Search results for: anodic alumina oxide

Authors: Gyung Soo Jeon, Hong Bae Kim, Chi Jung Oh

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In order to prepare the α-alumina with low content of sodium oxide from aluminum trihydroxide as a reactant, three kinds of methods were employed as follows; the mixture of Chamotte (aggregate composed of silica and alumina), ammonium chloride and aluminum fluoride with aluminum trihydroxide under 1600°C, respectively. The sodium oxide in α-alumina produced above methods was analyzed by XRF and the particle size distribution was determined by particle size analyzer, and the specific surface area of α-alumina was measured by BET method, and phase of α-alumina produced was confirmed by XRD. Acknowledgement: This research was supported by Development Program of Technical Innovation funded by Korea Technology and Information Promotion Agency for SMEs (KTIP-2016-S2401821).

Keywords: α-alumina, sodium oxide, aluminum trihydroxide, Chamotte, ammonium chloride, aluminum fluoride

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Authors: W. J. Stępniowski, W. Florkiewicz, M. Norek, M. Michalska-Domańska, E. Kościuczyk, T. Czujko

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In this paper, two options of anodic alumina barrier layer thinning have been demonstrated. The approaches varied with the duration of the voltage step. It was found that too long step of the barrier layer thinning process leads to chemical etching of the nanopores on their top. At the bottoms pores are not fully opened what is disadvantageous for further applications in nanofabrication. On the other hand, while the duration of the voltage step is controlled by the current density (value of the current density cannot exceed 75% of the value recorded during previous voltage step) the pores are fully opened. However, pores at the bottom obtained with this procedure have smaller diameter, nevertheless this procedure provides electric contact between the bare aluminum (substrate) and electrolyte, what is suitable for template assisted electrodeposition, one of the most cost-efficient synthesis method in nanotechnology.

Keywords: anodic aluminum oxide, anodization, barrier layer thinning, nanopores

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Authors: Hang Zhou, Limin Zhu

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This paper investigates the fabrication of microstructures on Si surfaces by using electrochemical anodic oxidation with agarose stamps. The fabricating process is based on a selective anodic oxidation reaction that occurs in the contact area between a stamp and a Si substrate. The stamp which is soaked in electrolyte previously acts as a current flow channel. After forming the oxide patterns as an etching mask, a KOH aqueous is used for the wet etching of Si. A complicated microstructure array of 1 cm2 was fabricated by the method with high accuracy.

Keywords: microstructures, anodic oxidation, silicon, agarose stamps

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Authors: Amine Mezni, Merfat Algethami, Ali Aldalbahi, Arwa Alrooqi, Abel Santos, Dusan Losic, Sarah Alharthi, Tariq Altalhi

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In situ synthesis of carbon nanotubes featuring different diameters (10-200 nm), lengths (1 to 100 µm) and periodically nanostructured shape was performed in a custom designed chemical vapor deposition (CVD) system using nanoporous anodic alumina (NAA) under different conditions. The morphology of the resulting CNTs/NAA composites and free-standing CNTs were analyzed by transmission electron microscopy (TEM) and scanning electron microscopy (SEM). The results confirm that highly ordered arrays of CNTs with precise control of nanotube dimensions in the range 20-200 nm with tube length in the range < 1 µm to > 100 μm and with periodically shaped morphology can be fabricated using nanostructured NAA templates prepared by anodization. This technique allows us to obtain tubes open at one / both ends with a uniform diameter along the pore length without using any metal catalyst. Our finding suggests that this fabrication strategy for designing new CNTs membranes and structures can be significant for emerging applications as molecular separation/transport, optical biosensing, and drug delivery.

Keywords: carbon nanotubes, CVD approach, composites membrane, nanoporous anodic alumina

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Authors: T. Taşköprü, M. Zor, E. Turan

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The advantages of nickel oxide as an electrochromic material are its good contrast of transmittance and its suitable use as a secondary electrochromic film with WO3 for electrochromic devices. Electrochromic nickel oxide film was prepared by using a simple and inexpensive chemical deposition bath (CBD) technique onto fluorine-doped tin oxide (FTO) coated glass substrates from nickel nitrate solution. The films were ace centered cubic NiO with preferred orientation in the (2 0 0) direction. The electrochromic (EC) properties of the films were studied as a function of pH (8, 9, 10 and 11) in an aqueous alkaline electrolyte (0.3 M KOH) using cyclic voltammetry (CV). The EC cell was formed with the following configuration; FTO/nickel oxide film/0.3 M KOH/Pt The potential was cycled from 0.1 to 0.6V at diffferent potential sweep rates in the range 10- 50 mV/s. The films exhibit anodic electrochromism, changing colour from transparent to black.CV results of a nickel oxide film showed well-resolved anodic current peak at potential; 45 mV and cathodic peak at potential 28 mV. The structural, morphological, and optical changes in NiO film following the CV were investigated by means of X-ray diffractometer (XRD), field emission electron microscopy (FESEM) and UV-Vis- NIR spectrophotometry. No change was observed in XRD, besides surface morphology undergoes change due to the electrical discharge. The change in tansmittance between the bleached and colored state is 68% for the film deposited with pH=11 precursor.

Keywords: nickel oxide, XRD, SEM, cyclic voltammetry

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Authors: Kanayo Kenneth Asogwa

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The influence of the flow of nanoparticles in nanofluids across a vertical surface is significant, and its application in medical sciences, engineering, pharmaceutical, and food industries is enormous & widely published. However, the comparative examination of alumina nanoparticles with cupric nanoparticles past a rapid progressive Riga plate remains unknown. Thus, this report investigates water-based alumina and cupric nanoparticles passing through an exponentially accelerated Riga plate. Nanofluids containing copper (II) oxide (CuO) and aluminum oxide (Al2O3) nanoparticles are considered. The Laplace transform technique is used to solve the partial differential equations guiding the flow. The effect of various factors on skin friction coefficient, Nusselt number, velocity and temperature profiles is investigated and reported in tabular and graphical form. The upsurge of Modified Hartmann number and radiative impact improves copper (II) oxide nanofluid compared to aluminum oxide nanofluid due to Lorentz force and since CuO is a better heat conductor. At the same time, heat absorption and reactive species favor a slight decline in Alumina nanofluid than Cupric nanofluid in the thermal and velocity fields. The higher density of Cupric nanofluid is enhanced by increasing nanoparticle volume fraction over Alumina nanofluid with a decline in velocity distribution.

Keywords: alumina, cupric, nanoparticles, water-based

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Authors: Yu-Wei Chang, Hsuan-Yu Ku, Jo-Shan Chiu, Shao-Fu Chang, Chien-Chon Chen

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This paper aims to discuss the hydrophilicity about the anodic aluminum oxide (AAO) template with titania nanotubes (NTs). The AAO templates with pore size diameters of 20-250 nm were generated by anodizing 6061 aluminum alloy substrates in acid solution of sulfuric acid (H₂SO₄), oxalic acid (COOH)₂, and phosphoric acid (H₃PO₄), respectively. TiO₂-NTs were grown on AAO templates by the sol-gel deposition process successfully. The water contact angle on AAO/TiO₂-NTs surface was lower compared to the water contact angle on AAO surface. So, the characteristic of hydrophilicity was significantly associated with the AAO pore size and what kinds of materials were immersed variables.

Keywords: AAO, nanotube, sol-gel, anodization, hydrophilicity

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Authors: Loai Ben Naji, Osama M. Ibrahim, Khaled J. Al-Fadhalah

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The objective of this paper is to investigate the formation and adhesion of a protective aluminum-oxide (Al₂O₃, alumina) layer on the surface of Iron-Chromium-Aluminum Alloy (Fe-Cr-Al) sintered-metal-fibers. The oxide-scale layer was developed via multi-stage thermal oxidation at 930 ^oC for 1 hour, followed by 1 hour at 960 ^oC, and finally at 990 ^oC for 2 hours. Scanning Electron Microscope (SEM) images show that the multi-stage thermal oxidation resulted in the formation of predominantly Al₂O₃ platelets-like and whiskers. SEM images also reveal non-uniform oxide-scale growth on the surface of the fibers. Furthermore, peeling/spalling of the alumina protective layer occurred after minimum handling, which indicates weak adhesion forces between the protective layer and the base metal alloy.  Energy Dispersive Spectroscopy (EDS) analysis of the heat-treated Fe-Cr-Al sintered-metal-fibers confirmed the high aluminum content on the surface of the protective layer, and the low aluminum content on the exposed base metal alloy surface. In conclusion, the failure of the oxide-scale protective layer exposes the base metal alloy to further oxidation, and the fragile non-uniform oxide-scale is not suitable as a support for catalysts.

Keywords: high-temperature oxidation, iron-chromium-aluminum alloy, alumina protective layer, sintered-metal-fibers

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Authors: Natia Jalagonia, Jimsher Maisuradze, Karlo Barbakadze, Tinatin Kuchukhidze

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At present intensive scientific researches of ceramics, cermets and metal alloys have been conducted for improving materials physical-mechanical characteristics. In purpose of increasing impact strength of ceramics based on alumina, simple method of graphene homogenization was developed. Homogeneous distribution of graphene (homogenization) in pressing composite became possible through the connection of functional groups of graphene oxide (-OH, -COOH, -O-O- and others) and alumina superficial OH groups with aluminum organic compounds. These two components connect with each other with -O-Al–O- bonds, and by their thermal treatment (300–500°C), graphene and alumina phase are transformed. Thus, choosing of aluminum organic compounds for modification is stipulated by the following opinion: aluminum organic compounds fragments fixed on graphene and alumina finally are transformed into an integral part of the matrix. By using of other elements as modifier on the matrix surface (Al2O3) other phases are transformed, which change sharply physical-mechanical properties of ceramic composites, for this reason, effect caused by the inclusion of graphene will be unknown. Fixing graphene fragments on alumina surface by alumoorganic compounds result in new type graphene-alumina complex, in which these two components are connected by C-O-Al bonds. Part of carbon atoms in graphene oxide are in sp3 hybrid state, so functional groups (-OH, -COOH) are located on both sides of graphene oxide layer. Aluminum organic compound reacts with graphene oxide at the room temperature, and modified graphene oxide is obtained: R2Al-O-[graphene]–COOAlR2. Remaining Al–C bonds also reacts rapidly with surface OH groups of alumina. In a result of these process, pressing powdery composite [Al2O3]-O-Al-O-[graphene]–COO–Al–O–[Al2O3] is obtained. For the purpose, graphene oxide suspension in dry toluene have added alumoorganic compound Al(iC4H9)3 in toluene with equimolecular ratio. Obtained suspension has put in the flask and removed solution in a rotary evaporate presence nitrogen atmosphere. Obtained powdery have been researched and used to consolidation of ceramic materials based on alumina. Ceramic composites are obtained in high temperature vacuum furnace with different temperature and pressure conditions. Received ceramics do not have open pores and their density reaches 99.5 % of TD. During the work, the following devices have been used: High temperature vacuum furnace OXY-GON Industries Inc (USA), device of spark-plasma synthesis, induction furnace, Electronic Scanning Microscopes Nikon Eclipse LV 150, Optical Microscope NMM-800TRF, Planetary mill Pulverisette 7 premium line, Shimadzu Dynamic Ultra Micro Hardness Tester DUH-211S, Analysette 12 Dynasizer and others.

Keywords: graphene oxide, alumo-organic, ceramic

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Authors: M. Diafi, M. Omari, B. Gasmi

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Perovskite-type La1−xCaxAlO3 were synthesized at 1000◦C by a co- precipitation method. The synthesized oxide powders were characterized by X-ray diffraction (XRD) and the oxide powders were produced in the form of films on pretreated Ni-supports by an oxide-slurry painting technique their electrocatalytic activities towards methanol oxidation in alkaline solutions at 25°C using cyclic voltammetry, chronoamperometry, and anodic Tafel polarization techniques. The oxide catalysts followed the rhombohedral hexagonal crystal geometry. The rate of electro-oxidation of methanol was found to increase with increasing substitution of La by Ca in the oxide matrix. The reaction indicated a Tafel slope of ~2.303RT/F, The electrochemical apparent activation energy (〖∆H〗_el^(°#)) was observed to decrease on increasing Ca content. The results point out the optimum electrode activity and stability of the Ca is x=0.6 of composition.

Keywords: electrocatalysis, oxygen evolution, perovskite-type La1−x Cax AlO3, methanol oxidation

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Authors: S. Tayyebi, F. Mirjalili, H. Samadi, A. Nemati

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In this study, hydroxyapatite-Alumina nano composite powder, containing 15,20 and 25% weight percent of reinforced alumina were prepared by chemical precipitation from the reaction between calcium nitrate tetrahydrate and di-ammonium hydrogen phosphate with ratio of Ca / p = 1.67 and different percentage of aluminum nitrate nona hydrate in different pH of 9,10 and 11. The microstructure and thermal stability of samples were measured by X-ray diffraction (XRD), infrared spectroscopy (FT-IR) and transmission electron microscopy (TEM). The results showed that the presence of reinforced alumina phase reduced the degree of crystallinity of hydroxyapatite phase and increased its decomposition to tricalcium phosphate phase. Microstructural analysis showed that the hydroxyapatite-alumina nano composite powder was obtained with spherical shape and size of less than 100 nm.

Keywords: biomaterial, hydroxyapatite, alumina, nano composite, precipitation method

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Authors: Mohamed Abbas, Ramesh Singh

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This study investigates the hydrothermal aging behavior of undoped and copper oxide-doped alumina-toughened zirconia (ATZ). The ATZ ceramic composites underwent conventional sintering at temperatures ranging from 1250 to 1500°C with a holding time of 12 minutes. XRD analysis revealed a stable 100% tetragonal phase for conventionally sintered ATZ samples up to 1450°C, even after 100 hours of exposure. At 1500℃, XRD patterns of both undoped and doped ATZ samples showed no phase transformation after up to 3 hours of exposure to superheated steam. Extended exposure, however, resulted in phase transformation beyond 10 hours. CuO-doped ATZ samples initially exhibited lower monoclinic content, gradually increasing with aging. Undoped ATZ demonstrated better-aging resistance, maintaining ~40% monoclinic content after 100 hours. FESEM images post-aging revealed surface roughness changes due to the tetragonal-to-monoclinic phase transformation, with limited nucleation in the largest tetragonal grains. Fracture analysis exhibited macrocracks and microcracks on the transformed surface layer after aging. This study found that 0.2wt% CuO doping did not prevent the low-temperature degradation (LTD) phenomenon at elevated temperatures. Transformation zone depth (TZD) calculations supported the trend observed in the transformed monoclinic phase.

Keywords: alumina toughened zirconia, conventional sintering, copper oxide, hydrothermal ageing

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Authors: Chien Chon Chen, Chun Mei Chu, Chuan Ju Wang, Chih Yuan Chen, Ker Jer Huang

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Cesiumiodide with Na doping (CsI(Na)) solution or melt is easily forming three- dimension dendrites on the free surface. The defects or bobbles form inside the CsI(Na) during the solution or melt solidification. The defects or bobbles can further effect the x-ray path in the CsI(Na) crystal and decrease the scintillation characteristics of CsI(Na). In order to enhance the CsI(Na) scintillated property we made single crystal of CsI(Na) column in the anodic aluminum oxide (AAO) template by hydraulic pressure injection method. It is interesting that when CsI(Na) melt is confined in the small AAO channels, the column grow as stable single column without any dendrites. The high aspect ratio (100~10000) of AAO and nano to sub-micron channel structure which is a suitable template for single of crystal CsI(Na) formation. In this work, a new low-cost approach to fabricate scintillator crystals using anodic aluminum oxide (AAO) rather than Si is reported, which can produce scintillator crystals with a wide range of controllable size to optimize their performance in X-ray detection.

Keywords: cesiumiodide, AAO, scintillator, crystal, X-ray

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Authors: C. C. Chen, C. W. Hun, C. J. Wang, C. Y. Chen, J. S. Lin, K. J. Huang

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Cesium iodide (CsI) melt was injected into anodic aluminum oxide (AAO) template and was solidified to CsI column. The controllable AAO channel size (10~500 nm) can makes CsI column size from 10 to500 nm in diameter. In order to have a shorter light irradiate from each singe CsI column top to bottom the AAO template was coated a TiO2 nano-film. The TiO2 film acts a refraction film and makes X-ray has a shorter irradiation path in the CsI crystal making a stronger the photo-electron signal. When the incidence light irradiate from air (R=1.0) to CsI’s first surface (R=1.84) the first refraction happen, the first refraction continue into TiO2 film (R=2.88) and produces the low angle of the second refraction. Then the second refraction continue into AAO wall (R=1.78) and produces the third refraction after refractions between CsI and AAO wall (R=1.78) produce the fourth refraction. The incidence light after through CsI and TiO2 film refractions arrive to the CsI second surface. Therefore, the TiO2 film can has shorter refraction path of incidence light and increase the photo-electron conversion efficiency.

Keywords: cesium iodide, anodic aluminum oxide (AAO), TiO2, refraction, X-ray

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Authors: D. Aboutaleb, B. Safi

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The borate glasses are known by their structural characterized by existence of unit’s structural composed by triangles and tetrahedrons boron in different configurations depending on the percentage of B2O3 in the glass chemical composition. In this paper, effect of lithium oxide addition on the thermal and physical properties of an alumina borate glass, was investigated. It was found that the boron abnormality has a significant effect in the change of glass properties according to the addition rate of lithium oxide.

Keywords: borate glasses, triangles and tetrahedrons boron, lithium oxide, boron anomaly, thermal properties, physical properties

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Authors: Mahendran Samykano, Ram Mohan, Shyam Aravamudhan

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The objective of this work is to study the effect of two key factors-external magnetic field and applied current density during the template-based electrodeposition of nickel nanowires using an electrode distance of 20 mm. Morphology, length, crystallite size, and crystallographic characterization of the grown nickel nanowires at an electrode distance of 20mm are presented. For this electrode distance of 20 mm, these two key electrodeposition factors when coupled was found to reduce crystallite size with a higher growth length and preferred orientation of Ni crystals. These observed changes can be inferred to be due to coupled interaction forces induced by the intensity of applied electric field (current density) and external magnetic field known as magnetohydrodynamic (MHD) effect during the electrodeposition process.

Keywords: anodic alumina oxide, electrodeposition, nanowires, nickel

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Authors: Luc Conti, Dimitry Dumont-Fillon, Harald van Lintel, Eric Chappel

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Flow control valves comprise a silicon flexible membrane that deflects against a substrate, usually made of glass, containing pillars, an outlet hole, and anti-stiction features. However, there is a strong interest in using silicon instead of glass as substrate material, as it would simplify the process flow by allowing the use of well controlled anisotropic etching. Moreover, specific devices demanding a bending of the substrate would also benefit from the inherent outstanding mechanical strength of monocrystalline silicon. Unfortunately, direct Si-Si bonding is not easily achieved with highly structured wafers since residual stress may prevent the good adhesion between wafers. Using a thermoplastic polymer, such as parylene, as intermediate layer is not well adapted to this design as the wafer-to-wafer alignment is critical. An alternative anodic bonding method using an intermediate borosilicate layer has been successfully tested. This layer has been deposited onto the silicon substrate. The bonding recipe has been adapted to account for the presence of the SOI buried oxide and intermediate glass layer in order not to exceed the breakdown voltage. Flow control valves dedicated to infusion of viscous fluids at very high pressure have been made and characterized. The results are compared to previous data obtained using the standard anodic bonding method.

Keywords: anodic bonding, evaporated glass, flow control valve, drug delivery

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Authors: P. Rutkowski, G. Górny, L. Stobierski, D. Zientara, W. Piekarczyk, K. Tran

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The polycrystalline dense alumina shows thermal conductivity about 30 W/mK and very high electrical resistivity. These last two properties can be modified by introducing commercial relatively cheap graphene nanoparticles which, as two-dimensional flakes show very high thermal and electrical properties. The aim of this work is to show that it is possible to manufacture the anisotropic alumina-graphene material with directed multilayer graphene particles. Such materials can show the anisotropic properties mentioned before.

Keywords: alumina, composite, hot-pressed, graphene, properties

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Authors: Olga Tkacheva, Pavel Arkhipov, Alexey Rudenko, Yurii Zaikov

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The aluminum electrolysis process in the conventional cryolite-alumina electrolyte with cryolite ratio of 2.7 was carried out at an initial temperature of 970 °C and the anode current density of 0.5 A/cm² in a 15A lab-scale cell in order to study the formation of the side ledge during electrolysis and the alumina distribution between electrolyte and side ledge. The alumina contained 35.97% α-phase and 64.03% γ-phase with the particles size in the range of 10-120 μm. The cryolite ratio and the alumina concentration were determined in molten electrolyte during electrolysis and in frozen bath after electrolysis. The side ledge in the electrolysis cell was formed only by the 13^th hour of electrolysis. With a slight temperature decrease a significant increase in the side ledge thickness was observed. The basic components of the side ledge obtained by the XRD phase analysis were Na₃AlF₆, Na₅Al₃F₁₄, Al₂O₃, and NaF^.5CaF₂^.AlF₃. As in the industrial cell, the increased alumina concentration in the side ledge formed on the cell walls and at the ledge-electrolyte-aluminum three-phase boundary during aluminum electrolysis in the lab cell was found (FTP No 05.604.21.0239, IN RFMEFI60419X0239).

Keywords: alumina distribution, aluminum electrolyzer, cryolie-alumina electrolyte, side ledge

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Authors: Krzysztof Zieliński, Dariusz Kierzek

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The addition of a small amount of alumina cement to Portland cement results in immediate setting, a rapid increase in the compressive strength and a clear increase of the adhesion to concrete substrate. This phenomenon is used, among others, for the production of liquid floor self-levelling compounds. Alumina cement is several times more expensive than Portland cement and is a component having a significant impact on prices of products manufactured with its use. For the production of liquid floor self-levelling compounds, low-alumina cement containing approximately 40% Al₂O₃ is normally used. The aim of the study was to determine the impact of Portland cement with the addition of alumina cement on the basic physical and mechanical properties of cement slurries and mortars. CEM I 42.5R and three types of alumina cement containing 40%, 50% and 70% of Al₂O₃ were used for the tests. Mixes containing 4%, 6%, 8%, 10% and 12% of different varieties of alumina cement were prepared; for which, the time of initial and final setting, compressive and flexural strength and adhesion to concrete substrate were determined. The analysis of the obtained test results showed that a similar immediate setting effect and clearly better adhesion strength can be obtained using the addition of 6% of high-alumina cement than 12% of low-alumina cement. As the prices of these cements are similar, this can give significant financial savings in the production of liquid floor self-levelling compounds.

Keywords: alumina cement, immediate setting, compression strength, adhesion to substrate

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Authors: Alireza Rafieerad, Bushroa Abd Razak, Bahman Nasiri Tabrizi, Jamunarani Vadivelu

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Recently, reports on the fabrication of nanotubular arrays have generated considerable scientific interest, owing to the broad range of applications of the oxide nanotubes in solar cells, orthopedic and dental implants, photocatalytic devices as well as lithium-ion batteries. A more attractive approach for the fabrication of oxide nanotubes with controllable morphology is the electrochemical anodization of substrate in a fluoride-containing electrolyte. Consequently, titanium dioxide nanotubes (TiO2 NTs) have been highly considered as an applicable material particularly in the district of artificial implants. In addition, regarding long-term efficacy and reasons of failing and infection after surgery of currently used dental implants required to enhance the cytocompatibility properties of Ti-based bone-like tissue. As well, graphene oxide (GO) with relevant biocompatibility features in tissue sites, osseointegration and drug delivery functionalization was fully understood. Besides, the boasting antibacterial ability of silver (Ag) remarkably provided for implantable devices without infection symptoms. Here, surface modification of Ti–6Al–7Nb implants (Ti67IMP) by the development of Ag/GO co-decorated TiO2 NTs was examined. Initially, the anodic TiO2 nanotubes obtained at a constant potential of 60 V were annealed at 600 degree centigrade for 2 h to improve the adhesion of the coating. Afterward, the Ag/GO co-decorated TiO2 NTs were developed by spin coating on Ti67IM. The microstructural features, phase composition and wettability behavior of the nanostructured coating were characterized comparably. In a nutshell, the results of the present study may contribute to the development of the nanostructured Ti67IMP with improved surface properties.

Keywords: anodic tio2 nanotube, biomedical applications, graphene oxide, silver, spin coating

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Authors: M. El Hajji, A. Hallaoui, L. Bazzi, A. Benlhachemi, O. Jbara, A. Tara, B. Bakiz, L. Bazzi, M. Hilali

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The objective of this study was the development of zinc-copper binary oxide "Cu2O-ZnO" thin films by the electrochemical method "cathodic electrodeposition" and their uses for the degradation of a basic dye "Congo Red" by direct anodic oxidation. The anode materials synthesized were characterized by X-ray diffraction "XRD" and by scanning electron microscopy "SEM" coupled to EDS.

Keywords: Cu2O-ZnO thin films, cathodic electrodeposition, electrodegradation, Congo Red, BDD

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Authors: Hyeonseok Yoo, Kiseok Oh, Jinsub Choi

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Titanium oxide nanotubes have attracted great attention because of its photocatalytic activity and large surface area. For enhancing electrochemical properties, catalysts should be doped into the structure because titanium oxide nanotubes themselves have low electroconductivity and catalytic activity. It has been reported that Ru and Ir doped titanium oxide electrodes exhibit high efficiency and low overpotential in the oxygen evolution reaction (OER) for water splitting. In general, titanium oxide nanotubes with high aspect ratio cannot be easily doped by conventional complex methods. Herein, two types of facile routes, namely single step anodization and potential shock, for Ru doping into high aspect ratio titanium oxide nanotubes are introduced in detail. When single step anodization was carried out, stability of electrodes were increased. However, onset potential was shifted to anodic direction. On the other hand, when high potential shock voltage was applied, a large amount of ruthenium/ruthenium oxides were doped into titanium oxide nanotubes and thick barrier oxide layers were formed simultaneously. Regardless of doping routes, ruthenium/ ruthenium oxides were homogeneously doped into titanium oxide nanotubes. In spite of doping routes, doping in aqueous solution generally led to incorporate high amount of Ru in titanium oxide nanotubes, compared to that in non-aqueous solution. The amounts of doped catalyst were analyzed by X-ray photoelectron spectroscopy (XPS). The optimum condition for water splitting was investigated in terms of the amount of doped Ru and thickness of barrier oxide layer.

Keywords: doping, potential shock, single step anodization, titanium oxide nanotubes

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Authors: J. Martin, A. Nominé, T. Czerwiec, G. Henrion, T. Belmonte

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The plasma electrolytic oxidation (PEO) is a particular electrochemical process to produce protective oxide ceramic coatings on light-weight metals (Al, Mg, Ti). When applied to aluminum alloys, the resulting PEO coating exhibit improved wear and corrosion resistance because thick, hard, compact and adherent crystalline alumina layers can be achieved. Several investigations have been carried out to improve the efficiency of the PEO process and one particular way consists in tuning the suitable electrical regime. Despite the considerable interest in this process, there is still no clear understanding of the underlying discharge mechanisms that make possible metal oxidation up to hundreds of µm through the ceramic layer. A key parameter that governs the PEO process is the numerous short-lived micro-discharges (micro-plasma in liquid) that occur continuously over the processed surface when the high applied voltage exceeds the critical dielectric breakdown value of the growing ceramic layer. By using a bipolar pulsed current to supply the electrodes, we previously observed that micro-discharges are delayed with respect to the rising edge of the anodic current. Nevertheless, explanation of the origin of such phenomena is still not clear and needs more systematic investigations. The aim of the present communication is to identify the relationship that exists between this delay and the mechanisms responsible of the oxide growth. For this purpose, the delay of micro-discharges ignition is investigated as the function of various electrical parameters such as the current density (J), the current pulse frequency (F) and the anodic to cathodic charge quantity ratio (R = Qp/Qn) delivered to the electrodes. The PEO process was conducted on Al2214 aluminum alloy substrates in a solution containing potassium hydroxide [KOH] and sodium silicate diluted in deionized water. The light emitted from micro-discharges was detected by a photomultiplier and the micro-discharge parameters (number, size, life-time) were measured during the process by means of ultra-fast video imaging (125 kfr./s). SEM observations and roughness measurements were performed to characterize the morphology of the elaborated oxide coatings while XRD was carried out to evaluate the amount of corundum -Al203 phase. Results show that whatever the applied current waveform, the delay of micro-discharge appearance increases as the process goes on. Moreover, the delay is shorter when the current density J (A/dm2), the current pulse frequency F (Hz) and the ratio of charge quantity R are high. It also appears that shorter delays are associated to stronger micro-discharges (localized, long and large micro-discharges) which have a detrimental effect on the elaborated oxide layers (thin and porous). On the basis of the results, a model for the growth of the PEO oxide layers will be presented and discussed. Experimental results support that a mechanism of electrical charge accumulation at the oxide surface / electrolyte interface takes place until the dielectric breakdown occurs and thus until micro-discharges appear.

Keywords: aluminium, micro-discharges, oxidation mechanisms, plasma electrolytic oxidation

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Authors: A. Guemache, M. Omari

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Oxides with formula Ca1-xSrx MnO3(0≤x≤0.2) were synthesized using co precipitation method. The identification of the obtained phase was carried out using infrared spectroscopy and x-ray diffraction. Thermogravimetric and differential analysis was permitted to characterize different transformations of precursors which take place during one heating cycle. The study of electrochemical behavior was carried out by cyclic voltammetry and impedance spectroscopy. The obtained results show that apparent catalytic activity improved when increasing the concentration of strontium. Anodic current densities varies from 1.3 to 5.9 mA/cm2 at the rate scan of 20 mV.s-1 and a potential 0.8 V for oxides with composition x=0 to 0.2.

Keywords: oxide, co-precipitation, thermal analysis, electrochemical properties

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Authors: Krasimir I. Ivanov, Elitsa N. Kolentsova, Dimitar Y. Dimitrov, Georgi V. Avdeev, Tatyana T. Tabakova

Abstract:

In recent research copper and manganese systems were found to be the most active in CO and organic compounds oxidation among the base catalysts. The mixed copper manganese oxide has been widely studied in oxidation reactions because of their higher activity at low temperatures in comparison with single oxide catalysts. The results showed that the formation of spinel CuxMn3−xO4 in the oxidized catalyst is responsible for the activity even at room temperature. That is why most of the investigations are focused on the hopcalite catalyst (CuMn2O4) as the best copper-manganese catalyst. Now it’s known that this is true only for CO oxidation, but not for mixture of CO and VOCs. The purpose of this study is to investigate the alumina supported copper-manganese catalysts with different Cu/Mn molar ratio in terms of oxidation of CO, methanol and dimethyl ether. The catalysts were prepared by impregnation of γ-Al2O3 with copper and manganese nitrates and the catalytic activity measurements were carried out in continuous flow equipment with a four-channel isothermal stainless steel reactor. Gas mixtures on the input and output of the reactor were analyzed with a gas chromatograph, equipped with FID and TCD detectors. The texture characteristics were determined by low-temperature (- 196 oС) nitrogen adsorption in a Quantachrome Instruments NOVA 1200e (USA) specific surface area&pore analyzer. Thermal, XRD and TPR analyses were performed. It was established that the active component of the mixed Cu-Mn/γ–alumina catalysts strongly depends on the Cu/Mn molar ratio. Highly active alumina supported Cu-Mn catalysts for CO, methanol and DME oxidation were synthesized. While the hopcalite is the best catalyst for CO oxidation, the best compromise for simultaneous oxidation of all components is the catalyst with Cu/Mn molar ratio 1:5.

Keywords: supported copper-manganese catalysts, CO, VOCs oxidation, combustion of exhaust gases

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Authors: Reim A. Almotiri, Manal M. Alkhamisi

Abstract:

Ternary nanocomposites based on hydroxyapatite (HAP) and alumina (Al2O3) were embedded through graphene oxide (GO) nanosheets to be investigated for medical applications. The composition of the preparations has been confirmed by X-ray photoelectron spectroscopy, energy-dispersive X-ray analysis, and Fourier-Transform infrared spectroscopy. Scanning and transmission electron microscopy have shown the typical morphologies of the components of the nanocomposites with hydroxyapatite nanorods reaching an average diameter of 22.26±2 nm and an average length of 69.56±19.25 nm in the ternary nanocomposites. The ternary nanocomposite has a microhardness of 5.8±0.1 GPa and a higher average roughness of 6.5 nm compared to pure HAP preparation with an average roughness of 2.7 nm. All preparations have shown an acceptable cytotoxicity profile with a percent osteoblasts cell viability of 98.6±1.3% after culturing with the ternary nanocomposite. The TNC has also shown the highest antibacterial activity compared to preparations of each of its constituents and their nanocomposites, with a zone of inhibition’s diameter of 14.1±0.8 mm and 13.6±0.6 mm against Staphylococcus aureus and Escherichia coli, respectively, compared to no zone of inhibition for the pure hydroxyapatite preparation.

Keywords: hydroxypatite, cytotoxicity, nanocomposites, X-ray analysis

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Authors: Waqas Hassan Tanveer, Yoon Ho Lee, Taehyun Park, Wonjong Yu, Yaegeun Lee, Yusung Kim, Suk Won Cha

Abstract:

Nickel-Gadolinium Doped Ceria (Ni-GDC) cermet anodic thin films were prepared on Scandia Stabilized Zirconia (ScSZ) electrolyte supports by radio frequency (RF) sputtering, with a range of different sputtering powers (50 – 200W) and background Ar gas pressures (30 – 90mTorr). The effects of varying sputtering power and pressure on the properties of Ni-GDC films were studied using Focused Ion Beam (FIB), X-ray Photoelectron Spectroscopy (XPS), X-ray Diffraction (XRD), Energy Dispersive X-ray (EDX), and Atomic Force Microscopy (AFM) techniques. The Ni content was found to be always higher than the Ce content, at all sputtering conditions. This increased Ni content was attributed to significantly higher energy transfer efficiency of Ni ions as compared to Ce ions with Ar background sputtering gas. The solid oxide fuel cell configuration was completed by using lanthanum strontium manganite (LSM/YSZ) cathodes on the other side of ScSZ supports. Performance comparison of cells was done by Voltage-Current-Power (VIP) curves, while the resistances of various cell components were observed by nyquist plots. Initial results showed that anode films made by higher powered RF sputtering performed better than lower powered ones for a specific Ar pressure. Interestingly, however, anodes made at highest power and pressure, were not the ones that showed the maximum power output at an intermediate solid oxide fuel cell temperature of 800°C. Finally, an optimal sputtering condition was reported for high performance Ni-GDC anodes.

Keywords: intermediate temperature solid oxide fuel cells, nickel-cermet anodic thin films, nyquist plots, radio frequency sputtering

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Authors: Abdul Mutalib Md Jani, Abdul Hadi Mahmud, Mohd Tajuddin Mohd Ali

Abstract:

The rapid growth of interest in surface modification of nanostructures materials that exhibit improved structural and functional properties is attracting more researchers. The unique properties of highly ordered nanoporous anodic aluminium oxide (NAAO) membrane have been proposed as a platform for biosensing applications. They exhibit excellent physical and chemical properties with high porosity, high surface area, tunable pore sizes and excellent chemical resistance. In this study, NAAO was functionalized with 3-aminopropyltriethoxysilane (APTES) to prepared silane-modified NAAO. Amine functional groups are formed on the surface of NAAO during silanization and were characterized using Fourier Transform Infrared spectroscopy (FTIR). The synthesis of multi segment of peptide on NAAO surfaces can be realized by changing the surface chemistry of the NAAO membrane via click chemistry. By click reactions, utilizing alkyne terminated with amino group, various peptides tagged on NAAO can be envisioned from chiral natural or unnatural amino acids using standard coupling methods (HOBt, EDCI and HBTU). This strategy seemly versatile since coupling strategy of dipeptide with another amino acids, leading to tripeptide, tetrapeptide or pentapeptide, can be synthesized without purification. When an appropriate terminus is selected, multiple segments of amino acids can be successfully synthesized on the surfaces. The immobilized NAAO should be easily separated from the reaction medium by conventional filtration, thus avoiding complicated purification methods. Herein, we proposed to synthesize multi fragment peptide as a model for capturing and attaching various small biomolecules on NAAO surfaces and can be also applied as biosensing device, drug delivery systems and biocatalyst.

Keywords: nanoporous anodic aluminium oxide, silanization, peptide synthesise, click chemistry

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Authors: Shalini Arora, Sri Sivakumar

Abstract:

The deep removal of high molecular weight sulphur compounds (e.g., 4,6, dimethyl dibenzothiophene) is challenging due to their steric hindrance. Hydrogenation desulfurization (HYD) pathway is the main pathway to remove these sulfur compounds, and it is mainly governed by the number of type 2 sites. The formation of type 2 sites can be enhanced by modulating the pore structure and the interaction between the active metal and support. To this end, we report the enhanced HDS catalytic activity of ultrasmall NiMo supported on amorphous alumina (A-Al₂O₃) catalysts by one pot colloidal synthesis method followed by calcination and sulfidation. The amorphous alumina (A-Al₂O₃) was chosen as the support due to its lower surface energy, better physicochemical properties, and enhanced acidic sites (due to the dominance of tetra and penta coordinated [Al] sites) than crystalline alumina phase. At 20% metal oxide composition, NiMo supported on A-Al₂O₃ catalyst showed 1.4 and 1.2 times more reaction rate constant and turn over frequency (TOF) respectively than the conventional catalyst (wet impregnated NiMo catalysts) for HDS reaction of dibenzothiophene reactant molecule. A-Al₂O₃ supported catalysts represented enhanced type 2 sites formation (because this catalystpossesses higher sulfidation degree (80%) and NiMoS sites (19.3 x 10¹⁷ sites/mg) with desired optimum stacking degree (2.5) than wet impregnated catalyst at same metal oxide composition 20%) along with higher active metal dispersion, Mo edge site fraction. The experimental observations were also supported by DFT simulations. Lower heat of adsorption (< 4.2 ev for MoS2 interaction and < 3.15 ev for Ni doped MoS2 interaction) values for A-Al₂O₃ confirmed the presence of weaker metal-support interaction in A-Al₂O₃ in contrast to crystalline ℽ-Al₂O3. The weak metal-support interaction for prepared catalysts clearly suggests the higher formation of type 2 sites which leads to higher catalytic activity for HDS reaction.

Keywords: amorphous alumina, colloidal, desulfurization, metal-support interaction

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