Influence of the grain structure of yttria thin films on the hydrogen isotope permeation

Steel components are required in the infrastructure and the facilities of the hydrogen economy. The high hydrogen pressures in the hydrogen economy lead to embrittlement and surface corrosion of the steels. For the functionality of the facilities it is necessary to suppress the embrittlement and the surface corrosion of the steels by protective layers, e.g. ceramic thin films. With regard to fusion power plants ceramic thin films on the structural steel materials are also required. These thin films work as a tritium permeation barrier that is necessary to prevent the loss of the radioactive fuel inventory. Oxide thin films, e.g. Al₂O₃, Er₂O₃, and Y₂O₃, are promising candidates as tritium permeation barrier layers. In terms of the application in the first wall, this is especially true for yttrium due to its favorably short decay time after neutron activation compared to the other candidates. The Y₂O₃ layers with thicknesses of 0.5 μm–1 μm are deposited on both substrate sides by RF magnetron sputter deposition. Since the microstructure of the barrier layer plays an important role for the permeation reduction, layers with three different magnetron process modes and thus three different microstructures are prepared. After annealing the cubic crystal structure of all thin films is verified by X-ray diffraction and the different microstructures are investigated by scanning electron microscopy and transmission electron microscopy. The Y₂O₃ stoichiometry of all thin films and a chromium oxide material segregation at the interface are verified by analysis methods such as X-ray photoelectron spectroscopy. The permeation reduction factors of all thin films are determined in gas-driven deuterium permeation experiments. Corresponding to the three different microstructures, reduction factors of 25, 45, and 1100 are identified. Thus, the permeation reduction is strongly dependent on the Y₂O₃ microstructure. The measurement results suggest that a high density of grain boundaries leads to a high hydrogen permeation.     

Two-step sintering technique for enhancing mechanical and oxygen permeation properties of dual-phase oxygen transport membranes

The present work involved the application of a two-step sintering (TSS) technique for typical Ce_0.9Gd_0.1O_2?δ–La_0.6Sr_0.4Co_0.2Fe_0.8O_3–δ (GDC–LSCF) composites and its effect on the microstructure and resultantly mechanical and O₂-permeating properties. The samples obtained by conventional sintering (CS) performed at 1100, 1250, and 1400 °C for 3 h exhibited maximum flexural strength and hardness values of 142 MPa and 8.71 GPa, respectively. However, the application of a TSS procedure produced fine-grained microstructures with improved mechanical properties. In particular, with the use of a typical 1250/1200 TSS protocol, increases of approximately 31 % and 7% in the flexural strength and hardness values, respectively, were observed compared to those obtained using the CS method. Moreover, thick-film (～ 60 μm) GDC–LSCF membrane prepared by tape casting and the TSS technique showed remarkably 1.5–2 times higher oxygen permeation flux than membrane sintered by CS method. The results are discussed and explained in detail.     

Investigating the influence mechanism of hydrogen partial pressure on fracture toughness and fatigue life by in-situ hydrogen permeation

In this work, we investigate the influence mechanism of hydrogen partial pressure on fracture toughness and fatigue life of a high strength pipeline steel. Both fracture toughness test and fatigue life test are carried out under different hydrogen partial pressure. The experimental results show that with the increasing of hydrogen partial pressure, fracture toughness and fatigue life decrease and the decrease trends gradually flatten out. Hydrogen has a larger effect on fatigue life than fracture toughness. Only 3% hydrogen gas can cause a 67.7% decrease of fatigue life. The in-situ hydrogen permeation test is performed respectively in 2 MPa, 5 MPa and 8 MPa hydrogen partial pressure. With the increasing of hydrogen partial pressure, the increase trend of hydrogen permeation current gradually tends to be gentle, which indicates that the hydrogen atoms entering into the material gradually become saturated. This result can be used to clarify the influence mechanism of hydrogen partial pressure on fracture toughness and fatigue life.     

Synthesis at several length scales of zeolite A membranes using a continuous flow method

Zeolite A membranes were synthesized in the inner side of porous TiO₂ and α-Al₂O₃ tubular supports by a continuous method. The methodology was then used at several scales for preparing membranes on TiO₂ and α-Al₂O₃ supports with lengths of 6, 12 and 25 cm. Formation of an homogeneous zeolite film was confirmed by XRD and SEM in all supports. Single-gas permeation experiments (He, H₂, N₂ and n-C₃H₈) indicated that Knudsen diffusion was the predominant mechanism in both supports. All the synthesized membranes present high flux and moderate selectivity to water in water–ethanol mixtures.     

Hydrogen permeation in high strength steel under load in aqueous environment

Abstract

The hydrogen assisted cracking problem is one of the major causes of the failure occurring in the high strength steel structures used in various industries. In aqueous environment, hydrogen is generated by the hydrogen reduction reaction on the steel surface. With depletion of the high quality resources in oil and gas industry, the hydrogen assisted cracking problem becomes severe in sour environment, which contains high amount of H₂S. Understanding on the hydrogen permeation behaviour is crucial to deal properly with the hydrogen related problems since they are primarily determined by the hydrogen uptake and transport in the steel. The Devanathan–Stachurski method is widely used to evaluate electrochemically the hydrogen permeation behaviour. This method has been successfully used for the steel with no load. Under loading condition, this electrochemical test method has been modified to accommodate the externally applied load. However, the data require careful examination to validate the technical importance because of the stability and homogeneity of palladium layer coated on the steel surface under load. In this paper, the hydrogen permeation test method under loading condition will be reviewed for the high strength steels used in oil and gas industry. The factors affecting the hydrogen permeation in the high strength steel will be discussed in terms of the applied stress level and the sulphide film forming on the steel surface in sour environment.     

Hydrogen permeation across super‐thin membrane and the burning limitation in low‐temperature proton exchange membrane fuel cell

Hydrogen permeation across the membrane is unavoidable in proton exchange membrane fuel cells, especially for super‐thin membranes, which lowers the open‐circuit voltage and could even be a safety concern. In this paper, hydrogen permeation across two membranes (25‐um‐thick Nafion^® 211 and 18‐um‐thick reinforced composite membrane) are evaluated at various temperatures, relative humidity (RH), and gas pressure differences between the anode and cathode. The results indicate that the hydrogen permeation rate in both membranes increases almost exponentially with temperature and linearly with pressure differences. Compared with RH, the effects of temperature and pressure differences are more crucial to hydrogen permeability. However, the effect of RH on the hydrogen permeation is quite complicated. The permeability exhibits a minimum value at intermediate RH (approximately 40% RH) for both applied membranes. The permeability of Nafion^® 211 appears more sensitive to RH than that of reinforced composite membrane at elevated temperature. Copyright © 2013 John Wiley & Sons, Ltd.     

Mucoadhesive liposomes as ocular delivery system: physical,microbiological, and in vivo assessment

Background: Mucoadhesive drug delivery is a promising strategy to overcome ocular biopharmaceutical constraints. Objective and methods: Ciprofloxacin HCl-loaded reverse phase evaporation liposomes were coated with different concentrations and molecular weights of mucoadhesive biocompatible chitosan polymer to form chitosomes. This colloidal mucoadhesive system was evaluated in vitro and in vivo with respect to deliver the antibiotic to ocular surface. Results and conclusion: The results obtained pointed out that liposome coating process resulted in entrapment efficiency reduction and higher chitosan concentration, and molecular weight showed a more pronounced effect. No morphological differences between coated and uncoated liposomes were observed. Diffusion was the drug release mechanism from chitosomes. Concerning rheological behavior, pseudoplastic flow was characteristic to the prepared chitosomal dispersions. In addition, chitosan coating improved the ocular permeation of ciprofloxacin HCl. Microbiologically; this formulated system enhanced antimicrobial activity of ciprofloxacin HCl against both Gram-positive and Gram-negative bacteria. Moreover, this mucoadhesive system was able to inhibit the growth of Pseudomonas aeruginosa in rabbits' eyes for 24 hours when compared to the marketed preparation. In vivo bacterial conjunctivitis model elucidated that symptoms were controlled by the prolonged release formulation such as that done by the marketed product.     

A novel application of electrospinning technique in sublingual membrane: characterization,permeation and in vivo study

Isosorbide dinitrate–polyvinylpyrrolidone (ISDN–PVP) electrospinning fibers were formulated and explored as potentially sublingual membrane. The addition of polyethylene glycol (PEG) to the formulation improved flexibility and reduced fluffiness of the fiber mat. The scanning electron microscopy (SEM) demonstrated that the fibers tended to be cross-linking, and the crosslinking degree increased with the increase of PEG amount. The differential scanning calorimetry (DSC) indicated that ISDN existed in non-crystalline state in the fibers (except at the highest drug content). The infrared spectroscopy suggested that ISDN had better compatibility with the ingredients owing to the hydrogen bonding (or hydrophobic interactions). The fibers were highly favorable for the fabrication of sublingual membrane due to neutral pH, large folding endurance and rapid drug release (complete dissolution within 120 s). The permeation study of ISDN through both dialysis membrane (DM) and porcine sublingual mucosa (SM) were carried out. A significant relationship of drug permeation rate through DM and SM was built up, which indicated that DM could be used to partly simulate SM and assess formulation. The pharmacokinetic study in rats demonstrated that the electrospinning fiber membrane had a higher C_max and lower T_max compared to the reference preparation, and the relative bioavailability of the fiber membrane was 151.6%.     

浇筑式钢桥面铺装层推挤变形病害机理分析

以贵州省北盘江大桥钢桥面铺装层推挤变形病害为研究背景,采用凝胶渗透色谱法(GPC)和傅里叶变换红外光谱法(FTIR),从沥青分子尺度分析钢桥面铺装产生推挤变形的原因。分析结果表明:沥青老化并不是造成钢桥面铺装层推挤变形的主要原因;从现场调查可知,第2层粘层粘结能力的降低是造成钢桥面铺装层推挤变形病害的次要原因;通过级配分析发现,造成钢桥面铺装层推挤变形的主要原因是浇筑式沥青混合料(GA)级配偏细以及GA中集料颗粒的棱角性较差所致。     

In vitro comparative evaluation of monolayered multipolymeric films embedded with didanosine-loaded solid lipid nanoparticles: a potential buccal drug delivery system for ARV therapy

Drug delivery via the buccal route has emerged as a promising alternative to oral drug delivery. Didanosine (DDI) undergoes rapid degradation in the gastrointestinal tract, has a short half-life and low oral bioavailability, making DDI a suitable candidate for buccal delivery. Recent developments in buccal drug delivery show an increased interest toward nano-enabled delivery systems. The advantages of buccal drug delivery can be combined with that of nanoparticulate delivery systems to provide a superior delivery system. The aim of this study was to design and evaluate the preparation of novel nano-enabled films for buccal delivery of DDI. Solid lipid nanoparticles (SLNs) were prepared via hot homogenization followed by ultrasonication and were characterized before being incorporated into nano-enabled monolayered multipolymeric films (MMFs). Glyceryl tripalmitate with Poloxamer 188 was identified as most suitable for the preparation of DDI-loaded SLNs. SLNs with desired particle size (PS) (201?nm), polydispersity index (PDI) (0.168) and zeta potential (?18.8?mV) were incorporated into MMFs and characterized. Conventional and nano-enabled MMFs were prepared via solvent casting/evaporation using Eudragit RS100 and hydroxypropyl methylcellulose. Drug release from the nano-enabled films was found to be faster (56% versus 20% in first hour). Conventional MMFs exhibited higher mucoadhesion and mechanical strength than nano-enabled MMFs. SLNs did not adversely affect the steady state flux (71.63?±?13.54?µg/cm²?h versus 74.39?±?15.95?µg/cm²?h) thereby confirming the potential transbuccal delivery of DDI using nano-enabled MMFs. Nano-enabled buccal films for delivery of DDI can be successfully prepared, and these physico-mechanical studies serve as a platform for future formulation optimization work in this emerging field.