (optionally, graphite) rod having an outside diameter of 2 in. (approximately equal to 5.1 cm) and an inside diameter of 5/8 in. (approximately equal to 1.6 cm). The cathode is partly immersed in a water bath, such that it protrudes about 2 in. (about 5.1 cm) above the surface of the water. The bottom end of the cathode is held underwater by a clamp, to which is connected the grounding cable of the welding power source. The anode is a carbon rod 1/8 in. (approximately equal to 0.3 cm) in diameter. The assembly that holds the anode includes a thumbknob- driven mechanism for controlling the height of the anode. A small hood is placed over the anode to direct a flow of helium downward from the anode to the cathode during the welding process. A bell-shaped exhaust hood collects the helium and other gases from the process. During the process, as the anode is consumed, the height of the anode is adjusted to maintain an anode-to-cathode gap of 1 mm. The arc-welding process is continued until the upper end of the anode has been lowered to a specified height above the surface of the water bath. The process causes carbon nanotubes to form in the lowest 2.5 cm of the anode. It also causes a deposit reminiscent of a sandcastle to form on the cathode. The nanotube-containing material is harvested. The cathode and anode can then be cleaned (or the anode is replaced, if necessary) and the process repeated to produce more nanotubes. Tests have shown that the process results in approximately equal to 50-percent yield of carbon nanotubes (mostly of the single-wall type) of various sizes. Whereas the unit cost of purified single-wall carbon nanotubes produced by other process is about $1,000/g in the year 2000, it has been estimated that for the present process, the corresponding cost would be about $10/g.

Development and Testing of High Surface Area Iridium Anodes for Molten Oxide Electrolysis

NASA Technical Reports Server (NTRS)

Shchetkovskiy, Anatoliy; McKechnie, Timothy; Sadoway, Donald R.; Paramore, James; Melendez, Orlando; Curreri, Peter A.

2010-01-01

Processing of lunar regolith into oxygen for habitat and propulsion is needed to support future space missions. Direct electrochemical reduction of molten regolith is an attractive method of processing, because no additional chemical reagents are needed. The electrochemical processing of molten oxides requires high surface area, inert anodes. Such electrodes need to be structurally robust at elevated temperatures (1400-1600?C), be resistant to thermal shock, have good electrical conductivity, be resistant to attack by molten oxide (silicate), be electrochemically stable and support high current density. Iridium with its high melting point, good oxidation resistance, superior high temperature strength and ductility is the most promising candidate for anodes in high temperature electrochemical processes. Several innovative concepts for manufacturing such anodes by electrodeposition of iridium from molten salt electrolyte (EL-Form? process) were evaluated. Iridium electrodeposition to form of complex shape components and coating was investigated. Iridium coated graphite, porous iridium structure and solid iridium anodes were fabricated. Testing of electroformed iridium anodes shows no visible degradation. The result of development, manufacturing and testing of high surface, inert iridium anodes will be presented.

Development and Testing of High Surface Area Iridium Anodes for Molten Oxide Electrolysis

NASA Technical Reports Server (NTRS)

Shchetkovskiy, Anatoliy; McKechnie, Timothy; Sadoway, Donald R.; Paramore, James; Melendez, Orlando; Curreri, Peter A.

2010-01-01

Processing of lunar regolith into oxygen for habitat and propulsion is needed to support future space missions. Direct electrochemical reduction of molten regolith is an attractive method of processing, because no additional chemical reagents are needed. The electrochemical processing of molten oxides requires high surface area, inert anodes. Such electrodes need to be structurally robust at elevated temperatures (1400-1600 C), be resistant to thermal shock, have good electrical conductivity, be resistant to attack by molten oxide (silicate), be electrochemically stable and support high current density. Iridium with its high melting point, good oxidation resistance, superior high temperature strength and ductility is the most promising candidate for anodes in high temperature electrochemical processes. Several innovative concepts for manufacturing such anodes by electrodeposition of iridium from molten salt electrolyte (EL-Form process) were evaluated. Iridium electrodeposition to form of complex shape components and coating was investigated. Iridium coated graphite, porous iridium structure and solid iridium anodes were fabricated. Testing of electroformed iridium anodes shows no visible degradation. The result of development, manufacturing and testing of high surface, inert iridium anodes will be presented.

Cognitive processing in the aftermath of relationship dissolution: Associations with concurrent and prospective distress and posttraumatic growth.

PubMed

Del Palacio-González, Adriana; Clark, David A; O'Sullivan, Lucia F

2017-12-01

Non-marital romantic relationship dissolution is amongst the most stressful life events experienced by young adults. Yet, some individuals experience posttraumatic growth following relationship dissolution. Little is known about the specific and differential contribution of trait-like and event-specific cognitive processing styles to each of these outcomes. A longitudinal design was employed in which trait-like (brooding and reflection) and dissolution-specific (intrusive and deliberate) cognitive processing was examined as predictors of growth (Posttraumatic Growth Inventory) and distress (Breakup Distress Scale) following a recent relationship dissolution. Initially, 148 participants completed measures of trait-like and dissolution-specific cognitive processing, growth, and distress (T1). A subsample completed a seven-month follow-up (T2). Higher frequency of relationship-dissolution intrusive thoughts predicted concurrent distress after accounting for brooding and relationship characteristics. Further, higher brooding and lower reflection predicted higher distress prospectively. Concurrent growth was predicted by both higher brooding and more deliberate relationship-dissolution thoughts. Prospectively, T1 dissolution intrusive thoughts predicted higher T2 deliberate thoughts, and the interaction between these two constructs predicted higher T2 growth. Therefore, deliberately thinking of the dissolution was related to positive psychological outcomes. In contrast, intrusive dissolution cognitions and a tendency for brooding had a mixed (paradoxical) association with psychological adjustment. Copyright © 2016 John Wiley & Sons, Ltd.

Modeling spray/puddle dissolution processes for deep-ultraviolet acid-hardened resists

NASA Astrophysics Data System (ADS)

Hutchinson, John M.; Das, Siddhartha; Qian, Qi-De; Gaw, Henry T.

1993-10-01

A study of the dissolution behavior of acid-hardened resists (AHR) was undertaken for spray and spray/puddle development processes. The Site Services DSM-100 end-point detection system is used to measure both spray and puddle dissolution data for a commercially available deep-ultraviolet AHR resist, Shipley SNR-248. The DSM allows in situ measurement of dissolution rate on the wafer chuck and hence allows parameter extraction for modeling spray and puddle processes. The dissolution data for spray and puddle processes was collected across a range of exposure dose and postexposure bake temperature. The development recipe was varied to decouple the contribution of the spray and puddle modes to the overall dissolution characteristics. The mechanisms involved in spray versus puddle dissolution and the impact of spray versus puddle dissolution on process performance metrics has been investigated. We used the effective-dose-modeling approach and the measurement capability of the DSM-100 and developed a lumped parameter model for acid-hardened resists that incorporates the effects of exposure, postexposure bake temperature and time, and development condition. The PARMEX photoresist-modeling program is used to determine parameters for the spray and for the puddle process. The lumped parameter AHR model developed showed good agreement with experimental data.

Modified low-temperture direct bonding method for vacuum microelectronics application

NASA Astrophysics Data System (ADS)

Ju, Byeong-Kwon; Lee, Duck-Jung; Choi, Woo-Beom; Lee, Yun-Hi; Jang, Jin; Lee, Kwang-Bae; Oh, Myung-Hwan

1997-06-01

This paper presents the process and experimental results for the improved silicon-to-glass bonding using silicon direct bonding (SDB) followed by anodic bonding. The initial bonding between glass and silicon was caused by the hydrophilic surfaces of silicon-glass ensemble using SDB method. Then the initially bonded specimen had to be strongly bonded by anodic bonding process. The effects of the bonding process parameters on the interface energy were investigated as functions of the bonding temperature and voltage. We found that the specimen which was bonded using SDB process followed by anodic bonding process had higher interface energy than one using anodic bonding process only. The main factor contributing to the higher interface energy in the glass-to-silicon assemble bonded by SDB followed by anodic bonding was investigated by secondary ion mass spectroscopy analysis.

Degradation Mechanisms of Magnesium Metal Anodes in Electrolytes Based on (CF 3SO 2) 2N – at High Current Densities

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yoo, Hyun Deog; Han, Sang-Don; Bolotin, Igor L.

The energy density of rechargeable batteries utilizing metals as anodes surpasses that of Li ion batteries, which employ carbon instead. Among possible metals, magnesium represents a potential alternative to the conventional choice, lithium, in terms of storage density, safety,stability, and cost. However, a major obstacle for metal-based batteries is the identification of electrolytes that show reversible deposition/dissolution of the metal anode and support reversible intercalation of ions into a cathode. Traditional Grignard-based Mg electrolytes are excellent with respect to the reversible deposition of Mg, but their limited anodic stability and compatibility with oxide cathodes hinder their applicability in Mg batteriesmore » with higher voltage. Non-Grignard electrolytes, which consist of ethereal solutions of magnesium(II) bis(trifluoromethanesulfonyl)imide (Mg(TFSI) 2), remain fairly stable near the potential of Mg deposition. The slight reactivity of these electrolytes toward Mg metal can be remedied by the addition of surface-protecting agents, such as MgCl 2. Hence, ethereal solutions of Mg(TFSI) 2 salt with MgCl 2 as an additive have been suggested as a representative non-Grignard Mg electrolyte. In this work, the degradation mechanisms of a Mg metal anode in the TFSI-based electrolyte were studied using a current density of 1 mA cm -2 and an areal capacity of ~0.4 mAh cm -2, which is close to those used in practical applications. The degradation mechanisms identified include the corrosion of Mg metal, which causes the loss of electronic pathways and mechanical integrity, the nonuniform deposition of Mg, and the decomposition of TFSI - anions. This study not only represents an assessment of the behavior of Mg metal anodes at practical current density and areal capacity but also details the outcomes of interfacial passivation, which was detected by simple cyclic voltammetry experiments. This study also points out the absolute absence of any passivation at the electrode-electrolyte interface for the premise of developing electrolytes compatible with a metal anode.« less

Degradation Mechanisms of Magnesium Metal Anodes in Electrolytes Based on (CF 3SO 2) 2N – at High Current Densities

DOE PAGES

Yoo, Hyun Deog; Han, Sang-Don; Bolotin, Igor L.; ...

2017-06-21

The energy density of rechargeable batteries utilizing metals as anodes surpasses that of Li ion batteries, which employ carbon instead. Among possible metals, magnesium represents a potential alternative to the conventional choice, lithium, in terms of storage density, safety,stability, and cost. However, a major obstacle for metal-based batteries is the identification of electrolytes that show reversible deposition/dissolution of the metal anode and support reversible intercalation of ions into a cathode. Traditional Grignard-based Mg electrolytes are excellent with respect to the reversible deposition of Mg, but their limited anodic stability and compatibility with oxide cathodes hinder their applicability in Mg batteriesmore » with higher voltage. Non-Grignard electrolytes, which consist of ethereal solutions of magnesium(II) bis(trifluoromethanesulfonyl)imide (Mg(TFSI) 2), remain fairly stable near the potential of Mg deposition. The slight reactivity of these electrolytes toward Mg metal can be remedied by the addition of surface-protecting agents, such as MgCl 2. Hence, ethereal solutions of Mg(TFSI) 2 salt with MgCl 2 as an additive have been suggested as a representative non-Grignard Mg electrolyte. In this work, the degradation mechanisms of a Mg metal anode in the TFSI-based electrolyte were studied using a current density of 1 mA cm -2 and an areal capacity of ~0.4 mAh cm -2, which is close to those used in practical applications. The degradation mechanisms identified include the corrosion of Mg metal, which causes the loss of electronic pathways and mechanical integrity, the nonuniform deposition of Mg, and the decomposition of TFSI - anions. This study not only represents an assessment of the behavior of Mg metal anodes at practical current density and areal capacity but also details the outcomes of interfacial passivation, which was detected by simple cyclic voltammetry experiments. This study also points out the absolute absence of any passivation at the electrode-electrolyte interface for the premise of developing electrolytes compatible with a metal anode.« less

Anodizing And Sealing Aluminum In Nonchromated Solutions

NASA Technical Reports Server (NTRS)

Emmons, John R.; Kallenborn, Kelli J.

1995-01-01

Improved process for anodizing and sealing aluminum involves use of 5 volume percent sulfuric acid in water as anodizing solution, and 1.5 to 2.0 volume percent nickel acetate in water as sealing solution. Replaces process in which sulfuric acid used at concentrations of 10 to 20 percent. Improved process yields thinner coats offering resistance to corrosion, fatigue life, and alloy-to-alloy consistency equal to or superior to those of anodized coats produced with chromated solutions.

Laser-Ultrasonic Measurement of Elastic Properties of Anodized Aluminum Coatings

NASA Astrophysics Data System (ADS)

Singer, F.

Anodized aluminum oxide plays a great role in many industrial applications, e.g. in order to achieve greater wear resistance. Since the hardness of the anodized films strongly depends on its processing parameters, it is important to characterize the influence of the processing parameters on the film properties. In this work the elastic material parameters of anodized aluminum were investigated using a laser-based ultrasound system. The anodized films were characterized analyzing the dispersion of Rayleigh waves with a one-layer model. It was shown that anodizing time and temperature strongly influence Rayleigh wave propagation.

Electrochemical mineral scale prevention and removal on electrically conducting carbon nanotube--polyamide reverse osmosis membranes.

PubMed

Duan, Wenyan; Dudchenko, Alexander; Mende, Elizabeth; Flyer, Celeste; Zhu, Xiaobo; Jassby, David

2014-05-01

The electrochemical prevention and removal of CaSO4 and CaCO3 mineral scales on electrically conducting carbon nanotube - polyamide reverse osmosis membrane was investigated. Different electrical potentials were applied to the membrane surface while filtering model scaling solutions with high saturation indices. Scaling progression was monitored through flux measurements. CaCO3 scale was efficiently removed from the membrane surface through the intermittent application of a 2.5 V potential to the membrane surface, when the membrane acted as an anode. Water oxidation at the anode, which led to proton formation, resulted in the dissolution of deposited CaCO3 crystals. CaSO4 scale formation was significantly retarded through the continuous application of 1.5 V DC to the membrane surface, when the membrane was operated as an anode. The continuous application of a sufficient electrical potential to the membrane surface leads to the formation of a thick layer of counter-ions along the membrane surface that pushed CaSO4 crystal formation away from the membrane surface, allowing the formed crystals to be carried away by the cross-flow. We developed a simple model, based on a modified Poisson-Boltzmann equation, which qualitatively explained our observed experimental results.

A Host-Configured Lithium-Sulfur Cell Built on 3D Nickel Photonic Crystal with Superior Electrochemical Performances.

PubMed

Lin, Shengxuan; Yan, Yang; Cai, Zihe; Liu, Lin; Hu, Xiaobin

2018-04-18

The insulator of the sulfur cathode and the easy dendrites growth of the lithium anode are the main barriers for lithium-sulfur cells in commercial application. Here, a 3D NPC@S/3D NPC@Li full cell is reported based on 3D hierarchical and continuously porous nickel photonic crystal (NPC) to solve the problems of sulfur cathode and lithium anode at the same time. In this case, the 3D NPC@S cathode can not only offer a fast transfer of electron and lithium ion, but also effectively prevent the dissolution of polysulfides and the tremendous volume change during cycling, and the 3D NPC@Li anode can efficiently inhibit the growth of lithium dendrites and volume expansion, too. As a result, the cell exhibits a high reversible capacity of 1383 mAh g -1 at 0.5 C (the current density of 837 mA g -1 ), superior rate ability (the reversible capacity of 735 mAh g -1 at the extremely high current density of 16 750 mA g -1 ) with excellent coulombic efficiency of about 100% and an excellent cycle life over 500 cycles with only about 0.026% capacity loss per cycle. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

The Synergistic Effect of Iodide and Sodium Nitrite on the Corrosion Inhibition of Mild Steel in Bicarbonate-Chloride Solution.

PubMed

Eyu, Gaius Debi; Will, Geoffrey; Dekkers, Willem; MacLeod, Jennifer

2016-10-26

The effect of potassium iodide (KI) and sodium nitrite (NaNO₂ inhibitor on the corrosion inhibition of mild steel in chloride bicarbonate solution has been studied using electrochemical techniques. Potentiodynamic polarisation data suggest that, when used in combination, KI and NaNO₂ function together to inhibit reactions at both the anode and the cathode, but predominantly anodic. KI/NO₂ - concentration ratios varied from 2:1 to 2:5; inhibition efficiency was optimized for a ratio of 1:1. The surface morphology and corrosion products were analysed using scanning electron microscopy (SEM) and X-ray diffractometry (XRD). The latter shows that the addition of I - to NO₂ facilitates the formation of a passivating oxide (γ-Fe₂O₃) as compared to NO₂ - alone, decreasing the rate of metal dissolution observed in electrochemical testing. The synergistic effect of KI/NO₂ - inhibition was enhanced under the dynamic conditions associated with testing in a rotating disc electrode.

Performance study of magnesium-sulfur battery using a graphene based sulfur composite cathode electrode and a non-nucleophilic Mg electrolyte.

PubMed

Vinayan, B P; Zhao-Karger, Zhirong; Diemant, Thomas; Chakravadhanula, Venkata Sai Kiran; Schwarzburger, Nele I; Cambaz, Musa Ali; Behm, R Jürgen; Kübel, Christian; Fichtner, Maximilian

2016-02-14

Here we report for the first time the development of a Mg rechargeable battery using a graphene-sulfur nanocomposite as the cathode, a Mg-carbon composite as the anode and a non-nucleophilic Mg based complex in tetraglyme solvent as the electrolyte. The graphene-sulfur nanocomposites are prepared through a new pathway by the combination of thermal and chemical precipitation methods. The Mg/S cell delivers a higher reversible capacity (448 mA h g(-1)), a longer cyclability (236 mA h g(-1) at the end of the 50(th) cycle) and a better rate capability than previously described cells. The dissolution of Mg polysulfides to the anode side was studied by X-ray photoelectron spectroscopy. The use of a graphene-sulfur composite cathode electrode, with the properties of a high surface area, a porous morphology, a very good electronic conductivity and the presence of oxygen functional groups, along with a non-nucleophilic Mg electrolyte gives an improved battery performance.

Computational Examination of Orientation-Dependent Morphological Evolution during the Electrodeposition and Electrodissolution of Magnesium

DOE PAGES

DeWitt, S.; Hahn, N.; Zavadil, K.; ...

2015-12-30

Here a new model of electrodeposition and electrodissolution is developed and applied to the evolution of Mg deposits during anode cycling. The model captures Butler-Volmer kinetics, facet evolution, the spatially varying potential in the electrolyte, and the time-dependent electrolyte concentration. The model utilizes a diffuse interface approach, employing the phase field and smoothed boundary methods. Scanning electron microscope (SEM) images of magnesium deposited on a gold substrate show the formation of faceted deposits, often in the form of hexagonal prisms. Orientation-dependent reaction rate coefficients were parameterized using the experimental SEM images. Three-dimensional simulations of the growth of magnesium deposits yieldmore » deposit morphologies consistent with the experimental results. The simulations predict that the deposits become narrower and taller as the current density increases due to the depletion of the electrolyte concentration near the sides of the deposits. Increasing the distance between the deposits leads to increased depletion of the electrolyte surrounding the deposit. Two models relating the orientation-dependence of the deposition and dissolution reactions are presented. Finally, the morphology of the Mg deposit after one deposition-dissolution cycle is significantly different between the two orientation-dependence models, providing testable predictions that suggest the underlying physical mechanisms governing morphology evolution during deposition and dissolution.« less

Single-step direct fabrication of pillar-on-pore hybrid nanostructures in anodizing aluminum for superior superhydrophobic efficiency.

PubMed

Jeong, Chanyoung; Choi, Chang-Hwan

2012-02-01

Conventional electrochemical anodizing processes of metals such as aluminum typically produce planar and homogeneous nanopore structures. If hydrophobically treated, such 2D planar and interconnected pore structures typically result in lower contact angle and larger contact angle hysteresis than 3D disconnected pillar structures and, hence, exhibit inferior superhydrophobic efficiency. In this study, we demonstrate for the first time that the anodizing parameters can be engineered to design novel pillar-on-pore (POP) hybrid nanostructures directly in a simple one-step fabrication process so that superior surface superhydrophobicity can also be realized effectively from the electrochemical anodization process. On the basis of the characteristic of forming a self-ordered porous morphology in a hexagonal array, the modulation of anodizing voltage and duration enabled the formulation of the hybrid-type nanostructures having controlled pillar morphology on top of a porous layer in both mild and hard anodization modes. The hybrid nanostructures of the anodized metal oxide layer initially enhanced the surface hydrophilicity significantly (i.e., superhydrophilic). However, after a hydrophobic monolayer coating, such hybrid nanostructures then showed superior superhydrophobic nonwetting properties not attainable by the plain nanoporous surfaces produced by conventional anodization conditions. The well-regulated anodization process suggests that electrochemical anodizing can expand its usefulness and efficacy to render various metallic substrates with great superhydrophilicity or -hydrophobicity by directly realizing pillar-like structures on top of a self-ordered nanoporous array through a simple one-step fabrication procedure.

Fabrication of Well-Ordered, Anodic Aluminum Oxide Membrane Using Hybrid Anodization.

PubMed

Kim, Jungyoon; Ganorkar, Shraddha; Choi, Jinnil; Kim, Young-Hwan; Kim, Seong-II

2017-01-01

Anodic Aluminum Oxide (AAO) is one of the most favorable candidates for fabrication of nano-meshed membrane for various applications due to its controllable pore size and self-ordered structure. The mechanism of AAO membrane is a simple and has been studied by many research groups, however the actual fabrication of membrane has several difficulties owing to its sensitivity of ordering, long anodizing time and unclearness of the pore. In this work, we have demonstrated enhanced process of fabrication symmetric AAO membrane by using “hybrid anodizing” (Hyb-A) method which include mild anodization (MA) followed by hard anodization (HA). This Hyb-A process can give highly ordered membrane with more vivid pore than two-step anodizing process. HA was implemented on the Al plate which has been already textured by MA for more ordered structure and HA plays a key role for formation of more obvious pore in Hyb-A. Our experimental results indicate that Hyb-A with proper process sequence would be one of the fast and useful fabrication methods for the AAO membrane.

Fault Detection and Diagnosis In Hall-Héroult Cells Based on Individual Anode Current Measurements Using Dynamic Kernel PCA

NASA Astrophysics Data System (ADS)

Yao, Yuchen; Bao, Jie; Skyllas-Kazacos, Maria; Welch, Barry J.; Akhmetov, Sergey

2018-04-01

Individual anode current signals in aluminum reduction cells provide localized cell conditions in the vicinity of each anode, which contain more information than the conventionally measured cell voltage and line current. One common use of this measurement is to identify process faults that can cause significant changes in the anode current signals. While this method is simple and direct, it ignores the interactions between anode currents and other important process variables. This paper presents an approach that applies multivariate statistical analysis techniques to individual anode currents and other process operating data, for the detection and diagnosis of local process abnormalities in aluminum reduction cells. Specifically, since the Hall-Héroult process is time-varying with its process variables dynamically and nonlinearly correlated, dynamic kernel principal component analysis with moving windows is used. The cell is discretized into a number of subsystems, with each subsystem representing one anode and cell conditions in its vicinity. The fault associated with each subsystem is identified based on multivariate statistical control charts. The results show that the proposed approach is able to not only effectively pinpoint the problematic areas in the cell, but also assess the effect of the fault on different parts of the cell.

A New Method to Determine the Half-Life for Penicillin Using Microcalorimeter

NASA Astrophysics Data System (ADS)

Li, Z. X.; Zhao, W. W.

2015-01-01

The dissolution process of penicillin in normal saline and isotonic glucose solution was reported using a microcalorimeter. Both the integral and differential heats of solution were measured. The quantitative relationships between the amount of heat released and the quantity of dissolved penicillin were established. Meanwhile, the kinetics and the half-life of the dissolution processes as well as the enthalpy of solution, the entropy of dissolution, and the free energy of dissolution were determined. The results showed that a change of the solvent from normal saline to isotonic glucose solution had little effect on the half-life of penicillin in the dissolution process, and there was no significant difference between the stabilities of penicillin in isotonic glucose solution and normal saline. Moreover, the dissolution process of penicillin in isotonic glucose solution followed the first-order kinetics. These results could provide a theoretical basis for the clinical applications of penicillin.

Influence of laser surface treated on the characterization and corrosion behavior of Al-Fe aerospace alloys

NASA Astrophysics Data System (ADS)

Pariona, Moisés Meza; Teleginski, Viviane; dos Santos, Kelly; de Lima, Angela A. O. C.; Zara, Alfredo J.; Micene, Katieli Tives; Riva, Rudimar

2013-07-01

In this research laser surface remelting without protective coating with a 2 kW Yb-fiber laser (IPG YLR-2000S) was applied in the Al-1.5 wt.%Fe alloy in order to investigate the layer treated with different techniques of superficial characterization, thereby, the technique of optical microscopy, atomic force microscopy and low-angle X-ray diffraction were used. The present work mainly focuses on the corrosion study by diverse techniques in aggressive environment of the laser-treated area and the substrate material was carried out, thereby, at open circuit potential testing, the results have shown a displacement to more anodic values in the corrosion potential for the laser-treated specimen when compared to the untreated specimen; in potentiodynamic polarization tests have shown that as a result of the laser treatment, the corrosion current can be reduced by as much as ten times, and a passive region was obtained, which served as an effective barrier for reducing anodic dissolution and finally, the result in cyclic polarization curves of the untreated sample there was a greater area of the hysteresis loop, implying that it is more susceptible to corrosion. This study was complemented by other techniques mentioned above in order to elucidate this study. Laser surface remelting process has definitely modified the surface film, which results in higher corrosion resistance, a large range of passivation and a lower area of the hysteresis loop.

Effect of electromagnetic interaction during fusion welding of AISI 2205 duplex stainless steel on the corrosion resistance

NASA Astrophysics Data System (ADS)

García-Rentería, M. A.; López-Morelos, V. H.; González-Sánchez, J.; García-Hernández, R.; Dzib-Pérez, L.; Curiel-López, F. F.

2017-02-01

The effect of electromagnetic interaction of low intensity (EMILI) applied during fusion welding of AISI 2205 duplex stainless steel on the resistance to localised corrosion in natural seawater was investigated. The heat affected zone (HAZ) of samples welded under EMILI showed a higher temperature for pitting initiation and lower dissolution under anodic polarisation in chloride containing solutions than samples welded without EMILI. The EMILI assisted welding process developed in the present work enhanced the resistance to localised corrosion due to a modification on the microstructural evolution in the HAZ and the fusion zone during the thermal cycle involved in fusion welding. The application of EMILI reduced the size of the HAZ, limited coarsening of the ferrite grains and promoted regeneration of austenite in this zone, inducing a homogeneous passive condition of the surface. EMILI can be applied during fusion welding of structural or functional components of diverse size manufactured with duplex stainless steel designed to withstand aggressive environments such as natural seawater or marine atmospheres.

The mutual co-regulation of extracellular polymeric substances and iron ions in biocorrosion of cast iron pipes.

PubMed

Jin, Juntao; Guan, Yuntao

2014-10-01

New insights into the biocorrosion process may be gained through understanding of the interaction between extracellular polymeric substances (EPS) and iron. Herein, the effect of iron ions on the formation of biofilms and production of EPS was investigated. Additionally, the impact of EPS on the corrosion of cast iron coupons was explored. The results showed that a moderate concentration of iron ions (0.06 mg/L) promoted both biofilm formation and EPS production. The presence of EPS accelerated corrosion during the initial stage, while inhibited corrosion at the later stage. The functional groups of EPS acted as electron shuttles to enable the binding of iron ions. Binding of iron ions with EPS led to anodic dissolution and promoted corrosion, while corrosion was later inhibited through oxygen reduction and availability of phosphorus from EPS. The presence of EPS also led to changes in crystalline phases of corrosion products. Copyright © 2014 Elsevier Ltd. All rights reserved.

Structure-Property Relationships of Organic Electrolytes and Their Effects on Li/S Battery Performance.

PubMed

Kaiser, Mohammad Rejaul; Chou, Shulei; Liu, Hua-Kun; Dou, Shi-Xue; Wang, Chunsheng; Wang, Jiazhao

2017-12-01

Electrolytes, which are a key component in electrochemical devices, transport ions between the sulfur/carbon composite cathode and the lithium anode in lithium-sulfur batteries (LSBs). The performance of a LSB mostly depends on the electrolyte due to the dissolution of polysulfides into the electrolyte, along with the formation of a solid-electrolyte interphase. The selection of the electrolyte and its functionality during charging and discharging is intricate and involves multiple reactions and processes. The selection of the proper electrolyte, including solvents and salts, for LSBs strongly depends on its physical and chemical properties, which is heavily controlled by its molecular structure. In this review, the fundamental properties of organic electrolytes for LSBs are presented, and an attempt is made to determine the relationship between the molecular structure and the properties of common organic electrolytes, along with their effects on the LSB performance. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Electrowinning process with electrode compartment to avoid contamination of electrolyte

DOEpatents

Poa, Davis S.; Pierce, R. Dean; Mulcahey, Thomas P.; Johnson, Gerald K.

1993-01-01

An electrolytic process and apparatus for reducing calcium oxide in a molten electrolyte of CaCl.sub.2 -CaF.sub.2 with a graphite anode in which particles or other contamination from the anode is restricted by the use of a porous barrier in the form of a basket surrounding the anode which may be removed from the electrolyte to burn the graphite particles, and wherein the calcium oxide feed is introduced to the anode compartment to increase the oxygen ion concentration at the anode.

Processing Ti-25Ta-5Zr Bioalloy via Anodic Oxidation Procedure at High Voltage

NASA Astrophysics Data System (ADS)

Ionita, Daniela; Grecu, Mihaela; Dilea, Mirela; Cojocaru, Vasile Danut; Demetrescu, Ioana

2011-12-01

The current paper reports the processing of Ti-25Ta-5Zr bioalloy via anodic oxidation in NH4BF4 solution under constant potentiostatic conditions at high voltage to obtain more suitable properties for biomedical application. The maximum efficiency of the procedure is reached at highest applied voltage, when the corrosion rate in Hank's solution is decreased approxomately six times. The topography of the anodic layer has been studied using atomic force microscopy (AFM), and the results indicated that the anodic oxidation process increases the surface roughness. The AFM images indicated a different porosity for the anodized surfaces as well. After anodizing, the hydrophilic character of Ti-25Ta-5Zr samples has increased. A good correlation between corrosion rate obtained from potentiodynamic curves and corrosion rate from ions release analysis was obtained.

Recovery of Silver and Gold from Copper Anode Slimes

NASA Astrophysics Data System (ADS)

Chen, Ailiang; Peng, Zhiwei; Hwang, Jiann-Yang; Ma, Yutian; Liu, Xuheng; Chen, Xingyu

2015-02-01

Copper anode slimes, produced from copper electrolytic refining, are important industrial by-products containing several valuable metals, particularly silver and gold. This article provides a comprehensive overview of the development of the extraction processes for recovering silver and gold from conventional copper anode slimes. Existing processes, namely pyrometallurgical processes, hydrometallurgical processes, and hybrid processes involving the combination of pyrometallurgical and hydrometallurgical technologies, are discussed based in part on a review of the form and characteristics of silver and gold in copper anode slimes. The recovery of silver and gold in pyrometallurgical processes is influenced in part by the slag and matte/metal chemistry and related characteristics, whereas the extraction of these metals in hydrometallurgical processes depends on the leaching reagents used to break the structure of the silver- and gold-bearing phases, such as selenides. By taking advantage of both pyrometallurgical and hydrometallurgical techniques, high extraction yields of silver and gold can be obtained using such combined approaches that appear promising for efficient extraction of silver and gold from copper anode slimes.

Porous carbon-free SnSb anodes for high-performance Na-ion batteries

NASA Astrophysics Data System (ADS)

Choi, Jeong-Hee; Ha, Choong-Wan; Choi, Hae-Young; Seong, Jae-Wook; Park, Cheol-Min; Lee, Sang-Min

2018-05-01

A simple melt-spinning/chemical-etching process is developed to create porous carbon-free SnSb anodes. Sodium ion batteries (SIBs) incorporating these anodes exhibit excellent electrochemical performances by accomodating large volume changes during repeated cycling. The porous carbon-free SnSb anode produced by the melt-spinning/chemical-etching process shows a high reversible capacity of 481 mAh g-1, high ICE of 80%, stable cyclability with a high capacity retention of 99% after 100 cycles, and a fast rate capability of 327 mAh g-1 at 4C-rate. Ex-situ X-ray diffraction and high resolution-transmission electron microscopy analyses demonstrate that the synthesized porous carbon-free SnSb anodes involve the highly reversible reaction with sodium through the conversion and recombination reactions during sodiation/desodiation process. The novel and simple melt-spinning/chemical-etching synthetic process represents a technological breakthrough in the commercialization of Na alloy-able anodes for SIBs.

Novel structure formation at the bottom surface of porous anodic alumina fabricated by single step anodization process.

PubMed

Ali, Ghafar; Ahmad, Maqsood; Akhter, Javed Iqbal; Maqbool, Muhammad; Cho, Sung Oh

2010-08-01

A simple approach for the growth of long-range highly ordered nanoporous anodic alumina film in H(2)SO(4) electrolyte through a single step anodization without any additional pre-anodizing procedure is reported. Free-standing porous anodic alumina film of 180 microm thickness with through hole morphology was obtained. A simple and single step process was used for the detachment of alumina from aluminum substrate. The effect of anodizing conditions, such as anodizing voltage and time on the pore diameter and pore ordering is discussed. The metal/oxide and oxide/electrolyte interfaces were examined by high resolution scanning transmission electron microscope. The arrangement of pores on metal/oxide interface was well ordered with smaller diameters than that of the oxide/electrolyte interface. The inter-pore distance was larger in metal/oxide interface as compared to the oxide/electrolyte interface. The size of the ordered domain was found to depend strongly upon anodizing voltage and time. (c) 2010 Elsevier Ltd. All rights reserved.

Light metal production

DOEpatents

Fan, Qinbai

2016-04-19

An electrochemical process for the production of light metals, particularly aluminum. Such a process involves contacting a light metal source material with an inorganic acid to form a solution containing the light metal ions in high concentration. The solution is fed to an electrochemical reactor assembly having an anode side containing an anode and a cathode side containing a cathode, with anode side and the cathode side separated by a bipolar membrane, with the solution being fed to the anode side. Light metal ions are electrochemically transferred through the bipolar membrane to the cathode side. The process further involves reducing the light metal ions to light metal powder. An associated processing system is also provided.

Glass fiber dissolution in simulated lung fluid and measures needed to improve consistency and correspondence to in vivo dissolution.

PubMed Central

Mattson, S M

1994-01-01

The dissolution of a range of glass fibers including commercial glass and mineral wools has been studied using a modification of Gamble's solution in a flow system at pH 7.4 and 37 degrees C. Dissolution has been followed by weight loss, effluent analysis, and morphology change of fibers and bulk glass. Flow per glass surface area can strongly affect both dissolution rate and morphology due to the effect of the dissolution process on the fluid. Effluent pH is shown to be a guide for choice of optimum flow/area conditions. These conditions provide measurable concentrations of dissolved glass in the effluent while maintaining their concentrations below the point at which they significantly affect the dissolution process. SiO2 and Al2O3 vary widely in the extent to which they are involved in the leaching process, which removes alkalis, alkaline earths, and B2O3. This makes analysis of a single component in the effluent unsuitable as a means of comparing the dissolution rates of a wide range of compositions. PMID:7882963

The alkaline zinc electrode as a mixed potential system

NASA Technical Reports Server (NTRS)

Fielder, W. L.

1979-01-01

Cathodic and anodic processes for the alkaline zinc electrode in 0.01 molar zincate electrolyte (9 molar hydroxide) were investigated. Cyclic voltammograms and current-voltage curves were obtained by supplying pulses through a potentiostat to a zinc rotating disk electrode. The data are interpreted by treating the system as one with a mixed potential; the processes are termed The zincate and corrosion reactions. The relative proportions of the two processes vary with the supplied potential. For the cathodic region, the cathodic corrosion process predominates at higher potentials while both processes occur simultaneously at a lower potential (i.e., 50 mV). For the anodic region, the anodic zincate process predominates at higher potentials while the anodic corrosion process is dominant at lower potential (i.e., 50 mV) if H2 is present.

Solid oxide membrane-assisted controllable electrolytic fabrication of metal carbides in molten salt.

PubMed

Zou, Xingli; Zheng, Kai; Lu, Xionggang; Xu, Qian; Zhou, Zhongfu

2016-08-15

Silicon carbide (SiC), titanium carbide (TiC), zirconium carbide (ZrC), and tantalum carbide (TaC) have been electrochemically produced directly from their corresponding stoichiometric metal oxides/carbon (MOx/C) precursors by electrodeoxidation in molten calcium chloride (CaCl2). An assembled yttria stabilized zirconia solid oxide membrane (SOM)-based anode was employed to control the electrodeoxidation process. The SOM-assisted controllable electrochemical process was carried out in molten CaCl2 at 1000 °C with a potential of 3.5 to 4.0 V. The reaction mechanism of the electrochemical production process and the characteristics of these produced metal carbides (MCs) were systematically investigated. X-ray diffraction, scanning electron microscopy, and transmission electron microscopy analyses clearly identify that SiC, TiC, ZrC, and TaC carbides can be facilely fabricated. SiC carbide can be controlled to form a homogeneous nanowire structure, while the morphologies of TiC, ZrC, and TaC carbides exhibit porous nodular structures with micro/nanoscale particles. The complex chemical/electrochemical reaction processes including the compounding, electrodeoxidation, dissolution-electrodeposition, and in situ carbonization processes in molten CaCl2 are also discussed. The present results preliminarily demonstrate that the molten salt-based SOM-assisted electrodeoxidation process has the potential to be used for the facile and controllable electrodeoxidation of MOx/C precursors to micro/nanostructured MCs, which can potentially be used for various applications.

Stainless steel anodes for alkaline water electrolysis and methods of making

DOEpatents

Soloveichik, Grigorii Lev

2014-01-21

The corrosion resistance of stainless steel anodes for use in alkaline water electrolysis was increased by immersion of the stainless steel anode into a caustic solution prior to electrolysis. Also disclosed herein are electrolyzers employing the so-treated stainless steel anodes. The pre-treatment process provides a stainless steel anode that has a higher corrosion resistance than an untreated stainless steel anode of the same composition.

Effect drug loading process on dissolution mechanism of encapsulated amoxicillin trihydrate in hydrogel semi-IPN chitosan methyl cellulose with pore forming agent KHCO3 as a floating drug delivery system

NASA Astrophysics Data System (ADS)

Fithawati, Garnis; Budianto, Emil

2018-04-01

Common treatment for Helicobacter pylori by repeated oral consumption of amoxicillin trihydrate is not effective. Amoxicillin trihydrate has a very short residence time in stomach which leads into its ineffectiveness. Residence time of amoxicillin trihydrate can be improved by encapsulating amoxicillin trihydrate into a floating drug delivery system. In this study, amoxicillin trihydrate is encapsulated into hydrogel semi-IPN chitosan methyl cellulose matrix as a floating drug delivery system and then treated with 20% KHCO3 as pore forming agent. Drug loading process used are in-situ loading and post loading. In-situ loading process has higher efficiency percentage and dissolution percentage than post loading process. In-situ loading process resulted 100% efficiency with 92,70% dissolution percentage. Post loading process resulted 98,7% efficiency with 90,42% dissolution percentage. Mechanism of drug dissolution study by kinetics approach showed both in-situ loading process and post loading process are diffusion and degradation process (n=0,4913) and (n=0,4602) respectively. These results are supported by characterization data from optical microscope and scanning electron microscopy (SEM). Data from optical microscope showed both loading process resulted in coarser hydrogel surface. Characterization using SEM showed elongated pores in both loading process after dissolution test.

Modelling the growth process of porous aluminum oxide film during anodization

NASA Astrophysics Data System (ADS)

Aryslanova, E. M.; Alfimov, A. V.; Chivilikhin, S. A.

2015-11-01

Currently it has become important for the development of metamaterials and nanotechnology to obtain regular self-assembled structures. One such structure is porous anodic alumina film that consists of hexagonally packed cylindrical pores. In this work we consider the anodization process, our model takes into account the influence of layers of aluminum and electrolyte on the rate of growth of aluminum oxide, as well as the effect of surface diffusion. In present work we consider those effects. And as a result of our model we obtain the minimum distance between centers of alumina pores in the beginning of anodizing process.

Direct electrolytic dissolution of silicate minerals for air CO2 mitigation and carbon-negative H2 production

PubMed Central

Rau, Greg H.; Carroll, Susan A.; Bourcier, William L.; Singleton, Michael J.; Smith, Megan M.; Aines, Roger D.

2013-01-01

We experimentally demonstrate the direct coupling of silicate mineral dissolution with saline water electrolysis and H2 production to effect significant air CO2 absorption, chemical conversion, and storage in solution. In particular, we observed as much as a 105-fold increase in OH− concentration (pH increase of up to 5.3 units) relative to experimental controls following the electrolysis of 0.25 M Na2SO4 solutions when the anode was encased in powdered silicate mineral, either wollastonite or an ultramafic mineral. After electrolysis, full equilibration of the alkalized solution with air led to a significant pH reduction and as much as a 45-fold increase in dissolved inorganic carbon concentration. This demonstrated significant spontaneous air CO2 capture, chemical conversion, and storage as a bicarbonate, predominantly as NaHCO3. The excess OH− initially formed in these experiments apparently resulted via neutralization of the anolyte acid, H2SO4, by reaction with the base mineral silicate at the anode, producing mineral sulfate and silica. This allowed the NaOH, normally generated at the cathode, to go unneutralized and to accumulate in the bulk electrolyte, ultimately reacting with atmospheric CO2 to form dissolved bicarbonate. Using nongrid or nonpeak renewable electricity, optimized systems at large scale might allow relatively high-capacity, energy-efficient (<300 kJ/mol of CO2 captured), and inexpensive (<$100 per tonne of CO2 mitigated) removal of excess air CO2 with production of carbon-negative H2. Furthermore, when added to the ocean, the produced hydroxide and/or (bi)carbonate could be useful in reducing sea-to-air CO2 emissions and in neutralizing or offsetting the effects of ongoing ocean acidification. PMID:23729814

Spontaneous Water Oxidation at Hematite (α-Fe2O3) Crystal Faces

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chatman, Shawn ME; Zarzycki, Piotr P.; Rosso, Kevin M.

2015-01-28

Hematite (α-Fe2O3) persists as a promising candidate for photoelectrochemical water splitting but a slow oxygen evolution reaction (OER) at its surfaces remains a limitation. Here we extend a series of studies that examine pH-dependent surface potentials and electron transfer properties of effectively perfect low-index crystal faces of hematite in contact with simple electrolyte. Zero resistance amperometry was performed in a two electrode configuration to quantify spontaneous dark current between hematite crystal face pairs (001)/(012), (001)/(113), and (012)/(113) at pH 3. Exponentially decaying currents initially of up to 200 nA were reported between faces over four minute experiments. Fourth order ZRAmore » kinetics indicated rate limitation by the OER for current that flows between (001)/(012) and (001)/(113) face pairs, with the (012) and (113) faces serving as the anodes when paired with (001). The cathodic partner reaction is reductive dissolution of the (001) face, converting surface Fe3+ to solubilized aqueous Fe2+, at a rate maintained by the OER at the anode. In contrast, OER rate limitation does not manifest for the (012)/(113) pair. The uniqueness of the (001) face is established in terms of a faster intrinsic ability to accept the protons required for the reductive dissolution reaction. OER rate limitation inversely may thus arise from sluggish kinetics of hematite surfaces to dispense with the protons that accompany the four-electron OER. The results are explained in terms of semi-quantitative energy band diagrams. The finding may be useful as a consideration for tailoring the design of polycrystalline hematite photoanodes that present multiple terminations to the interface with electrolyte.« less

Natural gas anodes for aluminium electrolysis in molten fluorides.

PubMed

Haarberg, Geir Martin; Khalaghi, Babak; Mokkelbost, Tommy

2016-08-15

Industrial primary production of aluminium has been developed and improved over more than 100 years. The molten salt electrolysis process is still suffering from low energy efficiency and considerable emissions of greenhouse gases (CO2 and PFC). A new concept has been suggested where methane is supplied through the anode so that the CO2 emissions may be reduced significantly, the PFC emissions may be eliminated and the energy consumption may decrease significantly. Porous carbon anodes made from different graphite grades were studied in controlled laboratory experiments. The anode potential, the anode carbon consumption and the level of HF gas above the electrolyte were measured during electrolysis. In some cases it was found that the methane oxidation was effectively participating in the anode process.

Surface characteristics, corrosion and bioactivity of chemically treated biomedical grade NiTi alloy.

PubMed

Chembath, Manju; Balaraju, J N; Sujata, M

2015-11-01

The surface of NiTi alloy was chemically modified using acidified ferric chloride solution and the characteristics of the alloy surface were studied from the view point of application as a bioimplant. Chemically treated NiTi was also subjected to post treatments by annealing at 400°C and passivation in nitric acid. The surface of NiTi alloy after chemical treatment developed a nanogrid structure with a combination of one dimensional channel and two dimensional network-like patterns. From SEM studies, it was found that the undulations formed after chemical treatment remained unaffected after annealing, while after passivation process the undulated surface was filled with oxides of titanium. XPS analysis revealed that the surface of passivated sample was enriched with oxides of titanium, predominantly TiO2. The influence of post treatment on the corrosion resistance of chemically treated NiTi alloy was monitored using Potentiodynamic Polarization and Electrochemical Impedance Spectroscopy (EIS) in Phosphate Buffered Saline (PBS) solution. In the chemically treated condition, NiTi alloy exhibited poor corrosion resistance due to the instability of the surface. On the other hand, the breakdown potential (0.8V) obtained was highest for the passivated samples compared to other surface treated samples. During anodic polarization, chemically treated samples displayed dissolution phenomenon which was predominantly activation controlled. But after annealing and passivation processes, the behavior of anodic polarization was typical of a diffusion controlled process which confirmed the enhanced passivity of the post treated surfaces. The total resistance, including the porous and barrier layer, was in the range of mega ohms for passivated surfaces, which could be attributed to the decrease in surface nickel content and formation of compact titanium oxide. The passivated sample displayed good bioactivity in terms of hydroxyapatite growth, noticed after 14days immersion in Hanks' solution. Copyright © 2015 Elsevier B.V. All rights reserved.

Effects of Bacillus subtilis endospore surface reactivity on the rate of forsterite dissolution

NASA Astrophysics Data System (ADS)

Harrold, Z.; Gorman-Lewis, D.

2013-12-01

Primary mineral dissolution products, such as silica (Si), calcium (Ca) and magnesium (Mg), play an important role in numerous biologic and geochemical cycles including microbial metabolism, plant growth and secondary mineral precipitation. The flux of these and other dissolution products into the environment is largely controlled by the rate of primary silicate mineral dissolution. Bacteria, a ubiquitous component in water-rock systems, are known to facilitate mineral dissolution and may play a substantial role in determining the overall flux of dissolution products into the environment. Bacterial cell walls are complex and highly reactive organic surfaces that can affect mineral dissolution rates directly through microbe-mineral adsorption or indirectly by complexing dissolution products. The effect of bacterial surface adsorption on chemical weathering rates may even outweigh the influence of active processes in environments where a high proportion of cells are metabolically dormant or cell metabolism is slow. Complications associated with eliminating or accounting for ongoing metabolic processes in long-term dissolution studies have made it challenging to isolate the influence of cell wall interactions on mineral dissolution rates. We utilized Bacillus subtilis endospores, a robust and metabolically dormant cell type, to isolate and quantify the effects of bacterial surface reactivity on forsterite (Mg2SiO4) dissolution rates. We measured the influence of both direct and indirect microbe-mineral interactions on forsterite dissolution. Indirect pathways were isolated using dialysis tubing to prevent mineral-microbe contact while allowing free exchange of dissolved mineral products and endospore-ion adsorption. Homogenous experimental assays allowed both direct microbe-mineral and indirect microbe-ion interactions to affect forsterite dissolution rates. Dissolution rates were calculated based on silica concentrations and zero-order dissolution kinetics. Additional analyses including Mg concentrations, microprobe and BET analyses support mineral dissolution rate calculations and stoichiometry considerations. All experimental assays containing endospores show increased forsterite dissolution rates relative to abiotic controls. Forsterite dissolution rates increased by approximately one order of magnitude in dialysis bound, biotic experiments relative to abiotic assays. Homogenous biotic assays exhibited a more complex dissolution rate profile that changes over time. All microbially mediated forsterite dissolution rates returned to abiotic control rates after 10 to 15 days of incubation. This shift in dissolution rate likely corresponds to maximum endospore surface adsorption capacity. The Bacillus subtilis endospore surface serves as a first-order proxy for studying the effect of metabolizing microbe surfaces on silicate dissolution rates. Comparisons with published abiotic, microbial, and organic acid mediated forsterite dissolution rates will provide insight on the importance of bacterial surfaces in primary mineral dissolution processes.

Preparation, characterization and in vivo evaluation of amorphous atorvastatin calcium nanoparticles using supercritical antisolvent (SAS) process.

PubMed

Kim, Min-Soo; Jin, Shun-Ji; Kim, Jeong-Soo; Park, Hee Jun; Song, Ha-Seung; Neubert, Reinhard H H; Hwang, Sung-Joo

2008-06-01

In this work, amorphous atorvastatin calcium nanoparticles were successfully prepared using the supercritical antisolvent (SAS) process. The effect of process variables on particle size and distribution of atorvastatin calcium during particle formation was investigated. Solid state characterization, solubility, intrinsic dissolution, powder dissolution studies and pharmacokinetic study in rats were performed. Spherical particles with mean particle size ranging between 152 and 863 nm were obtained by varying process parameters such as precipitation vessel pressure and temperature, drug solution concentration and feed rate ratio of CO2/drug solution. XRD, TGA, FT-IR, FT-Raman, NMR and HPLC analysis indicated that atorvastatin calcium existed as anhydrous amorphous form and no degradation occurred after SAS process. When compared with crystalline form (unprocessed drug), amorphous atorvastatin calcium nanoparticles were of better performance in solubility and intrinsic dissolution rate, resulting in higher solubility and faster dissolution rate. In addition, intrinsic dissolution rate showed a good correlation with the solubility. The dissolution rates of amorphous atorvastatin calcium nanoparticles were highly increased in comparison with unprocessed drug by the enhancement of intrinsic dissolution rate and the reduction of particle size resulting in an increased specific surface area. The absorption of atorvastatin calcium after oral administration of amorphous atorvastatin calcium nanoparticles to rats was markedly increased.

26 CFR 301.6501(d)-1 - Request for prompt assessment.

Code of Federal Regulations, 2014 CFR

2014-04-01

... which is contemplating dissolution, is in the process of dissolution, or has been dissolved, may be... that the corporation contemplates dissolution at or before the expiration of such 18-month period; the dissolution is in good faith begun before the expiration of such 18-month period; and the dissolution so begun...

27 CFR 70.74 - Request for prompt assessment.

Code of Federal Regulations, 2014 CFR

2014-04-01

... contemplating dissolution, is in the process of dissolution, or has been dissolved, may be liable, shall be... dissolution at or before the expirationof such 18-month period; the dissolution is in good faith begun before the expiration of such 18-month period; and the dissolution so begun is completed either before or...

27 CFR 70.74 - Request for prompt assessment.

Code of Federal Regulations, 2012 CFR

2012-04-01

... contemplating dissolution, is in the process of dissolution, or has been dissolved, may be liable, shall be... dissolution at or before the expirationof such 18-month period; the dissolution is in good faith begun before the expiration of such 18-month period; and the dissolution so begun is completed either before or...

27 CFR 70.74 - Request for prompt assessment.

Code of Federal Regulations, 2010 CFR

2010-04-01

... contemplating dissolution, is in the process of dissolution, or has been dissolved, may be liable, shall be... dissolution at or before the expirationof such 18-month period; the dissolution is in good faith begun before the expiration of such 18-month period; and the dissolution so begun is completed either before or...

27 CFR 70.74 - Request for prompt assessment.

Code of Federal Regulations, 2013 CFR

2013-04-01

... contemplating dissolution, is in the process of dissolution, or has been dissolved, may be liable, shall be... dissolution at or before the expirationof such 18-month period; the dissolution is in good faith begun before the expiration of such 18-month period; and the dissolution so begun is completed either before or...

26 CFR 301.6501(d)-1 - Request for prompt assessment.

Code of Federal Regulations, 2012 CFR

2012-04-01

... which is contemplating dissolution, is in the process of dissolution, or has been dissolved, may be... that the corporation contemplates dissolution at or before the expiration of such 18-month period; the dissolution is in good faith begun before the expiration of such 18-month period; and the dissolution so begun...

26 CFR 301.6501(d)-1 - Request for prompt assessment.

Code of Federal Regulations, 2011 CFR

2011-04-01

... which is contemplating dissolution, is in the process of dissolution, or has been dissolved, may be... that the corporation contemplates dissolution at or before the expiration of such 18-month period; the dissolution is in good faith begun before the expiration of such 18-month period; and the dissolution so begun...

27 CFR 70.74 - Request for prompt assessment.

Code of Federal Regulations, 2011 CFR

2011-04-01

... contemplating dissolution, is in the process of dissolution, or has been dissolved, may be liable, shall be... dissolution at or before the expirationof such 18-month period; the dissolution is in good faith begun before the expiration of such 18-month period; and the dissolution so begun is completed either before or...

26 CFR 301.6501(d)-1 - Request for prompt assessment.

Code of Federal Regulations, 2013 CFR

2013-04-01

... which is contemplating dissolution, is in the process of dissolution, or has been dissolved, may be... that the corporation contemplates dissolution at or before the expiration of such 18-month period; the dissolution is in good faith begun before the expiration of such 18-month period; and the dissolution so begun...

26 CFR 301.6501(d)-1 - Request for prompt assessment.

Code of Federal Regulations, 2010 CFR

2010-04-01

... which is contemplating dissolution, is in the process of dissolution, or has been dissolved, may be... that the corporation contemplates dissolution at or before the expiration of such 18-month period; the dissolution is in good faith begun before the expiration of such 18-month period; and the dissolution so begun...

Effect of alloying elements Al and Ca on corrosion resistance of plasma anodized Mg alloys

NASA Astrophysics Data System (ADS)

Anawati, Asoh, Hidetaka; Ono, Sachiko

2016-04-01

Plasma anodizing is a surface treatment used to form a ceramic-type oxide film on Mg alloys by the application of a high anodic voltage to create intense plasma near the metal surface. With proper selection of the process parameters, the technique can produce high quality oxide with superior adhesion, corrosion resistance, micro-hardness, wear resistance and strength. The effect of alloying element Al on plasma anodizing process of Mg alloys was studied by comparing the anodizing curves of pure Mg, AZ31, and AZ61 alloys while the effect of Ca were studied on AZ61 alloys containing 0, 1, and 2 wt% Ca. Anodizing was performed in 0.5 M Na3PO4 solution at a constant current density of 200 Am-2 at 25°C. Anodic oxide films with lava-like structure having mix composition of amorphous and crystal were formed on all of the alloys. The main crystal form of the oxide was Mg3(PO4)2 as analyzed by XRD. Alloying elements Al and Ca played role in modifying the plasma lifetime during anodization. Al tended to extend the strong plasma lifetime and therefore accelerated the film thickening. The effect of Ca on anodizing process was still unclear. The anodic film thickness and chemical composition were altered by the presence of Ca in the alloys. Electrochemical corrosion test in 0.9% NaCl solution showed that the corrosion behavior of the anodized specimens depend on the behavior of the substrate. Increasing Al and Ca content in the alloys tended to increase the corrosion resistance of the specimens. The corrosion resistance of the anodized specimens improved significantly about two orders of magnitude relative to the bare substrate.

Microbial fuel cell treatment of ethanol fermentation process water

DOEpatents

Borole, Abhijeet P [Knoxville, TN

2012-06-05

The present invention relates to a method for removing inhibitor compounds from a cellulosic biomass-to-ethanol process which includes a pretreatment step of raw cellulosic biomass material and the production of fermentation process water after production and removal of ethanol from a fermentation step, the method comprising contacting said fermentation process water with an anode of a microbial fuel cell, said anode containing microbes thereon which oxidatively degrade one or more of said inhibitor compounds while producing electrical energy or hydrogen from said oxidative degradation, and wherein said anode is in electrical communication with a cathode, and a porous material (such as a porous or cation-permeable membrane) separates said anode and cathode.

Dissolution profile of dolomite in chloric acid solution: The effect of chloric acid concentration and pulp density

NASA Astrophysics Data System (ADS)

Solihin, Indriani, Mubarok, M. Zaki

2018-05-01

Dolomite is one of carbonate minerals that contain magnesium. Magnesium is important element used in many aspects of life such as cofactor of many enzymes in human body, nutrient for plants, and raw material in automotive industry. Dolomite can be processed through low temperature process to obtain magnesium and calcium oxide that is needed in important applications such as base material for making drugs, raw material in the synthesize slow release fertilizer, materials for fire retardant, component for catalyst, etc. One of the important step of this low temperature process is dissolution of dolomite. Optimizing the dissolution process determines the % extraction of magnesium and calcium oxide from dolomite. The dissolution of dolomite from Gresik, East Java Provence Indonesia, in chloric acid solution has been conducted. Chloric acid concentration and pulp density are the variables that were observed. The dissolution of magnesium and calcium from Gresik dolomite was found to be very fast. The stable stage of dissolution can be reached for 5-10 seconds. The % extraction is mainly determined by the molar ratio of chloric acid / dolomite. At molar ratio of chloric acid / dolomite equal or above stoichiometric of dolomite dissolution, % extraction of magnesium is almost 100 %.

Investigation of carbon supported PtW catalysts as CO tolerant anodes at high temperature in proton exchange membrane fuel cell

NASA Astrophysics Data System (ADS)

Hassan, Ayaz; Paganin, Valdecir A.; Ticianelli, Edson A.

2016-09-01

The CO tolerance mechanism and the stability of carbon supported PtW electrocatalysts are evaluated in the anode of a proton exchange membrane fuel cell (PEMFC) at two different temperatures. The electrocatalysts are characterized by energy dispersive spectroscopy, X-ray diffraction, and transmission electron spectroscopy. Employed electrochemical techniques include cyclic voltammetry, CO stripping, fuel cell polarization, and online mass spectrometry. At a cell temperature of 85 °C, the PtW/C catalyst shows higher CO tolerance compared to Pt/C due an electronic effect of WOx in the Pt 5d band, which reduces the CO adsorption. An increase in hydrogen oxidation activity in the presence of CO is observed for both the catalysts at a higher temperature, due to the decrease of the Pt-CO coverage. A reduction in the current densities occurs for the PtW/C catalyst in both polarization curves and cyclic voltammograms after 5000 cycles of the anode in the range of 0.1-0.7 V vs. RHE at 50 mVs-1. This decrease in performance is assigned to the dissolution of W, with a consequent increase in the membrane resistivity. However, the observed decline of performance is small either in the presence of pure H2 or in the presence of H2/CO.

Lithium rich cathode/graphite anode combination for lithium ion cells with high tolerance to near zero volt storage

NASA Astrophysics Data System (ADS)

Crompton, K. R.; Staub, J. W.; Hladky, M. P.; Landi, B. J.

2017-03-01

Management of reversible lithium is an advantageous approach to design lithium ion cells that are tolerant to near zero volt (NZV) storage under fixed resistive load towards highly controllable, enhanced user-inactive safety. Presently, the first cycle loss from a high energy density Li-rich HE5050 cathode is used to provide excess reversible lithium when paired with an appropriately capacity matched mesocarbon microbead (MCMB) anode. Cells utilizing 1.2 M LiPF6 3:7 v/v ethylene carbonate:ethyl methyl carbonate electrolyte and a lithium reference were used for 3-electrode testing. After conditioning, a fixed resistive load was applied to 3-electrode cells for 72 or 168-h during which the anode potential and electrode asymptotic potential (EAP) remained less than the copper dissolution potential. After multiple storage cycles (room temperature or 40 °C), the NZV coulombic efficiency (cell reversibility) exceeded 97% and the discharge capacity retention was >98%. Conventional 2-electrode HE5050/MCMB pouch cells stored at NZV or open circuit for 3 days had nearly identical rate capability (up to 5C) and discharge performance stability (for 500 cycles under a 30% depth of discharge low-earth-orbit regime). Thus, lithium ion cells with appropriately capacity matched HE5050/MCMB electrodes have excellent tolerance to prolonged NZV storage, which can lead to enhanced user-inactive safety.

A Database Approach for Predicting and Monitoring Baked Anode Properties

NASA Astrophysics Data System (ADS)

Lauzon-Gauthier, Julien; Duchesne, Carl; Tessier, Jayson

2012-11-01

The baked anode quality control strategy currently used by most carbon plants based on testing anode core samples in the laboratory is inadequate for facing increased raw material variability. The low core sampling rate limited by lab capacity and the common practice of reporting averaged properties based on some anode population mask a significant amount of individual anode variability. In addition, lab results are typically available a few weeks after production and the anodes are often already set in the reduction cells preventing early remedial actions when necessary. A database approach is proposed in this work to develop a soft-sensor for predicting individual baked anode properties at the end of baking cycle. A large historical database including raw material properties, process operating parameters and anode core data was collected from a modern Alcoa plant. A multivariate latent variable PLS regression method was used for analyzing the large database and building the soft-sensor model. It is shown that the general low frequency trends in most anode physical and mechanical properties driven by raw material changes are very well captured by the model. Improvements in the data infrastructure (instrumentation, sampling frequency and location) will be necessary for predicting higher frequency variations in individual baked anode properties. This paper also demonstrates how multivariate latent variable models can be interpreted against process knowledge and used for real-time process monitoring of carbon plants, and detection of faults and abnormal operation.

Interface dissolution control of the 14C profile in marine sediment

USGS Publications Warehouse

Keir, R.S.; Michel, R.L.

1993-01-01

The process of carbonate dissolution at the sediment-water interface has two possible endmember boundary conditions. Either the carbonate particles dissolve mostly before they are incorporated into the sediment by bioturbation (interface dissolution), or the vertical mixing is rapid relative to their extermination rate (homogeneous dissolution). In this study, a detailed radiocarbon profile was determined in deep equatorial Pacific sediment that receives a high rate of carbonate supply. In addition, a box model of sediment mixing was used to simulate radiocarbon, carbonate content and excess thorium profiles that result from either boundary process following a dissolution increase. Results from homogeneous dissolution imply a strong, very recent erosional event, while interface dissolution suggests that moderately increased dissolution began about 10,000 years ago. In order to achieve the observed mixed layer radiocarbon age, increased homogeneous dissolution would concentrate a greater amount of clay and 230Th than is observed, while for interface dissolution the predicted concentrations are too small. These results together with small discontinuities beneath the mixed layer in 230Th profiles suggest a two-stage increase in interface dissolution in the deep Pacific, the first occurring near the beginning of the Holocene and the second more recently, roughly 5000 years ago. ?? 1993.

Improving operational anodising process performance using simulation approach

NASA Astrophysics Data System (ADS)

Liong, Choong-Yeun; Ghazali, Syarah Syahidah

2015-10-01

The use of aluminium is very widespread, especially in transportation, electrical and electronics, architectural, automotive and engineering applications sectors. Therefore, the anodizing process is an important process for aluminium in order to make the aluminium durable, attractive and weather resistant. This research is focused on the anodizing process operations in manufacturing and supplying of aluminium extrusion. The data required for the development of the model is collected from the observations and interviews conducted in the study. To study the current system, the processes involved in the anodizing process are modeled by using Arena 14.5 simulation software. Those processes consist of five main processes, namely the degreasing process, the etching process, the desmut process, the anodizing process, the sealing process and 16 other processes. The results obtained were analyzed to identify the problems or bottlenecks that occurred and to propose improvement methods that can be implemented on the original model. Based on the comparisons that have been done between the improvement methods, the productivity could be increased by reallocating the workers and reducing loading time.

The role of stress in self-ordered porous anodic oxide formation and corrosion of aluminum

NASA Astrophysics Data System (ADS)

Capraz, Omer Ozgur

The phenomenon of plastic flow induced by electrochemical reactions near room temperature is significant in porous anodic oxide (PAO) films, charging of lithium batteries and stress-corrosion cracking (SCC). As this phenomenon is poorly understood, fundamental insight into flow from our work may provide useful information for these problems. In-situ monitoring of the stress state allows direct correlation between stress and the current or potential, thus providing fundamental insight into technologically important deformation and failure mechanisms induced by electrochemical reactions. A phase-shifting curvature interferometry was designed to investigate the stress generation mechanisms on different systems. Resolution of our curvature interferometry was found to be ten times more powerful than that obtained by state-of-art multiple deflectometry technique and the curvature interferometry helps to resolve the conflicting reports in the literature. During this work, formation of surface patterns during both aqueous corrosion of aluminum and formation of PAO films were investigated. Interestingly, for both cases, stress induced plastic flow controls the formation of surface patterns. Pore formation mechanisms during anodizing of the porous aluminum oxide films was investigated . PAO films are formed by the electrochemical oxidation of metals such as aluminum and titanium in a solution where oxide is moderately soluble. They have been used extensively to design numerous devices for optical, catalytic, and biological and energy related applications, due to their vertically aligned-geometry, high-specific surface area and tunable geometry by adjusting process variables. These structures have developed empirically, in the absence of understanding the process mechanism. Previous experimental studies of anodizing-induced stress have extensively focused on the measurement of average stress, however the measurement of stress evolution during anodizing does not provide sufficient information to understand the potential stress mechanisms. We developed a new method, which enables us to discriminate the potential stress mechanisms during anodizing and characterize the evolution of the stress profile during film growth. Using stress measurement and characterization techniques, we demonstrated the evolution of the stress profile during the film formation and discussed the role of stress on the PAO film formation. Compressive stress builds up linearly during the anodizing, while barrier oxide film gets thicker until the onset of the pore initiation. Both barrier layer thickness and the integrated oxide stress decreased rapidly to the steady-state period when pore initiation began. The morphology change and stress transients points out the transition from elastic to plastic oxide behavior, similar to those observed in other situations such as lithium intercalation into silicon. The stress profile is consistent with the stress gradient needed to drive plastic flow observed experimentally. We also addressed the dependence of overall stress generation on applied current density. Apparently, stress caused by expansion or contraction of oxide and metal interface depends on the volume change due to overall reactions. In the last chapter, the stress generation during alkaline Al corrosion will be discussed. The enhancement of mechanical degradation by corrosion is the basis for the damage process such as stress-corrosion cracking. Understanding the synergistic effect of stress on stress-corrosion cracking mechanism is necessary to design new materials to improve the safety and viability of existing energy conversion systems. the high-resolution in-situ stress measurements during Al corrosion in alkaline solution was presented, supported by characterization techniques and Fast Fourier Transform analysis. Unprecedented curvature resolution of curvature interferometry permits the monitoring of stress during extended periods of corrosion of thick metal samples. Evolution of concaved-shaped surface patterns is in a great harmony with recorded tensile stress. Furthermore, absolute value of tensile stress onset of the plasticity depends on the dissolution rate of metal and yield stress of metal. The measurements reveal corrosion-induced tensile stress generation, leading to surface plasticity. This finding is evidence that corrosion can directly bring about plasticity, and may be relevant to mechanism of corrosion-induced degradation.

Exploring As-Cast PbCaSn-Mg Anodes for Improved Performance in Copper Electrowinning

NASA Astrophysics Data System (ADS)

Yuwono, Jodie A.; Clancy, Marie; Chen, Xiaobo; Birbilis, Nick

2018-06-01

Lead calcium tin (PbCaSn) alloys are the common anodes used in copper electrowinning (Cu EW). Given a large amount of energy consumed in Cu EW process, anodes with controlled oxygen evolution reaction (OER) kinetics and a lower OER overpotential are advantageous for reducing the energy consumption. To date, magnesium (Mg) has never been studied as an alloying element for EW anodes. As-cast PbCaSn anodes with the addition of Mg were examined herein, revealing an improved performance compared to that of the industrial standard PbCaSn anode. The alloy performances in the early stages of anode life and passivation were established from electrochemical studies which were designed to simulate industrial Cu EW process. The 24-hour polarization testing revealed that the Mg alloying depolarizes the anode potential up to 80 mV; thus, resulting in a higher Cu EW efficiency. In addition, scanning electron microscopy and X-ray photoelectron spectroscopy revealed that the alteration of the alloy microstructure and the corresponding interfacial reactions contribute to the changes of the anode electrochemical performances. The present study reveals for the first time the potency of Mg alloying in reducing the overpotential of PbCaSn anode.

Controlling the anodizing conditions in preparation of an nanoporous anodic aluminium oxide template

NASA Astrophysics Data System (ADS)

Nazemi, Azadeh; Abolfazl, Seyed; Sadjadi, Seyed

2014-12-01

Porous anodic aluminium oxide (AAO) template is commonly used in the synthesis of one-dimensional nanostructures, such as nanowires and nanorods, due to its simple fabrication process. Controlling the anodizing conditions is important because of their direct influence on the size of AAO template pores; it affects the size of nanostructures that are fabricated in AAO template. In present study, several alumina templates were fabricated by a two-step electrochemical anodization in different conditions, such as the time of first process, its voltage, and electrolyte concentration. The effect of these factors on pore diameters of AAO templates was investigated using scanning electron microscopy (SEM).

Optimization of an integrated electrodisinfection/electrocoagulation process with Al bipolar electrodes for urban wastewater reclamation.

PubMed

Cotillas, Salvador; Llanos, Javier; Cañizares, Pablo; Mateo, Sara; Rodrigo, Manuel A

2013-04-01

In this work, a novel integrated electrochemical process for urban wastewater regeneration is described. The electrochemical cell consists in a Boron Doped Diamond (BDD) or a Dimensionally Stable Anode (DSA) as anode, a Stainless Steel (SS) as cathode and a perforated aluminum plate, which behaves as bipolar electrode, between anode and cathode. Thus, in this cell, it is possible to carry out, at the same time, two different electrochemical processes: electrodisinfection (ED) and electrocoagulation (EC). The treatment of urban wastewater with different anodes and different operating conditions is studied. First of all, in order to check the process performance, experiments with synthetic wastewaters were carried out, showing that it is possible to achieve a 100% of turbidity removal by the electrodissolution of the bipolar electrode. Next, the effect of the current density and the anode material are studied during the ED-EC process of actual effluents. Results show that it is possible to remove Escherichia coli and turbidity simultaneously of an actual effluent from a WasteWater Treatment Facility (WWTF). The use of BDD anodes allows to remove the E. coli completely at an applied electric charge of 0.0077 A h dm(-3) when working with a current density of 6.65 A m(-2). On the other hand, with DSA anodes, the current density necessary to achieve the total removal of E. coli is higher (11.12 A m(-2)) than that required with BDD anodes. Finally, the influence of cell flow path and flow rate have been studied. Results show that the performance of the process strongly depends on the characteristics of the initial effluent (E. coli concentration and Cl(-)/NH(4)(+) initial ratio) and that a cell configuration cathode (inlet)-anode (outlet) and a higher flow rate enhance the removal of the turbidity from the treated effluent. Copyright © 2013 Elsevier Ltd. All rights reserved.

Nano structural anodes for radiation detectors

DOEpatents

Cordaro, Joseph V.; Serkiz, Steven M.; McWhorter, Christopher S.; Sexton, Lindsay T.; Retterer, Scott T.

2015-07-07

Anodes for proportional radiation counters and a process of making the anodes is provided. The nano-sized anodes when present within an anode array provide: significantly higher detection efficiencies due to the inherently higher electric field, are amenable to miniaturization, have low power requirements, and exhibit a small electromagnetic field signal. The nano-sized anodes with the incorporation of neutron absorbing elements (e.g., .sup.10B) allow the use of neutron detectors that do not use .sup.3He.

Application of fuel cell for pyrite and heavy metal containing mining waste

NASA Astrophysics Data System (ADS)

Keum, H.; Ju, W. J.; Jho, E. H.; Nam, K.

2015-12-01

Once pyrite and heavy metal containing mining waste reacts with water and air it produces acid mine drainage (AMD) and leads to the other environmental problems such as contamination of surrounding soils. Pyrite is the major source of AMD and it can be controlled using a biological-electrochemical dissolution method. By enhancing the dissolution of pyrite using fuel cell technology, not only mining waste be beneficially utilized but also be treated at the same time by. As pyrite-containing mining waste is oxidized in the anode of the fuel cell, electrons and protons are generated, and electrons moves through an external load to cathode reducing oxygen to water while protons migrate to cathode through a proton exchange membrane. Iron-oxidizing bacteria such as Acidithiobacillus ferrooxidans, which can utilize Fe as an electron donor promotes pyrite dissolution and hence enhances electrochemical dissolution of pyrite from mining waste. In this study mining waste from a zinc mine in Korea containing 17 wt% pyrite and 9% As was utilized as a fuel for the fuel cell inoculated with A. ferrooxidans. Electrochemically dissolved As content and chemically dissolved As content was compared. With the initial pH of 3.5 at 23℃, the dissolved As concentration increased (from 4.0 to 13 mg/L after 20 d) in the fuel cell, while it kept decreased in the chemical reactor (from 12 to 0.43 mg/L after 20 d). The fuel cell produced 0.09 V of open circuit voltage with the maximum power density of 0.84 mW/m2. Dissolution of As from mining waste was enhanced through electrochemical reaction. Application of fuel cell technology is a novel treatment method for pyrite and heavy metals containing mining waste, and this method is beneficial for mining environment as well as local community of mining areas.

Energy-Efficient and Environmentally Friendly Solid Oxide Membrane Electrolysis Process for Magnesium Oxide Reduction: Experiment and Modeling

NASA Astrophysics Data System (ADS)

Guan, Xiaofei; Pal, Uday B.; Powell, Adam C.

2014-06-01

This paper reports a solid oxide membrane (SOM) electrolysis experiment using an LSM(La0.8Sr0.2MnO3-δ)-Inconel inert anode current collector for production of magnesium and oxygen directly from magnesium oxide at 1423 K (1150 °C). The electrochemical performance of the SOM cell was evaluated by means of various electrochemical techniques including electrochemical impedance spectroscopy, potentiodynamic scan, and electrolysis. Electronic transference numbers of the flux were measured to assess the magnesium dissolution in the flux during SOM electrolysis. The effects of magnesium solubility in the flux on the current efficiency and the SOM stability during electrolysis are discussed. An inverse correlation between the electronic transference number of the flux and the current efficiency of the SOM electrolysis was observed. Based on the experimental results, a new equivalent circuit of the SOM electrolysis process is presented. A general electrochemical polarization model of SOM process for magnesium and oxygen gas production is developed, and the maximum allowable applied potential to avoid zirconia dissociation is calculated as well. The modeling results suggest that a high electronic resistance of the flux and a relatively low electronic resistance of SOM are required to achieve membrane stability, high current efficiency, and high production rates of magnesium and oxygen.

Dissecting anode swelling in commercial lithium-ion batteries

NASA Astrophysics Data System (ADS)

Zhang, Ningxin; Tang, Huaqiong

2012-11-01

An innovative method is applied to investigate anode swelling during electrochemical processes in commercial lithium-ion batteries. Cathode surface is partially covered with a piece of paste to block the transportation of lithium ion from active material during charging/discharging, and the corresponding part on the anode film shows no formation of Li-graphite compounds during different electrochemical processes, which is confirmed by XRD analysis. The increases of anode thickness within and outside lithiated zone are measured, and defined as electrochemical swelling and physical swelling respectively. The microscopic lattice expansion of graphite due to lithiation process correlates to mesoscopic electrochemical swelling synchronically, while physical swelling tends to decrease steadily with time. The relationship among the microscopic stress due to lithium-ion intercalation, the mesoscopic stress resulting in anode swelling, and the macroscopic rippling of pouch cell after a large number of cycle test, is analyzed and correlated in terms of stress evolution across different scales, and suggestions for solving anode swelling are provided.

Effect of TiO2 Addition on Grain Growth, Anodic Bubble Evolution and Anodic Overvoltage of NiFe2O4-Based Composite Inert Anodes

NASA Astrophysics Data System (ADS)

Wang, Bin; Du, Jinjing; Liu, Yihan; Fang, Zhao; Hu, Ping

2017-11-01

A two-step powder compaction and sintering process was employed to fabricate TiO2-doped NiFe2O4 ceramic-based inert anodes. Grain growth during isothermal sintering was analyzed using Brook grain growth model. The bubble behavior of NiFe2O4 ceramic-based inert anodes was investigated in a two-compartment see-through quartz cell for aluminum electrolysis process. Anodic overvoltage and potential decay curves of the inert anodes were measured by using the steady state and current interruption technique. The results showed that the kinetic index of grain growth decreased with an increase in temperature. The average activation energy of grain growth for 1.0 wt.% TiO2-doped NiFe2O4 ceramic samples with a sintering temperature range from 1373 to 1673 K dropped from 675.30 to 183.47 kJ/mol. The diameter size of bubbles before releasing from the bottom surface of the anodes was reduced with increasing the current density, and the larger average releasing bubble size for carbon anode at the same current density could be obtained, which was compared to the NiFe2O4 inert anodes. Besides, the cell voltage of carbon anodes fluctuated much more violently under the same experimental conditions. After adding small amount of TiO2, a minor reduction in anodic overvoltage of NiFe2O4-based anodes can be observed.

Optimal condition for fabricating superhydrophobic Aluminum surfaces with controlled anodizing processes

NASA Astrophysics Data System (ADS)

Saffari, Hamid; Sohrabi, Beheshteh; Noori, Mohammad Reza; Bahrami, Hamid Reza Talesh

2018-03-01

A single step anodizing process is used to produce micro-nano structures on Aluminum (1050) substrates with sulfuric acid as electrolyte. Therefore, surface energy of the anodized layer is reduced using stearic acid modification. Undoubtedly, effects of different parameters including anodizing time, electrical current, and type and concentration of electrolyte on the final contact angle are systemically studied and optimized. Results show that anodizing current of 0.41 A, electrolyte (sulfuric acid) concentration of 15 wt.% and anodizing time of 90 min are optimal conditions which give contact angle as high as 159.2° and sliding angle lower than 5°. Moreover, the study reveals that adding oxalic acid to the sulfuric acid cannot enhance superhydrophobicity of the samples. Also, scanning electron microscopy images of samples show that irregular (bird's nest) structures present on the surface instead of high-ordered honeycomb structures expecting from normal anodizing process. Additionally, X-ray diffraction analysis of the samples shows that only amorphous structures present on the surface. The Brunauer-Emmett-Teller (BET) specific surface area of the anodized layer is 2.55 m2 g-1 in optimal condition. Ultimately, the surface keeps its hydrophobicity in air and deionized water (DIW) after one week and 12 weeks, respectively.

Occurrence and Removal of Organic Micropollutants in Landfill Leachates Treated by Electrochemical Advanced Oxidation Processes.

PubMed

Oturan, Nihal; van Hullebusch, Eric D; Zhang, Hui; Mazeas, Laurent; Budzinski, Hélène; Le Menach, Karyn; Oturan, Mehmet A

2015-10-20

In recent years, electrochemical advanced oxidation processes have been shown to be an effective alternative for the removal of refractory organic compounds from water. This study is focused on the effective removal of recalcitrant organic matter (micropollutants, humic substances, etc.) present in municipal solid waste landfill leachates. A mixture of eight landfill leachates has been studied by the electro-Fenton process using a Pt or boron-doped diamond (BDD) anode and a carbon felt cathode or by the anodic oxidation process with a BDD anode. These processes exhibit great oxidation ability due to the in situ production of hydroxyl radicals ((•)OH), a highly powerful oxidizing species. Both electrochemical processes were shown to be efficient in the removal of dissolved total organic carbon (TOC) from landfill leachates. Regarding the electro-Fenton process, the replacement of the classical anode Pt by the anode BDD allows better performance in terms of dissolved TOC removal. The occurrence and removal yield of 19 polycyclic aromatic hydrocarbons, 15 volatile organic compounds, 7 alkylphenols, 7 polychlorobiphenyls, 5 organochlorine pesticides, and 2 polybrominated diphenyl ethers in landfill leachate were also investigated. Both electrochemical processes allow one to reach a quasicomplete removal (about 98%) of these organic micropollutants.

Quantification of the resist dissolution process: an in situ analysis using high speed atomic force microscopy

NASA Astrophysics Data System (ADS)

Santillan, Julius Joseph; Shichiri, Motoharu; Itani, Toshiro

2016-03-01

This work focuses on the application of a high speed atomic force microscope (HS-AFM) for the in situ visualization / quantification of the resist dissolution process. This technique, as reported in the past, has provided useful pointers on the formation of resist patterns during dissolution. This paper discusses about an investigation made on the quantification of what we refer to as "dissolution unit size" or the basic units of patterning material dissolution. This was done through the establishment of an originally developed analysis method which extracts the difference between two succeeding temporal states of the material film surface (images) to indicate the amount of change occurring in the material film at a specific span of time. Preliminary experiments with actual patterning materials were done using a positive-tone EUV model resist composed only of polyhydroxystyrene (PHS)-based polymer with a molecular weight of 2,500 and a polydispersity index of 1.2. In the absence of a protecting group, the material was utilized at a 50nm film thickness with post application bake of 90°C/60s. The resulting film is soluble in the alkali-based developer even without exposure. Results have shown that the dissolution components (dissolution unit size) of the PHS-based material are not of fixed size. Instead, it was found that aside from one constantly dissolving unit size, another, much larger dissolution unit size trend also occurs during material dissolution. The presence of this larger dissolution unit size suggests an occurrence of "polymer clustering". Such polymer clustering was not significantly present during the initial stages of dissolution (near the original film surface) but becomes more persistently obvious after the dissolution process reaches a certain film thickness below the initial surface.

Anodizing Process

NASA Technical Reports Server (NTRS)

1983-01-01

This anodizing process traces its origin to the 1960's when Reynolds Metals Company, under contract with Goddard Space Flight Center, developed a multipurpose anodizing electrolyte (MAE) process to produce a hard protective finish for spacecraft aluminum. MAE produces a high-density, abrasion-resistant film prior to the coloring step, in which the pores of the film are impregnated with a metallic form of salt. Tru-Color product applications include building fronts, railing, curtain walls, doors and windows.

Investigation on the Oxidation and Reduction of Titanium in Molten Salt with the Soluble TiC Anode

NASA Astrophysics Data System (ADS)

Wang, Shulan; Wan, Chaopin; Liu, Xuan; Li, Li

2015-12-01

To reveal the oxidation process of titanium from TiC anode and the reduction mechanism of titanium ions in molten NaCl-KCl, the polarization curve of TiC anode in molten NaCl-KCl and cyclic voltammograms of the molten salt after polarization were studied. Investigation on the polarization curve shows that titanium can be oxidized and dissociated from the TiC anode at very low potential. The cyclic voltammograms demonstrated that the reduction reaction of titanium ions in the molten salt is a one-step process. By potentiostatic electrolysis, dendritic titanium is obtained on the steel plate. The work promotes the understanding on the process of electrochemical oxidization/dissociation of titanium from TiC anode and the reduction mechanism of titanium ions in molten salt.

Electrokinetic treatment of an agricultural soil contaminated with heavy metals.

PubMed

Figueroa, Arylein; Cameselle, Claudio; Gouveia, Susana; Hansen, Henrik K

2016-07-28

The high organic matter content in agricultural soils tends to complex and retain contaminants such as heavy metals. Electrokinetic remediation was tested in an agricultural soil contaminated with Co(+2), Zn(+2), Cd(+2), Cu(+2), Cr(VI), Pb(+2) and Hg(+2). The unenhanced electrokinetic treatment was not able to remove heavy metals from the soil due to the formation of precipitates in the alkaline environment in the soil section close to the cathode. Moreover, the interaction between metals and organic matter probably limited metal transportation under the effect of the electric field. Citric acid and ethylenediaminetetraacetic acid (EDTA) were used in the catholyte as complexing agents in order to enhance the extractability and removal of heavy metals from soil. These complexing agents formed negatively charged complexes that migrated towards the anode. The acid front electrogenerated at the anode favored the dissolution of heavy metals that were transported towards the cathode. The combined effect of the soil pH and the complexing agents resulted in the accumulation of heavy metals in the center of the soil specimen.

Galvanic corrosion of nitinol under deaerated and aerated conditions.

PubMed

Pound, Bruce G

2016-10-01

Various studies have examined the corrosion rate of nitinol generally under deaerated conditions. Likewise, galvanic corrosion studies have typically involved deaerated solutions. This work addressed the effect of galvanic coupling on the corrosion current of electropolished nitinol in phosphate buffered saline and 0.9% sodium chloride under dearated and aerated conditions for times up to 24 h. Tests were performed on nitinol alone and coupled with MP35N in both the mechanically polished and passivated conditions. Aeration and galvanic coupling were found to have relatively little effect, indicating that the corrosion current is controlled by the anodic reaction. The current can be attributed entirely to Ni(2+) dissolution, which appears to be governed by solid-state mass transport of Ni(2+) through the passive oxide film. Because corrosion of EP nitinol is controlled by the anodic reaction, contact between EP nitinol and MP35N or other biomedical Co-Cr alloys is unlikely to result in significant galvanic effects in vivo. © 2015 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 104B: 1322-1327, 2016. © 2015 Wiley Periodicals, Inc.

Synthesis of zinc oxide porous structures by anodization with water as an electrolyte

NASA Astrophysics Data System (ADS)

Shetty, Amitha; Nanda, Karuna Kar

2012-10-01

We report a simple, reliable and one-step method of synthesizing ZnO porous structures at room temperature by anodization of zinc (Zn) sheet with water as an electrolyte and graphite as a counter electrode. We observed that the de-ionized (DI) water used in the experiment is slightly acidic (pH=5.8), which is due to the dissolution of carbon dioxide from the atmosphere forming carbonic acid. Porous ZnO is characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), Raman spectroscopy and photoluminescence (PL) studies. The current-transient measurement is carried out using a Gamry Instruments Reference 3000 and the thickness of the deposited films is measured using a Dektak surface profilometer. The PL, Raman and X-ray photoelectron spectroscopy are used to confirm the presence of ZnO phase. We have demonstrated that the hybrid structures of ZnO and poly (3,4-ethylenedioxythiophene):poly (styrene sulfonate) (PEDOT:PSS) exhibit good rectifying characteristics. The evaluated barrier height and the ideality factor are 0.45 eV and 3.6, respectively.

Development of 10×10 Matrix-anode MCP-PMT

NASA Astrophysics Data System (ADS)

Yang, Jie; Li, Yongbin; Xu, Pengxiao; Zhao, Wenjin

2018-02-01

10×10 matrix-anode is developed by high-temperature co-fired ceramics (HTCC) technology. Based on the new matrix-anode, a new kind of photon counting imaging detector - 10×10 matrix-anode MCP-PMT is developed, and its performance parameters are tested. HTCC technology is suitable for the MCP-PMT's air impermeability and its baking process. Its response uniformity is better than the metal-ceramic or metal-glass sealing anode, and it is also a promising method to realize a higher density matrix-anode.

Initial dissolution kinetics of cocrystal of carbamazepine with nicotinamide.

PubMed

Hattori, Yusuke; Sato, Maiko; Otsuka, Makoto

2015-11-01

Objectives of this study are investigating the initial dissolution kinetics of the cocrystal of carbamazepine (CBZ) with nicotinamide (NIC) and understanding its initial dissolution process. Cocrystal solids of CBZ with NIC were prepared by co-milling and solvent evaporation methods. The formation of cocrystal solid was verified via X-ray diffraction measurement. Dissolution tests of the solids were performed using an original flow cell and ultraviolet-visible spectroscopic detector. The spectra monitored in situ were analyzed to determine the dissolved compounds separately using the classical least squares regression method. The initial dissolution profiles were interpreted using simultaneous model of dissolution and phase changes. In the initial dissolution, CBZ in the cocrystal structure dissolved in water and it was suggested that CBZ reached a metastable intermediate state simultaneously with dissolution. The cocrystal solid prepared by solvent evaporation provided a higher rate constant of the phase change than that prepared by co-milling. Our results thus support the use of evaporation as the method of choice to produce ordered cocrystal structures. We suggest that CBZ forms dihydrate during the dissolution process; however, during the initial phase of dissolution, CBZ changes to a metastable intermediate phase. © 2015 Royal Pharmaceutical Society.

SiO2 decoration dramatically enhanced the stability of PtRu electrocatalysts with undetectable deterioration in fuel cell performance.

PubMed

Yu, Xinxin; Xu, Zejun; Yang, Zehui; Xu, Sen; Zhang, Quan; Ling, Ying; Zhang, Yunfeng; Cai, Weiwei

2018-06-15

Prevention of Ru dissolution is essential for steady CO tolerance of anodic electrocatalysts in direct methanol fuel cells. Here, we demonstrate a facile way to stabilize Ru atoms by decorating commercial CB/PtRu with SiO 2 , which shows a six-fold higher stability and similar activity toward a methanol oxidation reaction leading to no discernible degradation in fuel cell performance compared to commercial CB/PtRu electrocatalysts. The higher stability and stable CO tolerance of SiO 2 -decorated electrocatalysts originate from the SiO 2 coating, since Ru atoms are partially ionized during SiO 2 decorating, resulting in difficulties in dissolution; while, in the case of commercial CB/PtRu, the dissolved Ru offers active sites for Pt coalescences and CO species resulting in the rapid decay of the electrochemical surface area and fuel cell performance. To the best of our knowledge, this is the first study about the stabilization of Ru atoms by SiO 2 . The highest stability is obtained for a PtRu electrocatalyst with negligible effect on the electrochemical properties.

A study of X100 pipeline steel passivation in mildly alkaline bicarbonate solutions using electrochemical impedance spectroscopy under potentiodynamic conditions and Mott-Schottky

NASA Astrophysics Data System (ADS)

Gadala, Ibrahim M.; Alfantazi, Akram

2015-12-01

The key steps involved in X100 pipeline steel passivation in bicarbonate-based simulated soil solutions from the pre-passive to transpassive potential regions have been analyzed here using a step-wise anodizing-electrochemical impedance spectroscopy (EIS) routine. Pre-passive steps involve parallel dissolution-adsorption in early stages followed by clear diffusion-adsorption control shortly before iron hydroxide formation. Aggressive NS4 chlorides/sulfate promote steel dissolution whilst inhibiting diffusion in pre-passive steps. Diffusive and adsorptive effects remain during iron hydroxide formation, but withdraw shortly thereafter during its removal and the development of the stable iron carbonate passive layer. Passive layer protectiveness is evaluated using EIS fitting, current density analysis, and correlations with semiconductive parameters, consistently revealing improved robustness in colder, bicarbonate-rich, chloride/sulfate-free conditions. Ferrous oxide formation at higher potentials results in markedly lower impedances with disordered behavior, and the involvement of the iron(III) valence state is observed in Mott-Schottky tests exclusively for 75 °C conditions.

Negligible degradation upon in situ voltage cycling of a PEMFC using an electrospun niobium-doped tin oxide supported Pt cathode.

PubMed

Savych, Iuliia; Subianto, Surya; Nabil, Yannick; Cavaliere, Sara; Jones, Deborah; Rozière, Jacques

2015-07-14

Novel platinum-catalysed, corrosion-resistant, loose-tube-structured electrocatalysts for proton exchange membrane fuel cells have been obtained using single-needle electrospinning associated with a microwave-assisted polyol method. Monodisperse platinum particles supported on Nb-SnO2 demonstrated higher electrochemical stability than conventional Pt/C electrodes during ex situ potential cycling and comparable activity in the oxygen reduction reaction. In situ fuel cell operation under accelerated stress test conditions of a membrane electrode assembly elaborated using a Pt/C anode and Pt/Nb-SnO2 cathode confirmed that the voltage loss is significantly lower for the novel cathode than for an MEA prepared using conventional Pt/C supported electrocatalysts. Furthermore, the Nb-SnO2 stabilised the supported platinum nanoparticles against dissolution, migration and reprecipitation in the membrane. Pt/Nb-SnO2 loose-tubes constitute a mitigation strategy for two known degradation mechanisms in PEMFC: corrosion of the carbon support at the cathode, and dissolution of Pt at high cell voltages.

Friction Stir Welding of Al Alloy 2219-T8: Part II-Mechanical and Corrosion

NASA Astrophysics Data System (ADS)

Kang, Ju; Feng, Zhi-Cao; Li, Ji-Chao; Frankel, G. S.; Wang, Guo-Qing; Wu, Ai-Ping

2016-09-01

In Part I of this series, abnormal agglomerations of θ particles with size of about 100 to 1000 µm were observed in friction stir welded AA2219-T8 joints. In this work, the effects of these agglomerated θ particles on the mechanical and corrosion properties of the joints are studied. Tensile testing with in situ SEM imaging was utilized to monitor crack initiation and propagation in base metal and weld nugget zone (WNZ) samples. These tests showed that cracks initiated in the θ particles and at the θ/matrix interfaces, but not in the matrix. The WNZ samples containing abnormal agglomerated θ particles had a similar ultimate tensile stress but 3 pct less elongation than other WNZ samples with only normal θ particles. Measurements using the microcell technique indicated that the agglomerated θ particles acted as a cathode causing the dissolution of adjacent matrix. The abnormal θ particle agglomerations led to more severe localized attack due to the large cathode/anode ratio. Al preferential dissolution occurred in the abnormal θ particle agglomerations, which was different from the corrosion behavior of normal size θ particles.

Corrosion behavior of ODS steels with several chromium contents in hot nitric acid solutions

NASA Astrophysics Data System (ADS)

Tanno, Takashi; Takeuchi, Masayuki; Ohtsuka, Satoshi; Kaito, Takeji

2017-10-01

Oxide dispersion strengthened (ODS) steel cladding tubes have been developed for fast reactors. Tempered martensitic ODS steels with 9 and 11 wt% of chromium (9Cr-, 11Cr-ODS steel) are the candidate material in research being carried out at JAEA. In this work, fundamental immersion tests and electrochemical tests of 9 to 12Cr-ODS steels were systematically conducted in various nitric acid solutions at 95 °C. The corrosion rate decreased exponentially with effective solute chromium concentration (Creff) and nitric acid concentration. Addition of vanadium (V) and ruthenium (Ru) also decreased the corrosion rate. The combination of low Creff and dilute nitric acid could not avoid the active mass dissolution during active domain at the beginning of immersion, and the corrosion rate was high. Higher Creff decreased the partial anodic current during the active domain and assisted the passivation of the surface of the steel. Concentrated nitric acid and addition of Ru and V increased partial cathodic current and shifted the corrosion potential to noble side. These effects should have prevented the active mass dissolution and decreased the corrosion rate.

SiO2 decoration dramatically enhanced the stability of PtRu electrocatalysts with undetectable deterioration in fuel cell performance

NASA Astrophysics Data System (ADS)

Yu, Xinxin; Xu, Zejun; Yang, Zehui; Xu, Sen; Zhang, Quan; Ling, Ying; Zhang, Yunfeng; Cai, Weiwei

2018-06-01

Prevention of Ru dissolution is essential for steady CO tolerance of anodic electrocatalysts in direct methanol fuel cells. Here, we demonstrate a facile way to stabilize Ru atoms by decorating commercial CB/PtRu with SiO2, which shows a six-fold higher stability and similar activity toward a methanol oxidation reaction leading to no discernible degradation in fuel cell performance compared to commercial CB/PtRu electrocatalysts. The higher stability and stable CO tolerance of SiO2-decorated electrocatalysts originate from the SiO2 coating, since Ru atoms are partially ionized during SiO2 decorating, resulting in difficulties in dissolution; while, in the case of commercial CB/PtRu, the dissolved Ru offers active sites for Pt coalescences and CO species resulting in the rapid decay of the electrochemical surface area and fuel cell performance. To the best of our knowledge, this is the first study about the stabilization of Ru atoms by SiO2. The highest stability is obtained for a PtRu electrocatalyst with negligible effect on the electrochemical properties.

Buried anode lithium thin film battery and process for forming the same

DOEpatents

Lee, Se-Hee; Tracy, C. Edwin; Liu, Ping

2004-10-19

A reverse configuration, lithium thin film battery (300) having a buried lithium anode layer (305) and process for making the same. The present invention is formed from a precursor composite structure (200) made by depositing electrolyte layer (204) onto substrate (201), followed by sequential depositions of cathode layer (203) and current collector (202) on the electrolyte layer. The precursor is subjected to an activation step, wherein a buried lithium anode layer (305) is formed via electroplating a lithium anode layer at the interface of substrate (201) and electrolyte film (204). The electroplating is accomplished by applying a current between anode current collector (201) and cathode current collector (202).

Dissolution process analysis using model-free Noyes-Whitney integral equation.

PubMed

Hattori, Yusuke; Haruna, Yoshimasa; Otsuka, Makoto

2013-02-01

Drug dissolution process of solid dosages is theoretically described by Noyes-Whitney-Nernst equation. However, the analysis of the process is demonstrated assuming some models. Normally, the model-dependent methods are idealized and require some limitations. In this study, Noyes-Whitney integral equation was proposed and applied to represent the drug dissolution profiles of a solid formulation via the non-linear least squares (NLLS) method. The integral equation is a model-free formula involving the dissolution rate constant as a parameter. In the present study, several solid formulations were prepared via changing the blending time of magnesium stearate (MgSt) with theophylline monohydrate, α-lactose monohydrate, and crystalline cellulose. The formula could excellently represent the dissolution profile, and thereby the rate constant and specific surface area could be obtained by NLLS method. Since the long time blending coated the particle surface with MgSt, it was found that the water permeation was disturbed by its layer dissociating into disintegrant particles. In the end, the solid formulations were not disintegrated; however, the specific surface area gradually increased during the process of dissolution. The X-ray CT observation supported this result and demonstrated that the rough surface was dominant as compared to dissolution, and thus, specific surface area of the solid formulation gradually increased. Copyright © 2012 Elsevier B.V. All rights reserved.

A new structural approach for uniform sub-micrometer anode metallization of planar THz Schottky components

NASA Astrophysics Data System (ADS)

Cojocari, O.; Mottet, B.; Rodriguez-Girones, M.; Biber, S.; Marchand, L.; Schmidt, L.-P.; Hartnagel, H. L.

2004-03-01

This paper presents the evaluation of a Schottky contact technology based on electrochemical metal deposition. The results of a long-term systematic investigation and optimization of the anode formation process to improve the yield and performance of Schottky-based GaAs mixer diodes are detailed. Surface preparation prior to the Schottky-metal deposition and anode metallization as previously optimized for whisker-contacted diodes are successfully transferred to the fabrication of planar structures. This uses an auxiliary honeycomb array of anode-like structures called 'dummy anodes', which are processed simultaneously with the real anodes and then removed in the later technological processes. Consequently, the scattering of planar diodes electrical parameters is significantly reduced and the yield of the fabrication process increases from about 5% up to about 50%. Very good dc characteristics such as series resistance (Rs) below 8 OHgr, ideality factor (eegr) below 1.2 and saturation current (Isat) of the order of 10-17A are achieved for the anode diameter as small as 1 µm. An excellent IF-noise figure of 250 K at 4.8 GHz up to 280 K at 2.1 GHz with current bias up to 3 mA is obtained for non-cooled THz mixer planar diodes. The use of this technological approach has enabled the extraction of statistically significant data which have been used to characterize the criticality of each step of the fabrication process on the device performance.

Experimental Studies of the Effects of Anode Composition and Process Parameters on Anode Slime Adhesion and Cathode Copper Purity by Performing Copper Electrorefining in a Pilot-Scale Cell

NASA Astrophysics Data System (ADS)

Zeng, Weizhi; Wang, Shijie; Free, Michael L.

2016-10-01

Copper electrorefining tests were conducted in a pilot-scale cell under commercial tankhouse environment to study the effects of anode compositions, current density, cathode blank width, and flow rate on anode slime behavior and cathode copper purity. Three different types of anodes (high, mid, and low impurity levels) were used in the tests and were analyzed under SEM/EDS. The harvested copper cathodes were weighed and analyzed for impurities concentrations using DC Arc. The adhered slimes and released slimes were collected, weighed, and analyzed for compositions using ICP. It was shown that the lead-to-arsenic ratio in the anodes affects the sintering and coalescence of slime particles. High current density condition can improve anode slime adhesion and cathode purity by intensifying slime particles' coalescence and dissolving part of the particles. Wide cathode blanks can raise the anodic current densities significantly and result in massive release of large slime particle aggregates, which are not likely to contaminate the cathode copper. Low flow rate can cause anode passivation and increase local temperatures in front of the anode, which leads to very intense sintering and coalescence of slime particles. The results and analyses of the tests present potential solutions for industrial copper electrorefining process.

Improving Efficiency of Aluminium Sacrificial Anode Using Cold Work Process

NASA Astrophysics Data System (ADS)

Asmara, Y. P.; Siregar, J. P.; Tezara, C.; Ann, Chang Tai

2016-02-01

Aluminium is one of the preferred materials to be used as sacrificial anode for carbon steel protection. The efficiency of these can be low due to the formation of oxide layer which passivate the anodes. Currently, to improve its efficiency, there are efforts using a new technique called surface modifications. The objective of this research is to study corrosion mechanism of aluminium sacrificial anode which has been processed by cold work. The cold works are applied by reducing the thickness of aluminium sacrificial anodes at 20% and 40% of thickness reduction. The cathodic protection experiments were performed by immersion of aluminium connected to carbon steel cylinder in 3% NaCl solutions. Visual inspections using SEM had been conducted during the experiments and corrosion rate data were taken in every week for 8 weeks of immersion time. Corrosion rate data were measured using weight loss and linear polarization technique (LPR). From the results, it is observed that cold worked aluminium sacrificial anode have a better corrosion performance. It shows higher corrosion rate and lower corrosion potential. The anodes also provided a long functional for sacrificial anode before it stop working. From SEM investigation, it is shown that cold works have changed the microstructure of anodes which is suspected in increasing corrosion rate and cause de-passivate of the surface anodes.

Relaxation process of the discharge channel near the anode in long air gaps under positive impulse voltages

NASA Astrophysics Data System (ADS)

Zhao, Xiangen; He, Junjia; Luo, Bing; Jia, Lei; Yang, Yongchao; Xiao, Pei

2017-12-01

The relaxation process of the discharge channel near the anode in a long air gap was observed using a Schlieren system with a temporal resolution of 5 µs and a spatial resolution of 70 µm. The dynamic characteristics of the decay process in the vicinity of the anode are obtained. The discharge channel evolves just as a growing mushroom in nature during the relaxation phase. Two physical quantities, angle θ and velocity v, are defined to describe the process in this paper. The average value of the angle and velocity under lightning impulses are 71.7° and 3.3 m s-1 respectively, while 7.7 m s-1 under switching impulses. A simplified model was established to simulate the formation of mushroom-shaped channel. The simulation and experimental results show that the formation and development of the mushroom-shaped channel are due to two factors. One is the convection of the high temperature and high pressure air near the anode produced by the first corona discharge; the other is the ionic migration. These two factors result in the phenomena that the cooling process in the vicinity of the anode is much more efficient than further into the gap, whereas the thermal conductivity of the anode may have little contribution to that.

The electrochemical reduction processes of solid compounds in high temperature molten salts.

PubMed

Xiao, Wei; Wang, Dihua

2014-05-21

Solid electrode processes fall in the central focus of electrochemistry due to their broad-based applications in electrochemical energy storage/conversion devices, sensors and electrochemical preparation. The electrolytic production of metals, alloys, semiconductors and oxides via the electrochemical reduction of solid compounds (especially solid oxides) in high temperature molten salts has been well demonstrated to be an effective and environmentally friendly process for refractory metal extraction, functional materials preparation as well as spent fuel reprocessing. The (electro)chemical reduction of solid compounds under cathodic polarizations generally accompanies a variety of changes at the cathode/melt electrochemical interface which result in diverse electrolytic products with different compositions, morphologies and microstructures. This report summarizes various (electro)chemical reactions taking place at the compound cathode/melt interface during the electrochemical reduction of solid compounds in molten salts, which mainly include: (1) the direct electro-deoxidation of solid oxides; (2) the deposition of the active metal together with the electrochemical reduction of solid oxides; (3) the electro-inclusion of cations from molten salts; (4) the dissolution-electrodeposition process, and (5) the electron hopping process and carbon deposition with the utilization of carbon-based anodes. The implications of the forenamed cathodic reactions on the energy efficiency, chemical compositions and microstructures of the electrolytic products are also discussed. We hope that a comprehensive understanding of the cathodic processes during the electrochemical reduction of solid compounds in molten salts could form a basis for developing a clean, energy efficient and affordable production process for advanced/engineering materials.

Activated microporous-mesoporous carbon derived from chestnut shell as a sustainable anode material for high performance microbial fuel cells.

PubMed

Chen, Qin; Pu, Wenhong; Hou, Huijie; Hu, Jingping; Liu, Bingchuan; Li, Jianfeng; Cheng, Kai; Huang, Long; Yuan, Xiqing; Yang, Changzhu; Yang, Jiakuan

2018-02-01

Microbial fuel cells (MFCs) are promising biotechnologies tool to harvest electricity by decomposing organic matter in waste water, and the anode material is a critical factor in determining the performance of MFCs. In this study, chestnut shell is proposed as a novel anode material with mesoporous and microporous structure prepared via a simple carbonization procedure followed by an activation process. The chemical activation process successfully modified the macroporous structure, created more mesoporous and microporous structure and decreased the O-content and pyridinic/pyrrolic N groups on the biomass anode, which were beneficial for improving charge transfer efficiency between the anode surface and microbial biofilm. The MFC with activated biomass anode achieved a maximum power density (23.6 W m -3 ) 2.3 times higher than carbon cloth anode (10.4 W m -3 ). This study introduces a promising and feasible strategy for the fabrication of high performance anodes for MFCs derived from cost-effective, sustainable natural materials. Copyright © 2017 Elsevier Ltd. All rights reserved.

Study on the influences of reduction temperature on nickel-yttria-stabilized zirconia solid oxide fuel cell anode using nickel oxide-film electrode

NASA Astrophysics Data System (ADS)

Jiao, Zhenjun; Ueno, Ai; Suzuki, Yuji; Shikazono, Naoki

2016-10-01

In this study, the reduction processes of nickel oxide at different temperatures were investigated using nickel-film anode to study the influences of reduction temperature on the initial performances and stability of nickel-yttria-stabilized zirconia anode. Compared to conventional nickel-yttria-stabilized zirconia composite cermet anode, nickel-film anode has the advantage of direct observation at nickel-yttria-stabilized zirconia interface. The microstructural changes were characterized by scanning electron microscopy. The reduction process of nickel oxide is considered to be determined by the competition between the mechanisms of volume reduction in nickel oxide-nickel reaction and nickel sintering. Electrochemical impedance spectroscopy was applied to analyze the time variation of the nickel-film anode electrochemical characteristics. The anode performances and microstructural changes before and after 100 hours discharging and open circuit operations were analyzed. The degradation of nickel-film anode is considered to be determined by the co-effect between the nickel sintering and the change of nickel-yttria-stabilized zirconia interface bonding condition.

In vitro dissolution kinetic study of theophylline from hydrophilic and hydrophobic matrices.

PubMed

Maswadeh, Hamzah M; Semreen, Mohammad H; Abdulhalim, Abdulatif A

2006-01-01

Oral dosage forms containing 300 mg theophylline in matrix type tablets, were prepared by direct compression method using two kinds of matrices, glycerylbehenate (hydrophobic), and (hydroxypropyl)methyl cellulose (hydrophilic). The in vitro release kinetics of these formulations were studied at pH 6.8 using the USP dissolution apparatus with the paddle assemble. The kinetics of the dissolution process were studied by analyzing the dissolution data using four kinetic equations, the zero-order equation, the first-order equation, the Higuchi square root equation and the Hixson-Crowell cube root law. The analysis of the dissolution kinetic data for the theophylline preparations in this study shows that it follows the first order kinetics and the release process involves erosion / diffusion and an alteration in the surface area and diameter of the matrix system, as well as in the diffusion path length from the matrix drug load during the dissolution process. This relation is best described by the use of both the first-order equation and the Hixson-Crowell cube root law.

Improving operational anodising process performance using simulation approach

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liong, Choong-Yeun, E-mail: lg@ukm.edu.my; Ghazali, Syarah Syahidah, E-mail: syarah@gapps.kptm.edu.my

The use of aluminium is very widespread, especially in transportation, electrical and electronics, architectural, automotive and engineering applications sectors. Therefore, the anodizing process is an important process for aluminium in order to make the aluminium durable, attractive and weather resistant. This research is focused on the anodizing process operations in manufacturing and supplying of aluminium extrusion. The data required for the development of the model is collected from the observations and interviews conducted in the study. To study the current system, the processes involved in the anodizing process are modeled by using Arena 14.5 simulation software. Those processes consist ofmore » five main processes, namely the degreasing process, the etching process, the desmut process, the anodizing process, the sealing process and 16 other processes. The results obtained were analyzed to identify the problems or bottlenecks that occurred and to propose improvement methods that can be implemented on the original model. Based on the comparisons that have been done between the improvement methods, the productivity could be increased by reallocating the workers and reducing loading time.« less

Dissolution of covalent adaptable network polymers in organic solvent

NASA Astrophysics Data System (ADS)

Yu, Kai; Yang, Hua; Dao, Binh H.; Shi, Qian; Yakacki, Christopher M.

2017-12-01

It was recently reported that thermosetting polymers can be fully dissolved in a proper organic solvent utilizing a bond-exchange reaction (BER), where small molecules diffuse into the polymer, break the long polymer chains into short segments, and eventually dissolve the network when sufficient solvent is provided. The solvent-assisted dissolution approach was applied to fully recycle thermosets and their fiber composites. This paper presents the first multi-scale modeling framework to predict the dissolution kinetics and mechanics of thermosets in organic solvent. The model connects the micro-scale network dynamics with macro-scale material properties: in the micro-scale, a model is developed based on the kinetics of BERs to describe the cleavage rate of polymer chains and evolution of chain segment length during the dissolution. The micro-scale model is then fed into a continuum-level model with considerations of the transportation of solvent molecules and chain segments in the system. The model shows good prediction on conversion rate of functional groups, degradation of network mechanical properties, and dissolution rate of thermosets during the dissolution. It identifies the underlying kinetic factors governing the dissolution process, and reveals the influence of different material and processing variables on the dissolution process, such as time, temperature, catalyst concentration, and chain length between cross-links.

Thin-film sulfuric acid anodizing as a replacement for chromic acid anodizing

NASA Technical Reports Server (NTRS)

Kallenborn, K. J.; Emmons, J. R.

1995-01-01

Chromic acid has long been used to produce a thin, corrosion resistant (Type I) coating on aluminum. Following anodizing, the hardware was sealed using a sodium dichromate solution. Sealing closes up pores inherent in the anodized coating, thus improving corrosion resistance. The thinness of the brittle coating is desirable from a fatigue standpoint, and chromium was absorbed by the coating during the sealing process, further improving corrosion resistance. Unfortunately, both chromic acid and sodium dichromate contain carcinogenic hexavalent chromium. Sulfuric acid is being considered as a replacement for chromic acid. Sulfuric acid of 10-20 percent concentration has traditionally been used to produce relatively thick (Types II and III) or abrasion resistant (Type III) coatings. A more dilute, that is five weight percent, sulfuric acid anodizing process, which produces a thinner coating than Type II or III, with nickel acetate as the sealant has been developed. The process was evaluated in regard to corrosion resistance, throwing power, fatigue life, and processing variable sensitivity, and shows promise as a replacement for the chromic acid process.

Investigation of the mechanical and chemical characteristics of nanotubular and nano-pitted anodic films on grade 2 titanium dental implant materials.

PubMed

Weszl, Miklós; Tóth, Krisztián László; Kientzl, Imre; Nagy, Péter; Pammer, Dávid; Pelyhe, Liza; Vrana, Nihal E; Scharnweber, Dieter; Wolf-Brandstetter, Cornelia; Joób F, Árpád; Bognár, Eszter

2017-09-01

The objective of this study was to investigate the reproducibility, mechanical integrity, surface characteristics and corrosion behavior of nanotubular (NT) titanium oxide arrays in comparison with a novel nano-pitted (NP) anodic film. Surface treatment processes were developed to grow homogenous NT and NP anodic films on the surface of grade 2 titanium discs and dental implants. The effect of process parameters on the surface characteristics and reproducibility of the anodic films was investigated and optimized. The mechanical integrity of the NT and NP anodic films were investigated by scanning electron microscopy, surface roughness measurement, scratch resistance and screwing tests, while the chemical and physicochemical properties were investigated in corrosion tests, contact angle measurement and X-ray photoelectron spectroscopy (XPS). The growth of NT anodic films was highly affected by process parameters, especially by temperature, and they were apt to corrosion and exfoliation. In contrast, the anodic growth of NP film showed high reproducibility even on the surface of 3-dimensional screw dental implants and they did not show signs of corrosion and exfoliation. The underlying reason of the difference in the tendency for exfoliation of the NT and NP anodic films is unclear; however the XPS analysis revealed fluorine dopants in a magnitude larger concentration on NT anodic film than on NP surface, which was identified as a possible causative. Concerning other surface characteristics that are supposed to affect the biological behavior of titanium implants, surface roughness values were found to be similar, whereas considerable differences were revealed in the wettability of the NT and NP anodic films. Our findings suggest that the applicability of NT anodic films on the surface of titanium bone implants may be limited because of mechanical considerations. In contrast, it is worth to consider the applicability of nano-pitted anodic films over nanotubular arrays for the enhancement of the biological properties of titanium implants. Copyright © 2017 Elsevier B.V. All rights reserved.

Electrical characterization of anodic alumina substrate with via-in-pad structure

NASA Astrophysics Data System (ADS)

Kim, Moonjung

2013-10-01

An anodic alumina substrate has been developed as a package substrate for dynamic random access memory devices. Unlike the conventional package substrates commonly made by laminating an epoxy-based core and cladding with copper, this substrate is fabricated using aluminum anodization technology. The anodization process produces a thick aluminum oxide layer on the aluminum substrate to be used as a dielectric layer. Placing copper patterns on the anodic aluminum oxide layer forms a new substrate structure that consists of a layered structure of aluminum, anodic aluminum oxide, and copper. Using selective anodization in the fabrication process, a via structure connecting the top copper layer and bottom aluminum layer is demonstrated. Additionally, by putting vias directly in the bond and ball pads in the substrate design, the via-in-pad structure is applied in this work. These two-layer metal structures and via-in-pad arrangements make routing easier and thus provide more design flexibility. Additionally, this new package substrate has improved the power distribution network impedance given the characteristics of these structures.

Method of manufacturing carbon nanotubes

NASA Technical Reports Server (NTRS)

Benavides, Jeanette M. (Inventor); Leidecker, Henning W. (Inventor); Frazier, Jeffrey (Inventor)

2004-01-01

A process for manufacturing carbon nanotubes, including a step of inducing electrical current through a carbon anode and a carbon cathode under conditions effective to produce the carbon nanotubes, wherein the carbon cathode is larger than the carbon anode. Preferably, a welder is used to induce the electrical current via an arc welding process. Preferably, an exhaust hood is placed on the anode, and the process does not require a closed or pressurized chamber. The process provides high-quality, single-walled carbon nanotubes, while eliminating the need for a metal catalyst.

Effect of processing on structural features of anodic aluminum oxides

NASA Astrophysics Data System (ADS)

Erdogan, Pembe; Birol, Yucel

2012-09-01

Morphological features of the anodic aluminum oxide (AAO) templates fabricated by electrochemical oxidation under different processing conditions were investigated. The selection of the polishing parameters does not appear to be critical as long as the aluminum substrate is polished adequately prior to the anodization process. AAO layers with a highly ordered pore distribution are obtained after anodizing in 0.6 M oxalic acid at 20 °C under 40 V for 5 minutes suggesting that the desired pore features are attained once an oxide layer develops on the surface. While the pore features are not affected much, the thickness of the AAO template increases with increasing anodization treatment time. Pore features are better and the AAO growth rate is higher at 20 °C than at 5 °C; higher under 45 V than under 40 V; higher with 0.6 M than with 0.3 M oxalic acid.

How does natural groundwater flow affect CO2 dissolution in saline aquifers?

NASA Astrophysics Data System (ADS)

Rosenzweig, R.; Michel-Meyer, I.; Tsinober, A.; Shavit, U.

2017-12-01

The dissolution of supercritical CO2 in aquifer brine is one of the most important trapping mechanisms in CO2 geological storage. Diffusion-limited dissolution is a very slow process. However, since the CO2-rich water is slightly denser than the CO2-free water, when CO2-free water is overlaid by heavier CO2-rich water, convective instability results in fingers of dense CO2-rich water that propagate downwards, causing CO2-unsaturated water to move upwards. This convection process significantly accelerates the dissolution rate of CO2 into the aquifer water.Most previous works have neglected the effect of natural groundwater flow and assumed it has no effect on the dissolution dynamics. However, it was found that in some of the saline aquifers groundwater flow rate, although small, is not zero. In this research, we study the effect of groundwater flow on dissolution by performing laboratory experiments in a bead pack cell using a mixture of methanol and ethylene-glycol as a CO2 analog while varying the water horizontal flow rate. We find that water horizontal flow decreases the number of fingers, their wavelength and their propagation velocity. When testing high water flow rates, no fingers were developed and the dissolution process was entirely diffusive. The effect of water flow on the dissolution rate did not show a clear picture. When increasing the horizontal flow rate the convective dissolution flux slightly decreased and then increased again. It seems that the combination of density-driven flow, water horizontal flow, mechanical dispersion and molecular diffusion affect the dissolution rate in a complex and non-monotonic manner. These intriguing dynamics should be further studied to understand their effect on dissolution trapping.

Etching of semiconductor cubic crystals: Determination of the dissolution slowness surfaces

NASA Astrophysics Data System (ADS)

Tellier, C. R.

1990-03-01

Equations of the representative surface of dissolution slowness for cubic crystals are determined in the framework of a tensorial approach of the orientation-dependent etching process. The independent dissolution constants are deduced from symmetry considerations. Using previous data on the chemical etching of germanium and gallium arsenide crystals, some possible polar diagrams of the dissolution slowness are proposed. A numerical and graphical simulation method is used to obtain the derived dissolution shapes. The influence of extrema in the dissolution slowness on the successive dissolution shapes is also examined. A graphical construction of limiting shapes of etched crystals appears possible using the tensorial representation of the dissolution slowness.

Low-viscosity hydroxypropylcellulose (HPC) grades SL and SSL: versatile pharmaceutical polymers for dissolution enhancement, controlled release, and pharmaceutical processing.

PubMed

Sarode, Ashish; Wang, Peng; Cote, Catherine; Worthen, David R

2013-03-01

Hydroxypropylcellulose (HPC)-SL and -SSL, low-viscosity hydroxypropylcellulose polymers, are versatile pharmaceutical excipients. The utility of HPC polymers was assessed for both dissolution enhancement and sustained release of pharmaceutical drugs using various processing techniques. The BCS class II drugs carbamazepine (CBZ), hydrochlorthiazide, and phenytoin (PHT) were hot melt mixed (HMM) with various polymers. PHT formulations produced by solvent evaporation (SE) and ball milling (BM) were prepared using HPC-SSL. HMM formulations of BCS class I chlorpheniramine maleate (CPM) were prepared using HPC-SL and -SSL. These solid dispersions (SDs) manufactured using different processes were evaluated for amorphous transformation and dissolution characteristics. Drug degradation because of HMM processing was also assessed. Amorphous conversion using HMM could be achieved only for relatively low-melting CBZ and CPM. SE and BM did not produce amorphous SDs of PHT using HPC-SSL. Chemical stability of all the drugs was maintained using HPC during the HMM process. Dissolution enhancement was observed in HPC-based HMMs and compared well to other polymers. The dissolution enhancement of PHT was in the order of SE>BM>HMM>physical mixtures, as compared to the pure drug, perhaps due to more intimate mixing that occurred during SE and BM than in HMM. Dissolution of CPM could be significantly sustained in simulated gastric and intestinal fluids using HPC polymers. These studies revealed that low-viscosity HPC-SL and -SSL can be employed to produce chemically stable SDs of poorly as well as highly water-soluble drugs using various pharmaceutical processes in order to control drug dissolution.

Dissolution enhancement of Deflazacort using hollow crystals prepared by antisolvent crystallization process.

PubMed

Paulino, A S; Rauber, G; Campos, C E M; Maurício, M H P; de Avillez, R R; Capobianco, G; Cardoso, S G; Cuffini, S L

2013-05-13

Deflazacort (DFZ), a derivate of prednisolone, is a poorly soluble drug which has been proposed to have major advantages over other corticosteroids. Poorly soluble drugs present limited bioavailability due to their low solubility and dissolution rate and several strategies have been developed in order to find ways to improve them. In general, pharmaceutical laboratories use a micronized process to reduce the particle size in order to increase the dissolution of the drugs. However, this process causes changes such as polymorphic transitions, particle agglomeration and a reduction in fluidity and wettability. These solid-state properties affect the dissolution behavior and stability performance of drugs. Crystallization techniques are widely used in the pharmaceutical industry and antisolvent crystallization has been used to obtain ultrafine particles. In this study, DFZ was investigated in terms of its antisolvent crystallization in different solvents and under various preparation conditions (methanol/water ratio, stirring and evaporation rate, etc.), in order to compare the physicochemical properties between crystallized samples and raw materials available on the Brazilian market with and without micronization. Crystalline structure, morphology, and particle size, and their correlation with the Intrinsic Dissolution Rate (IDR) and dissolution profile as relevant biopharmaceutical properties were studied. Crystallization conditions were achieved which provided crystalline samples of hollow-shaped crystals with internal channels, which increased the dissolution rate of DFZ. The antisolvent crystallization process allowed the formation of hollow crystals, which demonstrated a better dissolution profile than the raw material (crystalline and micronized), making this a promising technique as a crystallization strategy for improving the dissolution and thus the bioavailability of poorly soluble drugs. Copyright © 2013 Elsevier B.V. All rights reserved.

A method for phenomenological and chemical kinetics study of autocatalytic reactive dissolution by optical microscopy. The case of uranium dioxide dissolution in nitric acid media

NASA Astrophysics Data System (ADS)

Marc, Philippe; Magnaldo, Alastair; Godard, Jérémy; Schaer, Éric

2018-03-01

Dissolution is a milestone of the head-end of hydrometallurgical processes, as the stabilization rates of the chemical elements determine the process performance and hold-up. This study aims at better understanding the chemical and physico-chemical phenomena of uranium dioxide dissolution reactions in nitric acid media in the Purex process, which separates the reusable materials and the final wastes of the spent nuclear fuels. It has been documented that the attack of sintering-manufactured uranium dioxide solids occurs through preferential attack sites, which leads to the development of cracks in the solids. Optical microscopy observations show that in some cases, the development of these cracks leads to the solid cleavage. It is shown here that the dissolution of the detached fragments is much slower than the process of the complete cleavage of the solid, and occurs with no disturbing phenomena, like gas bubbling. This fact has motivated the measurement of dissolution kinetics using optical microscopy and image processing. By further discriminating between external resistance and chemical reaction, the "true" chemical kinetics of the reaction have been measured, and the highly autocatalytic nature of the reaction confirmed. Based on these results, the constants of the chemical reactions kinetic laws have also been evaluated.

Dissolution of used nuclear fuel using recycled nitric acid

DOE Office of Scientific and Technical Information (OSTI.GOV)

Almond, Philip M.; Daniel, Jr., William E.; Rudisill, Tracy S.

An evaluation was performed on the feasibility of using HB-Line anion exchange column waste streams from Alternate Feedstock 2 (AFS-2) processing for the dissolver solution for used nuclear fuel (UNF) processing. The targeted UNF for dissolution using recycled solution are fuels similar to the University of Missouri Research Reactor (MURR) fuel. Furthermore, the objectives of this experimental program were to validate the feasibility of using impure dissolver solutions with the MURR dissolution flowsheet to verify they would not significantly affect dissolution of the UNF in a detrimental manner.

Dissolution of used nuclear fuel using recycled nitric acid

DOE PAGES

Almond, Philip M.; Daniel, Jr., William E.; Rudisill, Tracy S.

2017-03-20

An evaluation was performed on the feasibility of using HB-Line anion exchange column waste streams from Alternate Feedstock 2 (AFS-2) processing for the dissolver solution for used nuclear fuel (UNF) processing. The targeted UNF for dissolution using recycled solution are fuels similar to the University of Missouri Research Reactor (MURR) fuel. Furthermore, the objectives of this experimental program were to validate the feasibility of using impure dissolver solutions with the MURR dissolution flowsheet to verify they would not significantly affect dissolution of the UNF in a detrimental manner.

Low cost fuel cell diffusion layer configured for optimized anode water management

DOEpatents

Owejan, Jon P; Nicotera, Paul D; Mench, Matthew M; Evans, Robert E

2013-08-27

A fuel cell comprises a cathode gas diffusion layer, a cathode catalyst layer, an anode gas diffusion layer, an anode catalyst layer and an electrolyte. The diffusion resistance of the anode gas diffusion layer when operated with anode fuel is higher than the diffusion resistance of the cathode gas diffusion layer. The anode gas diffusion layer may comprise filler particles having in-plane platelet geometries and be made of lower cost materials and manufacturing processes than currently available commercial carbon fiber substrates. The diffusion resistance difference between the anode gas diffusion layer and the cathode gas diffusion layer may allow for passive water balance control.

Modelling and shadowgraph imaging of cocrystal dissolution and assessment of in vitro antimicrobial activity for sulfadimidine/4-aminosalicylic acid cocrystals.

PubMed

Serrano, Dolores R; Persoons, Tim; D'Arcy, Deirdre M; Galiana, Carolina; Dea-Ayuela, Maria Auxiliadora; Healy, Anne Marie

2016-06-30

The aim of this work was to evaluate the influence of crystal habit on the dissolution and in vitro antibacterial and anitiprotozoal activity of sulfadimidine:4-aminosalicylic acid cocrystals. Cocrystals were produced via milling or solvent mediated processes. In vitro dissolution was carried out in the flow-through apparatus, with shadowgraph imaging and mechanistic mathematical models used to observe and simulate particle dissolution. In vitro activity was tested using agar diffusion assays. Cocrystallisation via milling produced small polyhedral crystals with antimicrobial activity significantly higher than sulfadimidine alone, consistent with a fast dissolution rate which was matched only by cocrystals which were milled following solvent evaporation. Cocrystallisation by solvent evaporation (ethanol, acetone) or spray drying produced flattened, plate-like or quasi-spherical cocrystals, respectively, with more hydrophobic surfaces and greater tendency to form aggregates in aqueous media, limiting both the dissolution rate and in vitro activity. Deviation from predicted dissolution profiles was attributable to aggregation behaviour, supported by observations from shadowgraph imaging. Aggregation behaviour during dissolution of cocrystals with different habits affected the dissolution rate, consistent with in vitro activity. Combining mechanistic models with shadowgraph imaging is a valuable approach for dissolution process analysis. Copyright © 2016 Elsevier B.V. All rights reserved.

Nonlinear dynamics and instability of aqueous dissolution of silicate glasses and minerals

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, Yifeng; Jove-Colon, Carlos F.; Kuhlman, Kristopher L.

2016-07-22

Aqueous dissolution of silicate glasses and minerals plays a critical role in global biogeochemical cycles and climate evolution. The reactivity of these materials is also important to numerous engineering applications including nuclear waste disposal. The dissolution process has long been considered to be controlled by a leached surface layer in which cations in the silicate framework are gradually leached out and replaced by protons from the solution. This view has recently been challenged by observations of extremely sharp corrosion fronts and oscillatory zonings in altered rims of the materials, suggesting that corrosion of these materials may proceed directly through congruentmore » dissolution followed by secondary mineral precipitation. Here we show that complex silicate material dissolution behaviors can emerge from a simple positive feedback between dissolution-induced cation release and cation-enhanced dissolution kinetics. This self-accelerating mechanism enables a systematic prediction of the occurrence of sharp dissolution fronts (vs. leached surface layers), oscillatory dissolution behaviors and multiple stages of glass dissolution (in particular the alteration resumption at a late stage of a corrosion process). In conclusion, our work provides a new perspective for predicting long-term silicate weathering rates in actual geochemical systems and developing durable silicate materials for various engineering applications.« less

Porous membrane electrochemical cell for uranium and transuranic recovery from molten salt electrolyte

DOEpatents

Willit, James L [Ratavia, IL

2007-09-11

An improved process and device for the recovery of the minor actinides and the transuranic elements (TRU's) from a molten salt electrolyte. The process involves placing the device, an electrically non-conducting barrier between an anode salt and a cathode salt. The porous barrier allows uranium to diffuse between the anode and cathode, yet slows the diffusion of uranium ions so as to cause depletion of uranium ions in the catholyte. This allows for the eventual preferential deposition of transuranics present in spent nuclear fuel such as Np, Pu, Am, Cm. The device also comprises an uranium oxidation anode. The oxidation anode is solid uranium metal in the form of spent nuclear fuel. The spent fuel is placed in a ferric metal anode basket which serves as the electrical lead or contact between the molten electrolyte and the anodic uranium metal.

Porous membrane electrochemical cell for uranium and transuranic recovery from molten salt electrolyte

DOEpatents

Willit, James L [Batavia, IL

2010-09-21

An improved process and device for the recovery of the minor actinides and the transuranic elements (TRU's) from a molten salt electrolyte. The process involves placing the device, an electrically non-conducting barrier between an anode salt and a cathode salt. The porous barrier allows uranium to diffuse between the anode and cathode, yet slows the diffusion of uranium ions so as to cause depletion of uranium ions in the catholyte. This allows for the eventual preferential deposition of transuranics present in spent nuclear fuel such as Np, Pu, Am, Cm. The device also comprises an uranium oxidation anode. The oxidation anode is solid uranium metal in the form of spent nuclear fuel. The spent fuel is placed in a ferric metal anode basket which serves as the electrical lead or contact between the molten electrolyte and the anodic uranium metal.

Study the effect of striping in two-step anodizing process on pore arrangement of nano-porous alumina

NASA Astrophysics Data System (ADS)

Rahimi, M. H.; Saramad, S.; Tabaian, S. H.; Marashi, S. P.; Zolfaghari, A.; Mohammadalinezhad, M.

2009-10-01

Two-step anodic oxidation of aluminum is generally employed to produce the ordered porous anodized alumina (PAA). Dissolving away (striping) the oxide film after the first anodizing step plays a key role in the final arrangement of nano-pores. In this work, different striping durations between 1 and 6 h were applied to the sample that was initially anodized at a constant voltage of 40 V at 17 °C for 15 h. The striping duration of 3 h was realized as the optimum time for achieving the best ordering degree for the pores. Scanning electron microscopy (SEM) was used during and at the end of the process to examine the cross section and finishing surface of the specimens. Linear-angular fast Fourier transform (LA-FFT), an in-house technique based on MATLAB software, was employed to assess the ordering degree of the anodized samples.

Nanosizing of drugs: Effect on dissolution rate

PubMed Central

Dizaj, S. Maleki; Vazifehasl, Zh.; Salatin, S.; Adibkia, Kh.; Javadzadeh, Y.

2015-01-01

The solubility, bioavailability and dissolution rate of drugs are important parameters for achieving in vivo efficiency. The bioavailability of orally administered drugs depends on their ability to be absorbed via gastrointestinal tract. For drugs belonging to Class II of pharmaceutical classification, the absorption process is limited by drug dissolution rate in gastrointestinal media. Therefore, enhancement of the dissolution rate of these drugs will present improved bioavailability. So far several techniques such as physical and chemical modifications, changing in crystal habits, solid dispersion, complexation, solubilization and liquisolid method have been used to enhance the dissolution rate of poorly water soluble drugs. It seems that improvement of the solubility properties ofpoorly water soluble drugscan translate to an increase in their bioavailability. Nowadays nanotechnology offers various approaches in the area of dissolution enhancement of low aqueous soluble drugs. Nanosizing of drugs in the form of nanoparticles, nanocrystals or nanosuspensions not requiring expensive facilities and equipment or complicated processes may be applied as simple methods to increase the dissolution rate of poorly water soluble drugs. In this article, we attempted to review the effects of nanosizing on improving the dissolution rate of poorly aqueous soluble drugs. According to the reviewed literature, by reduction of drug particle size into nanometer size the total effective surface area is increased and thereby dissolution rate would be enhanced. Additionally, reduction of particle size leads to reduction of the diffusion layer thickness surrounding the drug particles resulting in the increment of the concentration gradient. Each of these process leads to improved bioavailability. PMID:26487886

Effects of half-wave and full-wave power source on the anodic oxidation process on AZ91D magnesium alloy

NASA Astrophysics Data System (ADS)

Wang, Ximei; Zhu, Liqun; Li, Weiping; Liu, Huicong; Li, Yihong

2009-03-01

Anodic films have been prepared on the AZ91D magnesium alloys in 1 mol/L Na 2SiO 3 with 10 vol.% silica sol addition under the constant voltage of 60 V at room temperature by half-wave and full-wave power sources. The weight of the anodic films has been scaled by analytical balance, and the thickness has been measured by eddy current instrument. The surface morphologies, chemical composition and structure of the anodic films have been characterized by scanning electron microscopy (SEM), energy dispersion spectrometry (EDS), X-ray diffraction (XRD) and transmission electron microscopy (TEM). The results show that the thickness and weight of the anodic films formed by the two power sources both increase with the anodizing time, and the films anodized by full-wave power source grow faster than that by half-wave one. Furthermore, we have fitted polynomial to the scattered data of the weight and thickness in a least-squares sense with MATLAB, which could express the growth process of the anodic films sufficiently. The full-wave power source is inclined to accelerate the growth of the anodic films, and the half-wave one is mainly contributed to the uniformity and fineness of the films. The anodic film consists of crystalline Mg 2SiO 4 and amorphous SiO 2.

Fabrication of Self-Ordered Alumina Films with Large Interpore Distance by Janus Anodization in Citric Acid

NASA Astrophysics Data System (ADS)

Ma, Yingjun; Wen, Yihao; Li, Juan; Li, Yuxin; Zhang, Zhiying; Feng, Chenchen; Sun, Runguang

2016-12-01

Self-organized porous anodic alumina (PAA) formed by electrochemical anodization have become a fundamental tool to develop various functional nanomaterials. However, it is still a great challenge to break the interpore distance (Dint) limit (500 nm) by using current anodization technologies of mild anodization (MA) and hard anodization (HA). Here, we reported a new anodization mode named “Janus anodization” (JA) to controllably fabricate self-ordered PAA with large Dint at high voltage of 350-400 V. JA naturally occurs as anodizing Al foils in citric acid solution, which possessing both the characteristics of MA and HA. The process can be divided into two stages: I, slow pore nucleation stage similar to MA; II, unequilibrium self-organization process similar to HA. The as-prepared films had the highest modulus (7.0 GPa) and hardness (127.2 GPa) values compared with the alumina obtained by MA and HA. The optical studies showed that the black films have low reflectance (<10 %) in the wavelength range of 250-1500 nm and photoluminescence property. Dint can be tuned between 645-884 nm by controlling citric acid concentration or anodization voltage. JA is a potential technology to efficiently and controllably fabricate microstructured or hybrid micro- and nanostructured materials with novel properties.

Fabrication of Self-Ordered Alumina Films with Large Interpore Distance by Janus Anodization in Citric Acid

PubMed Central

Ma, Yingjun; Wen, Yihao; Li, Juan; Li, Yuxin; Zhang, Zhiying; Feng, Chenchen; Sun, Runguang

2016-01-01

Self-organized porous anodic alumina (PAA) formed by electrochemical anodization have become a fundamental tool to develop various functional nanomaterials. However, it is still a great challenge to break the interpore distance (Dint) limit (500 nm) by using current anodization technologies of mild anodization (MA) and hard anodization (HA). Here, we reported a new anodization mode named “Janus anodization” (JA) to controllably fabricate self-ordered PAA with large Dint at high voltage of 350–400 V. JA naturally occurs as anodizing Al foils in citric acid solution, which possessing both the characteristics of MA and HA. The process can be divided into two stages: I, slow pore nucleation stage similar to MA; II, unequilibrium self-organization process similar to HA. The as-prepared films had the highest modulus (7.0 GPa) and hardness (127.2 GPa) values compared with the alumina obtained by MA and HA. The optical studies showed that the black films have low reflectance (<10 %) in the wavelength range of 250–1500 nm and photoluminescence property. Dint can be tuned between 645–884 nm by controlling citric acid concentration or anodization voltage. JA is a potential technology to efficiently and controllably fabricate microstructured or hybrid micro- and nanostructured materials with novel properties. PMID:27958365

Effects of Complex Structured Anodic Oxide Dielectric Layer Grown in Pore Matrix for Aluminum Capacitor.

PubMed

Shin, Jin-Ha; Yun, Sook Young; Lee, Chang Hyoung; Park, Hwa-Sun; Suh, Su-Jeong

2015-11-01

Anodization of aluminum is generally divided up into two types of anodic aluminum oxide structures depending on electrolyte type. In this study, an anodization process was carried out in two steps to obtain high dielectric strength and break down voltage. In the first step, evaporated high purity Al on Si wafer was anodized in oxalic acidic aqueous solution at various times at a constant temperature of 5 degrees C. In the second step, citric acidic aqueous solution was used to obtain a thickly grown sub-barrier layer. During the second anodization process, the anodizing potential of various ranges was applied at room temperature. An increased thickness of the sub-barrier layer in the porous matrix was obtained according to the increment of the applied anodizing potential. The microstructures and the growth of the sub-barrier layer were then observed with an increasing anodizing potential of 40 to 300 V by using a scanning electron microscope (SEM). An impedance analyzer was used to observe the change of electrical properties, including the capacitance, dissipation factor, impedance, and equivalent series resistance (ESR) depending on the thickness increase of the sub-barrier layer. In addition, the breakdown voltage was measured. The results revealed that dielectric strength was improved with the increase of sub-barrier layer thickness.

Osteoconductivity and Hydrophilicity of TiO2 Coatings on Ti Substrates Prepared by Different Oxidizing Processes

PubMed Central

Yamamoto, Dai; Kawai, Ikki; Kuroda, Kensuke; Ichino, Ryoichi; Okido, Masazumi; Seki, Azusa

2012-01-01

Various techniques for forming TiO2 coatings on Ti have been investigated for the improvement of the osteoconductivity of Ti implants. However, it is not clear how the oxidizing process affects this osteoconductivity. In this study, TiO2 coatings were prepared using the following three processes: anodizing in 0.1 M H3PO4 or 0.1 M NaOH aqueous solution; thermal oxidation at 673 K for 2 h in air; and a two-step process of anodizing followed by thermal oxidation. The oxide coatings were evaluated using SEM, XRD, and XPS. The water contact angle on the TiO2 coatings was measured as a surface property. The osteoconductivity of these samples was evaluated by measuring the contact ratio of formed hard tissue on the implanted samples (defined as the R B-I value) after 14 d implantation in rats' tibias. Anatase was formed by anodizing and rutile by thermal oxidation, but the difference in the TiO2 crystal structure did not influence the osteoconductivity. Anodized TiO2 coatings were hydrophilic, but thermally oxidized TiO2 coatings were less hydrophilic than anodized TiO2 coatings because they lacked in surface OH groups. The TiO2 coating process using anodizing without thermal oxidation gave effective improvement of the osteoconductivity of Ti samples. PMID:23316128

Discharge properties of Mg-Al-Mn-Ca and Mg-Al-Mn alloys as anode materials for primary magnesium-air batteries

NASA Astrophysics Data System (ADS)

Yuasa, Motohiro; Huang, Xinsheng; Suzuki, Kazutaka; Mabuchi, Mamoru; Chino, Yasumasa

2015-11-01

The discharge behaviors of rolled Mg-6 mass%Al-0.3 mass%Mn-2 mass%Ca (AMX602) and Mg-6 mass%Al-0.3 mass%Mn (AM60) alloys used as anodes for Magnesium-air batteries were investigated. The AMX602 alloy exhibited superior discharge properties compared to the AM60 alloy, especially at low current density. The discharge products of the AMX602 alloy were dense and thin, and many cracks were observed at all current densities. In addition, the discharge products were detached at some sites. These sites often corresponded to the positions of Al2Ca particles. The comparison of the discharge and corrosion tests indicated that the dense and thin discharge products of AMX602 were easily cracked by dissolution of the Mg matrix around Al2Ca particles, and the cracks promoted the penetration of the electrolyte into the discharge products, retaining the discharge activity. In contrast, concerning the AM60 alloy, thick discharge products were formed on the surface during discharge, and cracking of the discharge products hardly occurred, degrading the discharge properties. Localized and deeply corroded pits that could result from the detachment of metal pieces from the anode during discharge were partly observed in the AM60 alloy. It is suggested that these detached metal pieces are another reason for the low discharge properties of the AM60 alloy.

Morphology and Mechanism of Benign Inhibitors

DTIC Science & Technology

2012-07-01

AAO resulting in much lower SLD. ....... 84 xiv List of Acronyms AA: Aluminum alloy; AAO : Anodic aluminum oxide ; AMCC: Advanced Materials...shown, we achieved excellent vanadate, trivalent chromium process (TCP) and anodic aluminum oxide ( AAO ) films. We also tried Ce but Ce did not form a...we also initiated the study of anodizing of aluminum . According to the literature anodic aluminum oxide

The Kinetics of Dissolution Revisited

NASA Astrophysics Data System (ADS)

Antonel, Paula S.; Hoijemberg, Pablo A.; Maiante, Leandro M.; Lagorio, M. Gabriela

2003-09-01

An experiment analyzing the kinetics of dissolution of a solid with cylindrical geometry in water is presented. The dissolution process is followed by measuring the solid mass and its size parameters (thickness and diameter) as a function of time. It is verified that the dissolution rate follows the Nernst model. Data treatment is compared with the dissolution of a spherical solid previously described. Kinetics, diffusion concepts, and polynomial fitting of experimental data are combined in this simple experiment.

Effective regeneration of anode material recycled from scrapped Li-ion batteries

NASA Astrophysics Data System (ADS)

Zhang, Jin; Li, Xuelei; Song, Dawei; Miao, Yanli; Song, Jishun; Zhang, Lianqi

2018-06-01

Recycling high-valuable metal elements (such as Li, Ni, Co, Al and Cu elements) from scrapped lithium ion batteries can bring significant economic benefits. However, recycling and reusing anode material has not yet attracted wide attention up to now, due to the lower added-value than the above valuable metal materials and the difficulties in regenerating process. In this paper, a novel regeneration process with significant green advance is proposed to regenerate anode material recycled from scrapped Li-ion batteries for the first time. After regenerated, most acetylene black (AB) and all the styrene butadiene rubber (SBR), carboxymethylcellulose sodium (CMC) in recycled anode material are removed, and the surface of anode material is coated with pyrolytic carbon from phenolic resin again. Finally, the regenerated anode material (graphite with coating layer, residual AB and a little CMC pyrolysis product) is obtained. As expected, all the technical indexs of regenerated anode material exceed that of a midrange graphite with the same type, and partial technical indexs are even closed to that of the unused graphite. The results indicate the effective regeneration of anode material recycled from scrapped Li-ion batteries is really achieved.

In situ fabrication of high-performance Ni-GDC-nanocube core-shell anode for low-temperature solid-oxide fuel cells

PubMed Central

Yamamoto, Kazuhiro; Qiu, Nan; Ohara, Satoshi

2015-01-01

A core–shell anode consisting of nickel–gadolinium-doped-ceria (Ni–GDC) nanocubes was directly fabricated by a chemical process in a solution containing a nickel source and GDC nanocubes covered with highly reactive {001} facets. The cermet anode effectively generated a Ni metal framework even at 500 °C with the growth of the Ni spheres. Anode fabrication at such a low temperature without any sintering could insert a finely nanostructured layer close to the interface between the electrolyte and the anode. The maximum power density of the attractive anode was 97 mW cm–2, which is higher than that of a conventional NiO–GDC anode prepared by an aerosol process at 55 mW cm–2 and 600 °C, followed by sintering at 1300 °C. Furthermore, the macro- and microstructure of the Ni–GDC-nanocube anode were preserved before and after the power-generation test at 700 °C. Especially, the reactive {001} facets were stabled even after generation test, which served to reduce the activation energy for fuel oxidation successfully. PMID:26615816

Mathematical modeling of drug dissolution.

PubMed

Siepmann, J; Siepmann, F

2013-08-30

The dissolution of a drug administered in the solid state is a pre-requisite for efficient subsequent transport within the human body. This is because only dissolved drug molecules/ions/atoms are able to diffuse, e.g. through living tissue. Thus, generally major barriers, including the mucosa of the gastro intestinal tract, can only be crossed after dissolution. Consequently, the process of dissolution is of fundamental importance for the bioavailability and, hence, therapeutic efficacy of various pharmaco-treatments. Poor aqueous solubility and/or very low dissolution rates potentially lead to insufficient availability at the site of action and, hence, failure of the treatment in vivo, despite a potentially ideal chemical structure of the drug to interact with its target site. Different physical phenomena are involved in the process of drug dissolution in an aqueous body fluid, namely the wetting of the particle's surface, breakdown of solid state bonds, solvation, diffusion through the liquid unstirred boundary layer surrounding the particle as well as convection in the surrounding bulk fluid. Appropriate mathematical equations can be used to quantify these mass transport steps, and more or less complex theories can be developed to describe the resulting drug dissolution kinetics. This article gives an overview on the current state of the art of modeling drug dissolution and points out the assumptions the different theories are based on. Various practical examples are given in order to illustrate the benefits of such models. This review is not restricted to mathematical theories considering drugs exhibiting poor aqueous solubility and/or low dissolution rates, but also addresses models quantifying drug release from controlled release dosage forms, in which the process of drug dissolution plays a major role. Copyright © 2013 Elsevier B.V. All rights reserved.

Assessment of anodal and cathodal transcranial direct current stimulation (tDCS) on MMN-indexed auditory sensory processing.

PubMed

Impey, Danielle; de la Salle, Sara; Knott, Verner

2016-06-01

Transcranial direct current stimulation (tDCS) is a non-invasive form of brain stimulation which uses a very weak constant current to temporarily excite (anodal stimulation) or inhibit (cathodal stimulation) activity in the brain area of interest via small electrodes placed on the scalp. Currently, tDCS of the frontal cortex is being used as a tool to investigate cognition in healthy controls and to improve symptoms in neurological and psychiatric patients. tDCS has been found to facilitate cognitive performance on measures of attention, memory, and frontal-executive functions. Recently, a short session of anodal tDCS over the temporal lobe has been shown to increase auditory sensory processing as indexed by the Mismatch Negativity (MMN) event-related potential (ERP). This preliminary pilot study examined the separate and interacting effects of both anodal and cathodal tDCS on MMN-indexed auditory pitch discrimination. In a randomized, double blind design, the MMN was assessed before (baseline) and after tDCS (2mA, 20min) in 2 separate sessions, one involving 'sham' stimulation (the device is turned off), followed by anodal stimulation (to temporarily excite cortical activity locally), and one involving cathodal stimulation (to temporarily decrease cortical activity locally), followed by anodal stimulation. Results demonstrated that anodal tDCS over the temporal cortex increased MMN-indexed auditory detection of pitch deviance, and while cathodal tDCS decreased auditory discrimination in baseline-stratified groups, subsequent anodal stimulation did not significantly alter MMN amplitudes. These findings strengthen the position that tDCS effects on cognition extend to the neural processing of sensory input and raise the possibility that this neuromodulatory technique may be useful for investigating sensory processing deficits in clinical populations. Copyright © 2016 Elsevier Inc. All rights reserved.

31 CFR 353.83 - Reissue or payment on dissolution of corporation or partnership.

Code of Federal Regulations, 2011 CFR

2011-07-01

... 31 Money and Finance:Treasury 2 2011-07-01 2011-07-01 false Reissue or payment on dissolution of... Reissue or payment on dissolution of corporation or partnership. (a) Corporations. A bond registered in the name of a private corporation which is in the process of dissolution will be paid to the...

31 CFR 315.83 - Reissue or payment on dissolution of corporation or partnership.

Code of Federal Regulations, 2014 CFR

2014-07-01

... 31 Money and Finance: Treasury 2 2014-07-01 2014-07-01 false Reissue or payment on dissolution of... and Officers § 315.83 Reissue or payment on dissolution of corporation or partnership. (a) Corporations. A bond registered in the name of a private corporation which is in the process of dissolution...

31 CFR 353.83 - Reissue or payment on dissolution of corporation or partnership.

Code of Federal Regulations, 2013 CFR

2013-07-01

... 31 Money and Finance:Treasury 2 2013-07-01 2013-07-01 false Reissue or payment on dissolution of... Reissue or payment on dissolution of corporation or partnership. (a) Corporations. A bond registered in the name of a private corporation which is in the process of dissolution will be paid to the...

31 CFR 315.83 - Reissue or payment on dissolution of corporation or partnership.

Code of Federal Regulations, 2010 CFR

2010-07-01

... 31 Money and Finance: Treasury 2 2010-07-01 2010-07-01 false Reissue or payment on dissolution of... and Officers § 315.83 Reissue or payment on dissolution of corporation or partnership. (a) Corporations. A bond registered in the name of a private corporation which is in the process of dissolution...

31 CFR 353.83 - Reissue or payment on dissolution of corporation or partnership.

Code of Federal Regulations, 2012 CFR

2012-07-01

... 31 Money and Finance:Treasury 2 2012-07-01 2012-07-01 false Reissue or payment on dissolution of... Reissue or payment on dissolution of corporation or partnership. (a) Corporations. A bond registered in the name of a private corporation which is in the process of dissolution will be paid to the...

31 CFR 353.83 - Reissue or payment on dissolution of corporation or partnership.

Code of Federal Regulations, 2010 CFR

2010-07-01

... 31 Money and Finance: Treasury 2 2010-07-01 2010-07-01 false Reissue or payment on dissolution of... Reissue or payment on dissolution of corporation or partnership. (a) Corporations. A bond registered in the name of a private corporation which is in the process of dissolution will be paid to the...

31 CFR 315.83 - Reissue or payment on dissolution of corporation or partnership.

Code of Federal Regulations, 2011 CFR

2011-07-01

... 31 Money and Finance:Treasury 2 2011-07-01 2011-07-01 false Reissue or payment on dissolution of... and Officers § 315.83 Reissue or payment on dissolution of corporation or partnership. (a) Corporations. A bond registered in the name of a private corporation which is in the process of dissolution...

31 CFR 315.83 - Reissue or payment on dissolution of corporation or partnership.

Code of Federal Regulations, 2012 CFR

2012-07-01

... 31 Money and Finance:Treasury 2 2012-07-01 2012-07-01 false Reissue or payment on dissolution of... and Officers § 315.83 Reissue or payment on dissolution of corporation or partnership. (a) Corporations. A bond registered in the name of a private corporation which is in the process of dissolution...

31 CFR 353.83 - Reissue or payment on dissolution of corporation or partnership.

Code of Federal Regulations, 2014 CFR

2014-07-01

... 31 Money and Finance: Treasury 2 2014-07-01 2014-07-01 false Reissue or payment on dissolution of... Reissue or payment on dissolution of corporation or partnership. (a) Corporations. A bond registered in the name of a private corporation which is in the process of dissolution will be paid to the...

31 CFR 315.83 - Reissue or payment on dissolution of corporation or partnership.

Code of Federal Regulations, 2013 CFR

2013-07-01

... 31 Money and Finance:Treasury 2 2013-07-01 2013-07-01 false Reissue or payment on dissolution of... and Officers § 315.83 Reissue or payment on dissolution of corporation or partnership. (a) Corporations. A bond registered in the name of a private corporation which is in the process of dissolution...

Carbonate fuel cell anodes

DOEpatents

Donado, R.A.; Hrdina, K.E.; Remick, R.J.

1993-04-27

A molten alkali metal carbonates fuel cell porous anode of lithium ferrite and a metal or metal alloy of nickel, cobalt, nickel/iron, cobalt/iron, nickel/iron/aluminum, cobalt/iron/aluminum and mixtures thereof wherein the total iron content including ferrite and iron of the composite is about 25 to about 80 percent, based upon the total anode, provided aluminum when present is less than about 5 weight percent of the anode. A process is described for production of the lithium ferrite containing anode by slipcasting.

Carbonate fuel cell anodes

DOEpatents

Donado, Rafael A.; Hrdina, Kenneth E.; Remick, Robert J.

1993-01-01

A molten alkali metal carbonates fuel cell porous anode of lithium ferrite and a metal or metal alloy of nickel, cobalt, nickel/iron, cobalt/iron, nickel/iron/aluminum, cobalt/iron/aluminum and mixtures thereof wherein the total iron content including ferrite and iron of the composite is about 25 to about 80 percent, based upon the total anode, provided aluminum when present is less than about 5 weight percent of the anode. A process for production of the lithium ferrite containing anode by slipcasting.

Justification of disintegration testing beyond current FDA criteria using in vitro and in silico models.

PubMed

Uebbing, Lukas; Klumpp, Lukas; Webster, Gregory K; Löbenberg, Raimar

2017-01-01

Drug product performance testing is an important part of quality-by-design approaches, but this process often lacks the underlying mechanistic understanding of the complex interactions between the disintegration and dissolution processes involved. Whereas a recent draft guideline by the US Food and Drug Administration (FDA) has allowed the replacement of dissolution testing with disintegration testing, the mentioned criteria are not globally accepted. This study provides scientific justification for using disintegration testing rather than dissolution testing as a quality control method for certain immediate release (IR) formulations. A mechanistic approach, which is beyond the current FDA criteria, is presented. Dissolution testing via United States Pharmacopeial Convention Apparatus II at various paddle speeds was performed for immediate and extended release formulations of metronidazole. Dissolution profile fitting via DDSolver and dissolution profile predictions via DDDPlus™ were performed. The results showed that Fickian diffusion and drug particle properties (DPP) were responsible for the dissolution of the IR tablets, and that formulation factors (eg, coning) impacted dissolution only at lower rotation speeds. Dissolution was completely formulation controlled if extended release tablets were tested and DPP were not important. To demonstrate that disintegration is the most important dosage form attribute when dissolution is DPP controlled, disintegration, intrinsic dissolution and dissolution testing were performed in conventional and disintegration impacting media (DIM). Tablet disintegration was affected by DIM and model fitting to the Korsmeyer-Peppas equation showed a growing effect of the formulation in DIM. DDDPlus was able to predict tablet dissolution and the intrinsic dissolution profiles in conventional media and DIM. The study showed that disintegration has to occur before DPP-dependent dissolution can happen. The study suggests that disintegration can be used as performance test of rapidly disintegrating tablets beyond the FDA criteria. The scientific criteria and justification is that dissolution has to be DPP dependent, originated from active pharmaceutical ingredient characteristics and formulations factors have to be negligible.

Justification of disintegration testing beyond current FDA criteria using in vitro and in silico models

PubMed Central

Uebbing, Lukas; Klumpp, Lukas; Webster, Gregory K; Löbenberg, Raimar

2017-01-01

Drug product performance testing is an important part of quality-by-design approaches, but this process often lacks the underlying mechanistic understanding of the complex interactions between the disintegration and dissolution processes involved. Whereas a recent draft guideline by the US Food and Drug Administration (FDA) has allowed the replacement of dissolution testing with disintegration testing, the mentioned criteria are not globally accepted. This study provides scientific justification for using disintegration testing rather than dissolution testing as a quality control method for certain immediate release (IR) formulations. A mechanistic approach, which is beyond the current FDA criteria, is presented. Dissolution testing via United States Pharmacopeial Convention Apparatus II at various paddle speeds was performed for immediate and extended release formulations of metronidazole. Dissolution profile fitting via DDSolver and dissolution profile predictions via DDDPlus™ were performed. The results showed that Fickian diffusion and drug particle properties (DPP) were responsible for the dissolution of the IR tablets, and that formulation factors (eg, coning) impacted dissolution only at lower rotation speeds. Dissolution was completely formulation controlled if extended release tablets were tested and DPP were not important. To demonstrate that disintegration is the most important dosage form attribute when dissolution is DPP controlled, disintegration, intrinsic dissolution and dissolution testing were performed in conventional and disintegration impacting media (DIM). Tablet disintegration was affected by DIM and model fitting to the Korsmeyer–Peppas equation showed a growing effect of the formulation in DIM. DDDPlus was able to predict tablet dissolution and the intrinsic dissolution profiles in conventional media and DIM. The study showed that disintegration has to occur before DPP-dependent dissolution can happen. The study suggests that disintegration can be used as performance test of rapidly disintegrating tablets beyond the FDA criteria. The scientific criteria and justification is that dissolution has to be DPP dependent, originated from active pharmaceutical ingredient characteristics and formulations factors have to be negligible. PMID:28442890

Nanopatterning of Crystalline Silicon Using Anodized Aluminum Oxide Templates for Photovoltaics

NASA Astrophysics Data System (ADS)

Chao, Tsu-An

A novel thin film anodized aluminum oxide templating process was developed and applied to make nanopatterns on crystalline silicon to enhance the optical properties of silicon. The thin film anodized aluminum oxide was created to improve the conventional thick aluminum templating method with the aim for potential large scale fabrication. A unique two-step anodizing method was introduced to create high quality nanopatterns and it was demonstrated that this process is superior over the original one-step approach. Optical characterization of the nanopatterned silicon showed up to 10% reduction in reflection in the short wavelength range. Scanning electron microscopy was also used to analyze the nanopatterned surface structure and it was found that interpore spacing and pore density can be tuned by changing the anodizing potential.

Large area organic light emitting diodes with multilayered graphene anodes

NASA Astrophysics Data System (ADS)

Moon, Jaehyun; Hwang, Joohyun; Choi, Hong Kyw; Kim, Taek Yong; Choi, Sung-Yool; Joo, Chul Woong; Han, Jun-Han; Shin, Jin-Wook; Lee, Bong Joon; Cho, Doo-Hee; Huh, Jin Woo; Park, Seung Koo; Cho, Nam Sung; Chu, Hye Yong; Lee, Jeong-Ik

2012-09-01

In this work, we demonstrate fully uniform blue fluorescence graphene anode OLEDs, which have an emission area of 10×7 mm2. Catalytically grown multilayered graphene films have been used as the anode material. In order to compensate the current drop, which is due to the graphene's electrical resistance, we have furnished metal bus lines on the support. Processing and optical issues involved in graphene anode OLED fabrications are presented. The fabricated OLEDs with graphene anode showed comparable performances to that of ITO anode OLEDs. Our works shows that metal bus furnished graphene anode can be extended into large area OLED lighting applications in which flexibility and transparency is required.

Novel Bonding Technology for Hermetically Sealed Silicon Micropackage

NASA Astrophysics Data System (ADS)

Lee, Duck-Jung; Ju, Byeong-Kwon; Choi, Woo-Beom; Jeong, Jee-Won; Lee, Yun-Hi; Jang, Jin; Lee, Kwang-Bae; Oh, Myung-Hwan

1999-01-01

We performed glass-to-silicon bonding and fabricated a hermetically sealed silicon wafer using silicon direct bonding followed by anodic bonding (SDAB). The hydrophilized glass and silicon wafers in solution were dried and initially bonded in atmosphere as in the silicon direct bonding (SDB) process, but annealing at high temperature was not performed. Anodic bonding was subsequently carried out for the initially bonded specimens. Then the wafer pairs bonded by the SDAB method were different from those bonded by the anodic bonding process only. The effects of the bonding process on the bonded area and tensile strength were investigated as functions of bonding temperature and voltage. Using scanning electron microscopy (SEM), the cross-sectional view of the bonded interface region was observed. In order to investigate the migration of the sodium ions in the bonding process, the concentration of the bonded glass was compared with that of standard glass. The specimen bonded using the SDAB process had higher efficiency than that using the anodic bonding process only.

Collective acceleration of ions in a system with an insulated anode

NASA Astrophysics Data System (ADS)

Bystritskii, V. M.; Didenko, A. N.; Krasik, Ya. E.; Lopatin, V. S.; Podkatov, V. I.

1980-11-01

An investigation was made of the processes of collective acceleration of protons in vacuum in a system with an insulated anode and trans-anode electrodes, which were insulated or grounded, in high-current Tonus and Vera electron accelerators. The influence of external conditions and parameters of the electron beam on the efficiency of acceleration processes was investigated. Experiments were carried out in which protons were accelerated in a system with trans-anode electrodes. A study was made of the influence of a charge prepulse and of the number of trans-anode electrodes on the energy of the accelerated electrons. A system with a single anode produced Np=1014 protons of 2Ee < Ep < 3Ee energy. Suppression of a charge prepulse increased the proton energy to (6 8)Ee and the yield was then 1013. The maximum proton energy of 14Ee was obtained in a system with three trans-anode electrodes. A possible mechanism of proton acceleration was analyzed. The results obtained were compared with those of other investigations. Ways of increasing the efficiency of this acceleration method were considered.

Improved performance of anodic titanium oxide nanotube arrays synthesized by sonoelectrochemical anodization method for dye-sensitized solar cells

NASA Astrophysics Data System (ADS)

Peighambardoust, Naeimeh-Sadat; Khameneh-Asl, Shahin; Azimi, Hamid

2017-05-01

With rising demand for using solar cell systems for energy and environmental applications, considerable interest in anode materials of these cells has dramatically emerged. In this work, TiO2 nanotubular electrodes of varying thicknesses as anode were fabricated using effective process in a short time by sonoelectrochemical anodizing of Ti using an organic electrolyte, containing Na2[H2EDTA]. Long TiO2 nanotubes about 30-40 μm thick containing ordered hexagonal TiO2 were achieved through manipulating anodization parameters. Dye-sensitized solar cells (DSSCs) with different TiO2 electrode morphologies of varying thicknesses were compared to DSSCs based on TiO2 Nanoparticle electrodes. The effect of controlling parameters of the sonoelectrochemical process including surface preparation and anodizing time was investigated. This report brings to attention the desirable properties of the structurally oriented TiO2 for dye-sensitized solar cell applications. It found that the best cell performance was achieved about 3.14% in the case of using TiO2 NT layers that were treated by TiCl4 treatment.

Process for producing a high emittance coating and resulting article

NASA Technical Reports Server (NTRS)

Le, Huong G. (Inventor); O'Brien, Dudley L. (Inventor)

1993-01-01

Process for anodizing aluminum or its alloys to obtain a surface particularly having high infrared emittance by anodizing an aluminum or aluminum alloy substrate surface in an aqueous sulfuric acid solution at elevated temperature and by a step-wise current density procedure, followed by sealing the resulting anodized surface. In a preferred embodiment the aluminum or aluminum alloy substrate is first alkaline cleaned and then chemically brightened in an acid bath The resulting cleaned substrate is anodized in a 15% by weight sulfuric acid bath maintained at a temperature of 30.degree. C. Anodizing is carried out by a step-wise current density procedure at 19 amperes per square ft. (ASF) for 20 minutes, 15 ASF for 20 minutes and 10 ASF for 20 minutes. After anodizing the sample is sealed by immersion in water at 200.degree. F. and then air dried. The resulting coating has a high infrared emissivity of about 0.92 and a solar absorptivity of about 0.2, for a 5657 aluminum alloy, and a relatively thick anodic coating of about 1 mil.

Research on rechargeable oxygen electrodes.

NASA Technical Reports Server (NTRS)

Giner, J.; Holleck, G.; Malachesky, P. A.

1970-01-01

A research program is described which consisted of studying the effects of electrode cycling in very pure KOH solutions, with and without controlled additions of impurities, on oxide formation, oxygen evolution kinetics, oxygen reduction kinetics (including hydrogen peroxide formation), and changes in electrode structure. Bright platinum, platinized platinum, and Teflon-bonded platinum black electrodes were studied. Three main problem areas are identified: the buildup of a refractory anodic layer on prolonged cycling, which leads to a degradation of performance; the dissolution and subsequent deposition of dendritic platinum in the separator, leading to short-circuit ing and loss of electrocatalyst; and the disruptive effect of bubbling during gas evolution on charge. Each of these problem areas is analyzed, and remedial solutions are proposed.

Influence of Dy in solid solution on the degradation behavior of binary Mg-Dy alloys in cell culture medium.

PubMed

Yang, Lei; Ma, Liangong; Huang, Yuanding; Feyerabend, Frank; Blawert, Carsten; Höche, Daniel; Willumeit-Römer, Regine; Zhang, Erlin; Kainer, Karl Ulrich; Hort, Norbert

2017-06-01

Rare earth element Dy is one of the promising alloying elements for magnesium alloy as biodegradable implants. To understand the effect of Dy in solid solution on the degradation of Mg-Dy alloys in simulated physiological conditions, the present work studied the microstructure and degradation behavior of Mg-Dy alloys in cell culture medium. It is found the corrosion resistance enhances with the increase of Dy content in solid solution in Mg. This can be attributed to the formation of a relatively more corrosion resistant Dy-enriched film which decreases the anodic dissolution of Mg. Copyright © 2017 Elsevier B.V. All rights reserved.

Aluminothermic Reduction-Molten Salt Electrolysis Using Inert Anode for Oxygen and Al-Base Alloy Extraction from Lunar Soil Simulant

NASA Astrophysics Data System (ADS)

Xie, Kaiyu; Shi, Zhongning; Xu, Junli; Hu, Xianwei; Gao, Bingliang; Wang, Zhaowen

2017-10-01

Aluminothermic reduction-electrolysis using an inert anode process is proposed to extract oxygen and metals from Minnesota Lunar Simulant-1 (MLS-1). Effective aluminothermic reduction between dissolved MLS-1 and dissolved metal aluminum was achieved in cryolite salt media. The product phases obtained by aluminothermic reduction at 980°C for 4 h were Al, Si, and Al5FeSi, while the chemical components were 79.71 mass% aluminum, 12.03 mass% silicon, 5.91 mass% iron, and 2.35 mass% titanium. The cryolite salt containing Al2O3 was subsequently electrolyzed with Fe0.58-Ni0.42 inert anode at 960°C for 4 h. Oxygen was evolved at the anode with an anodic current efficiency of 78.28%. The results demonstrate that this two-step process is remarkably feasible for the extraterrestrial extraction of oxygen and metals. This process will help expand the existing in situ resource utilization methods.

Humectants to augment current from metallized zinc cathodic protection systems on concrete : final report.

DOT National Transportation Integrated Search

2002-12-01

Cathodic protection (CP) systems using thermal-sprayed zinc anodes are employed to mitigate the corrosion process in reinforced concrete structures. However, the performance of the anodes is improved by moisture at the anode-concrete interface. Resea...

A three-mask process for fabricating vacuum-sealed capacitive micromachined ultrasonic transducers using anodic bonding.

PubMed

Yamaner, F Yalçın; Zhang, Xiao; Oralkan, Ömer

2015-05-01

This paper introduces a simplified fabrication method for vacuum-sealed capacitive micromachined ultrasonic transducer (CMUT) arrays using anodic bonding. Anodic bonding provides the established advantages of wafer-bondingbased CMUT fabrication processes, including process simplicity, control over plate thickness and properties, high fill factor, and ability to implement large vibrating cells. In addition to these, compared with fusion bonding, anodic bonding can be performed at lower processing temperatures, i.e., 350°C as opposed to 1100°C; surface roughness requirement for anodic bonding is more than 10 times more relaxed, i.e., 5-nm rootmean- square (RMS) roughness as opposed to 0.5 nm for fusion bonding; anodic bonding can be performed on smaller contact area and hence improves the fill factor for CMUTs. Although anodic bonding has been previously used for CMUT fabrication, a CMUT with a vacuum cavity could not have been achieved, mainly because gas is trapped inside the cavities during anodic bonding. In the approach we present in this paper, the vacuum cavity is achieved by opening a channel in the plate structure to evacuate the trapped gas and subsequently sealing this channel by conformal silicon nitride deposition in the vacuum environment. The plate structure of the fabricated CMUT consists of the single-crystal silicon device layer of a silicon-on-insulator wafer and a thin silicon nitride insulation layer. The presented fabrication approach employs only three photolithographic steps and combines the advantages of anodic bonding with the advantages of a patterned metal bottom electrode on an insulating substrate, specifically low parasitic series resistance and low parasitic shunt capacitance. In this paper, the developed fabrication scheme is described in detail, including process recipes. The fabricated transducers are characterized using electrical input impedance measurements in air and hydrophone measurements in immersion. A representative design is used to demonstrate immersion operation in conventional, collapse-snapback, and collapse modes. In collapsemode operation, an output pressure of 1.67 MPa pp is shown at 7 MHz on the surface of the transducer for 60-Vpp, 3-cycle sinusoidal excitation at 30-V dc bias.

The use of ordered mixtures for improving the dissolution rate of low solubility compounds.

PubMed

Nyström, C; Westerberg, M

1986-03-01

The dissolution rate of micronized griseofulvin has been investigated, both for the agglomerated raw material and the material formulated as an ordered mixture, by means of the USP XX paddle method. During the experiments, which were performed at sink condition and constant temperature, the effects of adding a surfactant and of agitation were tested. The ordered mixture with sodium chloride gave a fast dissolution rate, practically independent of the test parameters. Micronized griseofulvin alone gave dissolution profiles that were improved by adding polysorbate 80 and by increased agitation, but the dissolution rates obtained were much lower than those for the ordered mixture. It was concluded that the rate limiting step in the dissolution of griseofulvin as the raw material is the penetration of the dissolution medium into the agglomerates. With an ordered mixture, these agglomerates were deaggregated during the mixing process, producing a system in which the entire external surface area of the primary particles was exposed to the dissolution medium. This conclusion was supported by calculation of the contact surface areas taking part in the dissolution process for the systems tested. The procedure developed in this study could be applied to preformulation work where a cohesive, low solubility drug of hydrophobic nature is to be formulated.

Surface characterization of anodized zirconium for biomedical applications

NASA Astrophysics Data System (ADS)

Sanchez, A. Gomez; Schreiner, W.; Duffó, G.; Ceré, S.

2011-05-01

Mechanical properties and corrosion resistance of zirconium make this material suitable for biomedical implants. Its good in vivo performance is mainly due to the presence of a protective oxide layer that minimizes corrosion rate, diminishes the amount of metallic ions released to the biological media and facilitates the osseointegration process. Since the implant surface is the region in contact with living tissues, the characteristics of the surface film are of great interest. Surface modification is a route to enhance both biocompatibility and corrosion resistance of permanent implant materials. Anodizing is presented as an interesting process to modify metal surfaces with good reproducibility and independence of the geometry. In this work the surface of zirconium before and after anodizing in 1 mol/L phosphoric acid solution at a fixed potential between 3 and 30 V, was characterized by means of several surface techniques. It was found that during anodization the surface oxide grows with an inhomogeneous coverage on zirconium surface, modifying the topography. The incorporation of P from the electrolyte to the surface oxide during the anodizing process changes the surface chemistry. After 30 days of immersion in Simulated Body Fluid (SBF) solution, Ca-P rich compounds were present on anodized zirconium.

Preparation and Characterization of Anode-Supported YSZ Thin Film Electrolyte by Co-Tape Casting and Co-Sintering Process

NASA Astrophysics Data System (ADS)

Liu, Q. L.; Fu, C. J.; Chan, S. H.; Pasciak, G.

2011-06-01

In this study, a co-tape casting and co-sintering process has been developed to prepare yttria-stabilized zirconia (YSZ) electrolyte films supported on Ni-YSZ anode substrates in order to substantially reduce the fabrication cost of solid oxide fuel cells (SOFC). Through proper control of the process, the anode/electrolyte bilayer structures with a size of 7.8cm × 7.8cm were achieved with good flatness. Scanning electron microscopy (SEM) observation indicated that the YSZ electrolyte film was about 16 μm in thickness, highly dense, crack free and well-bonded to the anode support. The electrochemical properties of the prepared anode-supported electrolyte film was evaluated in a button cell mode incorporating a (LaSr)MnO3-YSZ composite cathode. With humidified hydrogen as the fuel and stationary air as the oxidant, the cell demonstrated an open-circuit voltage of 1.081 V and a maximum power density of 1.01 W/cm2 at 800°C. The obtained results represent the important progress in the development of anode-supported intermediate temperature SOFC with reduced fabrication cost.

Preparation of olanzapine and methyl-β-cyclodextrin complexes using a single-step, organic solvent-free supercritical fluid process: An approach to enhance the solubility and dissolution properties.

PubMed

Rudrangi, Shashi Ravi Suman; Trivedi, Vivek; Mitchell, John C; Wicks, Stephen Richard; Alexander, Bruce David

2015-10-15

The purpose of this study was to evaluate a single-step, organic solvent-free supercritical fluid process for the preparation of olanzapine-methyl-β-cyclodextrin complexes with an express goal to enhance the dissolution properties of olanzapine. The complexes were prepared by supercritical carbon dioxide processing, co-evaporation, freeze drying and physical mixing. The prepared complexes were then analysed by differential scanning calorimetry, X-ray powder diffraction, scanning electron microscopy, solubility and dissolution studies. Computational molecular docking studies were performed to study the formation of molecular inclusion complexation of olanzapine with methyl-β-cyclodextrin. All the binary mixtures of olanzapine with methyl-β-cyclodextrin, except physical mixture, exhibited a faster and greater extent of drug dissolution than the drug alone. Products obtained by the supercritical carbon dioxide processing method exhibited the highest apparent drug dissolution. The characterisation by different analytical techniques suggests complete complexation or amorphisation of olanzapine and methyl-β-cyclodextrin complexes prepared by supercritical carbon dioxide processing method. Therefore, organic solvent-free supercritical carbon dioxide processing method proved to be novel and efficient for the preparation of solid inclusion complexes of olanzapine with methyl-β-cyclodextrin. The preliminary data also suggests that the complexes of olanzapine with methyl-β-cyclodextrin will lead to better therapeutic efficacy due to better solubility and dissolution properties. Copyright © 2015 Elsevier B.V. All rights reserved.

Growth and Filling Regularities of Filamentary Channels in Non-Metallic Inorganic Coatings Under Anodic Oxidation of Valve Metals. Mathematical Modeling

NASA Astrophysics Data System (ADS)

Mamaev, A. I.; Mamaeva, V. A.; Kolenchin, N. F.; Chubenko, A. K.; Kovalskaya, Ya. B.; Dolgova, Yu. N.; Beletskaya, E. Yu.

2015-12-01

Theoretical models are developed for growth and filling processes in filamentary channels of nanostructured non-metallic coatings produced by anodizing and microplasma oxidation. Graphical concentration distributions are obtained for channel-reacting anions, cations, and sparingly soluble reaction products depending on the time of electric current transmission and the length of the filamentary channel. Graphical distributions of the front moving velocity for the sparingly soluble compound are presented. The resulting model representation increases the understanding of the anodic process nature and can be used for a description and prediction of porous anodic film growth and filling. It is shown that the character of the filamentary channel growth and filling causes a variety of processes determining the textured metal - nonmetallic inorganic coating phase boundary formation.

A new, bright and hard aluminum surface produced by anodization

NASA Astrophysics Data System (ADS)

Hou, Fengyan; Hu, Bo; Tay, See Leng; Wang, Yuxin; Xiong, Chao; Gao, Wei

2017-07-01

Anodized aluminum (Al) and Al alloys have a wide range of applications. However, certain anodized finishings have relatively low hardness, dull appearance and/or poor corrosion resistance, which limited their applications. In this research, Al was first electropolished in a phosphoric acid-based solution, then anodized in a sulfuric acid-based solution under controlled processing parameters. The anodized specimen was then sealed by two-step sealing method. A systematic study including microstructure, surface morphology, hardness and corrosion resistance of these anodized films has been conducted. Results show that the hardness of this new anodized film was increased by a factor of 10 compared with the pure Al metal. Salt spray corrosion testing also demonstrated the greatly improved corrosion resistance. Unlike the traditional hard anodized Al which presents a dull-colored surface, this newly developed anodized Al alloy possesses a very bright and shiny surface with good hardness and corrosion resistance.

Thermal investigation of an electrical high-current arc with porous gas-cooled anode

NASA Technical Reports Server (NTRS)

Eckert, E. R. G.; Schoeck, P. A.; Winter, E. R. F.

1984-01-01

The following guantities were measured on a high-intensity electric arc with tungsten cathode and transpiration-cooled graphite anode burning in argon: electric current and voltage, cooling gas flow rate (argon), surface temperature of the anode and of the anode holder, and temperature profile in three cross-sections of the arc are column. The last mentioned values were obtained from spectroscopic photographs. From the measured quantities, the following values were calculated: the heat flux into the anode surface, the heat loss of the anode by radiation and conduction, and the heat which was regeneratively transported by the cooling gas back into the arc space. Heat balances for the anode were also obtained. The anode losses (which are approximately 80% of the total arc power for free burning arcs) were reduced by transpiration cooling to 20%. The physical processes of the energy transfer from the arc to the anode are discussed qualitatively.

Lanthanum doped strontium titanate - ceria anodes: deconvolution of impedance spectra and relationship with composition and microstructure

NASA Astrophysics Data System (ADS)

Burnat, Dariusz; Nasdaurk, Gunnar; Holzer, Lorenz; Kopecki, Michal; Heel, Andre

2018-05-01

Electrochemical performance of ceramic (Ni-free) SOFC anodes based on La0.2Sr0.7TiO3-δ (LST) and Gd0.1Ce0.9O1.95-δ (CGO) is thoroughly investigated. Microstructures and compositions are systematically varied around the percolation thresholds of both phases by modification of phase volume fractions, particle size distributions and firing temperature. Differential impedance spectroscopy was performed while varying gas composition, electrical potential and operating temperature, which allows determining four distinct electrode processes. Significant anode impedances are measured at low frequencies, which in contrast to the literature cannot be linked with gas concentration impedance. The dominant low frequency process (∼1 Hz) is attributed to the chemical capacitance. Combined EIS and microstructure investigations show that the chemical capacitance correlates inversely with the available surface area of CGO, indicating CGO surface reactions as the kinetic limitation for the dominant anode process and for the associated chemical capacitance. In anodes with a fine-grained microstructure this limitation is significantly smaller, which results in an impressive power output as high as 0.34 Wcm-2. The anodes show high redox stability by not only withstanding 30 isothermal redox cycles, but even improving the performance. Hence, compared to conventional Ni-cermet anodes the new LST-CGO material represents an interesting alternative with much improved redox-stability.

A new binder-free and conductive-additive-free TiO2/WO3-W integrative anode material produced by laser ablation

NASA Astrophysics Data System (ADS)

Su, Yibo; Zhang, Hongjun; Liang, Peng; Liu, Kai; Cai, Mingyong; Huang, Zeya; Wang, Chang-An; Zhong, Minlin

2018-02-01

Although transition metal oxides anodes have attracted lots of attention, there are still many problems to be resolved. Complicated fabrication process, high cost and poor electrochemical performances are the most important ones, together hindering transition metal oxides anodes for practical use. Herein, we provide a new approach to fabricate a binder-free and conductive-additive-free TiO2/WO3-W integrative anode material through the nanosecond laser ablation and dip-coating technology, which simplifies the entire anode preparation process with no need for a conventional tape-casting procedure. Using this method, great time cost, machine cost and labor cost related to mixing and tape-casting process can be saved on the basis of good electrochemical performances. The prepared TiO2/WO3-W integrative anode realizes a first Coulombic efficiency of 75.6% and attains to a stable capacity within the first five cycles. It can still maintain a capacity of 600 mAh g-1 in the range of 0.01-3 V vs. Li+/Li at a current rate of 0.2 C after 500 cycles. This work offers a new way to achieve a fast fabrication of the integrative anode for lithium ion battery, which is universal for other transition metals (such as Fe, Cu, Ni, Co, Mo, W etc.).

Fuzzy Multicriteria Ranking of Aluminium Coating Methods

NASA Astrophysics Data System (ADS)

Batzias, A. F.

2007-12-01

This work deals with multicriteria ranking of aluminium coating methods. The alternatives used are: sulfuric acid anodization, A1; oxalic acid anodization, A2; chromic acid anodization, A3; phosphoric acid anodization, A4; integral color anodizing, A5; chemical conversion coating, A6; electrostatic powder deposition, A7. The criteria used are: cost of production, f1; environmental friendliness of production process, f2; appearance (texture), f3; reflectivity, f4; response to coloring, f5; corrosion resistance, f6; abrasion resistance, f7; fatigue resistance, f8. Five experts coming from relevant industrial units set grades to the criteria vector and the preference matrix according to a properly modified Delphi method. Sensitivity analysis of the ranked first alternative A1 against the `second best', which was A3 at low and A7 at high resolution levels proved that the solution is robust. The dependence of anodized products quality on upstream processes is presented and the impact of energy price increase on industrial cost is discussed.

Determination of sulfuric acid concentration for anti-cavitation characteristics of Al alloy by two step anodizing process to forming nano porous.

PubMed

Lee, Seung-Jun; Kim, Seong-Kweon; Jeong, Jae-Yong; Kim, Seong-Jong

2014-12-01

Al alloy is a highly active metal but forms a protective oxide film having high corrosion resistance in atmosphere environment. However, the oxide film is not suitable for practical use, since the thickness of the film is not uniform and it is severly altered with formation conditions. This study focused on developing an aluminum anodizing layer having hardness, corrosion resistance and abrasion resistance equivalent to a commercial grade protective layer. Aluminum anodizing layer was produced by two-step aluminum anodizing oxide (AAO) process with different sulfuric acid concentrations, and the cavitation characteristics of the anodized coating layer was investigated. In hardness measurement, the anodized coating layer produced with 15 vol.% of sulfuric acid condition had the highest value of hardness but exhibited poor cavitation resistance due to being more brittle than those with other conditions. The 10 vol.% of sulfuric acid condition was thus considered to be the optimum condition as it had the lowest weight loss and damage depth.

Synthesis and characterization of hybrid micro/nano-structured NiTi surfaces by a combination of etching and anodizing

NASA Astrophysics Data System (ADS)

Huan, Z.; Fratila-Apachitei, L. E.; Apachitei, I.; Duszczyk, J.

2014-02-01

The purpose of this study was to generate hybrid micro/nano-structures on biomedical nickel-titanium alloy (NiTi). To achieve this, NiTi surfaces were firstly electrochemically etched and then anodized in fluoride-containing electrolyte. With the etching process, the NiTi surface was micro-roughened through the formation of micropits uniformly distributed over the entire surface. Following the subsequent anodizing process, self-organized nanotube structures enriched in TiO2 could be superimposed on the etched surface under specific conditions. Furthermore, the anodizing treatment significantly reduced water contact angles and increased the surface free energy compared to the surfaces prior to anodizing. The results of this study show for the first time that it is possible to create hybrid micro/nano-structures on biomedical NiTi alloys by combining electrochemical etching and anodizing under controlled conditions. These novel structures are expected to significantly enhance the surface biofunctionality of the material when compared to conventional implant devices with either micro- or nano-structured surfaces.

Synthesis and characterization of hybrid micro/nano-structured NiTi surfaces by a combination of etching and anodizing.

PubMed

Huan, Z; Fratila-Apachitei, L E; Apachitei, I; Duszczyk, J

2014-02-07

The purpose of this study was to generate hybrid micro/nano-structures on biomedical nickel-titanium alloy (NiTi). To achieve this, NiTi surfaces were firstly electrochemically etched and then anodized in fluoride-containing electrolyte. With the etching process, the NiTi surface was micro-roughened through the formation of micropits uniformly distributed over the entire surface. Following the subsequent anodizing process, self-organized nanotube structures enriched in TiO2 could be superimposed on the etched surface under specific conditions. Furthermore, the anodizing treatment significantly reduced water contact angles and increased the surface free energy compared to the surfaces prior to anodizing. The results of this study show for the first time that it is possible to create hybrid micro/nano-structures on biomedical NiTi alloys by combining electrochemical etching and anodizing under controlled conditions. These novel structures are expected to significantly enhance the surface biofunctionality of the material when compared to conventional implant devices with either micro- or nano-structured surfaces.

Controlling initial biodegradation of magnesium by a biocompatible strontium phosphate conversion coating.

PubMed

Chen, X B; Nisbet, D R; Li, R W; Smith, P N; Abbott, T B; Easton, M A; Zhang, D-H; Birbilis, N

2014-03-01

A simple strontium phosphate (SrP) conversion coating process was developed to protect magnesium (Mg) from the initial degradation post-implantation. The coating morphology, deposition rate and resultant phases are all dependent on the processing temperature, which determines the protective ability for Mg in minimum essential medium (MEM). Coatings produced at 80 °C are primarily made up of strontium apatite (SrAp) with a granular surface, a high degree of crystallinity and the highest protective ability, which arises from retarding anodic dissolution of Mg in MEM. Following 14 days' immersion in MEM, the SrAp coating maintained its integrity with only a small fraction of the surface corroded. The post-degradation effect of uncoated Mg and Mg coated at 40 and 80 °C on the proliferation and differentiation of human mesenchymal stem cells was also studied, revealing that the SrP coatings are biocompatible and permit proliferation to a level similar to that of pure Mg. The present study suggests that the SrP conversion coating is a promising option for controlling the early rapid degradation rate, and hence hydrogen gas evolution, of Mg implants without adverse effects on surrounding cells and tissues. Copyright © 2013 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

An empirical model for dissolution profile and its application to floating dosage forms.

PubMed

Weiss, Michael; Kriangkrai, Worawut; Sungthongjeen, Srisagul

2014-06-02

A sum of two inverse Gaussian functions is proposed as a highly flexible empirical model for fitting of in vitro dissolution profiles. The model was applied to quantitatively describe theophylline release from effervescent multi-layer coated floating tablets containing different amounts of the anti-tacking agents talc or glyceryl monostearate. Model parameters were estimated by nonlinear regression (mixed-effects modeling). The estimated parameters were used to determine the mean dissolution time, as well as to reconstruct the time course of release rate for each formulation, whereby the fractional release rate can serve as a diagnostic tool for classification of dissolution processes. The approach allows quantification of dissolution behavior and could provide additional insights into the underlying processes. Copyright © 2014 Elsevier B.V. All rights reserved.

Influence of anodization parameters on the volume expansion of anodic aluminum oxide formed in mixed solution of phosphoric and oxalic acids

NASA Astrophysics Data System (ADS)

Kao, Tzung-Ta; Chang, Yao-Chung

2014-01-01

The growth of anodic alumina oxide was conducted in the mixed solution of phosphoric and oxalic acids. The influence of anodizing voltage, electrolyte temperature, and concentration of phosphoric and oxalic acids on the volume expansion of anodic aluminum oxide has been investigated. Either anodizing parameter is chosen to its full extent of range that allows the anodization process to be conducted without electric breakdown and to explore the highest possible volume expansion factor. The volume expansion factors were found to vary between 1.25 and 1.9 depending on the anodizing parameters. The variation is explained in connection with electric field, ion transport number, temperature effect, concentration, and activity of acids. The formation of anodic porous alumina at anodizing voltage 160 V in 1.1 M phosphoric acid mixed with 0.14 M oxalic acid at 2 °C showed the peak volume expansion factor of 1.9 and the corresponding moderate growth rate of 168 nm/min.

Advanced electrolyte/additive for lithium-ion batteries with silicon anode

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhang, Shuo; He, Meinan; Su, Chi-Cheung

State-of-the-art lithium-ion batteries (LIBs) are based on a lithium transition metal oxide cathode, a graphite anode and a nonaqueous carbonate electrolyte. To further increase the energy and power density of LIBs, silicon anodes have been intensively explored due to their high theoretical capacity, low operation potential, and low cost. However, the main challenges for Si anode are the large volume change during lithiation/delithiation process and the instability of the solid-electrolyte-interphase associated with this process. Recently, significant progress has been achieved via advanced material fabrication technologies and rational electrolyte design in terms of improving the Coulombic efficiency and capacity retention. Inmore » this paper, new developments in advanced electrolyte and additive for LIBs with Si anode were systematically reviewed, and perspectives over future research were suggested.« less

Study of the highly ordered TiO2 nanotubes physical properties prepared with two-step anodization

NASA Astrophysics Data System (ADS)

Pishkar, Negin; Ghoranneviss, Mahmood; Ghorannevis, Zohreh; Akbari, Hossein

2018-06-01

Highly ordered hexagonal closely packed titanium dioxide nanotubes (TiO2 NTs) were successfully grown by a two-step anodization process. The TiO2 NTs were synthesized by electrochemical anodization of titanium foils in an ethylene glycol based electrolyte solution containing 0.3 wt% NH4F and 2 vol% deionized (DI) water at constant potential (50 V) for 1 h at room temperature. Physical properties of the TiO2 NTs, which were prepared via one and two-step anodization, were investigated. Atomic Force Microscopy (AFM) analysis revealed that anodization and subsequently peeled off the TiO2 NTs caused to the periodic pattern on the Ti surface. In order To study the nanotubes morphology, Field Emission Scanning Electron Microscopy (FESEM) was used, which was revealed that the two-step anodization resulted highly ordered hexagonal TiO2 NTs. Crystal structures of the TiO2 NTs were mainly anatase, determined by X-ray diffraction analysis. Optical studies were performed by Diffuse Reflection Spectra (DRS) and Photoluminescence (PL) analysis showed that the band gap of TiO2 NTs prepared via two-step anodization was lower than the band gap of samples prepared by one-step anodization process.

Automated Dissolution for Enteric-Coated Aspirin Tablets: A Case Study for Method Transfer to a RoboDis II.

PubMed

Ibrahim, Sarah A; Martini, Luigi

2014-08-01

Dissolution method transfer is a complicated yet common process in the pharmaceutical industry. With increased pharmaceutical product manufacturing and dissolution acceptance requirements, dissolution testing has become one of the most labor-intensive quality control testing methods. There is an increased trend for automation in dissolution testing, particularly for large pharmaceutical companies to reduce variability and increase personnel efficiency. There is no official guideline for dissolution testing method transfer from a manual, semi-automated, to automated dissolution tester. In this study, a manual multipoint dissolution testing procedure for an enteric-coated aspirin tablet was transferred effectively and reproducibly to a fully automated dissolution testing device, RoboDis II. Enteric-coated aspirin samples were used as a model formulation to assess the feasibility and accuracy of media pH change during continuous automated dissolution testing. Several RoboDis II parameters were evaluated to ensure the integrity and equivalency of dissolution method transfer from a manual dissolution tester. This current study provides a systematic outline for the transfer of the manual dissolution testing protocol to an automated dissolution tester. This study further supports that automated dissolution testers compliant with regulatory requirements and similar to manual dissolution testers facilitate method transfer. © 2014 Society for Laboratory Automation and Screening.

In-line ATR-UV and Raman Spectroscopy for Monitoring API Dissolution Process During Liquid-Filled Soft-Gelatin Capsule Manufacturing.

PubMed

Wan, Boyong; Zordan, Christopher A; Lu, Xujin; McGeorge, Gary

2016-10-01

Complete dissolution of the active pharmaceutical ingredient (API) is critical in the manufacturing of liquid-filled soft-gelatin capsules (SGC). Attenuated total reflectance UV spectroscopy (ATR-UV) and Raman spectroscopy have been investigated for in-line monitoring of API dissolution during manufacturing of an SGC product. Calibration models have been developed with both techniques for in-line determination of API potency. Performance of both techniques was evaluated and compared. The ATR-UV methodology was found to be able to monitor the dissolution process and determine the endpoint, but was sensitive to temperature variations. The Raman technique was also capable of effectively monitoring the process and was more robust to the temperature variation and process perturbations by using an excipient peak for internal correction. Different data preprocessing methodologies were explored in an attempt to improve method performance.

A novel microdialysis-dissolution/permeation system for testing oral dosage forms: A proof-of-concept study.

PubMed

Fong, Sophia Yui Kau; Poulsen, Jessie; Brandl, Martin; Bauer-Brandl, Annette

2017-01-01

A novel microdialysis-dissolution/permeation (M-D/P) system was developed for the biopharmaceutical assessment of oral drug formulations. This system consists of a side-by-side diffusion chamber, a microdialysis unit fixed within the dissolution chamber for continuous sampling, and a biomimetic Permeapad® as the intestinal barrier. In the M-D/P system, the concentration of the molecularly dissolved drug (with MWCO <20kDa) was measured over time in the dissolution compartment (representing the gastrointestinal tract) while the concentration of the permeated drug was measured in the acceptor compartment (representing the blood). The kinetics of both the dissolution process and the permeation process were simultaneously quantified under circumstances that mimic physiological conditions. For the current proof-of-concept study, hydrocortisone (HCS) in the form of slowly dissolving solvate crystals and buffer and the biorelevant fasted state simulated intestinal fluids (FaSSIF), were employed as the model drug and dissolution media, respectively. The applicability of the M-D/P system to dissolution and permeation profiling of HCS in buffer and in FaSSIF has been successfully demonstrated. Compared to the conventional direct sampling method (using filter of 0.1-0.45μm), sampling by the M-D/P system exhibited distinct advantages, including (1) showing minimal disturbance of the permeation process, (2) differentiating "molecularly" dissolved drugs from "apparently" dissolved drugs during dissolution of HCS in FaSSIF, and (3) being less laborious and having better sampling temporal resolution. M-D/P system appeared to be a promising, simple and routine tool that allows for the researchers' intensive comprehension of the interplay of dissolution and permeation thus helping for better oral formulation screening and as an ultimate goal, for better dosage forms assessment. Copyright © 2016. Published by Elsevier B.V.

Intensified nitrogen and phosphorus removal in a novel electrolysis-integrated tidal flow constructed wetland system.

PubMed

Ju, Xinxin; Wu, Shubiao; Zhang, Yansheng; Dong, Renjie

2014-08-01

A novel electrolysis-integrated tidal flow constructed wetland (CW) system was developed in this study. The dynamics of intensified nitrogen and phosphorus removal and that of hydrogen sulphide control were evaluated. Ammonium removal of up to 80% was achieved with an inflow concentration of 60 mg/L in wetland systems with and without electrolysis integration. Effluent nitrate concentration decreased from 2 mg/L to less than 0.5 mg/L with the decrease in current intensity from 1.5 mA/cm(2) to 0.57 mA/cm(2) in the electrolysis-integrated wetland system, thus indicating that the current intensity of electrolysis plays an important role in nitrogen transformations. Phosphorus removal was significantly enhanced, exceeding 95% in the electrolysis-integrated CW system because of the in-situ formation of a ferric iron coagulant through the electro-dissolution of a sacrificial iron anode. Moreover, the electrolyzed wetland system effectively inhibits sulphide accumulation as a result of a sulphide precipitation coupled with ferrous-iron electro-dissolution and/or an inhibition of bacterial sulphate reduction under increased aerobic conditions. Copyright © 2014 Elsevier Ltd. All rights reserved.

Secondary calcification and dissolution respond differently to future ocean conditions

NASA Astrophysics Data System (ADS)

Silbiger, N. J.; Donahue, M. J.

2015-01-01

Climate change threatens both the accretion and erosion processes that sustain coral reefs. Secondary calcification, bioerosion, and reef dissolution are integral to the structural complexity and long-term persistence of coral reefs, yet these processes have received less research attention than reef accretion by corals. In this study, we use climate scenarios from RCP 8.5 to examine the combined effects of rising ocean acidity and sea surface temperature (SST) on both secondary calcification and dissolution rates of a natural coral rubble community using a flow-through aquarium system. We found that secondary reef calcification and dissolution responded differently to the combined effect of pCO2 and temperature. Calcification had a non-linear response to the combined effect of pCO2 and temperature: the highest calcification rate occurred slightly above ambient conditions and the lowest calcification rate was in the highest temperature-pCO2 condition. In contrast, dissolution increased linearly with temperature-pCO2 . The rubble community switched from net calcification to net dissolution at +271 μatm pCO2 and 0.75 °C above ambient conditions, suggesting that rubble reefs may shift from net calcification to net dissolution before the end of the century. Our results indicate that (i) dissolution may be more sensitive to climate change than calcification and (ii) that calcification and dissolution have different functional responses to climate stressors; this highlights the need to study the effects of climate stressors on both calcification and dissolution to predict future changes in coral reefs.

Secondary calcification and dissolution respond differently to future ocean conditions

NASA Astrophysics Data System (ADS)

Silbiger, N. J.; Donahue, M. J.

2014-09-01

Climate change threatens both the accretion and erosion processes that sustain coral reefs. Secondary calcification, bioerosion, and reef dissolution are integral to the structural complexity and long-term persistence of coral reefs, yet these processes have received less research attention than reef accretion by corals. In this study, we use climate scenarios from RCP8.5 to examine the combined effects of rising ocean acidity and SST on both secondary calcification and dissolution rates of a natural coral rubble community using a flow-through aquarium system. We found that secondary reef calcification and dissolution responded differently to the combined effect of pCO2 and temperature. Calcification had a non-linear response to the combined effect of pCO2-temperature: the highest calcification rate occurred slightly above ambient conditions and the lowest calcification rate was in the highest pCO2-temperature condition. In contrast, dissolution increased linearly with pCO2-temperature. The rubble community switched from net calcification to net dissolution at +272 μatm pCO2 and 0.84 °C above ambient conditions, suggesting that rubble reefs may shift from net calcification to net dissolution before the end of the century. Our results indicate that dissolution may be more sensitive to climate change than calcification, and that calcification and dissolution have different functional responses to climate stressors, highlighting the need to study the effects of climate stressors on both calcification and dissolution to predict future changes in coral reefs.

Performance of (in)active anodic materials for the electrooxidation of phenolic wastewaters from cashew-nut processing industry.

PubMed

Oliveira, Edna M S; Silva, Francisco R; Morais, Crislânia C O; Oliveira, Thiago Mielle B F; Martínez-Huitle, Carlos A; Motheo, Artur J; Albuquerque, Cynthia C; Castro, Suely S L

2018-06-01

This study investigated the anodic oxidation of phenolic wastewater generated by cashew-nut processing industry (CNPI) using active (Ti/RuO 2 -TiO 2 ) and inactive (boron doped diamond, BDD) anodes. During electrochemical treatment, various operating parameters were investigated, such as current density, chemical oxygen demand (COD), total phenols, O 2 production, temperature, pH, as well as current efficiency and energy consumption. After electrolysis under optimized working conditions, samples were evaluated by chromatography and toxicological tests against L. sativa. When both electrode materials were compared under the same operating conditions, higher COD removal efficiency was achieved for BDD anode; achieving lower energy requirements when compared with the values estimated for Ti/RuO 2 -TiO 2 . The presence of Cl - in the wastewater promoted the electrogeneration of strong oxidant species as chlorine, hypochlorite and mainly hypochlorous acid, increasing the efficiency of degradation process. Regarding the temperature effect, BDD showed slower performances than those achieved for Ti/RuO 2 -TiO 2 . Chromatographic and phytotoxicity studies indicated formation of some by-products after electrolytic process, regardless of the anode evaluated, and phytotoxic action of the effluent. Results encourage the applicability of the electrochemical method as wastewater treatment process for the CNPI, reducing depuration time. Copyright © 2018. Published by Elsevier Ltd.

The charge-discharge characteristics and diffusion mechanism of Ti-Si-Al thin film anode using an electrically induced crystallization process

NASA Astrophysics Data System (ADS)

Chen, Yen-Ting; Hung, Fei-Yi; Lui, Truan-Sheng

2018-04-01

In this study, an Al-Si-Ti multilayer thin film structure is designed as the anode of a lithium ion battery. The novel structure restricts the expansion of Si during charge-discharge, and its battery capacity can reach 1112 mA h g-1 after a 100-cycle charge-charging test under a 0.2 C charge-discharge rate without annealing. Notably, after a 200 °C vacuum annealing process, the cyclic capacity of the anode rises to 1208 mA h g-1 through crystallization of the Al and Ti buffer layer. However, its thermal diffusion behavior in the Al/Si or Ti/Si interfaces seriously reduces the performance and restricts the expansion of Si. The electrically induced crystallization (EIC) process not only performs crystallization but also controls the interfacial stability, after which its capacity can obviously improve to 1602 mA h g-1 after 100 cycles. Using EIC, the electron flow drives the Cu and Al atoms to endow the Si matrix with doping properties and further increases the electron conductivity of the anode. This result demonstrates that the EIC process is a suitable post-treatment process for multilayer anodes and provides a reference for future battery designs.

The application of the barrier-type anodic oxidation method to thickness testing of aluminum films

NASA Astrophysics Data System (ADS)

Chen, Jianwen; Yao, Manwen; Xiao, Ruihua; Yang, Pengfei; Hu, Baofu; Yao, Xi

2014-09-01

The thickness of the active metal oxide film formed from a barrier-type anodizing process is directly proportional to its formation voltage. The thickness of the consumed portion of the metal film is also corresponding to the formation voltage. This principle can be applied to the thickness test of the metal films. If the metal film is growing on a dielectric substrate, when the metal film is exhausted in an anodizing process, because of the high electrical resistance of the formed oxide film, a sudden increase of the recorded voltage during the anodizing process would occur. Then, the thickness of the metal film can be determined from this voltage. As an example, aluminum films are tested and discussed in this work. This method is quite simple and is easy to perform with high precision.

Extended self-ordering regime in hard anodization and its application to make asymmetric AAO membranes for large pitch-distance nanostructures.

PubMed

Kim, Minwoo; Ha, Yoon-Cheol; Nguyen, Truong Nhat; Choi, Hae Young; Kim, Doohun

2013-12-20

We report here a fast and reliable hard anodization process to make asymmetric anodic aluminum oxide (AAO) membranes which can serve as a template for large pitch-distance nanostructures. In order to make larger pitch distances possible, the common burning failure associated with the high current density during the conventional constant voltage hard anodization, especially at a voltage higher than a known limit, i.e., 155 V for oxalic acid, was effectively suppressed by using a burning-protective agent. A new self-ordering regime beyond the voltage limit was observed with a different voltage-interpore distance relationship of 2.2 nm V(-1) compared to the reported 2.0 nm V(-1) for hard anodization. Combining a sulfuric acid mild anodization with this new regime of hard anodization, we further demonstrate a scalable process to make an asymmetric membrane with size up to ~47 mm in diameter and ~60 μm in thickness. This free-standing membrane can be used as a template for novel nanopatterned structures such as arrays of quantum dots, nanowires or nanotubes with diameters of a few tens of nanometers and pitch distance of over 400 nm.

Extended self-ordering regime in hard anodization and its application to make asymmetric AAO membranes for large pitch-distance nanostructures

NASA Astrophysics Data System (ADS)

Kim, Minwoo; Ha, Yoon-Cheol; Nhat Nguyen, Truong; Choi, Hae Young; Kim, Doohun

2013-12-01

We report here a fast and reliable hard anodization process to make asymmetric anodic aluminum oxide (AAO) membranes which can serve as a template for large pitch-distance nanostructures. In order to make larger pitch distances possible, the common burning failure associated with the high current density during the conventional constant voltage hard anodization, especially at a voltage higher than a known limit, i.e., 155 V for oxalic acid, was effectively suppressed by using a burning-protective agent. A new self-ordering regime beyond the voltage limit was observed with a different voltage-interpore distance relationship of 2.2 nm V-1 compared to the reported 2.0 nm V-1 for hard anodization. Combining a sulfuric acid mild anodization with this new regime of hard anodization, we further demonstrate a scalable process to make an asymmetric membrane with size up to ˜47 mm in diameter and ˜60 μm in thickness. This free-standing membrane can be used as a template for novel nanopatterned structures such as arrays of quantum dots, nanowires or nanotubes with diameters of a few tens of nanometers and pitch distance of over 400 nm.

Anodized Steel Electrodes for Supercapacitors.

PubMed

Sagu, Jagdeep S; Wijayantha, K G Upul; Bohm, Mallika; Bohm, Siva; Kumar Rout, Tapan

2016-03-09

Steel was anodized in 10 M NaOH to enhance its surface texture and internal surface area for application as an electrode in supercapacitors. A mechanism was proposed for the anodization process. Field-emission gun scanning electron microscopy (FEGSEM) studies of anodized steel revealed that it contains a highly porous sponge like structure ideal for supercapacitor electrodes. X-ray photoelectron spectroscopy (XPS) measurements showed that the surface of the anodized steel was Fe2O3, whereas X-ray diffraction (XRD) measurements indicated that the bulk remained as metallic Fe. The supercapacitor performance of the anodized steel was tested in 1 M NaOH and a capacitance of 18 mF cm(-2) was obtained. Cyclic voltammetry measurements showed that there was a large psueudocapacitive contribution which was due to oxidation of Fe to Fe(OH)2 and then further oxidation to FeOOH, and the respective reduction of these species back to metallic Fe. These redox processes were found to be remarkably reversible as the electrode showed no loss in capacitance after 10000 cycles. The results demonstrate that anodization of steel is a suitable method to produce high-surface-area electrodes for supercapacitors with excellent cycling lifetime.

20 CFR 295.6 - Disclosure of information.

Code of Federal Regulations, 2010 CFR

2010-04-01

... suit for divorce, dissolution, annulment or legal separation, or otherwise subjected to the... documents, and like state process issued in connection with a suit for divorce, dissolution, annulment or... divorce, dissolution, annulment or legal separation may be made by the General Counsel or his or her...

20 CFR 295.6 - Disclosure of information.

Code of Federal Regulations, 2011 CFR

2011-04-01

... suit for divorce, dissolution, annulment or legal separation, or otherwise subjected to the... documents, and like state process issued in connection with a suit for divorce, dissolution, annulment or... divorce, dissolution, annulment or legal separation may be made by the General Counsel or his or her...

20 CFR 295.6 - Disclosure of information.

Code of Federal Regulations, 2012 CFR

2012-04-01

... suit for divorce, dissolution, annulment or legal separation, or otherwise subjected to the... documents, and like state process issued in connection with a suit for divorce, dissolution, annulment or... divorce, dissolution, annulment or legal separation may be made by the General Counsel or his or her...

Dissolution of Fe(III) (hydr) oxides by metal-EDTA complexes

NASA Astrophysics Data System (ADS)

Ngwack, Bernd; Sigg, Laura

1997-03-01

The dissolution of Fe(III)(hydr)oxides (goethite and hydrous ferric oxide) by metal-EDTA complexes occurs by ligand-promoted dissolution. The process is initiated by the adsorption of metal-EDTA complexes to the surface and is followed by the dissociation of the complex at the surface and the release of Fe(III)EDTA into solution. The dissolution rate is decreased to a great extent if EDTA is complexed by metals in comparison to the uncomplexed EDTA. The rate decreases in the order EDTA CaEDTA ≫ PbEDTA > ZnEDTA > CuEDTA > Co(II)EDTA > NiEDTA. Two different rate-limiting steps determine the dissolution process: (1) detachment of Fe(III) from the oxide-structure and (2) dissociation of the metal-EDTA complexes. In the case of goethite, step 1 is slower than step 2 and the dissolution rates by various metals are similar. In the case of hydrous ferric oxide, step 2 is rate-limiting and the effect of the complexed metal is very pronounced.

Role of Solvents in Improvement of Dissolution Rate of Drugs: Crystal Habit and Crystal Agglomeration

PubMed Central

Maghsoodi, Maryam

2015-01-01

Crystallization is often used for manufacturing drug substances. Advances of crystallization have achieved control over drug identity and purity, but control over the physical form remains poor. This review discusses the influence of solvents used in crystallization process on crystal habit and agglomeration of crystals with potential implication for dissolution. According to literature it has been known that habit modification of crystals by use of proper solvents may enhance the dissolution properties by changing the size, number and the nature of crystal faces exposed to the dissolution medium. Also, the faster dissolution rate of drug from the agglomerates of crystals compared with the single crystals may be related to porous structure of the agglomerates and consequently their better wettability. It is concluded from this review that in-depth understanding of role of the solvents in crystallization process can be applied to engineering of crystal habit or crystal agglomeration, and predictably dissolution improvement in poorly soluble drugs. PMID:25789214

Influence of oxalic acid on the dissolution kinetics of manganese oxide

NASA Astrophysics Data System (ADS)

Godunov, E. B.; Artamonova, I. V.; Gorichev, I. G.; Lainer, Yu. A.

2012-11-01

The kinetics and electrochemical processes of the dissolution of manganese oxides with various oxidation states in sulfuric acid solutions containing oxalate ion additives is studied under variable conditions (concentration, pH, temperature). The parameters favoring a higher degree of the dissolution of manganese oxides in acidic media are determined. The optimal conditions are found for the dissolution of manganese oxides in acidic media in the presence of oxalate ions. The mechanism proposed for the dissolution of manganese oxides in sulfuric acid solutions containing oxalic acid is based on the results of kinetic and electrochemical studies. The steps of the dissolution mechanism are discussed.

Investigation of the interactions of enteric and hydrophilic polymers to enhance dissolution of griseofulvin following hot melt extrusion processing.

PubMed

Bennett, Ryan C; Keen, Justin M; Bi, Yunxia Vivian; Porter, Stuart; Dürig, Thomas; McGinity, James W

2015-07-01

This study focuses on the application of hot melt extrusion (HME) to produce solid dispersions containing griseofulvin (GF) and investigates the in-vitro dissolution performance of HME powders and resulting tablet compositions containing HME-processed dispersions. Binary, ternary and quaternary dispersions containing GF, enteric polymer (Eudragit L100-55 or AQOAT-LF) and/or vinyl pyrrolidone-based polymer (Plasdone K-12 povidone or S-630 copovidone) were processed by HME. Two plasticizers, triethyl citrate (TEC) and acetyl tributyl citrate (ATBC), were incorporated to aid in melt processing and to modify release of GF in neutral media following a pH-change in dissolution. Products were characterized for GF recovery, degrees of compositional amorphous character, intermolecular interactions and non-sink dissolution performance. Binary dispersions exhibited lower maximum observed concentration values and magnitudes of supersaturated GF in neutral media dissolution in comparison with the ternary dispersions. The quaternary HME products, 1 : 2 : 1 : 0.6 GF : L100-55 : S-630 : ATBC and GF : AQOAT-LF : K-12 : ATBC, were determined as the most optimal concentration-enhancing compositions due to increased hydrogen bonding of enteric functional groups with carbonyl/acetate groups of vinyl pyrrolidone-based polymers, reduced compositional crystallinity and presence of incorporated hydrophobic plasticizer. HME products containing combinations of concentration-enhancing polymers can supersaturate and sustain GF dissolution to greater magnitudes in neutral media following the pH-transition and be compressed into immediate-release tablets exhibiting similar dissolution profiles. © 2015 Royal Pharmaceutical Society.

Model of dissolution in the framework of tissue engineering and drug delivery.

PubMed

Sanz-Herrera, J A; Soria, L; Reina-Romo, E; Torres, Y; Boccaccini, A R

2018-05-22

Dissolution phenomena are ubiquitously present in biomaterials in many different fields. Despite the advantages of simulation-based design of biomaterials in medical applications, additional efforts are needed to derive reliable models which describe the process of dissolution. A phenomenologically based model, available for simulation of dissolution in biomaterials, is introduced in this paper. The model turns into a set of reaction-diffusion equations implemented in a finite element numerical framework. First, a parametric analysis is conducted in order to explore the role of model parameters on the overall dissolution process. Then, the model is calibrated and validated versus a straightforward but rigorous experimental setup. Results show that the mathematical model macroscopically reproduces the main physicochemical phenomena that take place in the tests, corroborating its usefulness for design of biomaterials in the tissue engineering and drug delivery research areas.

Anode film formation and control

DOEpatents

Koski, Oscar; Marschman, Steven C.

1990-01-01

A protective film is created about the anode within a cryolite-based electrolyte during electrolytic production of aluminum from alumina. The film function to minimize corrosion of the anode by the cryolitic electrolyte and thereby extend the life of the anode. Various operating parameters of the electrolytic process are controlled to maintain the protective film about the anode in a protective state throughout the electrolytic reduction of alumina. Such parameters include electrolyte temperature, electrolyte ratio, current density, and Al.sub.2 O.sub.3 concentration. An apparatus is also disclosed to enable identification of the onset of anode corrosion due to disruption of the film to provide real time information regarding the state of the film.

Spontaneous oscillations of cell voltage, power density, and anode exit CO concentration in a PEM fuel cell.

PubMed

Lu, Hui; Rihko-Struckmann, Liisa; Sundmacher, Kai

2011-10-28

The spontaneous oscillations of the cell voltage and output power density of a PEMFC (with PtRu/C anode) using CO-containing H(2) streams as anodic fuels have been observed during galvanostatic operating. It is ascribed to the dynamic coupling of the CO adsorption (poisoning) and the electrochemical CO oxidation (reactivating) processes in the anode chamber of the single PEMFC. Accompanying the cell voltage and power density oscillations, the discrete CO concentration oscillations at the anode outlet of the PEMFC were also detected, which directly confirms the electrochemical CO oxidation taking place in the anode chamber during galvanostatic operating. This journal is © the Owner Societies 2011

Anode film formation and control

DOEpatents

Koski, O.; Marschman, S.C.

1990-05-01

A protective film is created about the anode within a cryolite-based electrolyte during electrolytic production of aluminum from alumina. The film functions to minimize corrosion of the anode by the cryolitic electrolyte and thereby extend the life of the anode. Various operating parameters of the electrolytic process are controlled to maintain the protective film about the anode in a protective state throughout the electrolytic reduction of alumina. Such parameters include electrolyte temperature, electrolyte ratio, current density, and Al[sub 2]O[sub 3] concentration. An apparatus is also disclosed to enable identification of the onset of anode corrosion due to disruption of the film to provide real time information regarding the state of the film. 3 figs.

U.sup.+4 generation in HTER

DOEpatents

Miller, William E [Naperville, IL; Gay, Eddie C [Park Forest, IL; Tomczuk, Zygmunt [Homer Glen, IL

2006-03-14

A improved device and process for recycling spent nuclear fuels, in particular uranium metal, that facilitates the refinement and recovery of uranium metal from spent metallic nuclear fuels. The electrorefiner device comprises two anodes in predetermined spatial relation to a cathode. The anodese have separate current and voltage controls. A much higher voltage than normal for the electrorefining process is applied to the second anode, thereby facilitating oxidization of uranium (III), U.sup.+, to uranium (IV), U.sup.+4. The current path from the second anode to the cathode is physically shorter than the similar current path from the second anode to the spent nuclear fuel contained in a first anode shaped as a basket. The resulting U.sup.+4 oxidizes and solubilizes rough uranium deposited on the surface of the cathode. A softer uranium metal surface is left on the cathode and is more readily removed by a scraper.

Electrochemical Performance Estimation of Anodized AZ31B Magnesium Alloy as Function of Change in the Current Density

NASA Astrophysics Data System (ADS)

Girón, L.; Aperador, W.; Tirado, L.; Franco, F.; Caicedo, J. C.

2017-08-01

The anodized AZ31B magnesium alloys were synthesized via electrodeposition processes. The aim of this work was to determine the electrochemical behavior of magnesium alloys by using anodized alloys as a protective coating. The anodized alloys were characterized by x-ray diffraction, exhibiting the crystallography orientation for Mg and MgO phases. The x-ray photoelectron spectroscopy was used to determine the chemical composition of anodized magnesium alloys. By using electrochemical impedance spectroscopy and Tafel curves, it was possible to estimate the electrochemical behavior of anodized AZ31B magnesium alloys in Hank's balanced salt solution (HBSS). Scanning electron microscopy was performed to analyze chemical changes and morphological surface changes on anodized Mg alloys due to the reaction in HBSS/anodized magnesium surface interface. Electrochemical behavior in HBSS indicates that the coatings may be a promising material for biomedical industry.

Fabrication of free standing anodic titanium oxide membranes with clean surface using recycling process.

PubMed

Meng, Xianhui; Lee, Tae-Young; Chen, Huiyu; Shin, Dong-Wook; Kwon, Kee-Won; Kwon, Sang Jik; Yoo, Ji-Beom

2010-07-01

Large area of self-organized, free standing anodic titanium oxide (ATO) nanotube membranes with clean surfaces were facilely prepared to desired lengths via electrochemical anodization of highly pure Ti sheets in an ethylene glycol electrolyte, with a small amount of NH4F and H2O at 50 V, followed by self-detachment of the ATO membrane from the Ti substrate using recycling processes. In the first anodization step, the nanowire oxide layer existed over the well-arranged ATO nanotube. After sufficiently rinsing with water, the whole ATO layer was removed from the Ti sheet by high pressure N2 gas, and a well-patterned dimple layer with a thickness of about 30 nm existed on the Ti substrate. By using these naturally formed nano-scale pits as templates, in the second and third anodization process, highly ordered, vertically aligned, and free standing ATO membranes with the anodic aluminum oxide (AAO)-like clean surface were obtained. The inter-pore distance and diameter was 154 +/- 2 nm and 91+/- 2 nm, the tube arrays lengths for 25 and 46 hours were 44 and 70 microm, respectively. The present study demonstrates a simple approach to producing high quality, length controllable, large area TiO2 membrane.

Influence of process parameters on plasma electrolytic surface treatment of tantalum for biomedical applications

NASA Astrophysics Data System (ADS)

Sowa, Maciej; Woszczak, Maja; Kazek-Kęsik, Alicja; Dercz, Grzegorz; Korotin, Danila M.; Zhidkov, Ivan S.; Kurmaev, Ernst Z.; Cholakh, Seif O.; Basiaga, Marcin; Simka, Wojciech

2017-06-01

This work aims to quantify the effect of anodization voltage and electrolyte composition used during DC plasma electrolytic oxidation (PEO), operated as a 2-step process, on the surface properties of the resulting oxide coatings on tantalum. The first step consisted of galvanostatic anodization (150 mA cm-2) of the tantalum workpiece up to several limiting voltages (200, 300, 400 and 500 V). After attaining the limiting voltage, the process was switched to voltage control, which resulted in a gradual decrease of the anodic current density. The anodic treatment was realized in a 0.5 M Ca(H2PO2)2 solution, which was then modified by the addition of 1.15 M Ca(HCOO)2 as well as 1.15 M and 1.5 M Mg(CH3COO)2. The increasing voltage of anodization led to the formation of thicker coatings, with larger pores and enriched with electrolytes species to a higher extent. The solutions containing HCOO- and CH3COO- ions caused the formation of coatings which were slightly hydrophobic (high contact angle). In the case of the samples anodized up to 500 V, scattered crystalline deposits were observed. Bioactive phases, such as hydroxyapatite, were detected in the treated oxide coatings by XRD and XPS.

Offset Initial Sodium Loss To Improve Coulombic Efficiency and Stability of Sodium Dual-Ion Batteries.

PubMed

Ma, Ruifang; Fan, Ling; Chen, Suhua; Wei, Zengxi; Yang, Yuhua; Yang, Hongguan; Qin, Yong; Lu, Bingan

2018-05-09

Sodium dual-ion batteries (NDIBs) are attracting extensive attention recently because of their low cost and abundant sodium resources. However, the low capacity of the carbonaceous anode would reduce the energy density, and the formation of the solid-electrolyte interphase (SEI) in the anode during the initial cycles will lead to large amount consumption of Na + in the electrolyte, which results in low Coulombic efficiency and inferior stability of the NDIBs. To address these issues, a phosphorus-doped soft carbon (P-SC) anode combined with a presodiation process is developed to enhance the performance of the NDIBs. The phosphorus atom doping could enhance the electric conductivity and further improve the sodium storage property. On the other hand, an SEI could preform in the anode during the presodiation process; thus the anode has no need to consume large amounts of Na + to form the SEI during the cycling of the NDIBs. Consequently, the NDIBs with P-SC anode after the presodiation process exhibit high Coulombic efficiency (over 90%) and long cycle stability (81 mA h g -1 at 1000 mA g -1 after 900 cycles with capacity retention of 81.8%), far more superior to the unsodiated NDIBs. This work may provide guidance for developing high performance NDIBs in the future.

Use of glancing angle X-ray powder diffractometry to depth-profile phase transformations during dissolution of indomethacin and theophylline tablets.

PubMed

Debnath, Smita; Predecki, Paul; Suryanarayanan, Raj

2004-01-01

The purpose of this study was (i) to develop glancing angle x-ray powder diffractometry (XRD) as a method for profiling phase transformations as a function of tablet depth; and (ii) to apply this technique to (a) study indomethacin crystallization during dissolution of partially amorphous indomethacin tablets and to (b) profile anhydrate --> hydrate transformations during dissolution of theophylline tablets. The intrinsic dissolution rates of indomethacin and theophylline were determined after different pharmaceutical processing steps. Phase transformations during dissolution were evaluated by various techniques. Transformation in the bulk and on the tablet surface was characterized by conventional XRD and scanning electron microscopy, respectively. Glancing angle XRD enabled us to profile these transformations as a function of depth from the tablet surface. Pharmaceutical processing resulted in a decrease in crystallinity of both indomethacin and theophylline. When placed in contact with the dissolution medium, while indomethacin recrystallized, theophylline anhydrate rapidly converted to theophylline monohydrate. Due to intimate contact with the dissolution medium, drug transformation occurred to a greater extent at or near the tablet surface. Glancing angle XRD enabled us to depth profile the extent of phase transformations as a function of the distance from the tablet surface. The processed sample (both indomethacin and theophylline) transformed more rapidly than did the corresponding unprocessed drug. Several challenges associated with the glancing angle technique, that is, the effects of sorbed water, phase transformations during the experimental timescale, and the influence of phase transformation on penetration depth, were addressed. Increased solubility, and consequently dissolution rate, is one of the potential advantages of metastable phases. This advantage is negated if, during dissolution, the metastable to stable transformation rate > dissolution rate. Glancing angle XRD enabled us to quantify and thereby profile phase transformations as a function of compact depth. The technique has potential utility in monitoring surface reactions, both chemical decomposition and physical transformations, in pharmaceutical systems.

Structural and characteristic variation of anodic oxide on pure Ti with anodization duration

NASA Astrophysics Data System (ADS)

Mizukoshi, Yoshiteru; Ohtsu, Naofhumi; Masahashi, Naoya

2013-10-01

Change in the structural and characteristic of the anodic oxide on pure Ti with the duration of anodization time was investigated. With the progress of the anodization, the phase of the formed TiO2 successively changed from anatase phase to rutile phase. In the transition process, peak intensities of rutile TiO2 1 0 1, 1 1 1 and 2 1 1 planes of X-ray diffraction characteristically increased. The contact angles of water droplets on the anodize TiO2 were monotonously decreased with the progress of the anodization except on the characteristically oriented rutile surface. In the evaluations of acetaldehyde photocatalysis under UV illumination, the anatase TiO2 anodized for short period exhibited high activities. On the other hand, when illuminated with visible light (>422 nm), rutile-structured TiO2 formed by anodization with a long duration exhibited superior photocatalytic activities probably due to high rutile fraction and sulfur incorporation from the electrolyte.

Microbial fuel cell treatment of fuel process wastewater

DOEpatents

Borole, Abhijeet P; Tsouris, Constantino

2013-12-03

The present invention is directed to a method for cleansing fuel processing effluent containing carbonaceous compounds and inorganic salts, the method comprising contacting the fuel processing effluent with an anode of a microbial fuel ell, the anode containing microbes thereon which oxidatively degrade one or more of the carbonaceous compounds while producing electrical energy from the oxidative degradation, and directing the produced electrical energy to drive an electrosorption mechanism that operates to reduce the concentration of one or more inorganic salts in the fuel processing effluent, wherein the anode is in electrical communication with a cathode of the microbial fuel cell. The invention is also directed to an apparatus for practicing the method.

Thermal dissolution of maize starches in aqueous medium

USDA-ARS?s Scientific Manuscript database

Starches are not soluble in neutral water at room temperature. However, if they are heated in a closed container beyond the boiling point of water, they eventually dissolve. The dissolution temperature depends on the type of starch. The dissolution process was monitored in real time by measuring ...

In situ monitoring of corrosion mechanisms and phosphate inhibitor surface deposition during corrosion of zinc-magnesium-aluminium (ZMA) alloys using novel time-lapse microscopy.

PubMed

Sullivan, James; Cooze, Nathan; Gallagher, Callum; Lewis, Tom; Prosek, Tomas; Thierry, Dominique

2015-01-01

In situ time-lapse optical microscopy was used to examine the microstructural corrosion mechanisms in three zinc-magnesium-aluminium (ZMA) alloy coated steels immersed in 1% NaCl pH 7. Preferential corrosion of MgZn(2) lamellae within the eutectic phases was observed in all the ZMA alloys followed by subsequent dissolution of Zn rich phases. The total extent and rate of corrosion, measured using time-lapse image analysis and scanning vibrating electrode technique (SVET) estimated mass loss, decreased as Mg and Al alloying additions were increased up to a level of 3 wt% Mg and 3.7 wt% Al. This was probably due to the increased presence of MgO and Al(2)O(3) at the alloy surface retarding the kinetics of cathodic oxygen reduction. The addition of 1 × 10(-2) mol dm(-3) Na(3)PO(4) to 1% NaCl pH 7 had a dramatic influence on the corrosion mechanism for a ZMA with passivation of anodic sites through phosphate precipitation observed using time-lapse image analysis. Intriguing rapid precipitation of filamentous phosphate was also observed and it is postulated that these filaments nucleate and grow due to super saturation effects. Polarisation experiments showed that the addition of 1 × 10(-2) mol dm(-3) Na(3)PO(4) to the 1% NaCl electrolyte promoted an anodic shift of 50 mV in open circuit potential for the ZMA alloy with a reduction in anodic current of 2.5 orders of magnitude suggesting that it was acting primarily as an anodic inhibitor supporting the inferences from the time-lapse investigations. These phosphate additions resulted in a 98% reduction in estimated mass loss as measured by SVET demonstrating the effectiveness of phosphate inhibitors for this alloy system.

The Weinstein conjecture with multiplicities on spherizations

NASA Astrophysics Data System (ADS)

Hertzberg, Benjamin J.

2011-07-01

Si-based anodes have recently received considerable attention for use in Li-ion batteries, due to their extremely high specific capacity---an order of magnitude beyond that offered by conventional graphite anode materials. However, during the lithiation process, Si-based anodes undergo extreme increases in volume, potentially by more than 300 %. The stresses produced within the electrode by these volume changes can damage the electrode binder, the active Si particles and the solid electrolyte interphase (SEI), causing the electrode to rapidly fail and lose capacity. These problems can be overcome by producing new anode materials incorporating both Si and C, which may offer a favorable combination of the best properties of both materials, and which can be designed with internal porosity, thereby buffering the high strains produced during battery charge and discharge with minimal overall volume changes. However, in order to develop useful anode materials, we must gain a thorough understanding of the structural, microstructural and chemical changes occurring within the electrode during the lithiation and delithiation process, and we must develop new processes for synthesizing composite anode particles which can survive the extreme strains produced during lithium intercalation of Si and exhibit no volume changes in spite of the volume changes in Si. In this work we have developed several novel synthesis processes for producing internally porous Si-C nanocomposite anode materials for Li-ion batteries. These nanocomposites possess excellent specific capacity, Coulombic efficiency, cycle lifetime, and rate capability. We have also investigated the influence of a range of different parameters on the electrochemical performance of these materials, including pore size and shape, carbon and silicon film thickness and microstructure, and binder chemistry.

Printed biofuel cells

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, Joseph; Windmiller, Joshua Ray; Jia, Wenzhao

2016-11-22

Methods, systems, and devices are disclosed for implementing a biofuel cell device for extracting energy from a biofuel. In one aspect, a biofuel cell device includes a substrate, an anode including a catalyst to facilitate the conversion of a fuel in a biological fluid in an oxidative process that releases electrons captured at the anode, thereby extracting energy from the fuel substance, a cathode configured on the substrate adjacent to the anode and separated from the anode by a spacing region, and a load electrically coupled to the anode and cathode via electrical interconnects to obtain the extracted energy asmore » electrical energy.« less

Evaluation of the impact of sodium lauryl sulfate source variability on solid oral dosage form development.

PubMed

Qiang, Dongmei; Gunn, Jocelyn A; Schultz, Leon; Li, Z Jane

2010-12-01

The objective of this study was to investigate the effects of sodium lauryl sulfate (SLS) from different sources on solubilization/wetting, granulation process, and tablet dissolution of BILR 355 and the potential causes. The particle size distribution, morphology, and thermal behaviors of two pharmaceutical grades of SLS from Spectrum and Cognis were characterized. The surface tension and drug solubility in SLS solutions were measured. The BILR 355 tablets were prepared by a wet granulation process and the dissolution was evaluated. The critical micelle concentration was lower for Spectrum SLS, which resulted in a higher BILR 355 solubility. During wet granulation, less water was required to reach the same end point using Spectrum than Cognis SLS. In general, BILR 355 tablets prepared with Spectrum SLS showed a higher dissolution than the tablets containing Cognis SLS. Micronization of SLS achieved the same improved tablet dissolution as micronized active pharmaceutical ingredient. The observed differences in wetting and solubilization were likely due to the different impurity levels in SLS from two sources. This study demonstrated that SLS from different sources could have significant impact on wet granulation process and dissolution. Therefore, it is critical to evaluate SLS properties from different suppliers, and then identify optimal formulation and process parameters to ensure robustness of drug product manufacture process and performance.

Latent variable modeling to analyze the effects of process parameters on the dissolution of paracetamol tablet

PubMed Central

Sun, Fei; Xu, Bing; Zhang, Yi; Dai, Shengyun; Shi, Xinyuan; Qiao, Yanjiang

2017-01-01

ABSTRACT The dissolution is one of the critical quality attributes (CQAs) of oral solid dosage forms because it relates to the absorption of drug. In this paper, the influence of raw materials, granules and process parameters on the dissolution of paracetamol tablet was analyzed using latent variable modeling methods. The variability in raw materials and granules was understood based on the principle component analysis (PCA), respectively. A multi-block partial least squares (MBPLS) model was used to determine the critical factors affecting the dissolution. The results showed that the binder amount, the post granulation time, the API content in granule, the fill depth and the punch tip separation distance were the critical factors with variable importance in the projection (VIP) values larger than 1. The importance of each unit of the whole process was also ranked using the block importance in the projection (BIP) index. It was concluded that latent variable models (LVMs) were very useful tools to extract information from the available data and improve the understanding on dissolution behavior of paracetamol tablet. The obtained LVMs were also helpful to propose the process design space and to design control strategies in the further research. PMID:27689242

Radiation imaging apparatus

DOEpatents

Anger, Hal O.; Martin, Donn C.; Lampton, Michael L.

1983-01-01

A radiation imaging system using a charge multiplier and a position sensitive anode in the form of periodically arranged sets of interconnected anode regions for detecting the position of the centroid of a charge cloud arriving thereat from the charge multiplier. Various forms of improved position sensitive anodes having single plane electrode connections are disclosed. Various analog and digital signal processing systems are disclosed, including systems which use the fast response of microchannel plates, anodes and preamps to perform scintillation pulse height analysis digitally.

Evaluation of various processes for simultaneous complexation and granulation to incorporate drug-cyclodextrin complexes into solid dosage forms.

PubMed

Gyanani, Vijay; Siddalingappa, Basavaraj; Betageri, Guru V

2015-01-01

Insoluble drugs often formulated with various excipients to enhance the dissolution. Cyclodextrins (CDs) are widely used excipients to improve dissolution profile of poorly soluble drugs. Drug-CD complexation process is complex and often requires multiple processes to produce solid dosage form. Hence, this study explored commonly used granulation processes for simultaneous complexation and granulation. Poorly soluble drugs ibuprofen and glyburide were selected as experimental drugs. Co-evaporation of drug:CD mixture from a solvent followed by wet granulation with water was considered as standard process for comparison. Spray granulation and fluid bed processing (FBP) using drug:CD solution in ethanol were evaluated as an alternative processes. The dissolution data of glyburide tablets indicated that tablets produced by spray granulation, FBP and co-evaporation-granulation have almost identical dissolution profile in water and 0.1% SLS (>70% in water and >60% in SLS versus 30 and 34%, respectively for plain tablet, in 120 min). Similarly, ibuprofen:CD tablets produced by co-evaporation-granulation and FBP displayed similar dissolution profile in 0.01 M HCl (pH 2.0) and buffer pH 5.5 (>90 and 100% versus 44 and 80% respectively for plain tablets, 120 min). Results of this study demonstrated that spray granulation is simple and cost effective process for low dose poorly soluble drugs to incorporate drug:CD complex into solid dosage form, whereas FBP is suitable for poorly soluble drugs with moderate dose.

Electrolytic production of high purity aluminum using inert anodes

DOEpatents

Ray, Siba P.; Liu, Xinghua; Weirauch, Jr., Douglas A.

2001-01-01

A method of producing commercial purity aluminum in an electrolytic reduction cell comprising inert anodes is disclosed. The method produces aluminum having acceptable levels of Fe, Cu and Ni impurities. The inert anodes used in the process preferably comprise a cermet material comprising ceramic oxide phase portions and metal phase portions.

Effect of Adding SiO2-Al2O3 Sol into Anodizing Bath on Corrosion Resistance of Oxidation Film on Magnesium Alloy

NASA Astrophysics Data System (ADS)

Liu, Huicong; Zhu, Liqun; Li, Weiping

Due to the widely use in automobile and construction field, AZ91D magnesium alloy need to be protected more effectively for its high chemical activity. In this paper, three kinds of films were formed on magnesium alloy. The first kind of film, named as anodic oxidation film, was prepared by anodic oxidation in the alkaline solution. The processes for preparing the second kind of film, named as multiple film, involved coating sol-gel on the samples and heat-treating before anodic oxidation. The third kind of film was prepared by anodic oxidation in the alkaline oxidation solution containning 5% (vol) SiO2-Al2O3 sol, named as modified oxidation film. The corrosion resistance of the three different films was investigated. The results showed that the modified oxidation film had the highest corrosion resistance due to the largest thickness and most dense surface morphology. Sol was discussed to react during the film forming process, which leaded to the difference between modified oxidation film and anodic oxidation film.

Porous aluminum room temperature anodizing process in a fluorinated-oxalic acid solution

NASA Astrophysics Data System (ADS)

Dhahri, S.; Fazio, E.; Barreca, F.; Neri, F.; Ezzaouia, H.

2016-08-01

Anodizing of aluminum is used for producing porous insulating films suitable for different applications in electronics and microelectronics. Porous-type aluminum films are most simply realized by galvanostatic anodizing in aqueous acidic solutions. The improvement in application of anodizing technique is associated with a substantial reduction of the anodizing voltage at appropriate current densities as well as to the possibility to carry out the synthesis process at room temperature in order to obtain a self-planarizing dielectric material incorporated in array of super-narrow metal lines. In this work, the anodizing of aluminum to obtain porous oxide was carried out, at room temperature, on three different substrates (glass, stainless steel and aluminum), using an oxalic acid-based electrolyte with the addition of a relatively low amount of 0.4 % of HF. Different surface morphologies, from nearly spherical to larger porous nanostructures with smooth edges, were observed by means of scanning electron microscopy. These evidences are explained by considering the formation, transport and adsorption of the fluorine species which react with the Al3+ ions. The behavior is also influenced by the nature of the original substrate.

Nernst-ping-pong model for evaluating the effects of the substrate concentration and anode potential on the kinetic characteristics of bioanode.

PubMed

Peng, Sikan; Liang, Da-Wei; Diao, Peng; Liu, Yanyan; Lan, Fei; Yang, Yuhan; Lu, Shanfu; Xiang, Yan

2013-05-01

Understanding the electron-transfer mechanism and kinetic characteristics of bioanodes is greatly significant to enhance the electron-generating efficiencies in bioelectrochemical systems (BESs). A Nernst-ping-pong model is proposed here to investigate the kinetics and biochemical processes of bioanodes in a microbial electrolysis cell. This model can accurately describe the effects of the substrate (including substrate inhibition) and the anode potential on the current of bioanodes. Results show that the half-wave potential positively shifts as the substrate concentration increases, indicating that the rate-determining steps of anodic processes change from substrate oxidation to intracellular electron transport reaction. The anode potential has negligible effects on the enzymatic catalysis of anodic microbes in the range of -0.25 V to +0.1 V vs. a saturated calomel electrode. It turns out that to reduce the anodic energy loss caused by overpotential, higher substrate concentrations are preferred, if the substrate do not significantly and adversely affect the output current. Copyright © 2013 Elsevier Ltd. All rights reserved.

Air plasma spray processing and electrochemical characterization of Cu-SDC coatings for use in solid oxide fuel cell anodes

NASA Astrophysics Data System (ADS)

Benoved, Nir; Kesler, O.

Air plasma spraying has been used to produce porous composite anodes based on Ce 0.8Sm 0.2O 1.9 (SDC) and Cu for use in solid oxide fuel cells (SOFCs). Preliminarily, a range of plasma conditions has been examined for the production of composite coatings from pre-mixed SDC and CuO powders. Plasma gas compositions were varied to obtain a range of plasma temperatures. After reduction in H 2, coatings were characterized for composition and microstructure using EDX and SEM. As a result of these tests, symmetrical sintered electrolyte-supported anode-anode cells were fabricated by air plasma spraying of the anodes, followed by in situ reduction of the CuO to Cu. Full cells deposited on SS430 porous substrates were then produced in one integrated process. Fine CuO and SDC powders have been used to produce homogeneously mixed anode coatings with higher surface area microstructures, resulting in area-specific polarization resistances of 4.8 Ω cm 2 in impedance tests in hydrogen at 712 °C.

Single-Wall Carbon Nanotube Production by the Arc Process: A Parametric Study

NASA Technical Reports Server (NTRS)

Scott, Carl D.; Gorelik, Olga; Proft, William J.

2000-01-01

Single wall carbon nanotubes are produced using the arc discharge process. Graphite anodes are filled with a mixture of nickel and yttrium metallic powders, then vaporized by creating a high current arc. By varying the current, gap distance, and ambient pressure it is shown that the best yield of single wall carbon nanotubes is obtained within a narrow range of conditions. The relative yield and purity of the product are indicated semi-quantitatively from scanning electric microscopy (SEM) and thermogravimetric analysis (TGA). Two types of anodes have been investigated. The first is hollow and filled with a powder mixture of graphite, nickel and yttrium. The second is filled with a paste made of a mixture of metal nitrates, graphite powder and carbon adhesive, then reduced in an argon atmosphere at high temperature. Product purity and yield will be compared for the two types of anodes. The graphite in the anodes may have hydrogen attached in the pores. To remove this impurity anodes have been baked up to 1400 - 1500 C. The effect of baking the anodes on impurities in the product will be given.

Hepa filter dissolution process

DOEpatents

Brewer, Ken N.; Murphy, James A.

1994-01-01

A process for dissolution of spent high efficiency particulate air (HEPA) filters and then combining the complexed filter solution with other radioactive wastes prior to calcining the mixed and blended waste feed. The process is an alternate to a prior method of acid leaching the spent filters which is an inefficient method of treating spent HEPA filters for disposal.

A mathematical analysis of drug dissolution in the USP flow through apparatus

NASA Astrophysics Data System (ADS)

McDonnell, David; D'Arcy, D. M.; Crane, L. J.; Redmond, Brendan

2018-03-01

This paper applies boundary layer theory to the process of drug dissolution in the USP (United States Pharmacopeia) Flow Through Apparatus. The mass transfer rate from the vertical planar surface of a compact within the device is examined. The theoretical results obtained are then compared with those of experiment. The paper also examines the effect on the dissolution process caused by the interaction between natural and forced convection within the apparatus and the introduction of additional boundaries.

Dissolution process for ZrO.sub.2 -UO.sub.2 -CaO fuels

DOEpatents

Paige, Bernice E.

1976-06-22

The present invention provides an improved dissolution process for ZrO.sub.2 -UO.sub.2 -CaO-type pressurized water reactor fuels. The zirconium cladding is dissolved with hydrofluoric acid, immersing the ZrO.sub.2 -UO.sub.2 -CaO fuel wafers in the resulting zirconium-dissolver-product in the dissolver vessel, and nitric acid is added to the dissolver vessel to facilitate dissolution of the uranium from the ZrO.sub.2 -UO.sub.2 -CaO fuel wafers.

Modelling the growth of porous alumina matrix for creating hyperbolic media

NASA Astrophysics Data System (ADS)

Aryslanova, E. M.; Alfimov, A. V.; Chivilikhin, S. A.

2016-08-01

Porous aluminum oxide is a regular self-assembled structure. During anodization it is possible to control nano-parameters of the structure using macroscopic parameters of anodization. Porous alumina films can be used as a template for the creation of hyperbolic media. In this work we consider the anodization process, our model takes into account the influence of layers of aluminum and electrolyte on the rate of growth of aluminum oxide, as well as the effect of surface diffusion. As a result of our model we obtain the minimum distance between centers of alumina pores in the beginning of anodizing process. We also present the results obtained by numerical modelling of hyperbolic media based on porous alumina film.

Facile preparation of porous alumina through-hole masks for sputtering by two-layer anodization

NASA Astrophysics Data System (ADS)

Yanagishita, Takashi; Masuda, Hideki

2016-08-01

Highly ordered porous alumina through-hole masks were fabricated on a substrate by combining two-layer anodization with subsequent through-holing by selective etching. This process allowed the fabrication of porous alumina masks without an increase in pore size during the etching performed for through-holing. Additionally, the process contributed to improved operability in the setting of the masks on substrates because the second anodizing layer acts as a supporting layer for the handling of the mask. The fabrication of ordered Au nanodot arrays was demonstrated as an example application of the through-hole masks obtained by the present process.

The role of halide ions on the electrochemical behaviour of iron in alkali solutions

NASA Astrophysics Data System (ADS)

Begum, S. Nathira; Muralidharan, V. S.; Basha, C. Ahmed

2008-02-01

Active dissolution and passivation of transition metals in alkali solutions is of technological importance in batteries. The performance of alkaline batteries is decided by the presence of halides as they influence passivation. Cyclic voltammetric studies were carried out on iron in different sodium hydroxide solutions in presence of halides. In alkali solutions iron formed hydroxo complexes and their polymers in the interfacial diffusion layer. With progress of time they formed a cation selective layer. The diffusion layer turned into bipolar ion selective layer consisted of halides, a selective inner sublayer to the metal side and cation selective outer layer to the solution side. At very high anodic potentials, dehydration and deprotonation led to the conversion of salt layer into an oxide.

Using Copper Nanoparticle Additive to Improve the Performance of Silicon Anodes in Lithium-Ion Batteries

NASA Astrophysics Data System (ADS)

Bachand, Gabrielle

In the foreseeable future, global energy demand is expected to rapidly increase as a result of the swelling population and higher standards of living. Current energy generation and transportation methods predominantly involve the combustion of non-renewable fossil fuels, and greenhouse gas emissions from these processes have been shown to contribute to global climate change and to be detrimental to human and environmental health. To satisfy future energy needs and to reduce greenhouse gas emissions, the advancement of renewable energy generation and electric vehicles is important. The proliferation of intermittent renewable energy sources (such as solar and wind) and electric vehicles depends upon reliable, high-capacity energy storage to serve the practical needs of society. The present-day lithium-ion battery offers excellent qualities for this purpose; however, improvements in the capacity and cost-effectiveness of these batteries are needed for further growth. As an anode material, silicon has exceptionally high theoretical capacity and is an earth-abundant, low-cost option. However, silicon also suffers from poor conductivity and long-term stability, prompting many studies to investigate the use of additive materials to mitigate these issues. This thesis focuses on the improvement of silicon anode performance by using a nanoparticulate copper additive to increase material conductivity and an inexpensive, industry-compatible anode fabrication process. Three main fabrication processes were explored using differing materials and heat treatment techniques for comparison. Anodes were tested using CR2032 type coin cells. The final anodes with the most-improved characteristics were fabricated using a high-temperature heating step for the anode material, and an additional batch was formed to test the viability of the copper additive functioning as a full substitute for carbon black, which is the traditional choice of conductive additive for electrode materials. Anodes materials were characterized using a variety of techniques including scanning electron microscopy (SEM), electron dispersive spectroscopy (EDS), inductively coupled plasma optical emission spectrometry (ICP-OES), Raman spectroscopy, and X-ray diffraction (XRD) to evaluate surface qualities and material content. Electrochemical techniques including electrochemical impedance spectroscopy (EIS) and charge/discharge cycling were also used to determine the conductivity and functional behavior of the anode materials. Anodes from the final experimental study achieved initial capacities of 309 mA/g and 957 mA/g for the silicon-only control and silicon with copper additive anodes, respectively, demonstrating an over 300% increase in specific capacity. Si-Cu (NC) anodes also showed superior performance over control anodes with an initial capacity of 775 mA/g. For all three anodes, high efficiencies of over 96% were achieved for the testing duration of 100 cycles and reached near or over 99% in final cycles. Results also show a significant decrease in the resistance of anodes with copper additive, contributing to the improved performance of these anodes.

Imidazole-based deep eutectic solvents for starch dissolution and plasticization.

PubMed

Zdanowicz, Magdalena; Spychaj, Tadeusz; Mąka, Honorata

2016-04-20

Potato starch and high-amylose starch were treated with imidazole-based deep eutectic solvents (DESs) as dissolution and plasticization media. Beside imidazole (IM) for two-component DESs preparation choline chloride (CC), glycerol (G) or carboxylic acids (citric or malic) were used. An influence of water content in starch (as well as an extra water in the starch/DES system) on polymer dissolution and plasticization processes was investigated. Dissolution and gelatinization of starch in DESs were followed via DSC and laser scanning microscopy. A rheometric characteristics revealed an influence of starch/DES system storage time on the plasticization process. The tendency to recrystallization of compression-molded-starch films was evaluated using XRD technique. High dissolution and plasticization effectiveness of CC/IM and G/IM and a low tendency to film retrogradation of thermoplasticized starch were noted. Copyright © 2015 Elsevier Ltd. All rights reserved.

Behavior of S.A.P. in the Mercury Catalyzed Nitric Acid Dissolution; COMPORTAMENTO DEL S.A.P. ALL'ATTACCO DI SOLUZIONI DI ACIDO NITRICO E NITRATO MERCURICO

DOE Office of Scientific and Technical Information (OSTI.GOV)

Beone, G.

1963-10-01

Plates of S.A.P. (sintered Aluminum Powder) were dissolved under different conditions in a nitric acid solution containing mercuric nitrate as a catalyst. These experiments nim at establishing a head-end dissolution process for S.A.P. cladded uranium oxide fuels. The results of preliminary dissolution experiments on simulated fuel rods are also described. The behavior of S.A.P. in the mercury catalyzed nitric acid dissolutions differs strongly from the behavior of aluminum: reaction rates are very low for S.A.P. and the dissolution time borders on being unacceptable in an industrial process. Settling rates of suspended alumina are however favorable. A tentative head end flowsheetmore » lay out for PRO second core fuel elements is included. (auth)« less

Dissolution kinetics of soluble nondisintegrating disks.

PubMed

de Blaey, C J; van der Graaff, H

1977-12-01

An equation describing the isotropical dissolution of soluble nondisintegrating disks was developed. It was equivalent to the cube root law only if the height and diameter of the disk were equal. The dissolution kinetics of sodium chloride disks were examined, using a beaker equipped with a centrifugal stirrer as the dissolution chamber. The fit of the experimental data to the cube root law had a coefficient of variation of about 4-5%. It was demonstrated statistically that a fit to a square root of mass versus time relation was significantly better. With increasing porosity, the dissolution process proceeded faster than predicted on the basis of the diffusion-convection model. An explanation is proposed by assuming an increased effective dissolution surface.

Lubricant-Induced Crystallization of Itraconazole From Tablets Made of Electrospun Amorphous Solid Dispersion.

PubMed

Démuth, Balázs; Farkas, Attila; Balogh, Attila; Bartosiewicz, Karolina; Kállai-Szabó, Barnabás; Bertels, Johny; Vigh, Tamás; Mensch, Jurgen; Verreck, Geert; Van Assche, Ivo; Marosi, György; Nagy, Zsombor K

2016-09-01

Investigation of downstream processing of nanofibrous amorphous solid dispersions to generate tablet formulation is in a quite early phase. Development of high speed electrospinning opened up the possibility to study tableting of electrospun solid dispersions (containing polyvinylpyrrolidone-vinyl acetate and itraconazole [ITR] in this case). This work was conducted to investigate the influence of excipients on dissolution properties and the feasibility of scaled-up rotary press tableting. The dissolution rates from tablets proved to be mainly composition dependent. Magnesium stearate acted as a nucleation promoting agent (providing an active hydrophobic environment for crystallization of ITR) hindering the total dissolution of ITR. This crystallization process proved to be temperature dependent as well. However, the extent of dissolution of more than 95% was realizable when a less hydrophobic lubricant, sodium stearyl fumarate (soluble in the medium), was applied. Magnesium stearate induced crystallization even if it was put in the dissolution medium next to proper tablets. After optimization of the composition, scaled-up tableting on a rotary press was carried out. Appropriate dissolution of ITR from tablets was maintained for 3 months at 25°C/60% relative humidity. HPLC measurements confirmed that ITR was chemically stable both in the course of downstream processing and storage. Copyright © 2016 American Pharmacists Association®. Published by Elsevier Inc. All rights reserved.

Solid Oxide Membrane (SOM) Process for Facile Electrosynthesis of Metal Carbides and Composites

NASA Astrophysics Data System (ADS)

Zou, Xingli; Chen, Chaoyi; Lu, Xionggang; Li, Shangshu; Xu, Qian; Zhou, Zhongfu; Ding, Weizhong

2017-02-01

Metal carbides (MCs) and composites including TiC, SiC, TaC, ZrC, NbC, Ti5Si3/TiC, and Nb/Nb5Si3 have been directly electrosynthesized from their stoichiometric metal oxides/carbon (MOs/C) mixture precursors by an innovative solid oxide membrane (SOM)-assisted electrochemical process. MOs/C mixture powders including TiO2/C, SiO2/C, Ta2O5/C, ZrO2/C, Nb2O5/C, TiO2/SiO2/C, Nb2O5/SiO2 were pressed to form porous pellets and then served as cathode precursors. A SOM-based anode, made from yttria-stabilized zirconia (YSZ)-based membrane, was used to control the electroreduction process. The SOM electrochemical process was performed at 1273 K (1000 °C) and 3.5 to 4.0 V in molten CaCl2. The oxygen component contained in the MOs/C precursors was gradually removed during electroreduction process, and thus, MOs/C can be directly converted into MCs and composites at the cathode. The reaction mechanism of the electroreduction process and the characteristics of the obtained MCs and composites products were systematically investigated. The results show that the electrosynthesis process typically involves compounding, electroreduction, dissolution-electrodeposition, and in situ carbonization processes. The products can be predesigned and controlled to form micro/nanostructured MCs and composites. Multicomponent multilayer composites (MMCs) have also been tried to electrosynthesize in this work. It is suggested that the SOM-assisted electroreduction process has great potential to be used for the facile and green synthesis of various MCs and composites.

Feasibility of Using Gluconolactone, Trehalose and Hydroxy-Propyl Gamma Cyclodextrin to Enhance Bendroflumethiazide Dissolution Using Lyophilisation and Physical Mixing Techniques.

PubMed

Saleh, Ashraf; McGarry, Kenneth; Chaw, Cheng Shu; Elkordy, Amal Ali

2018-02-01

Hydrophobic drugs are facing a major challenge in dissolution rate enhancement and solubility in aqueous solutions; therefore, a variety of methods have been used to improve dissolution rate and/or solubility of bendroflumethiazide as a model hydrophobic drug. In this study, two main methods (physical mixing and lyophilisation) were used with gluconolactone, hydroxyl propyl γ-ccyclodextrin, and trehalose to explore this challenge. Bendroflumethiazide, practically insoluble in water, was mixed with one of the three excipients gluconolactone, hydroxyl propyl γ-cyclodextrin, and trehalose in three different ratios 1:1, 1:2, 1:5. To the best of our knowledge, the dissolution of the drug has not been previously enhanced by using either these methods or any of the used excipients. Samples containing drug and each of the excipients were characterized via dissolution testing, Fourier Transform infra-red spectroscopy, differential scanning calorimetry, and scanning electron microscopy. The used methods showed a significant enhancement in dug dissolution rate; physical mixing significantly, p < 0.05, increased the percentage of the drug released with time; for example, bendroflumethiazide dissolution in distilled water was improved from less than 20% to 99.79% within 90 min for physically mixed drug-cyclodextrin 1:5. The lyophilisation process was enhanced and the drug dissolution rate and the highest drug dissolution was achieved for (drug-gluconolactone 1:1) with 98.98% drug release within 90 min. the physical mixing and freeze drying processes significantly increased the percentage of drug release with time.

Radiation imaging apparatus

DOEpatents

Anger, H.O.; Martin, D.C.; Lampton, M.L.

1983-07-26

A radiation imaging system using a charge multiplier and a position sensitive anode in the form of periodically arranged sets of interconnected anode regions for detecting the position of the centroid of a charge cloud arriving thereat from the charge multiplier. Various forms of improved position sensitive anodes having single plane electrode connections are disclosed. Various analog and digital signal processing systems are disclosed, including systems which use the fast response of microchannel plates, anodes and preamps to perform scintillation pulse height analysis digitally. 15 figs.

Localised anodic oxidation of aluminium material using a continuous electrolyte jet

NASA Astrophysics Data System (ADS)

Kuhn, D.; Martin, A.; Eckart, C.; Sieber, M.; Morgenstern, R.; Hackert-Oschätzchen, M.; Lampke, T.; Schubert, A.

2017-03-01

Anodic oxidation of aluminium and its alloys is often used as protection against material wearout and corrosion. Therefore, anodic oxidation of aluminium is applied to produce functional oxide layers. The structure and properties of the oxide layers can be influenced by various factors. These factors include for example the properties of the substrate material, like alloy elements and heat treatment or process parameters, like operating temperature, electric parameters or the type of the used electrolyte. In order to avoid damage to the work-piece surface caused by covering materials in masking applications, to minimize the use of resources and to modify the surface in a targeted manner, the anodic oxidation has to be localised to partial areas. Within this study a proper alternative without preparing the substrate by a mask is investigated for generating locally limited anodic oxidation by using a continuous electrolyte jet. Therefore aluminium material EN AW 7075 is machined by applying a continuous electrolyte jet of oxalic acid. Experiments were carried out by varying process parameters like voltage or processing time. The realised oxide spots on the aluminium surface were investigated by optical microscopy, SEM and EDX line scanning. Furthermore, the dependencies of the oxide layer properties from the process parameters are shown.

Anodization Mechanism on SiC Nanoparticle Reinforced Al Matrix Composites Produced by Power Metallurgy.

PubMed

Ferreira, Sonia C; Conde, Ana; Arenas, María A; Rocha, Luis A; Velhinho, Alexandre

2014-12-19

Specimens of aluminum-based composites reinforced by silicon carbide nanoparticles (Al/SiC np ) produced by powder metallurgy (PM) were anodized under voltage control in tartaric-sulfuric acid (TSA). In this work, the influence of the amount of SiC np on the film growth during anodizing was investigated. The current density versus time response and the morphology of the porous alumina film formed at the composite surface are compared to those concerning a commercial aluminum alloy (AA1050) anodized under the same conditions. The processing method of the aluminum alloys influences the efficiency of the anodizing process, leading to a lower thicknesses for the unreinforced Al-PM alloy regarding the AA1050. The current density versus time response is strongly dependent on the amount of SiC np . The current peaks and the steady-state current density recorded at each voltage step increases with the SiC np volume fraction due to the oxidation of the SiC np . The formation mechanism of the anodic film on Al/SiC np composites is different from that occurring in AA1050, partly due the heterogeneous distribution of the reinforcement particles in the metallic matrix, but also to the entrapment of SiC np in the anodic film.

Anodization Mechanism on SiC Nanoparticle Reinforced Al Matrix Composites Produced by Power Metallurgy

PubMed Central

Ferreira, Sonia C.; Conde, Ana; Arenas, María A.; Rocha, Luis A.; Velhinho, Alexandre

2014-01-01

Specimens of aluminum-based composites reinforced by silicon carbide nanoparticles (Al/SiCnp) produced by powder metallurgy (PM) were anodized under voltage control in tartaric-sulfuric acid (TSA). In this work, the influence of the amount of SiCnp on the film growth during anodizing was investigated. The current density versus time response and the morphology of the porous alumina film formed at the composite surface are compared to those concerning a commercial aluminum alloy (AA1050) anodized under the same conditions. The processing method of the aluminum alloys influences the efficiency of the anodizing process, leading to a lower thicknesses for the unreinforced Al-PM alloy regarding the AA1050. The current density versus time response is strongly dependent on the amount of SiCnp. The current peaks and the steady-state current density recorded at each voltage step increases with the SiCnp volume fraction due to the oxidation of the SiCnp. The formation mechanism of the anodic film on Al/SiCnp composites is different from that occurring in AA1050, partly due the heterogeneous distribution of the reinforcement particles in the metallic matrix, but also to the entrapment of SiCnp in the anodic film. PMID:28788295

Etching Behavior of Aluminum Alloy Extrusions

NASA Astrophysics Data System (ADS)

Zhu, Hanliang

2014-11-01

The etching treatment is an important process step in influencing the surface quality of anodized aluminum alloy extrusions. The aim of etching is to produce a homogeneously matte surface. However, in the etching process, further surface imperfections can be generated on the extrusion surface due to uneven materials loss from different microstructural components. These surface imperfections formed prior to anodizing can significantly influence the surface quality of the final anodized extrusion products. In this article, various factors that influence the materials loss during alkaline etching of aluminum alloy extrusions are investigated. The influencing variables considered include etching process parameters, Fe-rich particles, Mg-Si precipitates, and extrusion profiles. This study provides a basis for improving the surface quality in industrial extrusion products by optimizing various process parameters.

Electrolytic production of high purity aluminum using ceramic inert anodes

DOEpatents

Ray, Siba P.; Liu, Xinghua; Weirauch, Douglas A.; DiMilia, Robert A.; Dynys, Joseph M.; Phelps, Frankie E.; LaCamera, Alfred F.

2002-01-01

A method of producing commercial purity aluminum in an electrolytic reduction cell comprising ceramic inert anodes is disclosed. The method produces aluminum having acceptable levels of Fe, Cu and Ni impurities. The ceramic inert anodes used in the process may comprise oxides containing Fe and Ni, as well as other oxides, metals and/or dopants.

Developing a quality by design approach to model tablet dissolution testing: an industrial case study.

PubMed

Yekpe, Ketsia; Abatzoglou, Nicolas; Bataille, Bernard; Gosselin, Ryan; Sharkawi, Tahmer; Simard, Jean-Sébastien; Cournoyer, Antoine

2018-07-01

This study applied the concept of Quality by Design (QbD) to tablet dissolution. Its goal was to propose a quality control strategy to model dissolution testing of solid oral dose products according to International Conference on Harmonization guidelines. The methodology involved the following three steps: (1) a risk analysis to identify the material- and process-related parameters impacting the critical quality attributes of dissolution testing, (2) an experimental design to evaluate the influence of design factors (attributes and parameters selected by risk analysis) on dissolution testing, and (3) an investigation of the relationship between design factors and dissolution profiles. Results show that (a) in the case studied, the two parameters impacting dissolution kinetics are active pharmaceutical ingredient particle size distributions and tablet hardness and (b) these two parameters could be monitored with PAT tools to predict dissolution profiles. Moreover, based on the results obtained, modeling dissolution is possible. The practicality and effectiveness of the QbD approach were demonstrated through this industrial case study. Implementing such an approach systematically in industrial pharmaceutical production would reduce the need for tablet dissolution testing.

Atomic-scale imaging of the dissolution of NaCl islands by water at low temperature

NASA Astrophysics Data System (ADS)

Peng, Jinbo; Guo, Jing; Ma, Runze; Meng, Xiangzhi; Jiang, Ying

2017-03-01

The dissolution of sodium chloride (NaCl) in water is a frequently encountered process in our daily lives. While the NaCl dissolution process in liquid water has been extensively studied, whether and how the dissolution occurs below the freezing point is still not clear. Using a low-temperature scanning tunneling microscope (STM), here we were able to directly visualize the dissolution of Au-supported NaCl (0 0 1) bilayer islands by water at atomic level. We found that the single water molecule on the STM tip can assist the extraction of single Na+ from the NaCl surface even at 5 K, while leaving the Cl- intact. When covered with a full water monolayer, the NaCl islands started to dissolve from the step edges and also showed evidence of dissolution inside the terraces as the temperature was raised up to 145 K. At 155 K, the water molecules completely desorbed from the surface, which was accompanied with the decomposition and restructuring of the bilayer NaCl islands. Those results suggest that the dissolution of NaCl may occur well below the freezing point at the ice/NaCl interfaces and is mainly driven by the interaction between the water molecules and the Na+, which is in clear contrast with the NaCl dissolution in liquid water.

The effect of ethylene glycol on pore arrangement of anodic aluminium oxide prepared by hard anodization

NASA Astrophysics Data System (ADS)

Guo, Yang; Zhang, Li; Han, Mangui; Wang, Xin; Xie, Jianliang; Deng, Longjiang

2018-03-01

The influence of the addition of ethylene glycol (EG) on the pore self-ordering process in anodic aluminium oxide (AAO) membranes prepared by hard anodization (HA) was investigated. It was illustrated that EG has a substantial effect on the pore arrangement of AAO, and it was found that a smaller pore size can be obtained with an EG concentration reaching 20 wt% in aqueous electrolyte. The number of estimated defects of AAO increases significantly with an increase in EG concentration to 50 wt%. Excellent ordering of pores was realized when the samples were anodized in the 30 wt%-EG-containing aqueous electrolyte.

Thin film buried anode battery

DOEpatents

Lee, Se-Hee [Lakewood, CO; Tracy, C Edwin [Golden, CO; Liu, Ping [Denver, CO

2009-12-15

A reverse configuration, lithium thin film battery (300) having a buried lithium anode layer (305) and process for making the same. The present invention is formed from a precursor composite structure (200) made by depositing electrolyte layer (204) onto substrate (201), followed by sequential depositions of cathode layer (203) and current collector (202) on the electrolyte layer. The precursor is subjected to an activation step, wherein a buried lithium anode layer (305) is formed via electroplating a lithium anode layer at the interface of substrate (201) and electrolyte film (204). The electroplating is accomplished by applying a current between anode current collector (201) and cathode current collector (202).

HEPA filter dissolution process

DOEpatents

Brewer, K.N.; Murphy, J.A.

1994-02-22

A process is described for dissolution of spent high efficiency particulate air (HEPA) filters and then combining the complexed filter solution with other radioactive wastes prior to calcining the mixed and blended waste feed. The process is an alternate to a prior method of acid leaching the spent filters which is an inefficient method of treating spent HEPA filters for disposal. 4 figures.

Effect of fabrication parameters on coating properties of tubular solid oxide fuel cell electrolyte prepared by vacuum slurry coating

NASA Astrophysics Data System (ADS)

Son, Hui-Jeong; Song, Rak-Hyun; Lim, Tak-Hyoung; Lee, Seung-Bok; Kim, Sung-Hyun; Shin, Dong-Ryul

The process of vacuum slurry coating for the fabrication of a dense and thin electrolyte film on a porous anode tube is investigated for application in solid oxide fuel cells. 8 mol% yttria stabilized zirconia is coated on an anode tube by vacuum slurry-coating process as a function of pre-sintering temperature of the anode tube, vacuum pressure, slurry concentration, number of coats, and immersion time. A dense electrolyte layer is formed on the anode tube after final sintering at 1400 °C. With decrease in the pre-sintering temperature of the anode tube, the grain size of the coated electrolyte layer increases and the number of surface pores in the coating layer decreases. This is attributed to a reduced difference in the respective shrinkage of the anode tube and the electrolyte layer. The thickness of the coated electrolyte layer increases with the content of solid powder in the slurry, the number of dip-coats, and the immersion time. Although vacuum pressure has no great influence on the electrolyte thickness, higher vacuum produces a denser coating layer, as confirmed by low gas permeability and a reduced number of defects in the coating layer. A single cell with the vacuum slurry coated electrolyte shows a good performance of 620 mW cm -2 (0.7 V) at 750 °C. These experimental results indicate that the vacuum slurry-coating process is an effective method to fabricate a dense thin film on a porous anode support.

A Model of Anode Sheath Potential Evolution in a Transverse Magnetic Field

NASA Astrophysics Data System (ADS)

Foster, John E.; Gallimore, Alec D.

1996-11-01

It has been conjectured that the growth in the magnitude of the anode fall voltage with changing transverse magnetic field is a function of the ratio of available transverse current to the discharge current. It has been postulated that at small values of this ratio, the anode fall voltage and thus the near-anode electric field increases in order to assure that the prescribed discharge is maintained.footnote H. Hugel, IEEE Tran. Plas. Sci., PS-8,4, 1980 In this present work, a model is presented which predicts the behavior of the anode fall voltage as a function of transverse magnetic field. The model attempts to explain why the anode fall voltage depends so strongly on this ratio. In addition, it is further shown that because of the current ratio's strong dependence on local electron number density, ultimately it is the changes in near-anode ionization processes with varying transverse magnetic field that control the anode fall voltage.

Comparison of electrokinetic soil remediation methods using one fixed anode and approaching anodes.

PubMed

Shen, Zhemin; Chen, Xuejun; Jia, Jinping; Qu, Liya; Wang, Wenhua

2007-11-01

During the cation exchange membrane (CEM) enhanced electrokinetic (EK) soil remediation, the nearer to the anode, the higher are the H+ concentrations and the redox potentials. As both low pH and high redox potential are helpful to speed-up Cd electro-migration, soils near the anode can be quickly remedied. Usually EK process is operated with one fixed anode (FA). A novel CEM enhanced EK method with approaching anodes (AAs) is proposed to accelerate electro-migration effect. Several mesh Ti/Ru anodes were inserted as AAs in the treated soil. They were switched in turn from the anode towards the cathode. Thus high H+ ions concentrations and high redox potentials quickly migrate to the cathode. Consequently, soil remediation is accelerated and nearly 44% of energy and 40% of time can be saved. The mechanism of Cd electro-migration behavior in soils during CEM enhanced EK is described as the elution in an electrokinetically driven chromatogram.

Surface States and Effective Surface Area on Photoluminescent P-Type Porous Silicon

NASA Technical Reports Server (NTRS)

Weisz, S. Z.; Porras, A. Ramirez; Resto, O.; Goldstein, Y.; Many, A.; Savir, E.

1997-01-01

The present study is motivated by the possibility of utilizing porous silicon for spectral sensors. Pulse measurements on the porous-Si/electrolyte system are employed to determine the surface effective area and the surface-state density at various stages of the anodization process used to produce the porous material. Such measurements were combined with studies of the photoluminescence spectra. These spectra were found to shift progressively to the blue as a function of anodization time. The luminescence intensity increases initially with anodization time, reaches a maximum and then decreases with further anodization. The surface state density, on the other hand, increases with anodization time from an initial value of about 2 x 10(exp 12)/sq cm surface to about 1013 sq cm for the anodized surface. This value is attained already after -2 min anodization and upon further anodization remains fairly constant. In parallel, the effective surface area increases by a factor of 10-30. This behavior is markedly different from the one observed previously for n-type porous Si.

Properties of nanostructures obtained by anodization of aluminum in phosphoric acid at moderate potentials

NASA Astrophysics Data System (ADS)

Zaraska, L.; Sulka, G. D.; Jaskuła, M.

2009-01-01

The influence of the process duration, anodizing potential and methanol addition on the structural features of porous anodic alumina formed in a 0.3 M H3PO4 solutions by twostep self-organized anodizing was investigated for potentials ranging from 100 to 170 V. The structural features of porous structures including pore diameter and interpore distance were evaluated from FE-SEM top-view images for samples anodized in the presence and absence of methanol. For the highest studied anodizing time and methanol volume fraction, an excellent agreement between experimental values of the interpore distance and theoretical predictions was observed. The pore arrangement regularity was analyzed for various electrolyte compositions and anodizing potentials. It was found that the regularity ratio of porous alumina increases linearly with increasing anodizing potential and time. The addition of methanol improves the quality of nanostructures and especially better uniformity of pore sizes is observed in the presence of the highest studied methanol content.

Surface treatments for aluminium alloys

NASA Astrophysics Data System (ADS)

Ardelean, M.; Lascău, S.; Ardelean, E.; Josan, A.

2018-01-01

Typically, in contact with the atmosphere, the aluminium surface is covered with an aluminium oxide layer, with a thickness of less than 1-2μm. Due to its low thickness, high porosity and low mechanical strength, this layer does not protect the metal from corrosion. Anodizing for protective and decorative purposes is the most common method of superficial oxidation processes and is carried out through anodic oxidation. The oxide films, resulted from anodizing, are porous, have a thickness of 20-50μm, and are heat-resistant, stable to water vapour and other corrosion agents. Hard anodizing complies with the same obtains principles as well as decorative and protective anodization. The difference is in that hard anodizing is achieved at low temperatures and high intensity of electric current. In the paper are presented the results of decorative and hard anodization for specimens made from several aluminium alloys in terms of the appearance of the specimens and of the thickness of the anodized.

Enhancement of dissolution rate of poorly-soluble active ingredients by supercritical fluid processes. Part I: Micronization of neat particles.

PubMed

Perrut, M; Jung, J; Leboeuf, F

2005-01-06

In this first of two articles, we discuss some issues surrounding the dissolution rate enhancement of poorly-soluble active ingredients micronized into nano-particles using several supercritical fluid particle design processes including rapid expansion of supercritical solutions (RESS), supercritical anti-solvent (SAS) and particles from gas-saturated solutions/suspensions (PGSS). Experimental results confirm that dissolution rates do not only depend on the surface area and particle size of the processed powder, but are greatly affected by other physico-chemical characteristics such as crystal morphology and wettability that may reduce the benefit of micronization.

Optimization of Aluminum Anodization Conditions for the Fabrication of Nanowires by Electrodeposition

NASA Technical Reports Server (NTRS)

Fucsko, Viola

2005-01-01

Anodized alumina nanotemplates have a variety of potential applications in the development of nanotechnology. Alumina nanotemplates are formed by oxidizing aluminum film in an electrolyte solution.During anodization, aluminum oxidizes, and, under the proper conditions, nanometer-sized pores develop. A series of experiments was conducted to determine the optimal conditions for anodization. Three-micrometer thick aluminum films on silicon and silicon oxide substrates were anodized using constant voltages of 13-25 V. 0.1-0.3M oxalic acid was used as the electrolyte. The anodization time was found to increase and the overshooting current decreased as both the voltage and the electrolyte concentrations were decreased. The samples were observed under a scanning electron microscope. Anodizing with 25V in 0.3M oxalic acid appears to be the best process conditions. The alumina nanotemplates are being used to fabricate nanowires by electrodeposition. The current-voltage characteristics of copper nanowires have also been studied.

Analysis of cadmium in undissolved anode materials of Mark-IV electro-refiner

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yoo, Tae-Sic; Fredrickson, G.L.; Vaden, D.

2013-07-01

The Mark-IV electro-refiner (Mk-IV ER) is a unit process in the FCF (Fuel Conditioning Facility), which is primarily assigned to treating the used driver fuels. Mk-IV ER contains an electrolyte/molten cadmium system for refining uranium electrochemically. Typically, the anode of the Mk-IV ER consists of the chopped sodium-bonded metallic driver fuels, which have been primarily U-10Zr binary fuels. Chemical analysis of the residual anode materials after electrorefining indicates that a small amount of cadmium is removed from the Mk-IV ER along with the undissolved anode materials. Investigation of chemical analysis data indicates that the amount of cadmium in the undissolvedmore » anode materials is strongly correlated with the anode rotation speeds and the residence time of the anode in the Mk-IV ER. Discussions are given to explain the prescribed correlation. (authors)« less

Effect of modeling factors on the dissolution-diffusion-convection process during CO2 geological storage in deep saline formations

NASA Astrophysics Data System (ADS)

Zhang, Wei

2013-06-01

It is well known that during CO2 geological storage, density-driven convective activity can significantly accelerate the dissolution of injected CO2 into water. This action could limit the escape of supercritical CO2 from the storage formation through vertical pathways such as fractures, faults and abandoned wells, consequently increasing permanence and security of storage. First, we investigated the effect of numerical perturbation caused by time and grid resolution and the convergence criteria on the dissolution-diffusion-convection (DDC) process. Then, using the model with appropriate spatial and temporal resolution, some uncertainty parameters investigated in our previous paper such as initial gas saturation and model boundaries, and other factors such as relative liquid permeability and porosity modification were used to examine their effects on the DDC process. Finally, we compared the effect of 2D and 3D models on the simulation of the DDC process. The above modeling results should contribute to clear understanding and accurate simulation of the DDC process, especially the onset of convective activity, and the CO2 dissolution rate during the convection-dominated stage.

Electrochemical deposited nickel nanowires: influence of deposition bath temperature on the morphology and physical properties

NASA Astrophysics Data System (ADS)

Sofiah, A. G. N.; Kananathan, J.; Samykano, M.; Ulakanathan, S.; Lah, N. A. C.; Harun, W. S. W.; Sudhakar, K.; Kadirgama, K.; Ngui, W. K.; Siregar, J. P.

2017-10-01

This paper investigates the influence of the electrolytic bath temperature on the morphology and physical properties of nickel (Ni) nanowires electrochemically deposited into the anodic alumina oxide porous membrane (AAO). The synthesis was performed using nickel sulfate hexahydrate (NiSO4.6H2O) and boric acid (H3BO3) as an electrolytic bath for the electrochemical deposition of Ni nanowires. During the experiment, the electrolyte bath temperature varied from 40°C, 80°C, and 120°C. After the electrochemical deposition process, AAO templates cleaned with distilled water preceding to dissolution in sodium hydroxide (NaOH) solution to obtain free-standing Ni nanowires. Field Emission Scanning Electron Microscopy (FESEM), Energy Dispersive Spectroscopy (EDX) and X-ray Diffraction (XRD) analysis were employed to characterize the morphology and physical properties of the synthesized Ni nanowires. Finding reveals the electrodeposition bath temperature significantly influences the morphology and physical properties of the synthesized Ni nanowires. Rougher surface texture, larger crystal size, and longer Ni nanowires obtained as the deposition bath temperature increased. From the physical properties properties analysis, it can be concluded that deposition bath temperature influence the physical properties of Ni nanowires.

In situ spectroscopy and spectroelectrochemistry of uranium in high-temperature alkali chloride molten salts.

PubMed

Polovov, Ilya B; Volkovich, Vladimir A; Charnock, John M; Kralj, Brett; Lewin, Robert G; Kinoshita, Hajime; May, Iain; Sharrad, Clint A

2008-09-01

Soluble uranium chloride species, in the oxidation states of III+, IV+, V+, and VI+, have been chemically generated in high-temperature alkali chloride melts. These reactions were monitored by in situ electronic absorption spectroscopy. In situ X-ray absorption spectroscopy of uranium(VI) in a molten LiCl-KCl eutectic was used to determine the immediate coordination environment about the uranium. The dominant species in the melt was [UO 2Cl 4] (2-). Further analysis of the extended X-ray absorption fine structure data and Raman spectroscopy of the melts quenched back to room temperature indicated the possibility of ordering beyond the first coordination sphere of [UO 2Cl 4] (2-). The electrolytic generation of uranium(III) in a molten LiCl-KCl eutectic was also investigated. Anodic dissolution of uranium metal was found to be more efficient at producing uranium(III) in high-temperature melts than the cathodic reduction of uranium(IV). These high-temperature electrolytic processes were studied by in situ electronic absorption spectroelectrochemistry, and we have also developed in situ X-ray absorption spectroelectrochemistry techniques to probe both the uranium oxidation state and the uranium coordination environment in these melts.

Investigating the structural transitions of proteins during dissolution by mass spectrometry.

PubMed

Gong, Xiaoyun; Xiong, Xingchuang; Qi, Lin; Fang, Xiang

2017-03-01

An appropriate solvent environment is essential for the implementation of biological functions of proteins. Interactions between protein residues and solvent molecules are of great importance for proteins to maintain their active structure and catalyze biochemical reactions. In this study, we investigated such interactions and studied the structural transitions of proteins during their dissolution process. Our previously developed technique, namely solvent assisted electric field induced desorption/ionization, was used for the dissolution and immediate ionization of proteins. Different solvents and proteins were involved in the investigation. According to the results, cytochrome c underwent significant unfolding during dissolution in the most commonly used NH 4 Ac buffer. The unfolding got more serious when the concentration of NH 4 Ac was further increased. Extending the dissolution time resulted in the re-folding of cytochrome c. In comparison, no unfolding was observed if cytochrome c was pre-dissolved in NH 4 Ac buffer and detected by nano-ESI. Furthermore, no unfolding was observed during the dissolution process of cytochrome c in water. Interactions between the residues of cytochrome c and the solute of NH 4 Ac might be the reason for the unfolding phenomenon. Similar unfolding phenomenon was observed on holo-myoglobin. However, the observed dissolution feature of insulin was different. No unfolding was observed on insulin during dissolution in NH 4 Ac buffers. Insulin underwent observable unfolding when water was used for dissolution. This might be due to the structural difference between different proteins. The obtained results in the present study furthered our insights into the interactions between proteins and the solvents during the phase transition of dissolution. Copyright © 2016 Elsevier B.V. All rights reserved.

Progress in Nano-Engineered Anodic Aluminum Oxide Membrane Development.

PubMed

Poinern, Gerrard Eddy Jai; Ali, Nurshahidah; Fawcett, Derek

2011-02-25

The anodization of aluminum is an electro-chemical process that changes the surface chemistry of the metal, via oxidation, to produce an anodic oxide layer. During this process a self organized, highly ordered array of cylindrical shaped pores can be produced with controllable pore diameters, periodicity and density distribution. This enables anodic aluminum oxide (AAO) membranes to be used as templates in a variety of nanotechnology applications without the need for expensive lithographical techniques. This review article is an overview of the current state of research on AAO membranes and the various applications of nanotechnology that use them in the manufacture of nano-materials and devices or incorporate them into specific applications such as biological/chemical sensors, nano-electronic devices, filter membranes and medical scaffolds for tissue engineering.

Progress in Nano-Engineered Anodic Aluminum Oxide Membrane Development

PubMed Central

Poinern, Gerrard Eddy Jai; Ali, Nurshahidah; Fawcett, Derek

2011-01-01

The anodization of aluminum is an electro-chemical process that changes the surface chemistry of the metal, via oxidation, to produce an anodic oxide layer. During this process a self organized, highly ordered array of cylindrical shaped pores can be produced with controllable pore diameters, periodicity and density distribution. This enables anodic aluminum oxide (AAO) membranes to be used as templates in a variety of nanotechnology applications without the need for expensive lithographical techniques. This review article is an overview of the current state of research on AAO membranes and the various applications of nanotechnology that use them in the manufacture of nano-materials and devices or incorporate them into specific applications such as biological/chemical sensors, nano-electronic devices, filter membranes and medical scaffolds for tissue engineering. PMID:28880002

Remediation of phosphate-contaminated water by electrocoagulation with aluminium, aluminium alloy and mild steel anodes.

PubMed

Vasudevan, Subramanyan; Lakshmi, Jothinathan; Jayaraj, Jeganathan; Sozhan, Ganapathy

2009-05-30

The present study provides an electrocoagulation process for the remediation of phosphate-contaminated water using aluminium, aluminium alloy and mild steel as the anodes and stainless steel as the cathode. The various parameters like effect of anode materials, effect of pH, concentration of phosphate, current density, temperature and co-existing ions, and so forth, and the adsorption capacity was evaluated using both Freundlich and Langmuir isotherm models. The adsorption of phosphate preferably fitting the Langmuir adsorption isotherm suggests monolayer coverage of adsorbed molecules. The results showed that the maximum removal efficiency of 99% was achieved with aluminium alloy anode at a current density of 0.2 A dm(-2), at a pH of 7.0. The adsorption process follows second-order kinetics.

Numerical simulation of the baking of porous anode carbon in a vertical flue ring furnace

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jacobsen, M.; Melaaen, M.C.

The interaction of pitch pyrolysis in porous anode carbon during heating and volatiles combustion in the flue gas channel has been analyzed to gain insight in the anode baking process. A two-dimensional geometry of a flue gas channel adjacent to a porous flue gas wall, packing coke, and an anode was used for studying the effect of heating rate on temperature gradients and internal gas pressure in the anodes. The mathematical model included porous heat and mass transfer, pitch pyrolysis, combustion of volatiles, radiation, and turbulent channel flow. The mathematical model was developed through source code modification of the computationalmore » fluid dynamics code FLUENT. The model was useful for studying the effects of heating rate, geometry, and anode properties.« less

Single-step preparation and deagglomeration of itraconazole microflakes by supercritical antisolvent method for dissolution enhancement.

PubMed

Sathigari, Sateesh Kumar; Ober, Courtney A; Sanganwar, Ganesh P; Gupta, Ram B; Babu, R Jayachandra

2011-07-01

Itraconazole (ITZ) microflakes were produced by supercritical antisolvent (SAS) method and simultaneously mixed with pharmaceutical excipients in a single step to prevent drug agglomeration. Simultaneous ITZ particle formation and mixing with fast-flo lactose (FFL) was performed in a high-pressure stirred vessel at 116 bar and 40 °C by the SAS-drug excipient mixing (SAS-DEM) method. The effects of stabilizers, such as sodium dodecyl sulfate and poloxamer 407 (PLX), on particle formation and drug dissolution were studied. Drug-excipient formulations were characterized for surface morphology, crystallinity, drug-excipient interactions, drug content uniformity, and drug dissolution rate. Mixture of drug microflakes and FFL formed by the SAS-DEM process shows that the process was successful in overcoming drug-drug agglomeration. PLX produced crystalline drug flakes in loose agglomerates with superior dissolution and flow properties even at higher drug loadings. Characterization studies confirmed the crystallinity of the drug and absence of chemical interactions during the SAS process. The dissolution of ITZ was substantially higher due to SAS and SAS-DEM processes; this improvement can be attributed to the microflake particle structures, effective deagglomeration, and wetting of the drug flakes with the excipients. Copyright © 2011 Wiley-Liss, Inc. and the American Pharmacists Association

Process for liquefying carbonaceous materials of high molecular weight and for separating liquefaction products

DOEpatents

Malek, John M.

1977-01-01

Process characterized by comprising successively a dissolution zone fed with carbonaceous solids and with a solvent, a high pressure hydrogenation zone provided with a source of hydrogen, and a hydrogenation products separation zone, wherein the improvement consists mainly in chemical upgrading of the liquidform products derived from the separation zone, and recycling a part of the upgraded products to the dissolution zone, this recycled part being of either positively acidic or positively basic properties for enhancing the dissolution - decomposition of base-acid structures present in the carbonaceous solid feed.

PROCESS OF DISSOLVING ZIRCONIUM ALLOYS

DOEpatents

Shor, R.S.; Vogler, S.

1958-01-21

A process is described for dissolving binary zirconium-uranium alloys where the uranium content is about 2%. In prior dissolution procedures for these alloys, an oxidizing agent was added to prevent the precipitation of uranium tetrafluoride. In the present method complete dissolution is accomplished without the use of the oxidizing agent by using only the stoichiometric amount or slight excess of HF required by the zirconium. The concentration of the acid may range from 2M to 10M and the dissolution is advatageously carried out at a temperature of 80 deg C.

Effects of Heat Treatment on the Discharge Behavior of Mg-6wt.%Al-1wt.%Sn Alloy as Anode For Magnesium-Air Batteries

NASA Astrophysics Data System (ADS)

Xiong, Hanqing; Zhu, Hualong; Luo, Jie; Yu, Kun; Shi, Chunli; Fang, Hongjie; Zhang, Yu

2017-05-01

Mg-6wt.%Al-1wt.%Sn alloys under different conditions are prepared. Primary magnesium-air batteries are assembled using such experimental Mg-Al-Sn alloys as anodes. The discharge behaviors of different alloys are investigated in 3.5 wt.% NaCl solution. The results show that the solution treatment can facilitate the homogeneous distribution of alloy elements and reduce the accumulation of discharge products. The magnesium-air battery based on the solution-treated Mg-Al-Sn anode presents higher operating voltage and more stable discharge process than those on the as-cast and the aged ones. Although the solution treatment cannot effectively improve the capacity density and the anodic efficiency of the experimental Mg-Al-Sn alloy, it is an effective approach to increasing the power and the energy density during discharge process. Especially at the applied current density of 30 mA cm-2 for 5 h, the solution-treated anode supplies 1.212 V average operating voltage, the anode energy density reaches 1527.2 mWhg-1, while the cast one is 1481.3 mWhg-1 and the aged one is 1478.8 mWhg-1.

Facile Fabrication of Ordered Anodized Aluminum Oxide Membranes with Controlled Pore Size by Improved Hard Anodization.

PubMed

Fan, Jiangxia; Zhu, Xinxin; Wang, Kunzhou; Chen, Xiaoyuan; Wang, Xinqing; Yan, Minhao; Ren, Yong

2018-05-01

We have fabricated highly ordered anodized aluminum oxide (AAO) membranes with different diameter through improved hard anodization (HA) at high temperature. This process can generate thick AAO membranes (30 μm) in a short anodizing time with high growth rate 20-60 μm h-1 which is much faster than that in traditional mild two-step anodization. We enlarged the AAO pore diameter by adjusting the voltage rise rate at the same time, which has a great influence on current density and temperature. The AAO pore diameter varies from 60-110 nm to 160-190 nm. The pore diameter (Dp) of the AAO prepared by this improved process is much larger than that prepared by HA (40-60 nm) when H2C2O4 as electrolyte. It can expand potential use of the AAO membranes such as for the template-based synthesis of nanowires or nanotubes with modulated diameters and also for practical separation technology. We also has used the AAO with different diameters prepared by this improved HA to fabricate Co nanowires and γ-Fe2O3 superparamagnetic nanorods.

Process for forming sulfuric acid

DOEpatents

Lu, Wen-Tong P.

1981-01-01

An improved electrode is disclosed for the anode in a sulfur cycle hydrogen generation process where sulfur dioxie is oxidized to form sulfuric acid at the anode. The active compound in the electrode is palladium, palladium oxide, an alloy of palladium, or a mixture thereof. The active compound may be deposited on a porous, stable, conductive substrate.

More About Arc-Welding Process for Making Carbon Nanotubes

NASA Technical Reports Server (NTRS)

Benavides, Jeanette M.; Leidecker, Henning

2005-01-01

High-quality batches of carbon nanotubes are produced at relatively low cost in a modified atmospheric-pressure electric-arc welding process that does not include the use of metal catalysts. What would normally be a welding rod and a weldment are replaced by an amorphous carbon anode rod and a wider, hollow graphite cathode rod. Both electrodes are water-cooled. The cathode is immersed in ice water to about 0.5 cm from the surface. The system is shielded from air by flowing helium during arcing. As the anode is consumed during arcing at 20 to 25 A, it is lowered to maintain it at an approximately constant distance above the cathode. The process causes carbon nanotubes to form on the lowest 5 cm of the anode. The arcing process is continued until the anode has been lowered to a specified height. The nanotube-containing material is then harvested. The additional information contained in the instant report consists mostly of illustrations of carbon nanotubes and a schematic diagram of the arc-welding setup, as modified for the production of carbon nanotubes.

Towards a molecular understanding of cellulose dissolution in ionic liquids: anion/cation effect, synergistic mechanism and physicochemical aspects.

PubMed

Li, Yao; Wang, Jianji; Liu, Xiaomin; Zhang, Suojiang

2018-05-07

Cellulose is one of the most abundant bio-renewable materials on the earth and its conversion to biofuels provides an appealing way to satisfy the increasing global energy demand. However, before carrying out the process of enzymolysis to glucose or polysaccharides, cellulose needs to be pretreated to overcome its recalcitrance. In recent years, a variety of ionic liquids (ILs) have been found to be effective solvents for cellulose, providing a new, feasible pretreatment strategy. A lot of experimental and computational studies have been carried out to investigate the dissolution mechanism. However, many details are not fully understood, which highlights the necessity to overview the current knowledge of cellulose dissolution and identify the research trend in the future. This perspective summarizes the mechanistic studies and microscopic insights of cellulose dissolution in ILs. Recent investigations of the synergistic effect of cations/anions and the distinctive structural changes of cellulose microfibril in ILs are also reviewed. Besides, understanding the factors controlling the dissolution process, such as the structure of anions/cations, viscosity of ILs, pretreatment temperature, heating rate, etc. , has been discussed from a structural and physicochemical viewpoint. At the end, the existing problems are discussed and future prospects are given. We hope this article would be helpful for deeper understanding of the cellulose dissolution process in ILs and the rational design of more efficient and recyclable ILs.

Towards a molecular understanding of cellulose dissolution in ionic liquids: anion/cation effect, synergistic mechanism and physicochemical aspects

PubMed Central

Li, Yao; Wang, Jianji

2018-01-01

Cellulose is one of the most abundant bio-renewable materials on the earth and its conversion to biofuels provides an appealing way to satisfy the increasing global energy demand. However, before carrying out the process of enzymolysis to glucose or polysaccharides, cellulose needs to be pretreated to overcome its recalcitrance. In recent years, a variety of ionic liquids (ILs) have been found to be effective solvents for cellulose, providing a new, feasible pretreatment strategy. A lot of experimental and computational studies have been carried out to investigate the dissolution mechanism. However, many details are not fully understood, which highlights the necessity to overview the current knowledge of cellulose dissolution and identify the research trend in the future. This perspective summarizes the mechanistic studies and microscopic insights of cellulose dissolution in ILs. Recent investigations of the synergistic effect of cations/anions and the distinctive structural changes of cellulose microfibril in ILs are also reviewed. Besides, understanding the factors controlling the dissolution process, such as the structure of anions/cations, viscosity of ILs, pretreatment temperature, heating rate, etc., has been discussed from a structural and physicochemical viewpoint. At the end, the existing problems are discussed and future prospects are given. We hope this article would be helpful for deeper understanding of the cellulose dissolution process in ILs and the rational design of more efficient and recyclable ILs. PMID:29780532

Development of In Vitro-In Vivo Correlation for Amorphous Solid Dispersion Immediate-Release Suvorexant Tablets and Application to Clinically Relevant Dissolution Specifications and In-Process Controls.

PubMed

Kesisoglou, Filippos; Hermans, Andre; Neu, Colleen; Yee, Ka Lai; Palcza, John; Miller, Jessica

2015-09-01

Although in vitro-in vivo correlations (IVIVCs) are commonly pursued for modified-release products, there are limited reports of successful IVIVCs for immediate-release (IR) formulations. This manuscript details the development of a Multiple Level C IVIVC for the amorphous solid dispersion formulation of suvorexant, a BCS class II compound, and its application to establishing dissolution specifications and in-process controls. Four different 40 mg batches were manufactured at different tablet hardnesses to produce distinct dissolution profiles. These batches were evaluated in a relative bioavailability clinical study in healthy volunteers. Although no differences were observed for the total exposure (AUC) of the different batches, a clear relationship between dissolution and Cmax was observed. A validated Multiple Level C IVIVC against Cmax was developed for the 10, 15, 20, 30, and 45 min dissolution time points and the tablet disintegration time. The relationship established between tablet tensile strength and dissolution was subsequently used to inform suitable tablet hardness ranges within acceptable Cmax limits. This is the first published report for a validated Multiple Level C IVIVC for an IR solid dispersion formulation demonstrating how this approach can facilitate Quality by Design in formulation development and help toward clinically relevant specifications and in-process controls. © 2015 Wiley Periodicals, Inc. and the American Pharmacists Association.

Preparation, characterization and dissolution of passive oxide film on the 400 series stainless steel surfaces

NASA Astrophysics Data System (ADS)

Sathyaseelan, V. S.; Rufus, A. L.; Chandramohan, P.; Subramanian, H.; Velmurugan, S.

2015-12-01

Full system decontamination of Primary Heat Transport (PHT) system of Pressurised Heavy Water Reactors (PHWRs) resulted in low decontamination factors (DF) on stainless steel (SS) surfaces. Hence, studies were carried out with 403 SS and 410 SS that are the material of construction of "End-Fitting body" and "End-Fitting Liner tubes". Three formulations were evaluated for the dissolution of passive films formed over these alloys viz., i) Two-step process consisting of oxidation and reduction reactions, ii) Dilute Chemical Decontamination (DCD) and iii) High Temperature Process. The two-step and high temperature processes could dissolve the oxide completely while the DCD process could remove only 60%. Various techniques like XRD, Raman spectroscopy and SEM-EDX were used for assessing the dissolution process. The two-step process is time consuming, laborious while the high temperature process is less time consuming and is recommended for SS decontamination.

Leakage current and charging/discharging processes in barrier-type anodic alumina thin films for use in metal-insulator-metal capacitors

NASA Astrophysics Data System (ADS)

Hourdakis, E.; Koutsoureli, M.; Papaioannou, G.; Nassiopoulou, A. G.

2018-06-01

Barrier-type anodic alumina thin films are interesting for use in high capacitance density metal-insulator-metal capacitors due to their excellent dielectric properties at small thickness. This thickness is easily controlled by the anodization voltage. In previous papers we studied the main parameters of interest of the Al/barrier-type anodic alumina/Al structure for use in RF applications and showed the great potential of barrier-type anodic alumina in this respect. In this paper, we investigated in detail charging/discharging processes and leakage current of the above dielectric material. Two different sets of metal-insulator-metal capacitors were studied, namely, with the top Al electrode being either e-gun deposited or sputtered. The dielectric constant of the barrier-type anodic alumina was found at 9.3. Low leakage current was observed in all samples studied. Furthermore, depending on the film thickness, field emission following the Fowler-Nordheim mechanism was observed above an applied electric field. Charging of the anodic dielectric was observed, occurring in the bulk of the anodic layer. The stored charge was of the order of few μC/cm2 and the calculated trap density ˜2 × 1018 states/cm3, the most probable origin of charge traps being, in our opinion, positive electrolyte ions trapped in the dielectric during anodization. We do not think that oxygen vacancies play an important role, since their existence would have a more important impact on the leakage current characteristics, such as resistive memory effects or significant changes during annealing, which were not observed. Finally, discharging characteristic times as high as 5 × 109 s were measured.

Pulse-reverse electrodeposition for mesoporous metal films: combination of hydrogen evolution assisted deposition and electrochemical dealloying.

PubMed

Cherevko, Serhiy; Kulyk, Nadiia; Chung, Chan-Hwa

2012-01-21

Hydrogen evolution assisted electrodeposition is a new bottom-up technique allowing the fast and simple synthesis of nanometals. Electrochemical dealloying is a top-down approach with the same purpose. In this work, we show that a combination of these two methods in sequence by pulse-reverse electrodeposition can be used to prepare high-surface-area nanostructured metals. Highly porous adherent platinum is obtained by the deposition of CuPt alloy during the cathodic cycles and the selective dissolution of copper during the anodic cycles. The convection created by the movement of the hydrogen bubbles increases the deposition rate and removes the dissolved copper ions from the diffusion layer, which ensures the deposition of a film with the same stoichiometry throughout the whole process. Due to the relatively high ratio of copper atoms on the surface in the as-deposited layer, it is proposed that the dealloying kinetics is significantly higher than that usually observed during the dealloying process in a model system. The proposed approach has several advantages over other methods, such as a very high growth rate and needlessness of any post-treatment processes. A detailed analysis of the effect of pulse-reverse waveform parameters on the properties of the films is presented. Mesoporous platinum with pores and ligaments having characteristic sizes of less than 10 nm, an equivalent surface area of up to ca. 220 m(2) cm(-3), and a roughness factor of more than 1000 is fabricated.

Gamma-insensitive optical sensor

DOEpatents

Kruger, Hans W.

1994-01-01

An ultra-violet/visible/infra-red gamma-insensitive gas avalanche focal plane array comprising a planar photocathode and a planar anode pad array separated by a gas-filled gap and across which is applied an electric potential. Electrons ejected from the photocathode are accelerated sufficiently between collisions with the gas molecules to ionize them, forming an electron avalanche. The gap acts like a proportional counter. The array of anode pad are mounted on the front of an anode plate and are connected to matching contact pads on the back of the anode via feed through wires. Connection of the anode to signal processing electronics is made from the contact pads using standard indium bump techniques, for example.

The effect of ethylene glycol on pore arrangement of anodic aluminium oxide prepared by hard anodization.

PubMed

Guo, Yang; Zhang, Li; Han, Mangui; Wang, Xin; Xie, Jianliang; Deng, Longjiang

2018-03-01

The influence of the addition of ethylene glycol (EG) on the pore self-ordering process in anodic aluminium oxide (AAO) membranes prepared by hard anodization (HA) was investigated. It was illustrated that EG has a substantial effect on the pore arrangement of AAO, and it was found that a smaller pore size can be obtained with an EG concentration reaching 20 wt% in aqueous electrolyte. The number of estimated defects of AAO increases significantly with an increase in EG concentration to 50 wt%. Excellent ordering of pores was realized when the samples were anodized in the 30 wt%-EG-containing aqueous electrolyte.

The effect of ethylene glycol on pore arrangement of anodic aluminium oxide prepared by hard anodization

PubMed Central

Zhang, Li; Han, Mangui; Wang, Xin; Xie, Jianliang; Deng, Longjiang

2018-01-01

The influence of the addition of ethylene glycol (EG) on the pore self-ordering process in anodic aluminium oxide (AAO) membranes prepared by hard anodization (HA) was investigated. It was illustrated that EG has a substantial effect on the pore arrangement of AAO, and it was found that a smaller pore size can be obtained with an EG concentration reaching 20 wt% in aqueous electrolyte. The number of estimated defects of AAO increases significantly with an increase in EG concentration to 50 wt%. Excellent ordering of pores was realized when the samples were anodized in the 30 wt%-EG-containing aqueous electrolyte. PMID:29657754

DOE Office of Scientific and Technical Information (OSTI.GOV)

Meng, Ling-Jian

A gamma ray detector apparatus comprises a solid state detector that includes a plurality of anode pixels and at least one cathode. The solid state detector is configured for receiving gamma rays during an interaction and inducing a signal in an anode pixel and in a cathode. An anode pixel readout circuit is coupled to the plurality of anode pixels and is configured to read out and process the induced signal in the anode pixel and provide triggering and addressing information. A waveform sampling circuit is coupled to the at least one cathode and configured to read out and processmore » the induced signal in the cathode and determine energy of the interaction, timing of the interaction, and depth of interaction.« less

Dissolution mechanism of calcium apatites in acids: A review of literature

PubMed Central

Dorozhkin, Sergey V

2012-01-01

Eight dissolution models of calcium apatites (both fluorapatite and hydroxyapatite) in acids were drawn from the published literature, analyzed and discussed. Major limitations and drawbacks of the models were conversed in details. The models were shown to deal with different aspects of apatite dissolution phenomenon and none of them was able to describe the dissolution process in general. Therefore, an attempt to combine the findings obtained by different researchers was performed which resulted in creation of the general description of apatite dissolution in acids. For this purpose, eight dissolution models were assumed to complement each other and provide the correct description of the specific aspects of apatite dissolution. The general description considers all possible dissolution stages involved and points out to some missing and unclear phenomena to be experimentally studied and verified in future. This creates a new methodological approach to investigate reaction mechanisms based on sets of affine data, obtained by various research groups under dissimilar experimental conditions. PMID:25237611

Dissolution corrosion of 316L austenitic stainless steels in contact with static liquid lead-bismuth eutectic (LBE) at 500 °C

NASA Astrophysics Data System (ADS)

Lambrinou, Konstantina; Charalampopoulou, Evangelia; Van der Donck, Tom; Delville, Rémi; Schryvers, Dominique

2017-07-01

This work addresses the dissolution corrosion behaviour of 316L austenitic stainless steels. For this purpose, solution-annealed and cold-deformed 316L steels were simultaneously exposed to oxygen-poor (<10-8 mass%) static liquid lead-bismuth eutectic (LBE) for 253-3282 h at 500 °C. Corrosion was consistently more severe for the cold-drawn steels than the solution-annealed steel, indicating the importance of the steel thermomechanical state. The thickness of the dissolution-affected zone was non-uniform, and sites of locally-enhanced dissolution were occasionally observed. The progress of LBE dissolution attack was promoted by the interplay of certain steel microstructural features (grain boundaries, deformation twin laths, precipitates) with the dissolution corrosion process. The identified dissolution mechanisms were selective leaching leading to steel ferritization, and non-selective leaching; the latter was mainly observed in the solution-annealed steel. The maximum corrosion rate decreased with exposure time and was found to be inversely proportional to the depth of dissolution attack.

New generation photoelectric converter structure optimization using nano-structured materials

NASA Astrophysics Data System (ADS)

Dronov, A.; Gavrilin, I.; Zheleznyakova, A.

2014-12-01

In present work the influence of anodizing process parameters on PAOT geometric parameters for optimizing and increasing ETA-cell efficiency was studied. During the calculations optimal geometrical parameters were obtained. Parameters such as anodizing current density, electrolyte composition and temperature, as well as the anodic oxidation process time were selected for this investigation. Using the optimized TiO2 photoelectrode layer with 3,6 μm porous layer thickness and pore diameter more than 80 nm the ETA-cell efficiency has been increased by 3 times comparing to not nanostructured TiO2 photoelectrode.

Universal Linear Scaling of Permeability and Time for Heterogeneous Fracture Dissolution

NASA Astrophysics Data System (ADS)

Wang, L.; Cardenas, M. B.

2017-12-01

Fractures are dynamically changing over geological time scale due to mechanical deformation and chemical reactions. However, the latter mechanism remains poorly understood with respect to the expanding fracture, which leads to a positively coupled flow and reactive transport processes, i.e., as a fracture expands, so does its permeability (k) and thus flow and reactive transport processes. To unravel this coupling, we consider a self-enhancing process that leads to fracture expansion caused by acidic fluid, i.e., CO2-saturated brine dissolving calcite fracture. We rigorously derive a theory, for the first time, showing that fracture permeability increases linearly with time [Wang and Cardenas, 2017]. To validate this theory, we resort to the direct simulation that solves the Navier-Stokes and Advection-Diffusion equations with a moving mesh according to the dynamic dissolution process in two-dimensional (2D) fractures. We find that k slowly increases first until the dissolution front breakthrough the outbound when we observe a rapid k increase, i.e., the linear time-dependence of k occurs. The theory agrees well with numerical observations across a broad range of Peclet and Damkohler numbers through homogeneous and heterogeneous 2D fractures. Moreover, the theory of linear scaling relationship between k and time matches well with experimental observations of three-dimensional (3D) fractures' dissolution. To further attest to our theory's universality for 3D heterogeneous fractures across a broad range of roughness and correlation length of aperture field, we develop a depth-averaged model that simulates the process-based reactive transport. The simulation results show that, regardless of a wide variety of dissolution patterns such as the presence of dissolution fingers and preferential dissolution paths, the linear scaling relationship between k and time holds. Our theory sheds light on predicting permeability evolution in many geological settings when the self-enhancing process is relevant. References: Wang, L., and M. B. Cardenas (2017), Linear permeability evolution of expanding conduits due to feedback between flow and fast phase change, Geophys. Res. Lett., 44(9), 4116-4123, doi: 10.1002/2017gl073161.

Anion-Dependent Potential Precycling Effects on Lithium Deposition/Dissolution Reaction Studied by an Electrochemical Quartz Crystal Microbalance.

PubMed

Smaran, Kumar Sai; Shibata, Sae; Omachi, Asami; Ohama, Ayano; Tomizawa, Eika; Kondo, Toshihiro

2017-10-19

The electrochemical quartz crystal microbalance technique was employed to study the initial stage of the electrodeposition and dissolution of lithium utilizing three kinds of electrolyte solutions such as LiPF 6 , LiTFSI, or LiFSI in tetraglyme. The native-SEI (solid-electrolyte interphase) formed by a potential prescan before lithium deposition/dissolution in all three solutions. Simultaneous additional SEI (add-SEI) deposition and its dissolution with lithium deposition and dissolution, respectively, were observed in LiPF 6 and LiTFSI. Conversely, the add-SEI dissolution with lithium deposition and its deposition with lithium dissolution were observed in LiFSI. Additional potential precycling resulted in the accumulation of a "pre-SEI" layer over the native-SEI layer in all of the solutions. With the pre-SEI, only lithium deposition/dissolution were significantly observed in LiTFSI and LiFSI. On the basis of the potential dependences of the mass and resistance changes, the anion-dependent effects of such a pre-SEI layer presence/absence on the lithium deposition/dissolution processes were discussed.

Multiscale Interfacial Strategy to Engineer Mixed Metal-Oxide Anodes toward Enhanced Cycling Efficiency.

PubMed

Ma, Yue; Tai, Cheuk-Wai; Li, Shaowen; Edström, Kristina; Wei, Bingqing

2018-06-13

Interconnected macro/mesoporous structures of mixed metal oxide (MMO) are developed on nickel foam as freestanding anodes for Li-ion batteries. The sustainable production is realized via a wet chemical etching process with bio-friendly chemicals. By means of divalent iron doping during an in situ recrystallization process, the as-developed MMO anodes exhibit enhanced levels of cycling efficiency. Furthermore, this atomic-scale modification coherently synergizes with the encapsulation layer across a micrometer scale. During this step, we develop a quasi-gel-state tri-copolymer, i.e., F127-resorcinol-melamine, as the N-doped carbon source to regulate the interfacial chemistry of the MMO electrodes. Electrochemical tests of the modified Fe x Ni 1- x O@NC-NiF anode in both half-cell and full-cell configurations unravel the favorable suppression of the irreversible capacity loss and satisfactory cyclability at the high rates. This study highlights a proof-of-concept modification strategy across multiple scales to govern the interfacial chemical process of the electrodes toward better reversibility.

Estimating the time for dissolution of spent fuel exposed to unlimited water

DOE Office of Scientific and Technical Information (OSTI.GOV)

Leider, H.R.; Nguyen, S.N.; Stout, R.B.

1991-12-01

The release of radionuclides from spent fuel cannot be precisely predicted at this point because a satisfactory dissolution model based on specific chemical processes is not yet available. However, preliminary results on the dissolution rate of UO{sub 2} and spent fuel as a function of temperature and water composition have recently been reported. This information, together with data on fragment size distribution of spent fuel, are used to estimate the dissolution response of spent fuel in excess flowing water within the framework of a simple model. In this model, the reaction/dissolution front advances linearly with time and geometry is preserved.more » This also estimates the dissolution rate of the bulk of the fission products and higher actinides, which are uniformly distributed in the UO{sub 2} matrix and are presumed to dissolve congruently. We have used a fuel fragment distribution actually observed to calculate the time for total dissolution of spent fuel. A worst-case estimate was also made using the initial (maximum) rate of dissolution to predict the total dissolution time. The time for total dissolution of centimeter size particles is estimated to be 5.5 {times} 10{sup 4} years at 25{degrees}C.« less

Mechanism of Urea Crystal Dissolution in Water from Molecular Dynamics Simulation.

PubMed

Anand, Abhinav; Patey, G N

2018-01-25

Molecular dynamics simulations are used to determine the mechanism of urea crystal dissolution in water under sink conditions. Crystals of cubic and tablet shapes are considered, and results are reported for four commonly used water models. The dissolution rates for different water models can differ considerably, but the overall dissolution mechanism remains the same. Urea dissolution occurs in three stages: a relatively fast initial stage, a slower intermediate stage, and a final stage. We show that the long intermediate stage is well described by classical rate laws, which assume that the dissolution rate is proportional to the active surface area. By carrying out simulations at different temperatures, we show that urea dissolution is an activated process, with an activation energy of ∼32 kJ mol -1 . Our simulations give no indication of a significant diffusion layer, and we conclude that the detachment of molecules from the crystal is the rate-determining step for dissolution. The results we report for urea are consistent with earlier observations for the dissolution of NaCl crystals. This suggests that the three-stage mechanism and classical rate laws might apply to the dissolution of other ionic and molecular crystals.

Nafion-coating of the electrodes improves the flow-stability of the Ag/SiO2/Ag2O electroosmotic pump.

PubMed

Shin, Woonsup; Zhu, Enhua; Nagarale, Rajaram Krishna; Kim, Chang Hwan; Lee, Jong Myung; Shin, Samuel Jaeho; Heller, Adam

2011-06-15

When a current or a voltage is applied across the ceramic membrane of the nongassing Ag/Ag(2)O-SiO(2)-Ag/Ag(2)O pump, protons produced in the anodic reaction 2Ag(s) + H(2)O → Ag(2)O(s) + 2H(+) + 2e(-) are driven to the cathode, where they are consumed by the reaction Ag(2)O(s) + H(2)O + 2e(-) → 2Ag(s) + 2 OH(-). The flow of water is induced by momentum transfer from the electric field-driven proton-sheet at the surface of the ceramic membrane. About 10(4) water molecules flowed per reacted electron. Because dissolved ions decrease the field at the membrane surface, the flow decreases upon increasing the ionic strength. For this reason Ag(+) ions introduced through the anodic reaction and by dissolution of Ag(2)O decrease the flow. Their accumulation is reduced by applying Nafion-films to the electrodes. The 20 μL min(-1) flow rate of 6 mm i.d. pumps with Nafion coated electrodes operate daily for 5 min at 1 V for 1 month, for 70 h when the pump is pulsed for 30 s every 30 min, and for 2 h when operating continuously.

Gas Evolution in Operating Lithium-Ion Batteries Studied In Situ by Neutron Imaging

PubMed Central

Michalak, Barbara; Sommer, Heino; Mannes, David; Kaestner, Anders; Brezesinski, Torsten; Janek, Jürgen

2015-01-01

Gas generation as a result of electrolyte decomposition is one of the major issues of high-performance rechargeable batteries. Here, we report the direct observation of gassing in operating lithium-ion batteries using neutron imaging. This technique can be used to obtain qualitative as well as quantitative information by applying a new analysis approach. Special emphasis is placed on high voltage LiNi0.5Mn1.5O4/graphite pouch cells. Continuous gassing due to oxidation and reduction of electrolyte solvents is observed. To separate gas evolution reactions occurring on the anode from those associated with the cathode interface and to gain more insight into the gassing behavior of LiNi0.5Mn1.5O4/graphite cells, neutron experiments were also conducted systematically on other cathode/anode combinations, including LiFePO4/graphite, LiNi0.5Mn1.5O4/Li4Ti5O12 and LiFePO4/Li4Ti5O12. In addition, the data were supported by gas pressure measurements. The results suggest that metal dissolution in the electrolyte and decomposition products resulting from the high potentials adversely affect the gas generation, particularly in the first charge cycle (i.e., during graphite solid-electrolyte interface layer formation). PMID:26496823

Mechanism of Zn Insertion into Nanostructured δ-MnO 2 : A Nonaqueous Rechargeable Zn Metal Battery

DOE Office of Scientific and Technical Information (OSTI.GOV)

Han, Sang-Don; Kim, Soojeong; Li, Dongguo

2017-05-19

Unlike the more established lithium-ion based energy storage chemistries, the complex intercalation chemistry of multivalent cations in a host lattice is not well understood, especially the relationship between the intercalating species solution chemistry and the prevalence and type of side reactions. Among multivalent metals, a promising model system can be based on nonaqueous Zn2+ ion chemistry. Several examples of these systems support the use of a Zn metal anode, and reversible intercalation cathodes have been reported. This study utilizes a combination of analytical tools to probe the chemistry of a nanostructured delta-MnO2 cathode in association with a nonaqueous acetonitrile-Zn(TFSI)(2) electrolytemore » and a Zn metal anode. As many of the issues related to understanding a multivalent battery relate to the electrolyte electrode interface, the high surface area of a nanostructured cathode provides a significant interface between the electrolyte and cathode host that maximizes the spectroscopic signal of any side reactions or minor mechanistic pathways. Numerous factors affecting capacity fade and issues associated with the second phase formation including Mn dissolution in heavily cycled Zn/delta-MnO2 cells are presented including dramatic mechanistic differences in the storage mechanism of this couple when compared to similar aqueous electrolytes are noted.« less

Effects of NaCl, pH, and Potential on the Static Creep Behavior of AA1100

NASA Astrophysics Data System (ADS)

Wan, Quanhe; Quesnel, David J.

2013-03-01

The creep rates of AA1100 are measured during exposure to a variety of aggressive environments. NaCl solutions of various concentrations have no influence on the steady-state creep behavior, producing creep rates comparable to those measured in lab air at room temperature. However, after an initial incubation period of steady strain rate, a dramatic increase of strain rate is observed on exposure to HCl solutions and NaOH solutions, as well as during cathodic polarization of specimens in NaCl solutions. Creep strain produces a continuous deformation and elongation of the sample surface that is comparable to slow strain rates at crack tips thought to control the kinetics of crack growth during stress corrosion cracking (SCC). In this experiment, we separate the strain and surface deformation from the complex geometry of the crack tip to better understand the processes at work. Based on this concept, two possible explanations for the environmental influences on creep strain rates are discussed relating to the anodic dissolution of the free surface and hydrogen influences on deformation mechanisms. Consistencies of pH dependence between corrosion creep and SCC at low pH prove a creep-involved SCC mechanism, while the discrepancies between corrosion creep behavior and previous SCC results at high pH indicate a rate-limit step change in the crack propagation of the SCC process.

Simulation results of influence of constricted arc column on anode deformation and melting pool swirl in vacuum arcs with AMF contacts

NASA Astrophysics Data System (ADS)

Wang, Lijun; Zhang, Xiao; Huang, Xiaolong; Jia, Shenli

2017-11-01

In the process of vacuum arc breaking, the energy injected into the anode will cause anode melting, evaporation, and deformation, resulting in the formation of the anode melting pool. The anode activities have great influence on the arc behavior. When the arc current is large enough, even the influence of axial magnetic field is considered, the arc column still is in contraction state, which means the arc burns only on a part of the electrode. In this paper, the model of anode melting pool deformation and rotation is used, and the model includes anode melting and solidification module, magneto-hydro-dynamic module of the anode melting pool, the volume of fraction method, and the current continuity equation. In this paper, the diffuse arc area is selected as 100%, 75%, and 50%, respectively. The anode temperature and deformation, the anode melting layer thickness, and the rotational velocity of the anode melting pool are obtained. The results show that when the current is at 17.5 kA (rms) and the diffuse arc area is 100%, the anode's maximum temperature is 1477 K and the crater depth is 0.83 mm. But when the diffuse arc areas are 75% and 50%, the anode's maximum temperatures reach 1500 K and 1761 K, and the crater depths reach 1.2 mm and 3 mm, respectively. Arc contraction will lead to more serious anode deformation. A similar result is obtained when the simulation current is 12.5 kA. Under the similar situation, the simulation results in the crater depth, the residual melt layer thickness, the rotational speed of the melting pool, and the maximum temperature of the anode at current zero are in good agreement with the experimental results.

Preparation and pharmaceutical characterization of amorphous cefdinir using spray-drying and SAS-process.

PubMed

Park, Junsung; Park, Hee Jun; Cho, Wonkyung; Cha, Kwang-Ho; Kang, Young-Shin; Hwang, Sung-Joo

2010-08-30

The aim of this study was to investigate the effects of micronization and amorphorization of cefdinir on solubility and dissolution rate. The amorphous samples were prepared by spray-drying (SD) and supercritical anti-solvent (SAS) process, respectively and their amorphous natures were confirmed by DSC, PXRD and FT-IR. Thermal gravimetric analysis was performed by TGA. SEM was used to investigate the morphology of particles and the processed particle had a spherical shape, while the unprocessed crystalline particle had a needle-like shape. The mean particle size and specific surface area were measured by dynamic light scattering (DLS) and BET, respectively. The DLS result showed that the SAS-processed particle was the smallest, followed by SD and the unprocessed cefdinir. The BET result was the same as DLS result in that the SAS-processed particle had the largest surface area. Therefore, the processed cefdinir, especially the SAS-processed particle, appeared to have enhanced apparent solubility, improved intrinsic dissolution rate and better drug release when compared with SD-processed and unprocessed crystalline cefdinir due not only to its amorphous nature, but also its reduced particle size. Conclusions were that the solubility and dissolution rate of crystalline cefdinir could be improved by physically modifying the particles using SD and SAS-process. Furthermore, SAS-process was a powerful methodology for improving the solubility and dissolution rate of cefdinir. Copyright 2010 Elsevier B.V. All rights reserved.

Preparation of Ti/IrO2 Anode with Low Iridium Content by Thermal Decomposition Process: Electrochemical removal of organic pollutants in water

NASA Astrophysics Data System (ADS)

Yaqub, Asim; Isa, Mohamed Hasnain; Ajab, Huma; Kutty, S. R. M.; Ezechi, Ezerie H.; Farooq, Robina

2018-04-01

In this study IrO2 (Iridium oxide) was coated onto a titanium plate anode from a dilute (50 mg/10 ml) IrCl3×H2O salt solution. Coating was done at high temperature (550∘C) using thermal decomposition. Surface morphology and characteristics of coated surface of Ti/IrO2 anode were examined by FESEM and XRD. The coated anode was applied for electrochemical removal of organic pollutants from synthetic water samples in 100 mL compartment of batch electrochemical cell. About 50% COD removal was obtained at anode prepared with low Ir content solution while 72% COD removal was obtained with anode prepared at high Ir content. Maximum COD removal was obtained at 10 mA/cm2 current density.

A Universal Strategy To Prepare Sulfur-Containing Polymer Composites with Desired Morphologies for Lithium-Sulfur Batteries.

PubMed

Zeng, Shao-Zhong; Zeng, Xierong; Tu, Wenxuan; Huang, Haitao; Yu, Liang; Yao, Yuechao; Jin, Nengzhi; Zhang, Qi; Zou, Jizhao

2018-06-19

Lithium-sulfur (Li-S) batteries are probably the most promising candidates for the next-generation batteries owing to their high energy density. However, Li-S batteries face severe technical problems where the dissolution of intermediate polysulfides is the biggest problem because it leads to the degradation of the cathode and the lithium anode, and finally the fast capacity decay. Compared with the composites of elemental sulfur and other matrices, sulfur-containing polymers (SCPs) have strong chemical bonds to sulfur and therefore show low dissolution of polysulfides. Unfortunately, most SCPs have very low electron conductivity and their morphologies can hardly be controlled, which undoubtedly depress the battery performances of SCPs. To overcome these two weaknesses of SCPs, a new strategy was developed for preparing SCP composites with enhanced conductivity and desired morphologies. With this strategy, macroporous SCP composites were successfully prepared from hierarchical porous carbon. The composites displayed discharge/charge capacities up to 1218/1139, 949/922, and 796/785 mA h g -1 at the current rates of 5, 10, and 15 C, respectively. Considering the universality of this strategy and the numerous morphologies of carbon materials, this strategy opens many opportunities for making carbon/SCP composites with novel morphologies.

Pulsed electrodeposition of two-dimensional Ag nanostructures on Au(111).

PubMed

Borissov, D; Tsekov, R; Freyland, W

2006-08-17

One-step pulsed potential electrodeposition of Ag on Au(111) in the underpotential deposition (UPD) region has been studied in 0.5 mM Ag2SO4 + 0.1 M H2SO4 aqueous electrolyte at various pulse durations from 0.2 to 500 ms. Evolution of the deposited Ag nanostructures was followed by in situ scanning tunneling microscopy (STM) and by measurement of the respective current transients. At short pulse durations a relatively high number density (4 x 10(11) cm(-2)) of two-dimensional Ag clusters with a narrow size and distance distribution is observed. They exhibit a remarkably high stability characterized by a dissolution potential which lies about 200 mV more anodically than the typical potential of Ag-(1 x 1) monolayer dissolution. To elucidate the underlying nucleation and growth mechanism, two models have been considered: two-dimensional lattice incorporation and a newly developed coupled diffusion-adsorption model. The first one yields a qualitative description of the current transients, whereas the second one is in nearly quantitative agreement with the experimental data. In this model the transformation of a Ag-(3 x 3) into a Ag-(1 x 1) structure indicated in the cyclic voltammogram (peaks at 520 vs 20 mV) is taken into account.

Moisture-Induced Spallation and Interfacial Hydrogen Embrittlement of Alumina Scales

NASA Technical Reports Server (NTRS)

Smialek, James L.

2005-01-01

Thermal expansion mismatch stresses and interfacial sulfur activity are the major factors producing primary Al2O3 scale spallation on high temperature alloys. However, moisture-induced delayed spallation appears as a secondary, but often dramatic, illustration of an additional mechanistic detail. A historical review of delayed failure of alumina scales and TBC s on superalloys is presented herein. Similarities with metallic phenomena suggest that hydrogen embrittlement from ambient humidity, resulting from the reaction Al+3H2O=Al(OH)3+3H(+)+3e(-), is the operative mechanism. This proposal was tested by standard cathodic hydrogen charging in 1N H2SO4, applied to Rene N5 pre-oxidized at 1150 C for 1000 1-hr cycles, and monitored by weight change, induced current, and microstructure. Here cathodic polarization at -2.0 V abruptly stripped mature Al2O3 scales at the oxide-metal interface. Anodic polarization at +2.0 V, however, produced alloy dissolution. Finally, with no applied voltage, the electrolyte alone produced neither scale spallation nor alloy dissolution. These experiments thus highlight the detrimental effects of hydrogen charging on alumina scale adhesion. It is proposed that interfacial hydrogen embrittlement is produced by moist air and is the root cause of both moisture-induced, delayed scale spallation and desktop TBC failures.

Membrane-less hybrid flow battery based on low-cost elements

NASA Astrophysics Data System (ADS)

Leung, P. K.; Martin, T.; Shah, A. A.; Mohamed, M. R.; Anderson, M. A.; Palma, J.

2017-02-01

The capital cost of conventional redox flow batteries is relatively high (>USD 200/kWh) due to the use of expensive active materials and ion-exchange membranes. This paper presents a membrane-less hybrid organic-inorganic flow battery based on the low-cost elements zinc (92.7% with the use of carbon felt electrodes. In the presence of a fully oxidized active species close to its solubility limit, dissolution of the deposited anode is relatively slow (<2.37 g h-1 cm-2) with an equivalent corrosion current density of <1.9 mA cm-2. In a parallel plate flow configuration, the resulting battery was charge-discharge cycled at 30 mA cm-2 with average coulombic and energy efficiencies of c.a. 71.8 and c.a. 42.0% over 20 cycles, respectively.

DTT-doped MWCNT coating for checking shuttle effect of lithium-sulfur battery

NASA Astrophysics Data System (ADS)

Xiaogang, Sun; Jie, Wang; Xu, Li; Wei, Chen

2018-01-01

In order to improve the rate and reversible capacity of lithium-sulfur (Li-S) battery, a reagent of dithiothreitol (DTT) was utilized to check the dissolution and shuttle of long-chain lithium polysulfides (LiPSs) by cutting the disulfide bond (-S-S- bonds) in them. The slurry of DTT-doped multi-walled carbon nanotubes (MWCNTs) was coated on the surface of sulfur cathode as a shield to slice the long-chain LiPSs to short-chain ones for checking the dissolution and migration of LiPSs to lithium anode. The morphology and structure of the electrodes were observed by scanning electron microscopy (SEM). The electrochemical performance was tested by galvanostatic charge-discharge, cyclic voltammetry (CV), and electrochemical impedance spectroscopy (EIS). The initial discharge capacity of S-DTT- carbon nanotube paper (CNTP) electrode reached 1670 and 949 mAh/g at 0.05 and 2 C respectively with a coulombic efficiency of over 99%. The electrode maintained a reversible specific capacity of 949 mAh/g after 45 cycles at 2 C. This suggested that the DTT-doped MWCNT coating can restrain shuttle effect and improve the rate and capacity of Li-S battery. The S-DTT-CNTP electrode not only accommodates the volume expansion but also provides stable electronics and ions channels.

Preliminary studies of the CHIM electrogeochemical method at the Kokomo Mine, Russell Gulch, Colorado

USGS Publications Warehouse

Smith, D.B.; Hoover, D.B.; Sanzolone, R.F.

1993-01-01

The CHIM electrogeochemical exploration technique was developed in the former Soviet Union about 20 years ago and is claimed to be effective in exploration for concealed mineral deposits that are not detectable by other geochemical or geophysical techniques. The method involves providing a high-voltage direct current to an anode and an array of special collector cathodes. Cations mobile in the electric field are collected at the cathodes and their concentrations determined. The U.S. Geological Survey started a study of the CHIM method by conducting tests over a precious- and base-metal-bearing quartz vein covered with 3 m of colluvial soil and weathered bedrock near the Kokomo Mine, Colorado. The tests show that the CHIM method gives better definition of the vein than conventional soil geochemistry based on a total-dissolution technique. The CHIM technique gives reproducible geochemical anomaly patterns, but the absolute concentrations depend on local site variability as well as temporal variations. Weak partial dissolutions of soils at the Kokomo Mine by an enzyme leach, a dilute acetic acid leach, and a dilute hydrochloric acid leach show results comparable to those from the CHIM method. This supports the idea that the CHIM technique is essentially a weak in-situ partial extraction involving only ions able to move in a weak electric field. ?? 1993.

Solution-processed MoS(x) as an efficient anode buffer layer in organic solar cells.

PubMed

Li, Xiaodong; Zhang, Wenjun; Wu, Yulei; Min, Chao; Fang, Junfeng

2013-09-25

We reported a facile solution-processed method to fabricate a MoSx anode buffer layer through thermal decomposition of (NH4)2MoS4. Organic solar cells (OSCs) based on in situ growth MoSx as the anode buffer layer showed impressive improvements, and the power conversion efficiency was higher than that of conventional PEDOT:PSS-based device. The MoSx films obtained at different temperatures and the corresponding device performance were systematically studied. The results indicated that both MoS3 and MoS2 were beneficial to the device performance. MoS3 could result in higher Voc, while MoS2 could lead to higher Jsc. Our results proved that, apart from MoO3, molybdenum sulfides and Mo(4+) were also promising candidates for the anode buffer materials in OSCs.

Effect of temperature on the anodizing process of aluminum alloy AA 5052

NASA Astrophysics Data System (ADS)

Theohari, S.; Kontogeorgou, Ch.

2013-11-01

The effect of temperature (10-40 °C) during the anodizing process of AA 5052 for 40 min in 175 g/L sulfuric acid solution at constant voltage (15 V) was studied in comparison with pure aluminum. The incorporated magnesium species in the barrier layer result in the further increase of the minimum current density passed during anodizing, as the temperature increases, by about 42% up to 30 °C and then by 12% up to 40 °C. Then during the anodizing process for 40 min a blocking effect on oxide film growth was gradually observed as the temperature increased until 30 °C. The results of EDAX analysis on thick films reveal that the mean amount of the magnesium species inside the film is about 50-70% less than that in the bulk alloy, while it is higher at certain locations adjacent to the film surface at 30 °C. The increase of anodizing temperature does not influence the porosity of thin films (formed for short times) on pure aluminum, while it reduces it on the alloy. At 40 °C the above mentioned blocking effects disappear. It means that the presence of magnesium species causes an impediment to the effect of temperature on iss, on the film thickness and on the porosity of thin films, only under conditions where film growth takes place without significant loss of the anodizing charge to side reactions.

Melt-Spun Fe-Sb Intermetallic Alloy Anode for Performance Enhanced Sodium-Ion Batteries.

PubMed

Edison, Eldho; Sreejith, Sivaramapanicker; Madhavi, Srinivasan

2017-11-15

Owing to the high theoretical sodiation capacities, intermetallic alloy anodes have attracted considerable interest as electrodes for next-generation sodium-ion batteries (SIBs). Here, we demonstrate the fabrication of intermetallic Fe-Sb alloy anode for SIBs via a high-throughput and industrially viable melt-spinning process. The earth-abundant and low-cost Fe-Sb-based alloy anode exhibits excellent cycling stability with nearly 466 mAh g -1 sodiation capacity at a specific current of 50 mA g -1 with 95% capacity retention after 80 cycles. Moreover, the alloy anode displayed outstanding rate performance with ∼300 mAh g -1 sodiation capacity at 1 A g -1 . The crystalline features of the melt-spun fibers aid in the exceptional electrochemical performance of the alloy anode. Further, the feasibility of the alloy anode for real-life applications was demonstrated in a sodium-ion full-cell configuration which could deliver a sodiation capacity of over 300 mAh g -1 (based on anode) at 50 mA g -1 with more than 99% Coulombic efficiency. The results further exhort the prospects of melt-spun alloy anodes to realize fully functional sodium-ion batteries.

High-absorptance high-emittance anodic coating

NASA Technical Reports Server (NTRS)

Le, Huong Giang (Inventor); Chesterfield, John L. (Inventor)

1998-01-01

A colored anodic coating for use on surfaces of substrates, e.g. aluminum substrates in which it is desirable to maintain a high solar absorptance (a) and a high infrared emittance (e), particularly in low earth orbit space environments. This anodic coating is preferably a dark colored coating, and even more preferably a black coating. This coating allows a touch temperature within an acceptable design range to preclude burning of an astronaut in case of contact, but also allows a solar radiation absorption in an amount such that an a/e ratio of unity is achieved. The coating of the invention comprises a first layer in the form of an acid anodized colored anodic layer for achieving a high solar absorptance and a second or high emittance layer in the form of a clear acid anodized layer for achieving a high emittance. The entire coating is quite thin, e.g. 1-2 mils and is quite stable in a hostile space environment of the type encountered in a low earth orbit. The coating is obtained by first creating the high emittance clear anodized coating on the metal surface followed by anodizing using a colored anodizing process.

High-absorptance high-emittance anodic coating

NASA Technical Reports Server (NTRS)

Le, Huong Giang (Inventor); Chesterfield, John L. (Inventor)

1999-01-01

A colored anodic coating for use on surfaces of substrates, e.g. aluminum substrates in which it is desirable to maintain a high solar absorptance (.alpha.) and a high infrared emittance (.epsilon.), particularly in low earth orbit space environments. This anodic coating is preferably a dark colored coating, and even more preferably a black coating. This coating allows a touch temperature within an acceptable design range to preclude burning of an astronaut in case of contact, but also allows a solar radiation absorption in an amount such that an .alpha./.epsilon. ratio of unity is achieved. The coating of the invention comprises a first layer in the form of an acid anodized colored anodic layer for achieving a high solar absorptance and a second or high emittance layer in the form of a clear acid anodized layer for achieving a high emittance. The entire coating is quite thin, e.g. 1-2 mils and is quite stable in a hostile space environment of the type encountered in a low earth orbit. The coating is obtained by first creating the high emittance clear anodized coating on the metal surface followed by anodizing using a colored anodizing process.

Electrolyte additives for lithium metal anodes and rechargeable lithium metal batteries: progresses and perspectives.

PubMed

Zhang, Heng; Eshetu, Gebrekidan Gebresilassie; Judez, Xabier; Li, Chunmei; Rodriguez-Martínez, Lide M; Armand, Michel

2018-02-14

Lithium metal (Li°) - based rechargeable batteries (LMBs), such as Li° anode vs. intercalation and/or conversion type cathode batteries, lithium-sulphur (Li-S), and lithium-oxygen (O2)/air (Li-O2/air) are becoming increasingly important for electrifying the modern transportation system, enabling sustainable mobility in the near future. Though some rechargeable LMBs batteries (e.g., Li°/LiFePO4 batteries from Bolloré Bluecar®, Li-S batteries from OXIS Energy and Sion Power) are already commercially viable in niche applications, their large-scale deployment is still hampered due to the existence of a number of formidable challenges, including lithium dendrite growth, electrolyte instability towards high voltage intercalation type cathode, poor electronic and ionic conductivities of sulphur (S8) and O2, as well as their corresponding reduction products (e.g., Li2S and Li2O), dissolution and shuttling of polysulphide (PS) intermediates etc. This ultimately results in short cycle life, low coulombic/energy efficiency, poor safety, and a high self-discharge rate. Among other mitigating strategies, the use of electrolyte additives is considered as one of the most economical, and effective approach for circumventing these dilemmas. Set out to offer an in-depth insight into the rapidly growing research on the account of electrolyte additives for rechargeable LMBs, this review presents an overview of the various functional additives, that are being applied in Li-anode/intercalation cathode-based, Li-S and Li-O2 batteries. This review is believed to assess the status quo of the research and thereby arouse new thoughts and opportunities, opening new avenues for the practical realization of these appealing devices. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Activity and Stability of Dispersed Multi Metallic Pt-based Catalysts for CO Tolerance in Proton Exchange Membrane Fuel Cell Anodes.

PubMed

Hassan, Ayaz; Ticianelli, Edson A

2018-01-01

Studies aiming at improving the activity and stability of dispersed W and Mo containing Pt catalysts for the CO tolerance in proton exchange membrane fuel cell (PEMFC) anodes are revised for the following catalyst systems: (1) a carbon supported PtMo electrocatalyst submitted to heat treatments; (2) Pt and PtMo nanoparticles deposited on carbon-supported molybdenum carbides (Mo2C/C); (3) ternary and quaternary materials formed by PtMoFe/C, PtMoRu/C and PtMoRuFe/C and; (4) Pt nanoparticles supported on tungsten carbide/carbon catalysts and its parallel evaluation with carbon supported PtW catalyst. The heat-treated (600 oC) Pt-Mo/C catalyst showed higher hydrogen oxidation activity in the absence and in the presence of CO and better stability, compared to all other Mo-containing catalysts. PtMoRuFe, PtMoFe, PtMoRu supported on carbon and Pt supported on Mo2C/C exhibited similar CO tolerances but better stability, as compared to as-prepared PtMo supported on carbon. Among the tungsten-based catalysts, tungsten carbide supported Pt catalyst showed reasonable performance and reliable stability in comparison to simple carbon supported PtW catalyst, though an uneven level of catalytic activity towards H2 oxidation in presence of CO is observed for the former as compared to Mo containing catalyst. However, a small dissolution of Mo, Ru, Fe and W from the anodes and their migration toward cathodes during the cell operation is observed. These results indicate that the fuel cell performance and stability has been improved but not yet totally resolved.

Effect of inflammatory conditions and H2O2 on bare and coated Ti-6Al-4V surfaces: Corrosion behavior, metal ion release and Ca-P formation under long-term immersion in DMEM

NASA Astrophysics Data System (ADS)

Höhn, Sarah; Virtanen, Sannakaisa

2015-12-01

The surface oxide film and calcium-phosphate (Ca-P) formation on Ti-6Al-4V during long-term immersion in biological environments play a decisive role for the biocompatibility of the implant. Hence, the aim of the study was to evaluate the corrosion resistance, metal ion release and Ca-P formation in DMEM under physiological conditions at pH values of 7.4 and in comparison under simulated inflammatory conditions with pH 5 and in presence of H2O2. Furthermore, the influence of the immersion conditions was investigated on different surface treatments: on bare Ti-6Al-4V, after anodization, and for TiO2 nanoparticle (NP) and hydroxyapatite (HA)-incorporated TiO2-NP coatings. In the absence of H2O2, the impedance response indicated a stable thin oxide film and Ca-P formation after 28 days or 56 days depending on the coating, while under inflammatory conditions the Ca-P formation on the surface is time-delayed and dissolution of the anodized oxide layer as well as selective etching of the β-phase and phase boundaries in case of the bare alloy occur. Electrochemical impedance spectroscopy (EIS), however, indicates a good general corrosion behavior in all cases. The quantities of Ti, Al and V released from the bare and coated Ti-6Al-4V alloy markedly increased with decreasing pH (pH ≤ 5). Although the rapid increase of metal release was observed for all samples at pH 5, the quantities were significantly higher for the bare and anodized alloy than after coating with TiO2-NP or HA.

In vitro study of electrodeposited fluoridated hydroxyapatite coating on G-II titanium with a nanostructured TiO2 interlayer.

PubMed

Lin, Jin-Shyong; Tsai, Tzung-Bau; Say, Wen-Ching; Chiu, Chun; Chen, Shih-Hsun

2017-04-04

Titanium and its alloys have been widely used as orthopedic and dental implants for several decades due to their superior mechanical properties, corrosion resistance and biocompatibility. Recently, many researches revealed that the hydroxyapatite coatings on biomedical materials can further improve their biocompatibility and bioactivity. However, hydroxyapatite coatings are easily decomposed, weakening the bonding between implants and bone tissues and resulting in a high dissolution rate in the biological environment. Prolonging the lifetime of hydroxyapatite in implants is valuable for improving postoperative quality. Hydroxyapatite is the primary inorganic component of bones and teeth. A suitable amount of fluoride ions would be beneficial for the formation of fluoridated hydroxyapatite, which can enhance bone-cell response and the acid resistance of enamel. In this study, G-II titanium substrate was anodized to form a TiO 2 interlayer with a nanotube structure. An electrolyte composed of fluoride, calcium and phosphorus ions was prepared for electroplating fluoridated hydroxyapatite (FHA) coatings onto anodized G-II titanium substrates at a constant voltage. The obtained coatings were examined for their microstructure, mechanical properties; moreover, the changes of apatite structure, surface morphology and corrosion resistance were further investigated after immersion in simulated body fluid (SBF) for a number of weeks. The results show that FHA coatings have a higher surface roughness and hardness than plain hydroxyapatite. After immersion in SBF, the FHA coatings induced the nucleation and growth of apatite on the surface and increased their crystallinity. In a potentiodynamic polarization test, FHA coatings exhibited a better anti-corrosion ability than bare G-II titanium substrate in SBF. Additionally, the anodized TiO 2 nanotube improved the adhesion and corrosion resistance of FHA as well.

Evaluation of correlation between dissolution rates of loxoprofen tablets and their surface morphology observed by scanning electron microscope and atomic force microscope.

PubMed

Yoshikawa, Shinichi; Murata, Ryo; Shida, Shigenari; Uwai, Koji; Suzuki, Tsuneyoshi; Katsumata, Shunji; Takeshita, Mitsuhiro

2010-01-01

We observed the surface morphological structures of 60 mg tablets of Loxonin, Loxot, and Lobu using scanning electron microscope (SEM) and atomic force microscope (AFM) to evaluate the dissolution rates. We found a significant difference among the initial dissolution rates of the three kinds of loxoprofen sodium tablets. Petal forms of different sizes were commonly observed on the surface of the Loxonin and Loxot tablets in which loxoprofen sodium was confirmed by measuring the energy-dispersible X-ray (EDX) spectrum of NaKalpha using SEM. However, a petal form was not observed on the surface of the Lobu tablet, indicating differences among the drug production processes. Surface area and particle size of the principal ingredient in tablets are important factors for dissolution rate. The mean size of the smallest fine particles constituting each tablet was also determined with AFM. There was a correlation between the initial dissolution rate and the mean size of the smallest particles in each tablet. Visualizing tablet surface morphology using SEM and AFM provides information on the drug production processes and initial dissolution rate, and is associated with the time course of pharmacological activities after tablet administration.

Iron dissolution of dust source materials during simulated acidic processing: the effect of sulfuric, acetic, and oxalic acids.

PubMed

Chen, Haihan; Grassian, Vicki H

2013-09-17

Atmospheric organic acids potentially display different capacities in iron (Fe) mobilization from atmospheric dust compared with inorganic acids, but few measurements have been made on this comparison. We report here a laboratory investigation of Fe mobilization of coal fly ash, a representative Fe-containing anthropogenic aerosol, and Arizona test dust, a reference source material for mineral dust, in pH 2 sulfuric acid, acetic acid, and oxalic acid, respectively. The effects of pH and solar radiation on Fe dissolution have also been explored. The relative capacities of these three acids in Fe dissolution are in the order of oxalic acid > sulfuric acid > acetic acid. Oxalate forms mononuclear bidentate ligand with surface Fe and promotes Fe dissolution to the greatest extent. Photolysis of Fe-oxalate complexes further enhances Fe dissolution with the concomitant degradation of oxalate. These results suggest that ligand-promoted dissolution of Fe may play a more significant role in mobilizing Fe from atmospheric dust compared with proton-assisted processing. The role of atmospheric organic acids should be taken into account in global-biogeochemical modeling to better access dissolved atmospheric Fe deposition flux at the ocean surface.

FY-16 Technology Gap Study Technical Report: Analysis of Undissolved Anode Materials of Mark-IV Electrorefiner

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yoo, Tae-Sic; Vaden, DeeEarl; Westphal, Brian Robert

2016-01-01

The Experimental Breeder Reactor II (EBR-II) is a sodium cooled fast reactor developed at Argonne National Laboratory (ANL). The used fuels from the EBR-II are currently being treated in the Fuel Conditioning Facility (FCF) at the Idaho National Laboratory (INL). The Mark IV (Mk-IV) electrorefiner (ER) is a unit process in the FCF, which is primarily assigned to treating the used driver fuels. The stainless steel anode baskets hold the chopped spent driver fuel segments. During electrorefining, the anode baskets are immersed into the electrolyte and the used fuel is dissolved electrochemically. Perforated sides and bottoms allow the flow ofmore » the electrolyte into and out of the anode baskets. The steel cathode is also immersed into the electrolyte and collects the reduced products. The active metal contents in the used fuel (e.g., Cs, Sr, lanthanides, Pu, etc.) reacts with uranium cations in the electrolyte and progressively reports to the electrolyte. Noble metals are mostly retained in the cladding hulls. Varying quantities of zirconium are retained in the cladding hulls depending on the operational conditions of the Mk-IV ER. The undissolved anode materials are removed from the anode baskets and stored for subsequent metal waste form processing. These undissolved materials typically include undissolved fuels, stainless steel cladding, and adhering electrolyte. A couple of hulls are retrieved for chemical analysis and used for estimating the composition of the entire undissolved anode materials. The mass balance attempt based on this practice of estimating the undissolved anode materials has been a challenge due to inherently high sampling errors associated with heterogeneous undissolved material compositions. Responding to the prescribed challenge, this report investigates chemical analysis data as a whole and finds noticeable trends in the compositions of undissolved anode material samples with respect to the mass of the whole undissolved anode materials. Based upon this discovery, an empirical model is proposed.« less

Development of a low-energy charged particle detector with on-anode ASIC for in-situ plasma measurement in the Earth's magnetosphere

NASA Astrophysics Data System (ADS)

Saito, M.; Saito, Y.; Mukai, T.; Asamura, K.

2009-06-01

The future magnetospheric exploration missions (ex. SCOPE: cross Scale COupling in the Plasma universE) aim to obtain electron 3D distribution function with very fast time resolution below 10 ms to investigate the electron dynamics that is regarded as pivotal in understanding the space plasma phenomena such as magnetic reconnection. This can be achieved by developing a new plasma detector system which is fast in signal processing with small size, light weight and low power consumption. The new detector system consists of stacked micro channel plates and a position sensitive multi-anode detector with on-anode analogue ASIC (Application Specific Integrated Circuits). Multi-anode system usually suffers from false signals caused by mainly two effects. One is the effect of the electrostatic crosstalk between the discrete anodes since our new detector consists of many adjacent anodes with small gaps to increase the detection areas. Our experimental results show that there exists electrostatic crosstalk effect of approximately 10% from the adjacent anodes. The effect of 10% electrostatic crosstalk can be effectively avoided by a suitable discrimination level of the signal processing circuit. Non negligible charge cloud size on the anode also causes false counts. Optimized ASIC for in-situ plasma measurement in the Earth's magnetosphere is under development. The initial electron cloud at the MCP output has angular divergence. Furthermore, space charge effects may broaden the size of the charge cloud. We have obtained the charge cloud size both experimentally and theoretically. Our test model detector shows expected performance that is explained by our studies above.

Surface Modification of Porous Titanium Granules for Improving Bioactivity.

PubMed

Karaji, Zahra Gorgin; Houshmand, Behzad; Faghihi, Shahab

The highly porous titanium granules are currently being used as bone substitute material and for bone tissue augmentation. However, they suffer from weak bone bonding ability. The aim of this study was to create a nanostructured surface oxide layer on irregularly shaped titanium granules to improve their bioactivity. This could be achieved using optimized electrochemical anodic oxidation (anodizing) and heat treatment processes. The anodizing process was done in an ethylene glycol-based electrolyte at an optimized condition of 60 V for 3 hours. The anodized granules were subsequently annealed at 450°C for 1 hour. Scanning electron microscopy (SEM), energy-dispersive x-ray spectroscopy (EDS), and x-ray diffraction (XRD) were used to characterize the surface structure and morphology of the granules. The in vitro bioactivity of the samples was evaluated by immersion of specimens in simulated body fluid (SBF) for 1, 2, and 3 weeks. The human osteoblastic sarcoma cell line, MG63, was used to evaluate cell viability on the samples using dimethylthiazol-diphenyl tetrazolium bromide (MTT) assay. The results demonstrated the formation of amorphous nanostructured titanium oxide after anodizing, which transformed to crystalline anatase and rutile phases upon heat treatment. After immersion in SBF, spherical aggregates of amorphous calcium phosphate were formed on the surface of the anodized sample, which turned into crystalline hydroxyapatite on the surface of the anodized annealed sample. No cytotoxicity was detected among the samples. It is suggested that anodic oxidation followed by heat treatment could be used as an effective surface treatment procedure to improve bioactivity of titanium granules implemented for bone tissue repair and augmentation.

Effect of CrO3 Sealing Time on Anodized A12024-T3

NASA Astrophysics Data System (ADS)

Korda, Akhmad A.; Hidayat, R. Z.

2016-08-01

The effect of CrO3 sealing time on anodized aluminum alloy has been investigated. A1 2024-T3 were used as substrate. Anodizing was carried out using chromic acid. CrO3 sealing was conducted in CrO3 solution for 30, 60, 90, 120 and 150 minutes. As comparison, other specimens were also prepared as anodized and boiled water sealing. Thickness of the coating was observed by optical microscope. Anodized and sealing layer was analyzed by X- ray diffraction. The hardness of as anodized, boiled water sealing and CrO3 sealing were compared. The highest hardness is achieved by CrO3 sealed specimen and followed by boiled water sealing and as anodized specimens. The longer the processes of CrO3 sealing the higher layer thickness and therefore the higher hardness of the oxide layer. The best resistance to electrolyte penetration is achieved by the CrO3 sealed specimen followed by boiled water sealed and as anodized specimens. The higher thickness of oxide layer, the higher the resistance against electrolyte penetration.

Alternative Anodes for the Electrolytic Reduction of Uranium Dioxide

NASA Astrophysics Data System (ADS)

Merwin, Augustus

Reprocessing of spent nuclear fuel is an essential step in closing the nuclear fuel cycle. In order to consume current stockpiles, ceramic uranium dioxide spent nuclear fuel will be subjected to an electrolytic reduction process. The current reduction process employs a platinum anode and a stainless steel alloy 316 cathode in a molten salt bath consisting of LiCl-2wt% Li 2O and occurs at 700°C. A major shortcoming of the existing process is the degradation of the platinum anode under the severely oxidizing conditions encountered during electrolytic reduction. This work investigates alternative anode materials for the electrolytic reduction of uranium oxide. The high temperature and extreme oxidizing conditions encountered in these studies necessitated a unique set of design constraints on the system. Thus, a customized experimental apparatus was designed and constructed. The electrochemical experiments were performed in an electrochemical reactor placed inside a furnace. This entire setup was housed inside a glove box, in order to maintain an inert atmosphere. This study investigates alternative anode materials through accelerated corrosion testing. Surface morphology was studied using scanning electron microscopy. Surface chemistry was characterized using energy dispersive spectroscopy and Raman spectroscopy. Electrochemical behavior of candidate materials was evaluated using potentiodynamic polarization characteristics. After narrowing the number of candidate electrode materials, ferrous stainless steel alloy 316, nickel based Inconel 718 and elemental tungsten were chosen for further investigation. Of these materials only tungsten was found to be sufficiently stable at the anodic potential required for electrolysis of uranium dioxide in molten salt. The tungsten anode and stainless steel alloy 316 cathode electrode system was studied at the required reduction potential for UO2 with varying lithium oxide concentrations. Electrochemical impedance spectroscopy showed mixed (kinetic and diffusion) control and an overall low impedance due to extreme corrosion. It was observed that tungsten is sufficiently stable in LiCl - 2wt% Li 2O at 700°C at the required anodic potential for the reduction of uranium oxide. This study identifies tungsten to be a superior anode material to platinum for the electrolytic reduction of uranium oxide, both in terms of superior corrosion behavior and reduced cost, and thus recommends that tungsten be further investigated as an alternative anode for the electrolytic reduction of uranium dioxide.

Effects of anodic oxidation parameters on a modified titanium surface.

PubMed

Park, Il Song; Lee, Min Ho; Bae, Tae Sung; Seol, Kyeong Won

2008-02-01

Anodic oxidation is an electrochemical treatment that can be used to control the thickness of an oxide layer formed on a titanium surface. This procedure has the advantage of allowing the ions contained in an electrolyte to deposit onto the oxide layer. The characteristics of a layer treated with anodic oxidation can vary according to the type and concentration of the electrolytes as well as the processing variables used during anodic oxidation. In this study, the constant electrolyte for anodic oxidation was a mixed solution containing 0.02 M DL-alpha-glycerophosphate disodium salt and 0.2M calcium acetate. Anodic oxidation was carried out at different voltages, current densities, and duration of anodic oxidation. The results showed that the current density and variation in the duration of anodic oxidation did not have a large effect on the change in the characteristics of the layer. On the other hand, the size of the micropores was increased with increasing voltage of anodic oxidation, and anatase and rutile phases were found to co-exist in the porous titanium dioxide layer. In addition, the thickness of the oxide layer on titanium and the characteristic of corrosion resistance increased with increasing voltage. The MTT test showed that the cell viability was increased considerably as a result of anodic oxidation. The anodizing voltage is an important parameter that determines the characteristics of the anodic oxide layer of titanium. (c) 2007 Wiley Periodicals, Inc.

Electrochemical studies on the performance of SS316L electrode in electrokinetics

NASA Astrophysics Data System (ADS)

Choi, Jeong-Hee; Maruthamuthu, Sundaram; Lee, Hyun-Goo; Ha, Tae-Hyun; Bae, Jeong-Hyo

2009-10-01

Organic and trace metal pollutants are removed by employing various electrodes in an electrokinetic (EK) process. Stainless steel was used either as an anode or a cathode by various investigators in electroremediation systems. In the present study, the role of SS316L as an anode and cathode in EK system was studied by the measurements of pH, conductivity of electrolyte, and potential of the anode and cathode at different current densities. The weight loss of the anode and cathode and the leaching of chromium, iron, and nickel at different current densities were measured and discussed with an electroosmosis process. The electrochemical behavior of SS316L electrode in neutral, acidic and alkaline pH in soil environment was studied by an electrochemical technique viz. polarization study. Surface analysis of SS316L after EK was done by XPS and SEM. The higher conductivity was noticed at anolyte when compared to catholyte. The weight loss of the anode was in the following order 0.615 > 0.307 > 0.123 mA/cm2 and the cathode corrosion rate was vice versa. Peroxide production was also noticed at the anolyte, which may encourage the degradation of the total organic content (TOC) in the soil. The OCP (open circuit potential) of SS316L was about +75 mV vs SCE in the soil extract; while adding acetic acid, the potential shifted to the positive side, to about +380 mV vs SCE. The breakdown potential and the range of passivation potential were higher in acetic acid added system when compared to other systems. Pitting was observed on both the anode and cathode within 48 h during the EK process. The present study concludes that SS is not a proper electrode material for the EK process.

Complexity of Products of Tungsten Corrosion: Comparison of the 3D Pourbaix Diagrams with the Experimental Data

NASA Astrophysics Data System (ADS)

Nave, Maryana I.; Kornev, Konstantin G.

2017-03-01

Tungsten is one of the most attractive metals in applications where materials are subject to high temperature and strong fields. However, in harsh aqueous environment, tungsten is prone to corrosion. Control of tungsten corrosion in aqueous solutions is a challenging task: as a transition metal, tungsten is able to produce a vast variety of oxides and hydrates. To reveal the thermodynamic pathway of corrosion at different conditions, the 3D Pourbaix diagrams relating the reduction potential, pH, and concentration of different tungsten-based compounds were constructed. These diagrams allow one to identify the most thermodynamically stable tungsten-based compounds. The 3D Pourbaix diagrams were used to explain different regimes of anodic dissolution of tungsten in aqueous solutions of potassium hydroxide.

Investigation of hexagonal boron nitride as an atomically thin corrosion passivation coating in aqueous solution.

PubMed

Zhang, Jing; Yang, Yingchao; Lou, Jun

2016-09-09

Hexagonal boron nitride (h-BN) atomic layers were utilized as a passivation coating in this study. A large-area continuous h-BN thin film was grown on nickel foil using a chemical vapor deposition method and then transferred onto sputtered copper as a corrosion passivation coating. The corrosion passivation performance in a Na2SO4 solution of bare and coated copper was investigated by electrochemical methods including cyclic voltammetry (CV), Tafel polarization and electrochemical impedance spectroscopy (EIS). CV and Tafel analysis indicate that the h-BN coating could effectively suppress the anodic dissolution of copper. The EIS fitting result suggests that defects are the dominant leakage source on h-BN films, and improved anti-corrosion performances could be achieved by further passivating these defects.

Electrochemical behavior of tube-fin assembly for an aluminum automotive condenser with improved corrosion resistance

NASA Astrophysics Data System (ADS)

Pech-Canul, M. A.; Guía-Tello, J. C.; Pech-Canul, M. I.; Aguilar, J. C.; Gorocica-Díaz, J. A.; Arana-Guillén, R.; Puch-Bleis, J.

An aluminum automotive condenser was designed to exhibit high corrosion resistance in the seawater acetic acid test (SWAAT) combining zinc coated microchannel tubes and fins made with AA4343/AA3003(Zn)/AA4343 brazing sheet. Electrochemical measurements in SWAAT solution were carried out under laboratory conditions using tube-fin assembly and individual fin and tube samples withdrawn from the condenser core. The aim was to gain information on the protective role of the zinc sacrificial layer and about changes in corrosion behavior as a function of immersion time. External corrosion of the tube-fin system was simulated by immersion of mini-core samples under open circuit conditions. The corrosion rate increased rapidly during the first 6 h and slowly afterwards. The short time behavior was related to the dissolution of the oxide film and fast dissolution of the outermost part of the zinc diffusion layer. With the aid of cross-sectional depth corrosion potential profiles, it was shown that as the sacrificial layer gets dissolved, the surface concentration of zinc decreases and the potential shifts to less negative values. The results of galvanic coupling of tube and fins in a mini-cell showed that the tube became the anode while the fins exhibited cathodic behavior. An evolution in the galvanic interaction was observed, due to the progressive dissolution of the sacrificial zinc layer. The difference of uncoupled potentials between tube and fins decreased from 71 mV to 32 mV after 84 h of galvanic coupling. At the end of such period there was still a part of the zinc sacrificial layer remaining which would serve for protection of the tube material for even longer periods and there were indications of slight corrosion in the fins.

The effect of grain boundary chemistry on Intergranular stress corrosion cracking of Ni-Cr-Fe alloys in 50 Pct NaOH at 140 °C

NASA Astrophysics Data System (ADS)

Sung, J. K.; Koch, J.; Angeliu, T.; Was, G. S.

1992-10-01

The role of chromium, carbon, chromium carbides, and phosphorus on the intergranular stress corrosion cracking (IGSCC) resistance of Ni-Cr-Fe alloys in 50 pct NaOH at 140 °C is studied using controlled-purity alloys. The effect of carbon is studied using heats in which the carbon level is varied between 0.002 and 0.063 wt pct while the Cr level is fixed at 16.8 wt pct. The effect of Cr is studied using alloys with Cr concentrations between 5 and 30 wt pct. The effect of grain boundary Cr and C together is studied by heat-treating the nominal alloy composition of Ni-16Cr-9Fe-0.035C, and the effect of P is studied using a high-purity, P-doped alloy and a carbon-containing, P-doped alloy. Constant extension rate tensile (CERT) results show that the crack depth increases with decreasing alloy Cr content and increasing alloy C content. Crack- ing severity also correlates inversely with thermal treatment time at 700 °C, during which the grain boundary Cr content rises and the grain boundary C content falls. Phosphorus is found to have a slightly beneficial effect on IG cracking susceptibility. Potentiodynamic polarization and potentiostatic current decay experiments confirm that Cr depletion or grain boundary C enhances the dissolution at the grain boundary. Results support a film rupture-anodic dissolution model in which Cr depletion or grain boundary C (independently or additively) enhances dissolution of nickel from the grain boundary region and leads to increased IG cracking.

Environmental fatigue of an Al-Li-Cu alloy. Part 2: Microscopic hydrogen cracking processes

NASA Technical Reports Server (NTRS)

Piascik, Robert S.; Gangloff, Richard P.

1992-01-01

Based on a fractographic analysis of fatigue crack propagation (FCP) in Al-Li-Cu alloy 2090 stressed in a variety of inert and embrittling environments, microscopic crack paths are identified and correlated with intrinsic da/dN-delta K kinetics. FCP rates in 2090 are accelerated by hydrogen producing environments (pure water vapor, moist air, and aqueous NaCl), as defined in Part 1. For these cases, subgrain boundary fatigue cracking (SGC) dominates for delta K values where the crack tip process zone, a significant fraction of the cyclic plastic zone, is sufficiently large to envelop 5 micron subgrains in the unrecrystallized microstructure. SGC may be due to strong hydrogen trapping at T1 precipitates concentrated at sub-boundaries. At low delta K, the plastic zone diameter is smaller than the subgrain size and FCP progresses along (100) planes due to either local lattice decohesion or aluminum-lithium hydride cracking. For inert environments (vacuum, helium, and oxygen), or at high delta K where the hydrogen effect on da/dN is small, FCP is along (111) slip planes; this mode does not transition with increasing delta K and plastic zone size. The SGC and (100) crystallographic cracking modes, and the governing influence of the crack tip process zone volume (delta K), support hydrogen embrittlement rather than a surface film rupture and anodic dissolution mechanism for environmental FCP. Multi-sloped log da/dN-log delta K behavior is produced by changes in process zone hydrogen-microstructure interactions, and not by purely micromechanical-microstructure interactions, in contradiction to microstructural distance-based fatigue models.

Gold-coated silicon nanowire-graphene core-shell composite film as a polymer binder-free anode for rechargeable lithium-ion batteries

NASA Astrophysics Data System (ADS)

Kim, Han-Jung; Lee, Sang Eon; Lee, Jihye; Jung, Joo-Yun; Lee, Eung-Sug; Choi, Jun-Hyuk; Jung, Jun-Ho; Oh, Minsub; Hyun, Seungmin; Choi, Dae-Geun

2014-07-01

We designed and fabricated a gold (Au)-coated silicon nanowires/graphene (Au-SiNWs/G) hybrid composite as a polymer binder-free anode for rechargeable lithium-ion batteries (LIBs). A large amount of SiNWs for LIB anode materials can be prepared by metal-assisted chemical etching (MaCE) process. The Au-SiNWs/G composite film on current collector was obtained by vacuum filtration using an anodic aluminum oxide (AAO) membrane and hot pressing method. Our experimental results show that the Au-SiNWs/G composite has a stable reversible capacity of about 1520 mA h/g which was maintained for 20 cycles. The Au-SiNWs/G composite anode showed much better cycling performance than SiNWs/polyvinylidene fluoride (PVDF)/Super-P, SiNWs/G composite, and pure SiNWs anodes. The improved electrochemical properties of the Au-SiNWs/G composite anode material is mainly ascribed to the composite's porous network structure.

Self-consistent modeling of self-organized patterns of spots on anodes of DC glow discharges

NASA Astrophysics Data System (ADS)

Bieniek, M. S.; Almeida, P. G. C.; Benilov, M. S.

2018-05-01

Self-organized patterns of spots on a flat metallic anode in a cylindrical glow discharge tube are simulated. A standard model of glow discharges is used, comprising conservation and transport equations for a single species of ion and electrons, written with the use of the drift-diffusion and local-field approximations, and the Poisson equation. Only processes in the near-anode region are considered and the computation domain is the region between the anode and the discharge column. Multiple solutions, existing in the same range of discharge current and describing modes with and without anode spots, are computed for the first time. A reversal of the local anode current density in the spots was found, i.e. mini-cathodes are formed inside the spots or, as one could say, anode spots operate as a unipolar glow discharge. The solutions do not fit into the conventional pattern of self-organization in bistable nonlinear dissipative systems; In particular, the modes are not joined by bifurcations.

Superhydrophobic NiTi shape memory alloy surfaces fabricated by anodization and surface mechanical attrition treatment

NASA Astrophysics Data System (ADS)

Ou, Shih-Fu; Wang, Kuang-Kuo; Hsu, Yen-Chi

2017-12-01

This paper describes the fabrication of superhydrophobic NiTi shape memory alloy (SMA) surfaces using an environmentally friendly method based on an economical anodizing process. Perfluorooctyltriethoxysilane was used to reduce the surface energy of the anodized surfaces. The wettability, morphology, composition, and microstructure of the surfaces were investigated by scanning electron microscopy, transmission electron microscopy, and x-ray photoelectron spectroscopy. The surface of the treated NiTi SMA exhibited superhydrophobicity, with a water contact angle of 150.6° and sliding angle of 8°. The anodic film on the NiTi SMA comprised of TiO2 and NiO, as well as traces of TiCl3. In addition, before the NiTi SMA was anodized, it underwent a surface mechanical attrition treatment to grain-refine its surface. This method efficiently enhanced the growth rate of the anodic oxide film, and improved the hydrophobic uniformity of the anodized NiTi-SMA-surface.

DNAPL remediation with in situ chemical oxidation using potassium permanganate - Part I. Mineralogy of Mn oxide and its dissolution in organic acids

NASA Astrophysics Data System (ADS)

Li, X. David; Schwartz, Franklin W.

2004-01-01

Previous studies on in situ chemical oxidation of trichloroethylene (TCE) with potassium permanganate indicated that the solid reaction product, Mn oxide, could reduce the permeability of the porous medium and impact the success of dense non-aqueous phase liquid (DNAPL) removal. In order to address the issue of permeability reduction caused by precipitation, this study investigated the mineralogy of Mn oxides and the possibilities of removing the solid precipitates by dissolution. The solid reaction product from the oxidation of TCE by permanganate is semi-amorphous potassium-rich birnessite, which has a layered mineral structure with an interlayer spacing of 7.3 Å. The chemical formula is K 0.854Mn 1.786O 4·1.55H 2O. It has a relatively small specific surface area at 23.6±0.82 m 2/g. Its point of zero charge (pzc) was measured as 3.7±0.4. This birnessite is a relatively active species and could participate in various reactions with existing organic and inorganic matter. The dissolution kinetics of Mn oxide was evaluated in batch experiments using solutions of citric acid, oxalic acid, and ethylenediaminetetraacetic acid (EDTA). Initial dissolution rates were determined to be 0.126 mM/m 2/h for citric acid, 1.35 mM/m 2/h for oxalic acid, and 5.176 mM/m 2/h for EDTA. These rates compare with 0.0025 mM/m 2/h for nitric acid at pH=2. Organic acids dissolve Mn oxide quickly. Reaction rates increase with acid concentration, as tested with citric acid. The dissolution mechanism likely involves proton and ligand-promoted dissolution and reductive dissolution. Citric and oxalic acid can induce ligand-promoted dissolution, while EDTA can induce ligand-promoted and reductive dissolutions. At low pH, proton-promoted dissolution seems to occur with all the acids tested, but this process is not dominant. Reductive dissolution appears to be the most effective process in dissolving the solid, followed by ligand-promoted dissolution. These experiments indicate the significant potential in using these organic acids to remove precipitates formed during the oxidation reaction.

Dissolution enhancement of gliclazide using pH change approach in presence of twelve stabilizers with various physico-chemical properties.

PubMed

Talari, Roya; Varshosaz, Jaleh; Mostafavi, Seyed Abolfazl; Nokhodchi, Ali

2009-01-01

The micronization using milling process to enhance dissolution rate is extremely inefficient due to a high energy input, and disruptions in the crystal lattice which can cause physical or chemical instability. Therefore, the aim of the present study is to use in situ micronization process through pH change method to produce micron-size gliclazide particles for fast dissolution hence better bioavailability. Gliclazide was recrystallized in presence of 12 different stabilizers and the effects of each stabilizer on micromeritic behaviors, morphology of microcrystals, dissolution rate and solid state of recrystallized drug particles were investigated. The results showed that recrystallized samples showed faster dissolution rate than untreated gliclazide particles and the fastest dissolution rate was observed for the samples recrystallized in presence of PEG 1500. Some of the recrystallized drug samples in presence of stabilizers dissolved 100% within the first 5 min showing at least 10 times greater dissolution rate than the dissolution rate of untreated gliclazide powders. Micromeritic studies showed that in situ micronization technique via pH change method is able to produce smaller particle size with a high surface area. The results also showed that the type of stabilizer had significant impact on morphology of recrystallized drug particles. The untreated gliclazide is rod or rectangular shape, whereas the crystals produced in presence of stabilizers, depending on the type of stabilizer, were very fine particles with irregular, cubic, rectangular, granular and spherical/modular shape. The results showed that crystallization of gliclazide in presence of stabilizers reduced the crystallinity of the samples as confirmed by XRPD and DSC results. In situ micronization of gliclazide through pH change method can successfully be used to produce micron-sized drug particles to enhance dissolution rate.

Removal of ammonium ion from produced waters in petroleum offshore exploitation by a batch single-stage electrolytic process.

PubMed

de Lima, Rosilda Maria Gomes; da Silva Wildhagen, Glória Regina; da Cunha, José Waldemar Silva Dias; Afonso, Julio Carlos

2009-01-30

This work describes a batch single-stage electrochemical process to remove quantitatively the ammonium ion from produced waters from petroleum exploration of the Campos' Basin, seeking to fulfil the directories of the National Brazilian Environmental Council. The anode was made out of titanium covered by a layer of RuO(2)+TiO(2) oxides (Dimensionally Stable Anode), whereas the cathode was made out of pure titanium. Anodic and cathodic compartments were separated by a membrane. The applied current varied from 0.3 to 1.5A. As the current increased NH(4)(+) removal was faster and pH was rapidly decreased to 3. The pH of the anodic compartment increased to approximately 10. When the current was 0.92 A chlorine evolution was observed after 40 min or only 15 min when that current was 1.50 A. In this voltage a deposit containing alkali-earth metal hydroxides/sulphates was formed on the membrane surface of the cathode side, thus suggesting a diffusion process from the anodic to the cathodic compartment. The maximum current applied to the cell must not exceed approximately 0.70 A in order to avoid chlorine evolution. Ammonia removal was over 99.9 wt% at 0.68 A in about 75 min.

Atomic force microscopy of atomic-scale ledges and etch pits formed during dissolution of quartz

NASA Technical Reports Server (NTRS)

Gratz, A. J.; Manne, S.; Hansma, P. K.

1991-01-01

The processes involved in the dissolution and growth of crystals are closely related. Atomic force microscopy (AFM) of faceted pits (called negative crystals) formed during quartz dissolution reveals subtle details of these underlying physical mechanisms for silicates. In imaging these surfaces, the AFM detected ledges less than 1 nm high that were spaced 10 to 90 nm apart. A dislocation pit, invisible to optical and scanning electron microscopy measurements and serving as a ledge source, was also imaged. These observations confirm the applicability of ledge-motion models to dissolution and growth of silicates; coupled with measurements of dissolution rate on facets, these methods provide a powerful tool for probing mineral surface kinetics.

Dewetting kinetics of metallic liquid films: Competition between unbalanced Young's force and dissolutive reaction

NASA Astrophysics Data System (ADS)

Lu, Gui; Lin, Lin; Hui, Sheng; Wang, Shuo-Lin; Wang, Xiao-Dong; Lee, Duu-Jong

2017-11-01

Dewetting kinetics of Al and NiAl metallic liquid films on NiAl (1 0 0) substrates was studied using molecular dynamics simulations. A new dewetting-spreading transitional behavior was observed for high temperature dewetting. The dewetting-spreading transition comes from the competition between unbalanced Young's force and dissolutive reaction. Without dissolutive reaction, liquid films keep dewetting, but immediately turn into spreading when the dissolutive reaction involved. The dissolutive reaction depends on the initial Ni atom contents rather than the contact areas of dewetting films. The far-away-from saturated Ni content is the main mechanism which accelerates the wetting and reverses the dewetting process at high temperatures.

Dissolution Processes at Step Edges of Calcite in Water Investigated by High-Speed Frequency Modulation Atomic Force Microscopy and Simulation.

PubMed

Miyata, Kazuki; Tracey, John; Miyazawa, Keisuke; Haapasilta, Ville; Spijker, Peter; Kawagoe, Yuta; Foster, Adam S; Tsukamoto, Katsuo; Fukuma, Takeshi

2017-07-12

The microscopic understanding of the crystal growth and dissolution processes have been greatly advanced by the direct imaging of nanoscale step flows by atomic force microscopy (AFM), optical interferometry, and X-ray microscopy. However, one of the most fundamental events that govern their kinetics, namely, atomistic events at the step edges, have not been well understood. In this study, we have developed high-speed frequency modulation AFM (FM-AFM) and enabled true atomic-resolution imaging in liquid at ∼1 s/frame, which is ∼50 times faster than the conventional FM-AFM. With the developed AFM, we have directly imaged subnanometer-scale surface structures around the moving step edges of calcite during its dissolution in water. The obtained images reveal that the transition region with typical width of a few nanometers is formed along the step edges. Building upon insight in previous studies, our simulations suggest that the transition region is most likely to be a Ca(OH) 2 monolayer formed as an intermediate state in the dissolution process. On the basis of this finding, we improve our understanding of the atomistic dissolution model of calcite in water. These results open up a wide range of future applications of the high-speed FM-AFM to the studies on various dynamic processes at solid-liquid interfaces with true atomic resolution.

Surface modification of graphene using HBC-6ImBr in solution-processed OLEDs

NASA Astrophysics Data System (ADS)

Cheng, Tsung-Chin; Ku, Ting-An; Huang, Kuo-You; Chou, Ang-Sheng; Chang, Po-Han; Chang, Chao-Chen; Yue, Cheng-Feng; Liu, Chia-Wei; Wang, Po-Han; Wong, Ken-Tsung; Wu, Chih-I.

2018-01-01

In this work, we report a simple method for solution-processed organic light emitting devices (OLEDs), where single-layer graphene acts as the anode and the hexa-peri-hexabenzocoronene exfoliating agent (HBC-6ImBr) provides surface modification. In SEM images, the PEDOT:PSS solution fully covered the graphene electrode after coating with HBC-6ImBr. The fabricated solution-processed OLEDs with a single-layer graphene anode showed outstanding brightness at 3182 cd/m2 and current efficiency up to 6 cd/A which is comparable to that of indium tin oxide films, and the OLED device brightness performance increases six times compared to tri-layer graphene treated with UV-Ozone at the same driving voltage. This method can be used in a wide variety of solution-processed organic optoelectronics on surface-modified graphene anodes.