Search results for: nanoporous alumina

Authors: H. K. Shahzad, M. A. Hussein, F. Patel, N. Al-Aqeeli, T. Laoui

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The purpose of the present study was to use the adsorption mechanism with microfiltration synergistically for efficient heavy metal removal from contaminated water. Alumina (Al2O3) is commonly used for ceramic membranes development while recently carbon nanotubes (CNTs) have been considered among the best adsorbent materials for heavy metals. In this work, we combined both of these materials to prepare porous Al2O3-CNTs nanocomposite membranes via Spark Plasma Sintering (SPS) technique. Alumina was used as a base matrix while CNTs were added as filler. The SPS process parameters i.e. applied pressure, temperature, heating rate, and holding time were varied to obtain the best combination of porosity (64%, measured according to ASTM c373-14a) and strength (3.2 MPa, measured by diametrical compression test) of the developed membranes. The prepared membranes were characterized using X-ray diffraction (XRD), field emission secondary electron microscopy (FE-SEM), contact angle and porosity measurements. The results showed that properties of the synthesized membranes were highly influenced by the SPS process parameters. FE-SEM images revealed that CNTs were reasonably dispersed in the alumina matrix. The porous membranes were evaluated for their water flux transport as well as their capacity to adsorb heavy metals ions. Selected membranes were able to remove about 97% cadmium from contaminated water. Further work is underway to enhance the removal efficiency of the developed membranes as well as to remove other heavy metals such as arsenic and mercury.

Keywords: heavy metal removal, inorganic membrane, nanocomposite, spark plasma sintering

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Authors: L. Vivet, L. Benabou, O. Simon

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With highly demanding applications in the field of power electronics, there is an increasing need to have interconnection materials with properties that can ensure both good mechanical assembly and high thermal/electrical conductivities. So far, lead-free solders have been considered an attractive solution, but recently, sintered joints based on nano-silver paste have been used for die attach and have proved to be a promising solution offering increased performances in high-temperature applications. In this work, the main parameters of the bonding process using silver oxalates are studied, i.e., the heating rate and the bonding pressure mainly. Their effects on both the mechanical and thermal properties of the sintered layer are evaluated following an experimental design. Pairs of copper substrates with gold metallization are assembled through the sintering process to realize the samples that are tested using a micro-traction machine. In addition, the obtained joints are examined through microscopy to identify the important microstructural features in relation to the measured properties. The formation of an intermetallic compound at the junction between the sintered silver layer and the gold metallization deposited on copper is also analyzed. Microscopy analysis exhibits a nanoporous structure of the sintered material. It is found that higher temperature and bonding pressure result in higher densification of the sintered material, with higher thermal conductivity of the joint but less mechanical flexibility to accommodate the thermo-mechanical stresses arising during service. The experimental design allows hence the determination of the optimal process parameters to reach sufficient thermal/mechanical properties for a given application. It is also found that the interphase formed between silver and gold metallization is the location where the fracture occurred after the mechanical testing, suggesting that the inter-diffusion mechanism between the different elements of the assembly leads to the formation of a relatively brittle compound.

Keywords: nanoporous structure, silver oxalate, sintering, mechanical strength, thermal conductivity, microelectronic packaging

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

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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: Shalini Arora, Sri Sivakumar

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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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Authors: M. D. Levi, Netanel Shpigel, Sergey Sigalov, Gregory Salitra, Leonid Daikhin, Doron Aurbach

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We have developed an in-situ method for tracking ions adsorption into composite nanoporous carbon electrodes based on quartz-crystal microbalance (QCM). In these first papers QCM was used as a simple gravimetric probe of compositional changes in carbon porous composite electrodes during their charging since variation of the electrode potential did not change significantly width of the resonance. In contrast, when we passed from nanoporous carbons to a composite Li-ion battery material such as LiFePO4 olivine, the change in the resonance width was comparable with change of the resonance frequency (polymeric binder PVdF was shown to be completely rigid when used in aqueous solutions). We have provided a quantitative hydrodynamic admittance model of ion-insertion processes into electrode host accompanied by intercalation-induced dimensional changes of electrode particles, and hence the entire electrode coating. The change in electrode deformation and the related porosity modify hydrodynamic solid-liquid interactions tracked by QCM with dissipation monitoring. Using admittance modeling, we are able to evaluate the changes of effective thickness and permeability/porosity of composite electrode caused by applied potential and as a function of cycle number. This unique non-destructive technique may have great advantage in early diagnostics of cycling life durability of batteries and supercapacitors.

Keywords: Li-ion batteries, particles deformations, QCM-D, viscoelasticity

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Authors: David E. Esezobor, Friday I. Apeh, Harrison O. Onovo, Ademola A. Agbeleye

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Available indigenous refractory bricks in Nigeria can only be used in the lining of furnaces for melting of cast iron operating at less than 1,400°C or in preheating furnaces due to their low refractoriness less than 1,500°C. The bricks crack and shatter on heating at 1350 to 1450°C. In this paper, a simple and adaptable technology of manufacturing high-quality refractory bricks from selected Nigerian clays for furnace linings was developed. Fireclays from Onibode, Owode-Ketu in Ogun State and Kwoi in Kaduna State were crushed, ground, and sieved into various grain sizes using standard techniques. The pulverized clays were blended with alumina in various mix ratios and indurated in the furnace at 900 – 16000C. Their chemical, microstructure and mineralogical properties were characterized using atomic absorption spectrophotometry, scanning electron microscopy and x-ray diffraction spectrometry respectively. The mineralogical and spectrochemical analyses suggested that the clays are of siliceous alumino-silicate and acidic in nature. The appropriate blending of fireclays with alumina provided the tremendous improvement in the refractoriness of the bricks and other acceptable service properties comparable with imported refractory bricks. The change in microstructure from pseudo-hexagonal grains to equiaxed grains of well – ordered sequence of structural layers could be responsible for the improved properties.

Keywords: alumina, furnace, industry, manufacturing, refractoriness

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Authors: Lia Gventsadze, Elguja Kutelia, David Gventsadze

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The purpose of the article is to show the possibility for the development of a new generation, eco-friendly (asbestos free) nano-porous friction materials on the basis of Georgian raw materials, along with the determination of technological parameters for their production, as well as the optimization of tribological properties and the investigation of structural aspects of wear peculiarities of elaborated materials using the scanning electron microscopy (SEM) and Auger electron spectroscopy (AES) methods. The study investigated the tribological properties of the polymer friction materials on the basis of the phenol-formaldehyde resin using the porous diatomite filler modified by silane with the aim to improve the thermal stability, while the composition was modified by iron phosphate, technical carbon and basalt fibre. As a result of testing the stable values of friction factor (0.3-0,45) were reached, both in dry and wet friction conditions, the friction working parameters (friction factor and wear stability) remained stable up to 500 OC temperatures, the wear stability of gray cast-iron disk increased 3-4 times, the soundless operation of materials without squeaking were achieved. Herewith it was proved that small amount of ingredients (5-6) are enough to compose the nano-porous friction materials. The study explains the mechanism of the action of nano-porous composition base brake lining materials and its tribological efficiency on the basis of the triple phase model of the tribo-pair.

Keywords: brake lining, friction coefficient, wear, nanoporous composite, phenolic resin

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Authors: Krasimir Ivanov, Elitsa Kolentsova, Dimitar Dimitrov, Petya Petrova, Tatyana Tabakova

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This work studies the effect of chemical composition on the activity and selectivity of γ–alumina supported CuO/ MnO2/Cr2O3 catalysts toward deep oxidation of CO, dimethyl ether (DME) and methanol. The catalysts were prepared by impregnation of the support with an aqueous solution of copper nitrate, manganese nitrate and CrO3 under different conditions. Thermal, XRD and TPR analysis were performed. The catalytic measurements of single compounds oxidation were carried out on continuous flow equipment with a four-channel isothermal stainless steel reactor. Flow-line equipment with an adiabatic reactor for simultaneous oxidation of all compounds under the conditions that mimic closely the industrial ones was used. The reactant and product gases were analyzed by means of on-line gas chromatographs. On the basis of XRD analysis it can be concluded that the active component of the mixed Cu-Mn-Cr/γ–alumina catalysts consists of at least six compounds – CuO, Cr2O3, MnO2, Cu1.5Mn1.5O4, Cu1.5Cr1.5O4 and CuCr2O4, depending on the Cu/Mn/Cr molar ratio. Chemical composition strongly influences catalytic properties, this influence being quite variable with regards to the different processes. The rate of CO oxidation rapidly decrease with increasing of chromium content in the active component while for the DME was observed the reverse trend. It was concluded that the best compromise are the catalysts with Cu/(Mn + Cr) molar ratio 1:5 and Mn/Cr molar ratio from 1:3 to 1:4.

Keywords: Cu-Mn-Cr oxide catalysts, volatile organic compounds, deep oxidation, dimethyl ether (DME)

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Authors: Lucie Speyer, Vincent Lecocq, Séverine Humbert, Antoine Hugon

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Mesoporous alumina is commonly used as a catalyst support for the hydrotreating of heavy petroleum cuts. The process of fabrication usually involves: the synthesis of the boehmite AlOOH precursor, a kneading-extrusion step, and a calcination in order to obtain the final alumina extrudates. Alumina is described as a complex porous medium, generally agglomerates constituted of aggregated nanocrystallites. Its porous texture directly influences the active phase deposition and mass transfer, and the catalytic properties. Then, it is easy to figure out that each step of the fabrication of the supports has a role on the building of their porous network, and has to be well understood to optimize the process. The synthesis of boehmite by precipitation of aluminum salts was extensively studied in the literature and the effect of various parameters, such as temperature or pH, are known to influence the size and shape of the crystallites and the specific surface area of the support. The calcination step, through the topotactic transition from boehmite to alumina, determines the final properties of the support and can tune the surface area, pore volume and pore diameters from those of boehmite. However, the kneading extrusion step has been subject to a very few studies. It generally consists in two steps: an acid, then a basic kneading, where the boehmite powder is introduced in a mixer and successively added with an acid and a base solution to form an extrudable paste. During the acid kneading, the induced positive charges on the hydroxyl surface groups of boehmite create an electrostatic repulsion which tends to separate the aggregates and even, following the conditions, the crystallites. The basic kneading, by reducing the surface charges, leads to a flocculation phenomenon and can control the reforming of the overall structure. The separation and reassembling of the particles constituting the boehmite paste have a quite obvious influence on the textural properties of the material. In this work, we are focused on the influence of the kneading step on the alumina catalysts supports. Starting from an industrial boehmite, extrudates are prepared using various kneading conditions. The samples are studied by nitrogen physisorption in order to analyze the evolution of the textural properties, and by synchrotron small-angle X-ray scattering (SAXS), a more original method which brings information about agglomeration and aggregation of the samples. The coupling of physisorption and SAXS enables a precise description of the samples, as same as an accurate monitoring of their evolution as a function of the kneading conditions. These ones are found to have a strong influence of the pore volume and pore size distribution of the supports. A mechanism of evolution of the texture during the kneading step is proposed and could be attractive in order to optimize the texture of the supports and then, their catalytic performances.

Keywords: alumina catalyst support, kneading, nitrogen physisorption, small-angle X-ray scattering

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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: Nikoloz Jalabadze, Roin Chedia, Lili Nadaraia, Levan Khundadze

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Nanocrystalline materials in powder condition can be manufactured by a number of different methods, however manufacture of composite materials product in the same nanocrystalline state is still a problem because the processes of compaction and synthesis of nanocrystalline powders go with intensive growth of particles – the process which promotes formation of pieces in an ordinary crystalline state instead of being crystallized in the desirable nanocrystalline state. To date spark plasma sintering (SPS) has been considered as the most promising and energy efficient method for producing dense bodies of composite materials. An advantage of the SPS method in comparison with other methods is mainly low temperature and short time of the sintering procedure. That finally gives an opportunity to obtain dense material with nanocrystalline structure. Graphene has recently garnered significant interest as a reinforcing phase in composite materials because of its excellent electrical, thermal and mechanical properties. Graphene nanoplatelets (GNPs) in particular have attracted much interest as reinforcements for ceramic matrix composites (mostly in Al2O3, Si3N4, TiO2, ZrB2 a. c.). SPS has been shown to fully densify a variety of ceramic systems effectively including Al2O3 and often with improvements in mechanical and functional behavior. Alumina consolidated by SPS has been shown to have superior hardness, fracture toughness, plasticity and optical translucency compared to conventionally processed alumina. Knowledge of how GNPs influence sintering behavior is important to effectively process and manufacture process. In this study, the effects of GNPs on the SPS processing of Al2O3 are investigated by systematically varying sintering temperature, holding time and pressure. Our experiments showed that SPS process is also appropriate for the synthesis of nanocrystalline powders of alumina-graphene composites. Depending on the size of the molds, it is possible to obtain different amount of nanopowders. Investigation of the structure, physical-chemical, mechanical and performance properties of the elaborated composite materials was performed. The results of this study provide a fundamental understanding of the effects of GNP on sintering behavior, thereby providing a foundation for future optimization of the processing of these promising nanocomposite systems.

Keywords: alumina oxide, ceramic matrix composites, graphene nanoplatelets, spark-plasma sintering

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Authors: S. Toufigh Bararpour, Amir H. Soleimanisalim, Davood Karami, Nader Mahinpey

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The continued increase in the atmospheric concentration of CO2 is expected to have great impacts on the climate. In order to reduce CO2 emission to the atmosphere, an efficient and cost-effective technique is required. Using regenerable solid sorbents, especially K2CO3 is a promising method for low-temperature CO2 capture. Pure K2CO3 is a delinquent substance that requires modifications before it can be used for cyclic operations. For this purpose, various types of additives and supports have been used to improve the structure of K2CO3. However, hydrophilicity and reactivity of the support materials with K2CO3 have a negative effect on the CO2 capture capacity of the sorbents. In this research, two kinds of alumina supports (γ-Alumina and Boehmite) were used. In order to decrease the supports' hydrophilicity and reactivity with K2CO3, nonreactive additives such as Titania, Zirconia and Silisium were incorporated into their structures. These materials provide a shell around the alumina to protect it from undesirable reactions and improve its properties. K2CO3-based core/shell-supported sorbents were fabricated using two preparation steps. The sol-gel method was applied for shelling the supports. Then the shelled supports were impregnated on K2CO3. The physicochemical properties of the sorbents were determined using SEM and BET analyses, and their CO2 capture capacity was quantified using a thermogravimetric analyzer. It was shown that type of the shell's material had an important effect on the water adsorption capacity of the sorbents. Supported K2CO3 modified by Titania shell showed the lowest hydrophilicity among the prepared samples. Based on the obtained results, incorporating nonreactive additives in Boehmite had an outstanding impact on the CO2 capture performance of the sorbent. Incorporation of Titania into the Boehmite-supported K2CO3 enhanced its CO2 capture capacity significantly. Therefore, further study of this novel fabrication technique is highly recommended. In the second phase of this research project, the CO2 capture performance of the sorbents in fixed and fluidized bed reactors will be investigated.

Keywords: CO₂ capture, core/shell support, K₂CO₃, post-combustion

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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: Oluwagbenga B. Fatile, Felix U. Idu, Olajide T. Sanya

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This paper reports the viability of developing Zn-27Al alloy matrix hybrid composites reinforced with alumina, graphite and fly ash (a solid waste byproduct of coal in thermal power plants). This research work was aimed at developing low cost-high performance Zn-27Al matrix composite with low density. Alumina particulates (Al2O3), graphite added with 0, 2, 3, 4, and 5 wt% fly ash were utilized to prepare 10wt% reinforcing phase with Zn-27Al alloy as matrix using two-step stir casting method. Density measurement estimated percentage porosity, tensile testing, micro hardness measurement, and optical microscopy were used to assess the performance of the composites produced. The results show that the hardness, ultimate tensile strength, and percent elongation of the hybrid composites decrease with increase in fly ash content. The maximum decrease in hardness and ultimate tensile strength of 13.72% and 15.25% respectively were observed for composite grade containing 5wt% fly ash. The percentage elongation of composite sample without fly ash is 8.9% which is comparable with that of the sample containing 2wt% fly ash with percentage elongation of 8.8%. The fracture toughness of the fly ash containing composites was, however, superior to those of composites without fly ash with 5wt% fly ash containing composite exhibiting the highest fracture toughness. The results show that fly ash can be utilized as complementary reinforcement in ZA-27 alloy matrix composite to reduce cost.

Keywords: fly ash, hybrid composite, mechanical behaviour, stir-cast

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Authors: Francesca Risplendi, Li-Chiang Lin, Jeffrey C. Grossman, Giancarlo Cicero

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Desalination is one of the most employed approaches to supply water in the context of a rapidly growing global water shortage. However, the most popular water filtration method available is the reverse osmosis (RO) technique, still suffers from important drawbacks, such as a large energy demands and high process costs. In addition some serious limitations have been recently discovered, among them, the boron problem seems to have a critical meaning. Boron has been found to have a dual effect on the living systems on Earth and the difference between boron deficiency and boron toxicity levels is quite small. The aim of this project is to develop a new generation of RO membranes based on porous graphene or reduced graphene oxide (rGO) able to remove salts from seawater and to reduce boron concentrations in the permeate to the level that meets the drinking or process water requirements, by means of a theoretical approach based on density functional theory and classical molecular dynamics. Computer simulations have been employed to investigate the relationship between the atomic structure of nanoporous graphene or rGO monolayer and its membrane properties in RO applications (i.e. water permeability and resilience at RO pressures). In addition, an emphasis has been given to multilayer nanoporous rGO and rGO flakes based membranes. By means of non-equilibrium MD simulations, we investigated the water transport mechanism permeating through such multilayer membrane focusing on the effect of slit widths and sheet geometries. These simulations allowed us to establish the implications of these graphene based materials as promising membrane properties for desalination plants and as boron filtration.

Keywords: boron filtration, desalination, graphene membrane, reduced graphene oxide membrane

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Authors: Soroor Ghaziof, Wei Gao

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Sol-enhanced Zn-Ni-Al2O3 nano-composite coatings were electroplated on mild steel by our newly developed sol-enhanced electroplating method. In this method, transparent Al2O3 sol was added into the acidic Zn-Ni bath to produced Zn-Ni-Al2O3 nano-composite coatings. The chemical composition, microstructure and mechanical properties of the composite and alloy coatings deposited at two different agitation speed were investigated. The structure of all coatings was single γ-Ni5Zn21 phase. The composite coatings possess refined crystals with higher microhardness compared to Zn-Ni alloy coatings. The wear resistance of Zn-Ni coatings was improved significantly by incorporation of alumina nano particles into the coatings. Higher agitation speed provided more uniform coatings with smaller grain sized and slightly higher microhardness. Considering composite coatings, high agitation speeds may facilitate co-deposition of alumina in the coatings.

Keywords: microhardness, sol-enhanced electroplating, wear resistance, Zn-Ni-Al2O3 composite coatings

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Authors: Amir Mahmoudi

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In this research the effects of adding silica and alumina nanoparticles on flow ability and compressive strength of cementitious composites based on Portland cement were investigated. In the first stage, the rheological behavior of different samples containing nanosilica, nanoalumina and polypropylene, polyvinyl alcohol and polyethylene fibers were evaluated. With increasing of nanoparticles in fresh samples, the slump flow diameter reduced. Fibers reduced the flow ability of the samples and viscosity increased. With increasing of the micro silica particles to cement ratio from 2/1 to 2/2, the slump flow diameter increased. By adding silica and alumina nanoparticles up to 3% and 2% respectively, the compressive strength increased and after decreased. Samples containing silica nanoparticles and fibers had the highest compressive strength.

Keywords: Portland cement, composite, nanoparticles, compressive strength

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Authors: Noor-ul-Amin, Lubna Nawab, Sabiha Sultana

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Geopolymer with different silica to alumina ratio with iron have been synthesized using sodium silicate, aluminum, and iron salts as a source of silica, alumina and iron source, and sodium/potassium hydroxide as an alkaline medium. The iron source will be taken from iron (III) salts and laterite clay samples. Laterite has been used as a natural source of iron in modified geopolymer. The synthesized iron modified geopolymer was submitted to the different aggressive environment, including chloride and sulphate solutions in different concentration. Different experimental techniques, including XRF, XRD, and FTIR, were used to study the bonding nature and effect of aggressive environment on geopolymer. The major phases formed during geopolymerization are sodalite (Na₄Al₃Si₃O₁₂Cl), albite (NaAlSi₃O₈), hematite (Fe₂O₃), and chabazite as confirmed from the XRD results. The resulting geopolymer showed greater resistance to sulphate and chloride as compared to the normal geopolymer.

Keywords: modified geopolymer, laterite, chloride, sulphate

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Authors: S. Ghanaraja, Subrata Ray, S. K. Nath

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Particle reinforced Metal Matrix Composite (MMC) succeeds in synergizing the metallic matrix with ceramic particle reinforcements to result in improved strength, particularly at elevated temperatures, but adversely it affects the ductility of the matrix because of agglomeration and porosity. The present study investigates the outcome of tensile properties in a cast and hot forged composite reinforced simultaneously with coarse and fine particles. Nano-sized alumina particles have been generated by milling mixture of aluminum and manganese dioxide powders. Milled particles after drying are added to molten metal and the resulting slurry is cast. The microstructure of the composites shows good distribution of both the size categories of particles without significant clustering. The presence of nanoparticles along with coarser particles in a composite improves both strength and ductility considerably. Delay in debonding of coarser particles to higher stress is due to reduced mismatch in extension caused by increased strain hardening in presence of the nanoparticles. However, higher addition of powder mix beyond a limit results in deterioration of mechanical properties, possibly due to clustering of nanoparticles. The porosity in cast composite generally increases with the increasing addition of powder mix as observed during process and on forging it has got reduced. The base alloy and nanocomposites show improvement in flow stress which could be attributed to lowering of porosity and grain refinement as a consequence of forging.

Keywords: aluminium, alumina, nano-particle reinforced composites, porosity

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Authors: Hossein Tavallali, Mohammad Ali Karimi, Gohar Deilamy-Rad

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The proposed method for speciation, preconcentration and determination of Fe(II) and Fe(III) in pharmaceutical products was developed using of alumina-coated magnetite nanoparticles (Fe₃O₄/Al₂O₃ NPs) as solid phase extraction (SPE) sorbent in magnetic mixed hemimicell solid phase extraction (MMHSPE) technique followed by flame atomic absorption spectrometry analysis. The procedure is based on complexation of Fe(II) with 1, 10-phenanthroline (OP) as complexing reagent for Fe(II) that immobilized on the modified Fe₃O₄/Al₂O₃ NPs. The extraction and concentration process for pharmaceutical sample was carried out in a single step by mixing the extraction solvent, magnetic adsorbents under ultrasonic action. Then, the adsorbents were isolated from the complicated matrix easily with an external magnetic field. Fe(III) ions determined after facility reduced to Fe(II) by added a proper reduction agent to sample solutions. Compared with traditional methods, the MMHSPE method simplified the operation procedure and reduced the analysis time. Various influencing parameters on the speciation and preconcentration of trace iron, such as pH, sample volume, amount of sorbent, type and concentration of eluent, were studied. Under the optimized operating conditions, the preconcentration factor of the modified nano magnetite for Fe(II) 167 sample was obtained. The detection limits and linear range of this method for iron were 1.0 and 9.0 - 175 ng.mL⁻¹, respectively. Also the relative standard deviation for five replicate determinations of 30.00 ng.mL^-1 Fe²⁺ was 2.3%.

Keywords: Alumina-Coated magnetite nanoparticles, Magnetic Mixed Hemimicell Solid-Phase Extraction, Fe(ΙΙ) and Fe(ΙΙΙ), pharmaceutical sample

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Authors: Dileep Maarisetty, Janaki Komandur, Saroj S. Baral

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In the current work, photocatalytic degradation of phenol was carried both in UV and visible light to find the slowest step that is limiting the rate of photo-degradation process. Characterization such as XRD, SEM, FT-IR, TEM, XPS, UV-DRS, PL, BET, UPS, ESR and zeta potential experiments were conducted to assess the credibility of catalysts in boosting the photocatalytic activity. To explore the synergy, TiO₂ was doped with graphene and alumina. The orbital hybridization with alumina doping (mediated by graphene) resulted in higher electron transfer from the conduction band of TiO₂ to alumina surface where oxygen reduction reactions (ORR) occur. Besides, the doping of alumina and graphene introduced defects into Ti lattice and helped in improving the adsorptive properties of modified photo-catalyst. Results showed that these defects promoted the oxygen reduction reactions (ORR) on the catalyst’s surface. ORR activity aims at producing reactive oxygen species (ROS). These ROS species oxidizes the phenol molecules which is adsorbed on the surface of photo-catalysts, thereby driving the photocatalytic reactions. Since mass transfer is considered as rate limiting step, various mathematical models were applied to the experimental data to probe the best fit. By varying the parameters, it was found that intra-particle diffusion was the slowest step in the degradation process. Lagergren model gave the best R² values indicating the nature of rate kinetics. Similarly, different adsorption isotherms were employed and realized that Langmuir isotherm suits the best with tremendous increase in uptake capacity (mg/g) of TiO₂-rGO-Al₂O₃ as compared undoped TiO₂. This further assisted in higher adsorption of phenol molecules. The results obtained from experimental, kinetic modelling and adsorption isotherms; it is concluded that apart from changes in surface, optoelectronic and morphological properties that enhanced the photocatalytic activity, the intra-particle diffusion within the catalyst’s pores serve as rate-limiting step in deciding the fate of photo-catalytic degradation of phenol.

Keywords: ORR, phenol degradation, photo-catalyst, rate kinetics

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Authors: Chien-Wan Hun, Shao-Fu Chang, Jheng-En Yang, Chien-Chon Chen, Wern-Dare Jheng

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This research provides a systematic way to study and better understand double nano-tubular structure of alunina (Al2O3) and titania (TiO2). The TiO2 NT was prepared by immersing Al2O3 template in 0.02 M titanium fluoride (TiF4) solution (pH=3) at 25 °C for 120 min, followed by annealing at 450 °C for 1 h to obtain anatase TiO2 NT in the Al2O3 template. Large-scale development of film for nanotube-based CO2 capture and conversion can potentially result in more efficient energy harvesting. In addition, the production process will be relatively environmentally friendly. The knowledge generated by this research will significantly advance research in the area of Al2O3, TiO2, CaO, and Ca2O3 nano-structure film fabrication and applications for CO2 capture and conversion. This green energy source will potentially reduce reliance on carbon-based energy resources and increase interest in science and engineering careers.

Keywords: alumina, titania, nano-tubular, film, CO2

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Authors: Tatyana T. Tabakova, Elitsa N. Kolentsova, Dimitar Y. Dimitrov, Krasimir I. Ivanov, Yordanka G. Karakirova, Petya Cv. Petrova, Georgi V. Avdeev

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The catalytic oxidation of CO and volatile organic compounds (VOCs) is considered as one of the most efficient ways to reduce harmful emissions from various chemical industries. The effectiveness of gold-based catalysts for many reactions of environmental significance was proven during the past three decades. The aim of this work was to combine the favorable features of Au and Cu-Ce mixed oxides in the design of new catalytic materials of improved efficiency and economic viability for removal of air pollutants in waste gases from formaldehyde production. Supported oxides of copper and cerium with Cu: Ce molar ratio 2:1 and 1:5 were prepared by wet impregnation of g-alumina. Gold (2 wt.%) catalysts were synthesized by a deposition-precipitation method. Catalysts characterization was carried out by texture measurements, powder X-ray diffraction, temperature programmed reduction and electron paramagnetic resonance spectroscopy. The catalytic activity in the oxidation of CO, CH₃OH and (CH₃)₂O was measured using continuous flow equipment with fixed bed reactor. Both Cu-Ce/alumina samples demonstrated similar catalytic behavior. The addition of gold caused significant enhancement of CO and methanol oxidation activity (100 % degree of CO and CH₃OH conversion at about 60 and 140 ^oC, respectively). The composition of Cu-Ce mixed oxides affected the performance of gold-based samples considerably. Gold catalyst on Cu-Ce/γ-Al₂O₃ 1:5 exhibited higher activity for CO and CH₃OH oxidation in comparison with Au on Cu-Ce/γ-Al₂O₃ 2:1. The better performance of Au/Cu-Ce 1:5 was related to the availability of highly dispersed gold particles and copper oxide clusters in close contact with ceria.

Keywords: CO and VOCs oxidation, copper oxide, Ceria, gold catalysts

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Authors: Nurcan Tugrul, Funda Demir, Hilal Ozkan, Nur Olgun, Emek Derun

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Geopolymers are aluminosilicate-containing materials. The raw materials of the geopolymerization can be natural material such as kaolinite, metakaolin (calcined kaolinite), clay, diatomite, rock powder or can also be industrial by-products such as fly ash, silica fume, blast furnace slag, rice-husk ash, mine tailing, red mud, waste slag, etc. Reactivity of raw materials in geopolymer production is very important for achieving high reaction grade. Fly ash used in geopolymer production has been calcined to obtain tetrahedral SiO₂ and Al₂O₃ structures. In this study, fly ash calcined at different temperatures (700, 800 and 900 °C), and Al₂O₃ addition (Al₂O₃ at min (0%) and max (100%)) were used to produce geopolymers. HCl dissolution method was applied to determine the geopolymerization percentage of samples and Fourier Transform Infrared (FTIR) Spectroscopy was used to find out the optimum calcination temperature for geopolymerization. According to obtained results, the highest geopolymerization percentage (0% alumina added geopolymer equal to 35.789%; 100% alumina added geopolymer equal to 40.546%) was obtained in samples using fly ash calcined at 800 °C.

Keywords: geopolymer, fly ash, Al₂O₃ addition, calcination

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Authors: Reim A. Almotiri, Manal M. Alkhamisi

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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: S. Gowri, K. Narayanasamy, R. Krishnamurthy

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Plasma spraying, from the point of value engineering, is considered as a cost-effective technique to deposit high performance ceramic coatings on ferrous substrates for use in the aero,automobile,electronics and semiconductor industries. High-performance ceramics such as Alumina, Zirconia, and titania-based ceramics have become a key part of turbine blades,automotive cylinder liners,microelectronic and semiconductor components due to their ability to insulate and distribute heat. However, as the industries continue to advance, improved methods are needed to increase both the flexibility and speed of ceramic processing in these applications. The ceramics mentioned were individually coated on structural steel substrate with NiCr bond coat of 50-70 micron thickness with the final thickness in the range of 150 to 200 microns. Optimal spray parameters were selected based on bond strength and porosity. The 'optimal' processed specimens were super finished by lapping using diamond and green SiC abrasives. Interesting results could be observed as follows: The green SiC could improve the surface finish of lapped surfaces almost as that by diamond in case of alumina and titania based ceramics but the diamond abrasives could improve the surface finish of PSZ better than that by green SiC. The conventional random scratches could be absent in alumina and titania ceramics but in PS those marks were found to be less. However, the flatness accuracy could be improved unto 60 to 85%. The surface finish and geometrical accuracy were measured and modeled. The abrasives in the midrange of their particle size could improve the surface quality faster and better than the particles of size in low and high ranges. From the experimental investigations after lapping process, the optimal lapping time, abrasive size, lapping pressure etc could be evaluated.

Keywords: atmospheric plasma spraying, ceramics, lapping, surface qulaity, optimization

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Authors: Elitsa Kolentsova, Dimitar Dimitrov, Vasko Idakiev, Tatyana Tabakova, Krasimir Ivanov

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Formaldehyde production by selective oxidation of methanol is an important industrial process. The main by-products in the waste gas are CO and dimethyl ether (DME). The idea of this study is to combine the advantages of both Cu-Mn and Cu-Co catalytic systems by obtaining a new mixed Cu-Mn-Co catalyst with high activity and selectivity at the simultaneous oxidation of CO, methanol, and DME. Two basic Cu-Mn samples with high activity were selected for further investigation: (i) manganese-rich Cu-Mn/γ–Al2O3 catalyst with Cu/Mn molar ratio 1:5 and (ii) copper-rich Cu-Mn/γ-Al2O3 catalyst with Cu/Mn molar ratio 2:1. Manganese in these samples was replaced by cobalt in the whole concentration region, and catalytic properties were determined. The results show a general trend of decreasing the activity toward DME oxidation and increasing the activity toward CO and methanol oxidation with the increase of cobalt up to 60% for both groups of catalyst. This general trend, however, contains specific features, depending on the composition of the catalyst and the nature of the oxidized gas. The catalytic activity of the sample with Cu/(Mn+Co) molar ratio of 2:1 is gradually changed with increasing the cobalt content. The activity of the sample with Cu/(Mn+Co) molar ratio of 1: 5 passes through a maximum at 60% manganese replacement by cobalt, probably due to the formation of highly dispersed Co-based spinel structures (Co3O4 and/or MnCo2O4). In conclusion, the present study demonstrates that the Cu-Mn-Co/γ–alumina supported catalysts have enhanced activity toward CO, methanol and DME oxidation. Cu/(Mn+Co) molar ratio 1:5 and Co/Mn molar ratio 1.5 in the active component can ensure successful oxidation of CO, CH3OH and DME. The active component of the mixed Cu-Mn-Co/γ–alumina catalysts consists of at least six compounds - CuO, Co3O4, MnO2, Cu1.5Mn1.5O4, MnCo2O4 and CuCo2O4, depending on the Cu/Mn/Co molar ratio. Chemical composition strongly influences catalytic properties, this effect being quite variable with regards to the different processes.

Keywords: Cu-Mn-Co catalysts, oxidation, carbon oxide, VOCs

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Authors: Prateeksha Mahamallik, Anjali Pal

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In the present study, Co(II)-adsolubilized surfactant modified alumina (SMA) was prepared, and methylene blue (MB) degradation was carried out on Co-SMA surface by visible light photo-Fenton process. The entire reaction proceeded on solid surface as MB was embedded on Co-SMA surface. The reaction followed zero order kinetics. Response surface methodology (RSM) and artificial neural network (ANN) were used for modeling the decolorization of MB by photo-Fenton process as a function of dose of Co-SMA (10, 20 and 30 g/L), initial concentration of MB (10, 20 and 30 mg/L), concentration of H2O2 (174.4, 348.8 and 523.2 mM) and reaction time (30, 45 and 60 min). The prediction capabilities of both the methodologies (RSM and ANN) were compared on the basis of correlation coefficient (R2), root mean square error (RMSE), standard error of prediction (SEP), relative percent deviation (RPD). Due to lower value of RMSE (1.27), SEP (2.06) and RPD (1.17) and higher value of R2 (0.9966), ANN was proved to be more accurate than RSM in order to predict decolorization efficiency.

Keywords: adsolubilization, artificial neural network, methylene blue, photo-fenton process, response surface methodology

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Authors: Surya Prakash Gajagouni, Akram Alfantazi, Imad Barsoum

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Austenitic stainless steels are widely recognized for their exceptional corrosion resistance and mechanical properties, rendering them indispensable materials across various industries from construction to biomedical applications. However, in chloride and high temperature atmosphere it to further enhance their surface properties, anodization has emerged as a promising surface treatment technique. Anodization modifies the surface of stainless steels by creating a protective oxide layer, improving corrosion resistance and imparting additional functional characteristics. This paper explores the structural and corrosion characteristics of anodized austenitic stainless steels (AISI 304) using a two-step anodic technique. We utilized a perchloric acid-based electrolyte followed by an ammonium fluoride-based electrolyte. This sequential approach aimed to cultivate deeper and intricately self-ordered nanopore oxide arrays on a substrate made of 304 stainless steel. Electron Microscopic (SEM and TEM) images revealed nanoporous layered structures with increased length and crack development correlating with higher voltage and anodization time. Surface composition and chemical oxidation state of surface-treated SS were determined using X-ray photoelectron spectroscopy (XPS) techniques, revealing a surface layer rich in Ni and suppressed Cr, resulting in a thin film composed of Ni and Fe oxide compared to untreated SS. Electrochemical studies demonstrated enhanced corrosion resistance in a strong alkaline medium compared to untreated SS. Understanding the intricate relationship between the structural features of anodized stainless steels and their corrosion resistance is crucial for optimizing the performance of these materials in diverse applications. This study aims to contribute to the advancement of surface engineering strategies for enhancing the durability and functionality of austenitic stainless steels in aggressive environments.

Keywords: austenitic stainless steel, anodization, nanoporous oxides, marine corrosion

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