Search results for: deposition of liquid

Authors: Raimoana Frogier, Luc Girard, Pierre Bauduin, Diane Rebiscoul, Olivier Diat

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Nano-ions (NIs) are ionic species or clusters of nanometric size. Their low charge density and the delocalization of their charges give special properties to some of NIs belonging to chemical classes of polyoxometalates (POMs) or boron clusters. They have the particularity of interacting non-covalently with neutral hydrated surface or interfaces such as assemblies of surface-active molecules (micelles, vesicles, lyotropic liquid crystals), foam bubbles or emulsion droplets. This makes possible to classify those NIs in the Hofmeister series as superchaotropic ions. The mechanism of adsorption is complex, linked to the simultaneous dehydration of the ion and the molecule or supramolecular assembly with which it can interact, all with an enthalpic gain on the free energy of the system. This interaction process is reversible and is sufficiently pronounced to induce changes in molecular and supramolecular shape or conformation, phase transitions in the liquid phase, all at sub-millimolar ionic concentrations. This new property of some NIs opens up new possibilities for applications in fields as varied as biochemistry for solubilization, recovery of metals of interest by foams in the form of NIs... In order to better understand the physico-chemical mechanisms at the origin of this interaction, we use silicon wafers functionalized by non-ionic oligomers (polyethylene glycol chains or PEG) to study in situ by X-ray reflectivity this interaction of NIs with the grafted chains. This study carried out at ESRF (European Synchrotron Radiation Facility) and has shown that the adsorption of the NIs, such as POMs, has a very fast kinetics. Moreover the distribution of the NIs in the grafted PEG chain layer was quantify. These results are very encouraging and confirm what has been observed on soft interfaces such as micelles or foams. The possibility to play on the density, length and chemical nature of the grafted chains makes this system an ideal tool to provide kinetic and thermodynamic information to decipher the complex mechanisms at the origin of this adsorption.

Keywords: adsorption, nano-ions, solid-liquid interface, superchaotropicity

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Authors: Shoubhik Mandal, Debarghya Mallick, Abhishek Banerjee, R. Ganesan, P. S. Anil Kumar

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We report magnetotransport measurements in Bi₁Sb₁Te₁.₅Se₁.₅/RuCl₃ heterostructure nanodevices. Bi₁Sb₁Te₁.₅Se₁.₅ (BSTS) is a strong three-dimensional topological insulator (3D-TI) that hosts conducting topological surface states (TSS) enclosing an insulating bulk. α-RuCl₃ (namely, RuCl₃) is an anti-ferromagnet that is predicted to behave as a Kitaev-like quantum spin liquid carrying Majorana excitations. Temperature (T)-dependent resistivity measurements show the interplay between parallel bulk and surface transport channels. At T < 150 K, surface state transport dominates over bulk transport. Multi-channel weak anti-localization (WAL) is observed, as a sharp cusp in the magnetoconductivity, indicating strong spin-orbit coupling. The presence of top and bottom topological surface states (TSS), including a pair of electrically coupled Rashba surface states (RSS), are indicated. Non-linear Hall effect, explained by a two-band model, further supports this interpretation. Finally, a low-T logarithmic resistance upturn is analyzed using the Lu-Shen model, supporting the presence of gapless surface states with a π Berry phase.

Keywords: topological materials, electrical transport, Lu-Shen model, quantum spin liquid

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Authors: Sabah El-Sawalhi, Elie Fayad, Roula M. Abdel-Massih

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Ilex paraguariensis (Yerba Mate) is a medium to large tree commonly consumed by South Americans. Its leaves and stems are associated with different biological activities. The purpose of this study was to evaluate the antibacterial activity of Yerba Mate against Gram-positive and Gram-negative bacterial strains and its action against some resistant bacteria with different resistance profiles. Yerba Mate aqueous extracts were prepared at 70°C for 2 hrs, and the microdilution method was used to determine the minimum inhibitory concentration (MIC). Gram-positive bacteria exhibited a stronger antibacterial activity (MIC ranged between 0.468 mg/mL and 15 mg/mL) than Gram-negative bacteria. Yerba Mate was also extracted with acetone: water (1:1) and then further sub-fractionated with hexane, chloroform, and ethyl acetate. MIC values against Staphylococcus aureus ranged from 0.78 to 2.5 mg/ml for the chloroform fraction, from 1.56 to 3.75 mg/ml for the ethyl acetate fraction, and 0.78 to 1.87 mg/ml for the water fraction. The water fraction also exhibited antibacterial activity against Salmonella species (MIC ranged from 1.56 mg/ml to 3.12 mg/ml). The water fraction exhibited the highest antibacterial activity among all the fractions obtained. More studies are needed to determine the molecule or molecules responsible for this activity.

Keywords: antibacterial activity, bacterial resistance, minimum inhibitory concentration, yerba mate

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Authors: Niki K. Burns, James R. Pearson, Paul G. Stevenson, Xavier A. Conlan

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In Australian state Victoria, synthetic cannabinoids have recently been made illegal under an amendment to the drugs, poisons and controlled substances act 1981. Identification of synthetic cannabinoids in popular brands of ‘incense’ and ‘potpourri’ has been a difficult and challenging task due to the sample complexity and changes observed in the chemical composition of the cannabinoids of interest. This study has developed analytical methodology for the targeted extraction and determination of synthetic cannabinoids available pre-ban. A simple solvent extraction and solid phase extraction methodology was developed that selectively extracted the cannabinoid of interest. High performance liquid chromatography coupled with UV‐visible and chemiluminescence detection (acidic potassium permanganate and tris (2,2‐bipyridine) ruthenium(III)) were used to interrogate the synthetic cannabinoid products. Mass spectrometry and nuclear magnetic resonance spectroscopy were used for structural elucidation of the synthetic cannabinoids. The tris(2,2‐bipyridine)ruthenium(III) detection was found to offer better sensitivity than the permanganate based reagents. In twelve different brands of herbal incense, cannabinoids were extracted and identified including UR‐144, XLR 11, AM2201, 5‐F‐AKB48 and A796‐260.

Keywords: electrospray mass spectrometry, high performance liquid chromatography, solid phase extraction, synthetic cannabinoids

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Authors: Farusil Najeeb Mullaveettil, Rolanas Dauksevicius

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Cellular structures produced by additive manufacturing have earned wide research attention due to their unique specific strength and energy absorption potentiality. The literature review concludes that pattern type and density are vital parameters that affect the mechanical properties of parts formed by additive manufacturing techniques and have an influence on printing time and material consumption. Fused deposition modeling technique (FDM) is used here to produce Polyvinylidene fluoride (PVDF) parts. In this work, patterns are based on triply periodic minimal surfaces (TPMS) produced by PVDF-based filaments using the FDM technique. PVDF homopolymer filament Fluorinar-H™ and PVDF copolymer filament Fluorinar-C™ are printed with three types of TPMS patterns. The patterns printed are Gyroid, Schwartz diamond, and Schwartz primitive. Tensile, flexural, and compression tests under quasi-static loading conditions are performed in compliance with ISO standards. The investigation elucidates the deformation mechanisms and a study that establishes a relationship between the printed and nominal specimens' dimensional accuracy. In comparison to the examined TPMS pattern, Schwartz diamond showed a higher relative elastic modulus and strength than the other patterns in tensile loading, and the Gyroid pattern showed the highest mechanical characteristics in flexural loading. The concluded results could be utilized to produce informed cellular designs for biomedical and mechanical applications.

Keywords: additive manufacturing, FDM, PVDF, gyroid, schwartz primitive, schwartz diamond, TPMS, tensile, flexural

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Authors: Jinliang Yuan, Jong-Sung Yu, Bengt Sundén

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A computational fluid dynamics (CFD) model is developed for rechargeable non-aqueous electrolyte lithium-air batteries with a partial opening for oxygen supply to the cathode. Multi-phase transport phenomena occurred in the battery are considered, including dissolved lithium ions and oxygen gas in the liquid electrolyte, solid-phase electron transfer in the porous functional materials and liquid-phase charge transport in the electrolyte. These transport processes are coupled with the electrochemical reactions at the active surfaces, and effects of discharge reaction-generated solid Li2O2 on the transport properties and the electrochemical reaction rate are evaluated and implemented in the model. The predicted results are discussed and analyzed in terms of the spatial and transient distribution of various parameters, such as local oxygen concentration, reaction rate, variable solid Li2O2 volume fraction and porosity, as well as the effective diffusion coefficients. It is found that the effect of the solid Li2O2 product deposited at the solid active surfaces is significant on the transport phenomena and the overall battery performance.

Keywords: Computational Fluid Dynamics (CFD), modeling, multi-phase, transport phenomena, lithium-air battery

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Authors: Ahmad Shanei, Mohammad Mahdi Shanei

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When a liquid is irradiated with high intensities (> 1 W) and low frequencies (≤ 1 MHz) ultrasound, acoustic cavitation occurs. Acoustic cavitation generates free radicals from the breakdown of water and other molecules. The existence of particles in liquid provide nucleation sites for cavitation bubbles and lead to decrease the ultrasonic intensity threshold needed for cavitation onset. The study was designed to measure hydroxyl radicals in terephthalic acid solutions containing 30 nm gold nanoparticles in a near field of a 1 MHz sonotherapy probe. The effect of ultrasound irradiation parameters containing mode of sonication and ultrasound intensity in hydroxyl radicals production have been investigated by the spectrofluorometry method. Recorded fluorescence signal in terephthalic acid solution containing gold nanoparticles was higher than the terephthalic acid solution without gold nanoparticles. Also, the results showed that any increase in intensity of the sonication would be associated with an increase in the fluorescence intensity. Acoustic cavitation in the presence of gold nanoparticles has been introduced as a way for improving therapeutic effects on the tumors. Also, the terephthalic acid dosimetry is suitable for detecting and quantifying free hydroxyl radicals as a criterion of cavitation production over a range of condition in medical ultrasound fields.

Keywords: acoustic cavitation, gold nanoparticle, chemical dosimetry, terephthalic acid

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Authors: Adesoji Sodeinde

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Analytical derivatives has recently undergone an explosive growth in areas of separation techniques, likewise in detectability of certain compound/concentrated ions. The gloomy and depressing scenario which charaterized the application of analytical derivatives in areas of water analysis, water cycle and the environment should not be allowed to continue unabated. Due to technological advancement in various chemical/biochemical analysis separation techniques is widely used in areas of medical, forensic and to measure and assesses environment and social-economic impact of alternative control strategies. This technological improvement was dully established in the area of comparison between certain separation/detection techniques to bring about vital result in forensic[as Gas liquid chromatography reveals the evidence given in court of law during prosecution of drunk drivers]. The water quality analysis,pH and water temperature analysis can be performed in the field, the concentration of dissolved free amino-acid [DFAA] can also be detected through separation techniques. Some important derivatives/ions used in separation technique. Water analysis : Total water hardness [EDTA to determine ca and mg ions]. Gas liquid chromatography : innovative gas such as helium [He] or nitrogen [N] Water cycle : Animal bone charcoal,activated carbon and ultraviolet light [U.V light].

Keywords: analytical derivative, environment, water analysis, chemical/biochemical analysis

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Authors: C. Jouhar, B. Rajesh Kamath, M. K. Veeraiah, M. Z. Kurian

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Since long time ago, petroleum-based mineral oils have been used for liquid insulation in high voltage equipments. Mineral oils are widely used as insulation for transmission and distribution power transformers, capacitors and other high voltage equipment. Petroleum-based insulating oils have excellent dielectric properties such as high electric field strength, low dielectric losses and good long-term performance. Due to environmental consideration, an attempt to search the alternate liquid insulation is required. The influence of particles on the voltage breakdown in insulating oil and other liquids has been recognized for many years. Particles influence both AC and DC voltage breakdown in insulating oil. Experiments are conducted under AC voltage. The breakdown process starts with a microscopic bubble, an area of large distance where ions or electrons initiate avalanches. Insulating liquids drive their dielectric strength from the much higher density compare to gases. Experiments are carried out under High Voltage AC (HVAC) in different types of oils namely castor oil, vegetable oil and mineral oil. The Breakdown Voltage (BDV) with presence of moisture and particle contamination in different types of oils is studied. The BDV of vegetable oil is better when compared to other oils without contamination. The BDV of mineral oil is better when compared to other types of oils in presence of contamination.

Keywords: breakdown voltage, high voltage AC, insulating oil, oil breakdown

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Authors: Hassan Hussin Zwida

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The liquified LPG (Liquefied Petroleum Gas) drying system at the Complex is designed to remove water and mercaptans from the LPG stream. Upon saturation of the desiccant beds, a regeneration cycle becomes necessary. The original design routed the regeneration gas, produced during the LPG dryer heating cycle, to the sulfur recovery unit to the incineration. However, concerns regarding high temperatures and potential unit disruptions led to a modification where the gas is currently vented to the acid flare for the initial hour before being diverted to the LP network fuel gas system. While this addresses the temperature concerns, it generates significant smoke due to the presence of liquid hydrocarbons. This paper proposes an approach to recover the regeneration gas and redirect it back to the gas plant's (off-gas compressors) instead of sending it to the AC (Acid Flare), by utilizing the existing pipe 6” and connected to off gas compressor KO (Knock-Out ) Drums . This option is simple to operate, flexible, environment-friendly solution as long-term solution, lower in capital expenditure and increase the company's profitability. The feasibility of this proposal is supported by dynamic simulations. The simulations suggest the possibility of operating two out of the three off-gas compressors and LPG (Liquefied petroleum gas) as a liquid phase, is foreseen to be carried over and gathered at the bottom level of the KO (Knock-Out) Drum.

Keywords: thermal incinerator, off-gas compressors, environment, knock-out drums, acid flare

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Authors: Piotr Wisniewski, Sławomir Dykas

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Condensation has a negative impact on turbomachinery efficiency in many energy processes.In technical applications, it is often impossible to dry the working fluid at the nozzle inlet. One of the most popular working fluid is atmospheric air that always contains water in form of steam, liquid, or ice crystals. Moreover, it always contains some amount of suspended particles which influence the phase change process. It is known that the phenomena of evaporation or condensation are connected with release or absorption of latent heat, what influence the fluid physical properties and might affect the machinery efficiency therefore, the phase transition has to be taken under account. This researchpresents an attempt to evaluate the impact of solid and liquid particles suspended in the air on the expansion of moist air in a low expansion rate, i.e., with expansion rate, P≈1000s⁻¹. The numerical study supported by analytical and experimental research is presented in this work. The experimental study was carried out using an in-house experimental test rig, where nozzle was examined for different inlet air relative humidity values included in the range of 25 to 51%. The nozzle was tested for a supersonic flow as well as for flow with shock waves induced by elevated back pressure. The Schlieren photography technique and measurement of static pressure on the nozzle wall were used for qualitative identification of both condensation and shock waves. A numerical model validated against experimental data available in the literature was used for analysis of occurring flow phenomena. The analysis of the suspended particles number, diameter, and character (solid or liquid) revealed their connection with heterogeneous condensation importance. If the expansion of fluid without suspended particlesis considered, the condensation triggers so called condensation wave that appears downstream the nozzle throat. If the solid particles are considered, with increasing number of them, the condensation triggers upwind the nozzle throat, decreasing the condensation wave strength. Due to the release of latent heat during condensation, the fluid temperature and pressure increase, leading to the shift of normal shock upstream the flow. Owing relatively large diameters of the droplets created during heterogeneous condensation, they evaporate partially on the shock and continues to evaporate downstream the nozzle. If the liquid water particles are considered, due to their larger radius, their do not affect the expanding flow significantly, however might be in major importance while considering the compression phenomena as they will tend to evaporate on the shock wave. This research proves the need of further study of phase change phenomena in supersonic flow especially considering the interaction of droplets with the aerodynamic waves in the flow.

Keywords: aerodynamics, computational fluid dynamics, condensation, moist air, multi-phase flows

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Authors: Deepti Mishra, K. K Pant, Xiu Song Zhao, Muxina Konarova

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Catalytic transformation of simplest hydrocarbon methane into benzene and valuable chemicals over Mo/HZSM-5 has a great economic potential, however, it suffers serious hurdles due to the blockage in the micropores because of extensive coking at high temperature during methane dehydroaromatization (MDA). Under such conditions, it necessitates the design of micro/mesoporous ZSM-5, which has the advantages viz. uniform dispersibility of MoOx species, consequently the formation of active Mo sites in the micro/mesoporous channel and lower carbon deposition because of improved mass transfer rate within the hierarchical pores. In this study, we report a unique strategy to control the porous structures of ZSM-5 through a dual templating approach, utilizing C6 and C12 -surfactants as porogen. DFT studies were carried out to correlate the ZSM-5 framework development using the C6 and C12 surfactants with structure directing agent. The structural and morphological parameters of the synthesized ZSM-5 were explored in detail to determine the crystallinity, porosity, Si/Al ratio, particle shape, size, and acidic strength, which were further correlated with the physicochemical and catalytic properties of Mo modified HZSM-5 catalysts. After Mo incorporation, all the catalysts were tested for MDA reaction. From the activity test, it was observed that C6 surfactant-modified hierarchically porous Mo/HZSM-5(H) showed the highest benzene formation rate (1.5 μmol/gcat. s) and longer catalytic stability up to 270 min of reaction as compared to the conventional microporous Mo/HZSM-5(C). In contrary, C12 surfactant modified Mo/HZSM-5(D) is inferior towards MDA reaction (benzene formation rate: 0.5 μmol/gcat. s). We ascribed that the difference in MDA activity could be due to the hierarchically interconnected meso/microporous feature of Mo/HZSM-5(H) that precludes secondary reaction of coking from benzene and hence contributing substantial stability towards MDA reaction.

Keywords: hierarchical pores, Mo/HZSM-5, methane dehydroaromatization, coke deposition

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Authors: Kooshan Nayebzadeh, Maryam Enteshari

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In this study, the oxidative stability of soybean oil under different storage temperatures (4 and 25 ˚C) and during 6-month shelf-life was investigated by various analytical methods and headspace-liquid phase microextraction (HS-LPME) coupled to gas chromatography-mass spectrometry (GC-MS). Oxidation changes were monitored by analytical parameters consisted of acid value (AV), peroxide value (PV), p-Anisidine value (p-AV), thiobarbituric acid value (TBA), fatty acids profile, iodine value (IV) and oxidative stability index (OSI). In addition, concentrations of hexanal and heptanal as secondary volatile oxidation compounds were determined by HS-LPME/GC-MS technique. Rate of oxidation in soybean oil which stored at 25 ˚C was so higher. The AV, p-AV, and TBA were gradually increased during 6 months, while the amount of unsaturated fatty acids, IV, and OSI decreased. Other parameters included concentrations of both hexanal and heptanal, and PV exhibited increasing trend during primitive months of storage; then, at the end of third and fourth months a sudden decrement was understood for the concentrations of hexanal and heptanal and the amount of PV, simultaneously. The latter parameters increased again until the end of shelf-time. As a result, the temperature and time were effective factors in oxidative stability of soybean oil. Also intensive correlations were found for soybean oil at 4 ˚C between AV and TBA (r2=0.96), PV and p-AV (r2=0.9), IV and TBA (-r2=0.9), and for soybean oil stored at 4 ˚C between p-AV and TBA (r2=0.99).

Keywords: headspace-liquid phase microextraction, oxidation, shelf-life, soybean oil

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Authors: Asmaa Mandour, Ramzia El-Bagary, Asmaa El-Zaher, Ehab Elkady

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Background: An UHPLC (ultra high performance liquid chromatography) method for the simultaneous determination of norfloxacin (NOR), metronidazole (MET) and tinidazole (TNZ) using monolithic column is presented. Purpose: The method is considered an environmentally friendly method with relatively low organic composition of the mobile phase. Methods: The chromatographic separation was performed using Phenomenex® Onyex Monolithic C18 (50mmx 20mm) column. An elution program of mobile phase consisted of 0.5% aqueous phosphoric acid : methanol (85:15, v/v). Where elution of all drugs was completed within 3.5 min with 1µL injection volume. The UHPLC method was applied for the stability indication of NOR in the presence of its acid degradation product ND. Results: Retention times were 0.69, 1.19 and 3.23 min for MET, TNZ and NOR, respectively. While ND retention time was 1.06 min. Linearity, accuracy, and precision were acceptable over the concentration range of 5-50µg mL-1for all drugs. Conclusions: The method is simple, sensitive and suitable for the routine quality control and dosage form assay of the three drugs and can also be used for the stability indication of NOR in the presence of its acid degradation product.

Keywords: antibacterial, monolithic cilumn, simultaneous determination, UHPLC

Procedia PDF Downloads 244

Authors: Tahani Hallek, Dhaou Akrout, Riadh Ahmadi, Mabrouk Montacer

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The present work is an organic geochemical study of the Fahdene Formation outcrops at the Mahjouba region belonging to the Eastern part of the Kalaat Senan structure in northwestern Tunisia (the Kef-Tedjerouine area). The analytical study of the organic content of the samples collected, allowed us to point out that the Formation in question is characterized by an average to good oil potential. This fossilized organic matter has a mixed origin (type II and III), as indicated by the relatively high values of hydrogen index. This origin is confirmed by the C29 Steranes abundance and also by tricyclic terpanes C19/(C19+C23) and tetracyclic terpanes C24/(C24+C23) ratios, that suggest a marine environment of deposit with high plants contribution. We have demonstrated that the heterogeneity of organic matter between the marine aspect, confirmed by the presence of foraminifera, and the continental contribution, is the result of an episodic anomaly in relation to the sequential stratigraphy. Given that the study area is defined as an outer platform forming a transition zone between a stable continental domain to the south and a deep basin to the north, we have explained the continental contribution by successive forced regressions, having blocked the albian transgression, allowing the installation of the lowstand system tracts. This aspect is represented by the incised valleys filling, in direct contact with the pelagic and deep sea facies. Consequently, the Fahdene Formation, in the Kef-Tedjerouine area, consists of transgressive system tracts (TST) brutally truncated by extras of continental progradation; resulting in a mixed influence deposition having retained a heterogeneous organic material.

Keywords: molecular geochemistry, biomarkers, forced regression, deposit environment, mixed origin, Northern Tunisia

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Authors: A. Merzouki, N. Haddaoui

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Polymers have a large reputation as electric insulators. These materials are characterized by weak weight, reduced price and a large domain of physical and chemical properties. They conquered new application domains that were until a recent past the exclusivity of metals. In this work, we used some composite materials (polymers/conductive fillers), as electrodes and we try to cover them with metallic lead layers in order to use them as courant collector grids in lead-acid battery plates.

Keywords: electrodeposition, polymer composites, carbon black, acetylene black

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Authors: Wei-Shan Wang, Klaus Vogel, Felix Gabler, Maik Wiemer, Thomas Gessner

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Metallic glasses, which are free of grain boundaries, have superior properties including large elastic limits, high strength, and excellent wear and corrosion resistance. Therefore, bulk metallic glasses (BMG) and thin film metallic glasses (TFMG) have been widely developed and investigated. Among various kinds of metallic glasses, Pd-Cu-Si TFMG, which has lower elastic modulus and better resistance of oxidation and corrosions compared to Zr- and Fe-based TFMGs, can be a promising candidate for MEMS applications. However, the study of Pd-TFMG membrane is still limited. This paper presents free-standing Pd-based metallic glass membranes with large area fabricated on wafer level for the first time. Properties of Pd-Cu-Si thin film metallic glass (TFMG) with various deposition parameters are investigated first. When deposited at 25°C, compressive stress occurs in the Pd76Cu6Si18 thin film regardless of Ar pressure. When substrate temperature is increased to 275°C, the stress state changes from compressive to tensile. Thin film stresses are slightly decreased when Ar pressure is higher. To show the influence of temperature on Pd-TFMGs, thin films without and with post annealing below (275°C) and within (370°C) supercooled liquid region are investigated. Results of XRD and TEM analysis indicate that Pd-TFMGs remain amorphous structure with well-controlled parameters. After verification of amorphous structure of the Pd-TFMGs, free-standing Pd-Cu-Si membranes were fabricated by depositing Pd-Cu-Si thin films directly on 200nm-thick silicon nitride membranes, followed by post annealing and dry etching of silicon nitride layer. Post annealing before SiNx removal is used to further release internal stress of Pd-TFMGs. The edge length of the square membrane ranges from 5 to 8mm. The effect of post annealing on Pd-Cu-Si membranes are discussed as well. With annealing at 370°C for 5 min, Pd-MG membranes are fully distortion-free after removal of SiNx layer. Results show that, by introducing annealing process, the stress-relief, distortion-free Pd-TFMG membranes with large area can be a promising candidate for sensing applications such as pressure and gas sensors.

Keywords: amorphous alloy, annealing, metallic glasses, TFMG membrane

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Authors: Muzaffar Iqbal, Essam Ezzeldin, Khalid A. Al-Rashood

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Pomalidomide is a second generation oral immunomodulatory agent, being used for the treatment of multiple myeloma in patients with disease refractory to lenalidomide and bortezomib. In this study, a sensitive UPLC-MS/MS assay was developed and validated for high-throughput determination of pomalidomide in rat plasma using celecoxib as an internal standard (IS). Liquid liquid extraction using dichloromethane as extracting agent was employed to extract pomalidomide and IS from 200 µL of plasma. Chromatographic separation was carried on Acquity BEHTM C18 column (50 × 2.1 mm, 1.7 µm) using an isocratic mobile phase of acetonitrile:10 mM ammonium acetate (80:20, v/v), at a flow rate of 0.250 mL/min. Both pomalidomide and IS were eluted at 0.66 ± 0.03 and 0.80 ± 0.03 min, respectively with a total run time of 1.5 min only. Detection was performed on a triple quadrupole tandem mass spectrometer using electrospray ionization in negative mode. The precursor to product ion transitions of m/z 272.01 → 160.89 for pomalidomide and m/z 380.08 → 316.01 for IS were used to quantify them respectively, using multiple reaction monitoring mode. The developed method was validated according to regulatory guideline for bioanalytical method validation. The linearity in plasma sample was achieved in the concentration range of 0.47–400 ng/mL (r2 ≥ 0.997). The intra and inter-day precision values were ≤ 11.1% (RSD, %) whereas accuracy values ranged from - 6.8 – 8.5% (RE, %). In addition, other validation results were within the acceptance criteria and the method was successfully applied in a pharmacokinetic study of pomalidomide in rats.

Keywords: pomalidomide, pharmacokinetics, LC-MS/MS, celecoxib

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Authors: A. Kabir, D. Boulainine, I. Bouanane, N. Benslim, B. Boudjema, C. Sedrati

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SnO₂ is an n-type semiconductor with a direct gap of about 3.6 eV. It is largely used in several domains such as nanocrystalline photovoltaic cells. Due to its interesting physic-chemical properties, this material was elaborated in thin film forms using different deposition techniques. It was found that SnO₂ properties were directly affected by the deposition method parameters. In this work, the RGTO method (Rheotaxial Growth and Thermal Oxidation) was used to deposit elaborate SnO₂ thin films. This technique consists on thermal oxidation of the Sn films deposited onto a substrate heated to a temperature close to Sn melting point (232°C). Such process allows the preparation of high porosity tin oxide films which are very suitable for the gas sensing. The films structural, morphological and optical properties pre and post thermal oxidation were studied using X-ray diffraction (XRD), scanning electron microscopy (SEM), UV-Visible spectroscopy and Fourier transform infrared spectroscopy (FTIR) respectively. XRD patterns showed a polycrystalline structure of the cassiterite phase of SnO₂. The grain growth was found affected by the oxidation temperature. This grain size evolution was confronted to existing grain growth models in order to understand the growth mechanism. From SEM images, the as deposited Sn film was formed of difference diameter spherical agglomerations. As a function of the oxidation temperature, these spherical agglomerations shape changed due to the introduction of oxygen ions. The deformed spheres started to interconnect by forming bridges between them. The volume porosity, determined from the UV-Visible reflexion spectra, Changes as a function of the oxidation temperature. The variation of the crystalline fraction, determined from FTIR spectra, correlated with the variation of both the grain size and the volume porosity.

Keywords: tin oxide, RGTO, grain growth, volume porosity, crystalline fraction

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Authors: G. Lancellotta, G. Di Salvo, A. Rigazio, A. Davout, V. Pastore, G. Tonoli, A. Martin, P. Jullien, R. Jagow-Klaff, R. Wernecke

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Artificial ground freezing (AGF) technique is a well-proven soil improvement approach used worldwide to construct shafts, tunnels and many other civil structures in difficult subsoil or ambient conditions. As part of the extension of Line 14 of the Paris subway, a passenger interchange tunnel between the new station at Porte de CI ichy and the new Tribunal the Grand Instance has been successfully constructed using this technique. The paper presents the successful application of AGF by Liquid Nitrogen and Brine implemented to provide structural stability and groundwater cut-off around the passenger interchange tunnel. The working conditions were considered to be rather challenging, due to the proximity of a hundred-year-old existing service tunnel of the Line 13, and subsoil conditions on site. Laboratory tests were carried out to determine the relevant soil parameters for hydro-thermal-mechanical aspects and to implement numerical analyses. Monitoring data were used in order to check and control the development and the efficiency of the freezing process as well as to back analyze the parameters assumed for the design, both during the freezing and thawing phases.

Keywords: artificial ground freezing, brine method, case history, liquid nitrogen

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Authors: H. R. Kelidari, M. Saeedi, J. Akbari, K. Morteza-Semnani, H. Valizadeh

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Spironolactoe (SP) a synthetic steroid diuretic is a poorly water-soluble drug with a low and variable oral bioavailability. Regarding to the good solubility of SP in lipid materials, SP loaded Solid lipid nanoparticles (SP-SLNs) and nanostructured lipid carrier (SP-SLNs) were thus prepared in this work for accelerating dissolution of this drug. The SP loaded NLC with stearic acid (SA) as solid lipid and different Oleic Acid (OA) as liquid lipid content and SLN without OA were prepared by probe ultrasonication method. With increasing the percentage of OA from 0 to 30 wt% in SLN/NLC, the average size and zeta potential of nanoparticles felled down and entrapment efficiency (EE %) rose dramatically. The obtained micrograph particles showed pronounced spherical shape. Differential Scanning Calorimeter (DSC) measurements indicated that the presence of OA reduced the melting temperature and melting enthalpy of solid lipid in NLC structure. The results reflected good long-term stability of the nanoparticles and the measurements show that the particle size remains lower in NLC compare to SLN formulations, 6 months after production. Dissolution of SP-SLN and SP-NLC was about 5.1 and 7.2 times faster than raw drugs in 120 min respectively. These results indicated that the SP loaded NLC containing 70:30 solid lipid to liquid lipid ratio is a suitable carrier of SP with improved drug EE and steady drug release properties.

Keywords: drug release, lipid nanoparticles, spironolactone, stability

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Authors: Sharon Waichman, Shahaf Froim, Ido Zukerman, Shmuel Barzilai, Shmual Hayun, Avi Raveh

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Boron carbide is a ceramic material with superior properties such as high chemical and thermal stability, high hardness and high wear resistance. Moreover, it has a big cross section for neutron absorption and therefore can be employed in nuclear based applications. However, an efficient attachment of boron carbide to a metal such as aluminum can be very challenging, mainly because of the formation of aluminum-carbon bonds that are unstable in humid environment, the affinity of oxygen to the metal and the different thermal expansion coefficients of the two materials that may cause internal stresses and a subsequent failure of the bond. Here, we aimed to achieving a strong and a durable attachment between the boron carbide coating and the aluminum substrate. For this purpose, we applied Ti as a thin intermediate layer that provides a gradual change in the thermal expansion coefficients of the configured layers. This layer is continuous and therefore prevents the formation of aluminum-carbon bonds. Boron carbide coatings with a thickness of 1-5 µm were deposited on the aluminum substrate by pulse-DC magnetron sputtering. Prior to the deposition of the boron carbide layer, the surface was pretreated by energetic ion plasma followed by deposition of the Ti intermediate adhesive layer in a continuous process. The properties of the Ti intermediate layer were adjusted by the bias applied to the substrate. The boron carbide/aluminum bond was evaluated by various methods and complementary techniques, such as SEM/EDS, XRD, XPS, FTIR spectroscopy and Glow Discharge Spectroscopy (GDS), in order to explore the structure, composition and the properties of the layers and to study the adherence mechanism of the boron carbide/aluminum contact. Based on the interfacial bond characteristics, we propose a desirable solution for improved adhesion of boron carbide to aluminum using a highly efficient intermediate adhesive layer.

Keywords: adhesion, boron carbide coatings, ceramic/metal bond, intermediate layer, pulsed-DC magnetron sputtering

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Authors: Jingwei Wang, Anthony G. Fane, Jia Wei Chew

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The use of fluidized Granular Activated Carbon (GAC) as a means of mitigation membrane fouling in membrane bioreactors (MBRs) has received much attention in recent years, especially in anaerobic fluidized bed membrane bioreactors (AFMBRs). It has been affirmed that the unsteady-state tangential shear conferred by GAC fluidization on membrane surface suppressed the extent of membrane fouling with energy consumption much lower than that of bubbling (i.e., air sparging). In a previous work, the hydrodynamics of the fluidized GAC particles were correlated with membrane fouling mitigation effectiveness. Results verified that the momentum transfer from particle to membrane held a key in fouling mitigation. The goal of the current work is to understand the effect of fluidized GAC on membrane critical flux. Membrane critical flux values were measured by a vertical Direct Observation Through the Membrane (DOTM) setup. The polystyrene particles (known as latex particles) with the particle size of 5 µm were used as model foulant thus to give the number of the foulant on the membrane surface. Our results shed light on the positive effect of fluidized GAC enhancing the critical membrane flux by an order-of-magnitude as compared to that of liquid shear alone. Membrane fouling mitigation was benefitted by the increasing of power input.

Keywords: membrane fouling mitigation, liquid-solid fluidization, critical flux, energy input

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Authors: F. A. M. Safwan, H. N. N. Dilrukshi, P. U. S. Peiris

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Less availability of high quality green forages leads to low productivity of national dairy herd of Sri Lanka. Growing grass and fodder to suit the production system is an efficient and economical solution for this problem. CO-3 is placed in a higher category, especially on tillering capacity, green forage yield, regeneration capacity, leaf to stem ratio, high crude protein content, resistance to pests and diseases and free from adverse factors along with other fodder varieties grown within the country. An experiment was designed to determine the effect of organic sheep manure, inorganic fertilizers and liquid sheep manure on growth, yield and nutritive value of CO-3. The study was consisted with three treatments; sheep manure (T1), recommended inorganic fertilizers (T2) and liquid sheep manure (T3) which was prepared using bucket fermentation method and each treatment was consisted with three replicates and those were assigned randomly. First harvest was obtained after 40 days of plant establishment and number of leaves (NL), leaf area (LA), tillering capacity (TC), fresh weight (FW) and dry weight (DW) were recorded and second harvest was obtained after 30 days of first harvest and same set of data were recorded. SPSS 16 software was used for data analysis. For proximate analysis AOAC, 2000 standard methods were used. Results revealed that the plants treated with T1 recorded highest NL, LA, TC, FW and DW and were statistically significant at first and second harvest of CO-3 (p˂ 0.05) and it was found that T1 was statistically significant from T2 and T3. Although T3 was recorded higher than the T2 in almost all growth parameters; it was not statistically significant (p ˃0.05). In addition, the crude protein content was recorded highest in T1 with the value of 18.33±1.61 and was lowest in T2 with the value of 10.82±1.14 and was statistically significant (p˂ 0.05). Apart from this, other proximate composition crude fiber, crude fat, ash, moisture content and dry matter were not statistically significant between treatments (p ˃0.05). In accordance with the results, it was found that the organic fertilizer is the best fertilizer for CO-3 in terms of growth parameters and crude protein content.

Keywords: fertilizer, growth parameters, Hybrid Napier CO-3, proximate composition

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Authors: A. Kouloumpis, P. Zygouri, G. Potsi, K. Spyrou, D. Gournis

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Much of the research effort on graphene focuses on its use as building block for the development of new hybrid nanostructures with well-defined dimensions and behavior suitable for applications among else in gas storage, heterogeneous catalysis, gas/liquid separations, nanosensing and biology. Towards this aim, here we describe a new bottom-up approach, which combines the self-assembly with the Langmuir Schaefer technique, for the production of fullerene-intercalated graphene hybrid materials. This new method uses graphene nanosheets as a template for the grafting of various fullerene C60 molecules (pure C60, bromo-fullerenes, C60Br24, and fullerols, C60(OH)24) in a bi-dimensional array, and allows for perfect layer-by-layer growth with control at the molecular level. Our film preparation approach involves a bottom-up layer-by-layer process that includes the formation of a hybrid organo-graphene Langmuir film hosting fullerene molecules within its interlayer spacing. A dilute water solution of chemically oxidized graphene (GO) was used as subphase on the Langmuir-Blodgett deposition system while an appropriate amino surfactant (that binds covalently with the GO) was applied for the formation of hybridized organo-GO. After the horizontal lift of a hydrophobic substrate, a surface modification of the GO platelets was performed by bringing the surface of the transferred Langmuir film in contact with a second amino surfactant solution (capable to interact strongly with the fullerene derivatives). In the final step, the hybrid organo-graphene film was lowered in the solution of the appropriate fullerene derivative. Multilayer films were constructed by repeating this procedure. Hybrid fullerene-based thin films deposited on various hydrophobic substrates were characterized by X-ray diffraction (XRD) and X-ray reflectivity (XRR), FTIR, and Raman spectroscopies, Atomic Force Microscopy, and optical measurements. Acknowledgments. This research has been co‐financed by the European Union (European Social Fund – ESF) and Greek national funds through the Operational Program "Education and Lifelong Learning" of the National Strategic Reference Framework (NSRF)‐Research Funding Program: THALES. Investing in knowledge society through the European Social Fund (no. 377285).

Keywords: hybrids, graphene oxide, fullerenes, langmuir-blodgett, intercalated structures

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Authors: Asiye Aydilek, Harun Aydilek

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We investigate the costs of various suboptimal allocations in housing, consumption, bond and stock holdings of a retiree in a setting with recursive utility, considering the extensive empirical evidence that investors make suboptimal decisions in different ways. We find that suboptimal stock holdings impose only modest costs on the retiree. This may have a merit in explaining the limited stock investment in the data. The cost of suboptimal bond holdings is higher than that of stocks, but still small. This may partially explain why many more people hold bonds compared to stocks. We find that positive deviations from the optimal level are less costly relative to the negative ones in suboptimal housing allocations. This may help us to clarify why the elderly are over consuming housing, as seen in the housing data. The cost of suboptimal consumption is quite high and the highest of all. Our paper suggests that, in terms of welfare, the decisions of how much of liquid wealth to use for consumption and for saving are more important than the decision about the composition of liquid savings. Suboptimal stock holdings are twice more costly in power utility and suboptimal bond holdings are twenty times more costly in recursive utility. Recursive utility is superior to power utility in terms of rationalizing many people's preference for bonds instead of stocks in investment.

Keywords: housing, recursive utility, retirement, suboptimal decisions, welfare cost

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Authors: Mulatu Kassie Birhanu

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Electro-oxidation of glycerol is an important process to convert the less price glycerol into other expensive (essential) and energy-rich chemicals. In this study, nickel was electro-deposited on laboratory-made carbon ceramic electrode (CCE) substrate using electrochemical techniques that is cyclic voltammetry (CV) to prepare an electro-catalyst (Ni/CCE) for electro-oxidation of glycerol. Carbon ceramic electrode was prepared from graphite and methyl tri-methoxy silane (MTMOS) through the processes called hydrolysis and condensation with methanol in acidic media (HCl) by a sol-gel technique. Physico-chemical characterization of bare CCE and modified (deposited) CCE (Ni/CCE) was measured and evaluated by Fourier Transform Infrared spectroscopy (FTIR), Scanning Electron Microscopy (SEM) and X-ray diffraction (XRD). Electro-oxidation of glycerol was performed in 0.1 M glycerol in alkaline media (0.5 M NaOH). High-Performance Liquid Chromatography (HPLC) technique was used to identify and determine the concentration of glycerol, reaction intermediates and oxidized products of glycerol after its electro-oxidation is performed. The conversion (%) of electro-oxidation of glycerol during 9-hour oxidation was 73% and 36% at 1.8V and 1.6V vs. RHE, respectively. Formate, oxalate, glycolate and glycerate are the main oxidation products of glycerol with selectivity (%) of 75%, 8.6%, 1.1% and 0.95 % at 1.8 V vs. RHE and 55.4%, 2.2%, 1.0% and 0.6% at 1.6 V vs. RHE respectively. The result indicates that formate is the main product in the electro-oxidation of glycerol on Ni/CCE using the indicated applied potentials.

Keywords: carbon-ceramic electrode, electrodeposition, electro-oxidation, Methyltrimethoxysilane

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Authors: Maor Farid, Oleg Gendelman

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Equivalent mechanical model of liquid sloshing in partially-filled cylindrical vessel is treated in the cases of free oscillations and of horizontal base excitation. The model is designed to cover both the linear and essentially nonlinear sloshing regimes. The latter fluid behaviour might involve hydraulic impacts interacting with the inner walls of the tank. These impulsive interactions are often modeled by high-power potential and dissipation functions. For the sake of analytical description, we use the traditional approach by modeling the impacts with velocity-dependent restitution coefficient. This modelling is similar to vibro-impact nonlinear energy sink (VI NES) which was recently explored for its vibration mitigation performances and nonlinear response regimes. Steady-state periodic regimes and chaotic strongly modulated responses (CSMR) are detected. Those dynamical regimes were described by the system's slow motion on the slow invariant manifold (SIM). There is a good agreement between the analytical results and numerical simulations. Subsequently, Finite-Element (FE) method is used to determine and verify the model parameters and to identify dominant dynamical regimes, natural modes and frequencies. The tank failure modes are identified and critical locations are identified. Mathematical relation is found between degrees-of-freedom (DOFs) motion and the mechanical stress applied in the tank critical section. This is the prior attempt to take under consideration large-amplitude nonlinear sloshing and tank structure elasticity effects for design, regulation definition and resistance analysis purposes. Both linear (tuned mass damper, TMD) and nonlinear (nonlinear energy sink, NES) passive energy absorbers contribution to the overall system mitigation is firstly examined, in terms of both stress reduction and time for vibration decay.

Keywords: nonlinear energy sink (NES), reduced-order modelling, liquid sloshing, vibration mitigation, vibro-impact dynamics

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Authors: Ane Escobar, Paula Angelomé, Mihaela Delcea, Marek Grzelczak, Sergio Enrique Moya

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The antibacterial capacity of bone-anchoring implants can be improved by the use of antibiotics that can be delivered to the media after the surgery. Mesoporous films have shown great potential in drug delivery for orthopedic applications, since pore size and thickness can be tuned to produce different surface area and free volume inside the material. This work shows the synthesis of mesoporous titania films (MTF) by sol-gel chemistry and evaporation-induced self-assembly (EISA) on top of glass substrates. Pores with a diameter of 12nm were observed by Transmission Electron Microscopy (TEM). A film thickness of 100 nm was measured by Scanning Electron Microscopy (SEM). Gentamicin was used to study the antibiotic delivery from the film by means of High-performance liquid chromatography (HPLC). The Staphilococcus aureus strand was used to evaluate the effectiveness of the penicillin loaded films toward inhibiting bacterial colonization. MC3T3-E1 pre-osteoblast cell proliferation experiments proved that MTFs have a good biocompatibility and are a suitable surface for MC3T3-E1 cell proliferation. Moreover, images taken by Confocal Fluorescence Microscopy using labeled vinculin, showed good adhesion of the MC3T3-E1 cells to the MTFs, as well as complex actin filaments arrangement. In order to improve cell proliferation Bone Morphogenetic Protein-2 (BMP-2) was adsorbed on top of the mesoporous film. The deposition of the protein was proved by measurements in the contact angle, showing an increment in the hydrophobicity while the protein concentration is higher. By measuring the dehydrogenase activity in MC3T3-E1 cells cultured in dually functionalized mesoporous titatina films with gentamicin and BMP-2 is possible to find an improvement in cell proliferation. For this purpose, the absorption of a yellow-color formazan dye, product of a water-soluble salt (WST-8) reduction by the dehydrogenases, is measured. In summary, this study proves that by means of the surface modification of MTFs with proteins and loading of gentamicin is possible to achieve an antibacterial effect and a cell growth improvement.

Keywords: antibacterial, biocompatibility, bone morphogenetic protein-2, cell proliferation, gentamicin, implants, mesoporous titania films, osteoblasts

Procedia PDF Downloads 159

Authors: Barbara Urasinska-Wojcik, Neil Chilton, Peter Todd, Christopher Elsworthy, Gregory J. Gibbons

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The recent increase in the application of Additive Manufacturing (AM) of products has resulted in new demands on capability. The ability to integrate both form and function within printed objects is the next frontier in the 3D printing area. To move beyond prototyping into low volume production, we demonstrate a UK-designed and built AM hybrid system that combines polymer based structural deposition with digital deposition of electrically conductive elements. This hybrid manufacturing system is based on a multi-planar build approach to improve on many of the limitations associated with AM, such as poor surface finish, low geometric tolerance, and poor robustness. Specifically, the approach involves a multi-planar Material Extrusion (ME) process in which separated build stations with up to 5 axes of motion replace traditional horizontally-sliced layer modeling. The construction of multi-material architectures also involved using multiple print systems in order to combine both ME and digital deposition of conductive material. To demonstrate multi-material 3D printing, three thermoplastics, acrylonitrile butadiene styrene (ABS), polyamide 6,6/6 copolymers (CoPA) and polyamide 12 (PA) were used to print specimens, on top of which our high viscosity Ag-particulate ink was printed in a non-contact process, during which drop characteristics such as shape, velocity, and volume were assessed using a drop watching system. Spectroscopic analysis of these 3D printed materials in the IR region helped to determine the optimum in-situ curing system for implementation into the AM system to achieve improved adhesion and surface refinement. Thermal Analyses were performed to determine the printed materials glass transition temperature (Tg), stability and degradation behavior to find the optimum annealing conditions post printing. Electrical analysis of printed conductive tracks on polymer surfaces during mechanical testing (static tensile and 3-point bending and dynamic fatigue) was performed to assess the robustness of the electrical circuits. The tracks on CoPA, ABS, and PA exhibited low electrical resistance, and in case of PA resistance values of tracks remained unchanged across hundreds of repeated tensile cycles up to 0.5% strain amplitude. Our developed AM printer has the ability to fabricate fully functional objects in one build, including complex electronics. It enables product designers and manufacturers to produce functional saleable electronic products from a small format modular platform. It will make 3D printing better, faster and stronger.

Keywords: additive manufacturing, conductive tracks, hybrid 3D printer, integrated manufacture

Procedia PDF Downloads 162