Search results for: TiO2 nanotubes

Authors: Nayeli Camacho, Fernanda Lara-Perez, Carolina Ortega-Portilla, Diego G. Espinosa-Arbelaez, Juan M. Alvarado-Orozco, Guillermo C. Mondragon-Rodriguez

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Ultra-high molecular weight polyethylene (UHMWPE) has been the gold standard material for total knee replacements for almost five decades. Wear damage to UHMWPE articulating surface is inevitable due to the natural sliding and rolling movements of the knee. This generates a considerable amount of wear debris, which results in mechanical instability of the joint, reduces joint mobility, increases pain with detrimental biologic responses, and causes component loosening. The presence of wear particles has been closely related to adverse reactions in the knee joint surrounding tissue, especially for particles in the range of 0.3 to 2 μm. Carbon-based materials possess excellent mechanical properties and have shown great promise in tribological applications. In this study, diamond-like carbon coatings (DLC) and carbon nanotubes (CNTs) were used to decrease the wear rate of ultra-high molecular weight polyethylene. A titanium doped DLC (Ti-DLC) was deposited by magnetron sputtering on stainless steel precision spheres while CNTs were used as a second phase reinforcement in UHMWPE at a concentration of 1.25 wt.%. A comparative tribological analysis of the wear of UHMWPE and UHMWPE-CNTs with a stainless steel counterpart with and without Ti-DLC coating is presented. The experimental wear testing was performed on a pin-on-disc tribometer under dry conditions, using a reciprocating movement with a load of 1 N at a frequency of 2 Hz for 100,000 and 200,000 cycles. The wear tracks were analyzed with high-resolution scanning electron microscopy to determine wear modes and observe the size and shape of the wear debris. Furthermore, profilometry was used to study the depth of the wear tracks and to map the wear of the articulating surface. The wear tracks at 100,000 and 200,000 cycles on all samples were relatively shallow, and they were in the range of average roughness. It was observed that the Ti-DLC coating decreases the mass loss in the UHMWPE and the depth of the wear track. The combination of both carbon-based materials decreased the material loss compared to the system of stainless steel and UHMWPE. Burnishing of the surface was the predominant wear mode observed with all the systems, more subtle for the systems with Ti-DLC coatings. Meanwhile, in the system composed of stainless steel-UHMWPE, the intrinsic surface roughness of the material was completely replaced by the wear tracks.

Keywords: CNT reinforcement, self-lubricating materials, Ti-DLC, UHMWPE tribological performance

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Authors: Hamsasew Hankebo Lemago, Dóra Hessz, Zoltán Erdélyi, Imre Miklós Szilágyi

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Metal oxide inverse opals are a unique class of photocatalysts with a hierarchical structure that mimics the natural opal gemstone. They are composed of a network of interconnected pores, which provides a large surface area and efficient pathways for the transport of light and reactants. Atomic layer deposition (ALD) is a versatile technique for the synthesis of high-precision metal oxide thin films, including inverse opals. ALD allows for precise control over the thickness, composition, and morphology of the synthesized films, making it an ideal technique for the fabrication of photocatalysts with tailored properties. In this study, we report the synthesis of TiO2, ZnO, and Al2O3 inverse opal photocatalysts using thermal or plasma-enhanced ALD. The synthesized photocatalysts were characterized using a variety of techniques, including scanning electron microscopy (SEM)-energy dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), Raman spectroscopy, photoluminescence (PL), ellipsometry, and UV-visible spectroscopy. The results showed that the ALD-synthesized metal oxide inverse opals had a highly ordered structure and a tunable pore size. The PL spectroscopy results showed low recombination rates of photogenerated electron-hole pairs, while the ellipsometry and UV-visible spectroscopy results showed tunable optical properties and band gap energies. The photocatalytic activity of the samples was evaluated by the degradation of methylene blue under visible light irradiation. The results showed that the ALD-synthesized metal oxide inverse opals exhibited high photocatalytic activity, even under visible light irradiation. The composites photocatalysts showed even higher activity than the individual metal oxide inverse opals. The enhanced photocatalytic activity of the composites can be attributed to the synergistic effect between the different metal oxides. For example, Al2O3 can act as a charge carrier scavenger, which can reduce the recombination of photogenerated electron-hole pairs. The ALD-synthesized metal oxide inverse opals and their composites are promising photocatalysts for a variety of applications, such as wastewater treatment, air purification, and energy production. For example, they can be used to remove organic pollutants from wastewater, decompose harmful gases in the air, and produce hydrogen fuel from water.

Keywords: ALD, metal oxide inverse opals, composites, photocatalysis

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Authors: Anjali Vanpariya, Priyanka Marathey, Sakshum Khanna, Roma Patel, Indrajit Mukhopadhyay

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Silicon (Si) is a promising negative electrode material for lithium-ion batteries (LiBs) due to its low cost, non-toxicity, and a high theoretical capacity of 4200 mAhg⁻¹. The primary challenge of the application of Si-based LiBs is large volume expansion (~ 300%) during the charge-discharge process. Incorporation of graphene, carbon nanotubes (CNTs), morphological control, and nanoparticles was utilized as effective strategies to tackle volume expansion issues. However, molten salt methods can resolve the issue, but high-temperature requirement limits its application. For sustainable and practical approach, room temperature (RT) based methods are essentially required. Use of ionic liquids (ILs) for electrodeposition of Si nanostructures can possibly resolve the issue of temperature as well as greener media. In this work, electrodeposition of Si nanoparticles on gold substrate was successfully carried out in the presence of ILs media, 1-butyl-3-methylimidazolium-bis (trifluoromethyl sulfonyl) imide (BMImTf₂N) at room temperature. Cyclic voltammetry (CV) suggests the sequential reduction of Si⁴⁺ to Si²⁺ and then Si nanoparticles (SiNs). The structure and morphology of the electrodeposited SiNs were investigated by FE-SEM and observed interconnected Si nanoparticles of average particle size ⁓100-200 nm. XRD and XPS data confirm the deposition of Si on Au (111). The first discharge-charge capacity of Si anode material has been found to be 1857 and 422 mAhg⁻¹, respectively, at current density 7.8 Ag⁻¹. The irreversible capacity of the first discharge-charge process can be attributed to the solid electrolyte interface (SEI) formation via electrolyte decomposition, and trapped Li⁺ inserted into the inner pores of Si. Pulverization of SiNs results in the creation of a new active site, which facilitates the formation of new SEI in the subsequent cycles leading to fading in a specific capacity. After 20 cycles, charge-discharge profiles have been stabilized, and a reversible capacity of 150 mAhg⁻¹ is retained. Electrochemical impedance spectroscopy (EIS) data shows the decrease in Rct value from 94.7 to 47.6 kΩ after 50 cycles of charge-discharge, which demonstrates the improvements of the interfacial charge transfer kinetics. The decrease in the Warburg impedance after 50 cycles of charge-discharge measurements indicates facile diffusion in fragmented and smaller Si nanoparticles. In summary, Si nanoparticles deposited on gold substrate using ILs as media and characterized well with different analytical techniques. Synthesized material was successfully utilized for LiBs application, which is well supported by CV and EIS data.

Keywords: silicon nanoparticles, ionic liquid, electrodeposition, cyclic voltammetry, Li-ion battery

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Authors: Amir Nourbakhsh Habibabadi, Alireza Ashori

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Context: The growing concern over the management of plastic waste and the high demand for wood-based products have led to the development of wood-plastic composites. Agricultural residues, which are abundantly available, can be used as a source of lignocellulosic fibers in the production of these composites. The use of recycled polymers and nanomaterials is also a promising approach to enhance the mechanical and physical properties of the composites. Research Aim: The aim of this study was to investigate the feasibility of using recycled high-density polyethylene (rHDPE), polypropylene (rPP), and agricultural residues fibers for manufacturing wood-plastic nano-composites. The effects of these materials on the mechanical properties of the composites, specifically tensile and flexural strength, were studied. Methodology: The study utilized an experimental approach where extruders and hot presses were used to fabricate the composites. Five types of cellulosic residues fibers (bagasse, corn stalk, rice straw, sunflower, and canola stem), three levels of nanomaterials (carbon nanotubes, nano silica, and nanoclay), and coupling agent were used to chemically bind the wood/polymer fibers, chemicals, and reinforcement. The mechanical properties of the composites were then analyzed. Findings: The study found that composites made with rHDPE provided moderately superior tensile and flexural properties compared to rPP samples. The addition of agricultural residues in several types of wood-plastic nano-composites significantly improved their bending and tensile properties, with bagasse having the most significant advantage over other lignocellulosic materials. The use of recycled polymers, agricultural residues, and nano-silica resulted in composites with the best strength properties. Theoretical Importance: The study's findings suggest that using agricultural fiber residues as reinforcement in wood/plastic nanocomposites is a viable approach to improve the mechanical properties of the composites. Additionally, the study highlights the potential of using recycled polymers in the development of value-added products without compromising the product's properties. Data Collection and Analysis Procedures: The study collected data on the mechanical properties of the composites using tensile and flexural tests. Statistical analyses were performed to determine the significant effects of the various materials used. Question addressed: Can agricultural residues and recycled polymers be used to manufacture wood-plastic nano-composites with enhanced mechanical properties? Conclusion: The study demonstrates the feasibility of using agricultural residues and recycled polymers in the production of wood-plastic nano-composites. The addition of these materials significantly improved the mechanical properties of the composites, with bagasse being the most effective agricultural residue. The study's findings suggest that composites made from recycled materials can offer value-added products without sacrificing performance.

Keywords: polymer, composites, wood, nano

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Authors: R. Khare, R. V. Gelamo, M. A. More, D. J. Late, Chandra Sekhar Rout

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Graphene emerges out as a promising material for various applications ranging from complementary integrated circuits to optically transparent electrode for displays and sensors. The excellent conductivity and atomic sharp edges of unique two-dimensional structure makes graphene a propitious field emitter. Graphene analogues of other 2D layered materials have emerged in material science and nanotechnology due to the enriched physics and novel enhanced properties they present. There are several advantages of using 2D nanomaterials in field emission based devices, including a thickness of only a few atomic layers, high aspect ratio (the ratio of lateral size to sheet thickness), excellent electrical properties, extraordinary mechanical strength and ease of synthesis. Furthermore, the presence of edges can enhance the tunneling probability for the electrons in layered nanomaterials similar to that seen in nanotubes. Here we report electron emission properties of multilayer graphene and effect of plasma (CO2, O2, Ar and N2) treatment. The plasma treated multilayer graphene shows an enhanced field emission behavior with a low turn on field of 0.18 V/μm and high emission current density of 1.89 mA/cm2 at an applied field of 0.35 V/μm. Further, we report the field emission studies of layered WS2/RGO and SnS2/RGO composites. The turn on field required to draw a field emission current density of 1μA/cm2 is found to be 3.5, 2.3 and 2 V/μm for WS2, RGO and the WS2/RGO composite respectively. The enhanced field emission behavior observed for the WS2/RGO nanocomposite is attributed to a high field enhancement factor of 2978, which is associated with the surface protrusions of the single-to-few layer thick sheets of the nanocomposite. The highest current density of ~800 µA/cm2 is drawn at an applied field of 4.1 V/μm from a few layers of the WS2/RGO nanocomposite. Furthermore, first-principles density functional calculations suggest that the enhanced field emission may also be due to an overlap of the electronic structures of WS2 and RGO, where graphene-like states are dumped in the region of the WS2 fundamental gap. Similarly, the turn on field required to draw an emission current density of 1µA/cm2 is significantly low (almost half the value) for the SnS2/RGO nanocomposite (2.65 V/µm) compared to pristine SnS2 (4.8 V/µm) nanosheets. The field enhancement factor β (~3200 for SnS2 and ~3700 for SnS2/RGO composite) was calculated from Fowler-Nordheim (FN) plots and indicates emission from the nanometric geometry of the emitter. The field emission current versus time plot shows overall good emission stability for the SnS2/RGO emitter. The DFT calculations reveal that the enhanced field emission properties of SnS2/RGO composites are because of a substantial lowering of work function of SnS2 when supported by graphene, which is in response to p-type doping of the graphene substrate. Graphene and 2D analogue materials emerge as a potential candidate for future field emission applications.

Keywords: graphene, layered material, field emission, plasma, doping

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Authors: T. Kuchukhidze, N. Jalagonia, T. Archuadze, G. Bokuchava

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The growing scientific-technological progress in modern civilization causes actuality of producing construction materials which can successfully work in conditions of high temperature, radiation, pressure, speed, and chemically aggressive environment. Such extreme conditions can withstand very few types of materials and among them, ceramic materials are in the first place. Corundum ceramics is the most useful material for creation of constructive nodes and products of various purposes for its low cost, easy accessibility to raw materials and good combination of physical-chemical properties. However, ceramic composite materials have one disadvantage; they are less plastics and have lower toughness. In order to increase the plasticity, the ceramics are reinforced by various dopants, that reduces the growth of the cracks. It is shown, that adding of even small amount of carbon fibers and carbon nanotubes (CNT) as reinforcing material significantly improves mechanical properties of the products, keeping at the same time advantages of alundum ceramics. Graphene in composite material acts in the same way as inorganic dopants (MgO, ZrO2, SiC and others) and performs the role of aluminum oxide inhibitor, as it creates shell, that gives possibility to reduce sintering temperature and at the same time it acts as damper, because scattering of a shock wave takes place on carbon structures. Application of different structural modification of carbon (graphene, nanotube and others) as reinforced material, gives possibility to create multi-purpose highly requested composite materials based on alundum ceramics. In the present work offers simplified technology for obtaining of aluminum oxide ceramics, reinforced with carbon nanostructures, during which chemical modification with doping carbon nanostructures will be implemented in the process of synthesis of final powdery composite – Alumina. In charge doping carbon nanostructures connected to matrix substance with C-O-Al bonds, that provide their homogeneous spatial distribution. In ceramic obtained as a result of consolidation of such powders carbon fragments equally distributed in the entire matrix of aluminum oxide, that cause increase of bending strength and crack-resistance. The proposed way to prepare the charge simplifies the technological process, decreases energy consumption, synthesis duration and therefore requires less financial expenses. In the implementation of this work, modern instrumental methods were used: electronic and optical microscopy, X-ray structural and granulometric analysis, UV, IR, and Raman spectroscopy.

Keywords: ceramic materials, α-Al₂O₃, carbon nanostructures, composites, characterization, hot-pressing

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Authors: Jyh Sheen, Yong-Lin Wang

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This research dedicates to find a different measurement procedure of microwave dielectric properties of ceramic materials with high dielectric constants. For the composite of ceramic dispersed in the polymer matrix, the dielectric constants of the composites with different concentrations can be obtained by various mixture equations. The other development of mixture rule is to calculate the permittivity of ceramic from measurements on composite. To do this, the analysis method and theoretical accuracy on six basic mixture laws derived from three basic particle shapes of ceramic fillers have been reported for dielectric constants of ceramic less than 40 at microwave frequency. Similar researches have been done for other well-known mixture rules. They have shown that both the physical curve matching with experimental results and low potential theory error are important to promote the calculation accuracy. Recently, a modified of mixture equation for high dielectric constant ceramics at microwave frequency has also been presented for strontium titanate (SrTiO3) which was selected from five more well known mixing rules and has shown a good accuracy for high dielectric constant measurements. However, it is still not clear the accuracy of this modified equation for other high dielectric constant materials. Therefore, the five more well known mixing rules are selected again to understand their application to other high dielectric constant ceramics. The other high dielectric constant ceramic, TiO2 with dielectric constant 100, was then chosen for this research. Their theoretical error equations are derived. In addition to the theoretical research, experimental measurements are always required. Titanium dioxide is an interesting ceramic for microwave applications. In this research, its powder is adopted as the filler material and polyethylene powder is like the matrix material. The dielectric constants of those ceramic-polyethylene composites with various compositions were measured at 10 GHz. The theoretical curves of the five published mixture equations are shown together with the measured results to understand the curve matching condition of each rule. Finally, based on the experimental observation and theoretical analysis, one of the five rules was selected and modified to a new powder mixture equation. This modified rule has show very good curve matching with the measurement data and low theoretical error. We can then calculate the dielectric constant of pure filler medium (titanium dioxide) by those mixing equations from the measured dielectric constants of composites. The accuracy on the estimating dielectric constant of pure ceramic by various mixture rules will be compared. This modified mixture rule has also shown good measurement accuracy on the dielectric constant of titanium dioxide ceramic. This study can be applied to the microwave dielectric properties measurements of other high dielectric constant ceramic materials in the future.

Keywords: microwave measurement, dielectric constant, mixture rules, composites

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Authors: Augustus K. Lebechi, Kenneth I. Ozoemena

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Rechargeable zinc-air batteries (RZABs) have been described as one of the most viable next-generation ‘beyond-the-lithium-ion’ battery technologies with great potential for renewable energy storage. It is safe, with a high specific energy density (1086 Wh/kg), environmentally benign, and low-cost, especially in resource-limited African countries. For widespread commercialization, the sluggish oxygen reaction kinetics pose a major challenge that impedes the reversibility of the system. Hence, there is a need for low-cost and highly active bifunctional electrocatalysts. Manganese oxide catalysts on carbon conducting additives remain the best couple for the realization of such low-cost RZABs. In this work, hausmannite Mn₃O₄ nanoparticles were synthesized through the annealing method from commercial electrolytic manganese dioxide (EMD), multi-walled carbon nanotubes (MWCNTs) were synthesized via the chemical vapor deposition (CVD) method and carbon nanofibers (CNFs) were synthesized via the electrospinning process with subsequent carbonization. Both Mn₃O₄ catalysts and the carbon conducting additives (MWCNT and CNF) were thoroughly characterized using X-ray powder diffraction spectroscopy (XRD), scanning electron microscopy (SEM), thermogravimetry analysis (TGA) and X-ray photoelectron spectroscopy (XPS). Composite electrocatalysts (Mn₃O₄/CNT and Mn₃O₄/CNF) were investigated for oxygen evolution reaction (OER) and oxygen reduction reaction (ORR) in an alkaline medium. Using the established electrocatalytic modalities for evaluating the electrocatalytic performance of materials (including double layer, electrochemical active surface area, roughness factor, specific current density, and catalytic stability), CNFs proved to be the most efficient conducting additive material for the Mn₃O₄ catalyst. From the DFT calculations, the higher performance of the CNFs over the MWCNTs is related to the ability of the CNFs to allow for a more favorable distribution of the d-electrons of the manganese (Mn) and enhanced synergistic effect with Mn₃O₄ for weaker adsorption energies of the oxygen intermediates (O*, OH* and OOH*). In a proof-of-concept, Mn₃O₄/CNF was investigated as the air cathode for rechargeable zinc-air battery (RZAB) in a micro-3D-printed cell configuration. The RZAB showed good performance in terms of open circuit voltage (1.77 V), maximum power density (177.5 mW cm-2), areal-discharge energy and cycling stability comparable to Pt/C (20 wt%) + IrO2. The findings here provide fresh physicochemical perspectives on the future design and utility of CNFs for developing manganese-based RZABs.

Keywords: bifunctional electrocatalyst, oxygen evolution reaction, oxygen reduction reactions, rechargeable zinc-air batteries.

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Authors: Chiao-Cheng Huang, Pei-Te Chiueh, Ya-Hsuan Liou

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Chromium-contaminated wastewater from electroplating industrial activity has been a long-standing environmental issue, as it can degrade surface water quality and is harmful to soil ecosystems. The traditional method of treating chromium-contaminated wastewater has been to use chemical coagulation processes. However, this method consumes large amounts of chemicals such as sulfuric acid, sodium hydroxide, and sodium bicarbonate in order to remove chromium. However, a series of new methods for treating chromium-containing wastewater have been developed. This study aimed to compare the environmental impact of four different lab scale chromium removal processes: 1.) chemical coagulation process (the most common and traditional method), in which sodium metabisulfite was used as reductant, 2.) electrochemical process using two steel sheets as electrodes, 3.) reduction by iron-copper bimetallic powder, and 4.) photocatalysis process by TiO2. Each process was run in the lab, and was able to achieve 100% removal of chromium in solution. Then a Life Cycle Assessment (LCA) study was conducted based on the experimental data obtained from four different case studies to identify the environmentally preferable alternative to treat chromium wastewater. The model used for calculating the environmental impact was TRACi, and the system scope includes the production phase and use phase of chemicals and electricity consumed by the chromium removal processes, as well as the final disposal of chromium containing sludge. The functional unit chosen in this study was the removal of 1 mg of chromium. Solution volume of each case study was adjusted to 1 L in advance and the chemicals and energy consumed were proportionally adjusted. The emissions and resources consumed were identified and characterized into 15 categories of midpoint impacts. The impact assessment results show that the human ecotoxicity category accounts for 55 % of environmental impact in Case 1, which can be attributed to the sulfuric acid used for pH adjustment. In Case 2, production of steel sheet electrodes is an energy-intensive process, thus contributed to 20 % of environmental impact. In Case 3, sodium bicarbonate is used as an anti-corrosion additive, which results mainly in 1.02E-05 Comparative Toxicity Unit (CTU) in the human toxicity category and 0.54E-05 (CTU) in acidification of air. In Case 4, electricity consumption for power supply of UV lamp gives 5.25E-05 (CTU) in human toxicity category, 1.15E-05 (kg Neq) in eutrophication. In conclusion, Case 3 and Case 4 have higher environmental impacts than Case 1 and Case 2, which can be attributed mostly to higher energy and chemical consumption, leading to high impacts in the global warming and ecotoxicity categories.

Keywords: chromium, lab scale, life cycle assessment, wastewater

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Authors: Jana Andzane, Gunta Kunakova, Margarita Baitimirova, Mikelis Marnauza, Floriana Lombardi, Donats Erts

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Bismuth selenide (Bi₂Se₃) is known as a narrow band gap semiconductor with pronounced thermoelectric (TE) and topological insulator (TI) properties. Unique TI properties offer exciting possibilities for fundamental research as observing the exciton condensate and Majorana fermions, as well as practical application in spintronic and quantum information. In turn, TE properties of this material can be applied for wide range of thermoelectric applications, as well as for broadband photodetectors and near-infrared sensors. Nanostructuring of this material results in improvement of TI properties due to suppression of the bulk conductivity, and enhancement of TE properties because of increased phonon scattering at the nanoscale grains and interfaces. Regarding TE properties, crystallographic growth direction, as well as orientation of the nanostructures relative to the growth substrate, play significant role in improvement of TE performance of nanostructured material. For instance, Bi₂Se₃ layers consisting of randomly oriented nanostructures and/or of combination of them with planar nanostructures show significantly enhanced in comparison with bulk and only planar Bi₂Se₃ nanostructures TE properties. In this work, a catalyst-free vapour-solid deposition technique was applied for controlled obtaining of different types of Bi₂Se₃ nanostructures and continuous nanostructured layers for targeted applications. For example, separated Bi₂Se₃ nanoplates, nanobelts and nanowires can be used for investigations of TI properties; consisting from merged planar and/or randomly oriented nanostructures Bi₂Se₃ layers are useful for applications in heat-to-power conversion devices and infrared detectors. The vapour-solid deposition was carried out using quartz tube furnace (MTI Corp), equipped with an inert gas supply and pressure/temperature control system. Bi₂Se₃ nanostructures/nanostructured layers of desired type were obtained by adjustment of synthesis parameters (process temperature, deposition time, pressure, carrier gas flow) and selection of deposition substrate (glass, quartz, mica, indium-tin-oxide, graphene and carbon nanotubes). Morphology, structure and composition of obtained Bi₂Se₃ nanostructures and nanostructured layers were inspected using SEM, AFM, EDX and HRTEM techniques, as well as home-build experimental setup for thermoelectric measurements. It was found that introducing of temporary carrier gas flow into the process tube during the synthesis and deposition substrate choice significantly influence nanostructures formation mechanism. Electrical, thermoelectric, and topological insulator properties of different types of deposited Bi₂Se₃ nanostructures and nanostructured coatings are characterized as a function of thickness and discussed.

Keywords: bismuth seleinde, nanostructures, topological insulator, vapour-solid deposition

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Authors: Ahmad Kayvani Fard, Gordon Mckay, Muataz Hussien

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Adsorption/sorption is believed to be one of the optimal processes for the removal of heavy metals from water due to its low operational and capital cost as well as its high removal efficiency. Different materials have been reported in literature as adsorbent for heavy metal removal in waste water such as natural sorbents, organic polymers (synthetic) and mineral materials (inorganic). The selection of adsorbents and development of new functional materials that can achieve good removal of heavy metals from water is an important practice and depends on many factors, such as the availability of the material, cost of material, and material safety and etc. In this study we reported the synthesis of doped Activated carbon and Carbon nanotube (CNT) with different loading of metal oxide nanoparticles such as Fe2O3, Fe3O4, Al2O3, TiO2, SiO2 and Ag nanoparticles and their application in removal of heavy metals, hydrocarbon, and organics from waste water. Commercial AC and CNT with different loadings of mentioned nanoparticle were prepared and effect of pH, adsorbent dosage, sorption kinetic, and concentration effects are studied and optimum condition for removal of heavy metals from water is reported. The prepared composite sorbent is characterized using field emission scanning electron microscopy (FE-SEM), high transmission electron microscopy (HR-TEM), thermogravimetric analysis (TGA), X-ray diffractometer (XRD), the Brunauer, Emmett and Teller (BET) nitrogen adsorption technique, and Zeta potential. The composite materials showed higher removal efficiency and superior adsorption capacity compared to commercially available carbon based adsorbent. The specific surface area of AC increased by 50% reaching up to 2000 m2/g while the CNT specific surface area of CNT increased by more than 8 times reaching value of 890 m2/g. The increased surface area is one of the key parameters along with surface charge of the material determining the removal efficiency and removal efficiency. Moreover, the surface charge density of the impregnated CNT and AC have enhanced significantly where can benefit the adsorption process. The nanoparticles also enhance the catalytic activity of material and reduce the agglomeration and aggregation of material which provides more active site for adsorbing the contaminant from water. Some of the results for treating wastewater includes 100% removal of BTEX, arsenic, strontium, barium, phenolic compounds, and oil from water. The results obtained are promising for the use of AC and CNT loaded with metal oxide nanoparticle in treatment and pretreatment of waste water and produced water before desalination process. Adsorption can be very efficient with low energy consumption and economic feasibility.

Keywords: carbon nanotube, activated carbon, adsorption, heavy metal, water treatment

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Authors: A. Saravanan, B. R. Huang, C. J. Yeh, K. C. Leou, I. N. Lin

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A new class of ultra-nano diamond-graphite nano-hybrid (DGH) composite materials containing nano-sized diamond needles was developed at low temperature process. Such kind of diamond- graphite nano-hybrid composite nanowires exhibit high electrical conductivity and excellent electron field emission (EFE) properties. Few earlier reports mention that addition of N2 gas to the growth plasma requires high growth temperature (800°C) to trigger the dopants to generate the conductivity in the films. High growth temperature is not familiar with the Si-based device fabrications. We have used a novel process such as bias-enhanced-grown (beg) MPECVD process to grow diamond films at low substrate temperature (450°C). We observed that the beg-N/UNCD films thus obtained possess high conductivity of σ=987 S/cm, ever reported for diamond films with excellent Electron field emission (EFE) properties. TEM investigation indicated that these films contain needle-like diamond grains about 5 nm in diameter and hundreds of nanometers in length. Each of the grains was encased in graphitic layers about tens of nano-meters in thickness. These materials properties suitable for more specific applications, such as high conductivity for electron field emitters, high robustness for microplasma cathodes and high electrochemical activity for electro-chemical sensing. Subsequently, other hand, the highly conducting DGH films were coated on vertically aligned ZnO nanorods, there is no prior nucleation or seeding process needed due to the use of BEG method. Such a composite structure provides significant enhancement in the field emission characteristics of the cold cathode was observed with ultralow turn on voltage 1.78 V/μm with high EFE current density of 3.68 mA/ cm2 (at 4.06V/μm) due to decoration of DGH material on ZnO nanorods. The DGH/ZNRs based device get stable emission for longer duration of 562min than bare ZNRs (104min) without any current degradation because the diamond coating protects the ZNRs from ion bombardment when they are used as the cathode for microplasma devices. The potential application of these materials is demonstrated by the plasma illumination measurements that ignited the plasma at the minimum voltage by 290 V. The photoresponse (Iphoto/Idark) behavior of the DGH/ZNRs based photodetectors exhibits a much higher photoresponse (1202) than bare ZNRs (229). During the process the electron transport is easy from ZNRs to DGH through graphitic layers, the EFE properties of these materials comparable to other primarily used field emitters like carbon nanotubes, graphene. The DGH/ZNRs composite also providing a possibility of their use in flat panel, microplasma and vacuum microelectronic devices.

Keywords: bias-enhanced nucleation and growth, ZnO nanorods, electrical conductivity, electron field emission, photo-detectors

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Authors: Ana M. Antolín, Sandra Contreras, Francesc Medina, Didier Tichit

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Introduction: High levels of nitrates (> 50 ppm NO3-) in drinking water are potentially risky to human health. In the recent years, the trend of nitrate concentration in groundwater is rising in the EU and other countries. Conventional catalytic nitrate reduction processes into N2 and H2O lead to some toxic intermediates and by-products, such as NO2-, NH4+, and NOx gases. Alternatively, photocatalytic nitrate removal using solar irradiation and heterogeneous catalysts is a very promising and ecofriendly technique. It has been scarcely performed and more research on highly efficient catalysts is still needed. In this work, different nanocatalysts supported on Aeroxide Titania P25 (P25) have been prepared varying: 0.5-4 % wt. Ag); Pt (2, 4 % wt.); Pt precursor (H2PtCl6/K2PtCl6); and impregnation order of both metals. Pt was chosen in order to increase the selectivity to N2 and decrease that to NO2-. Catalysts were characterized by nitrogen physisorption, X-Ray diffraction, UV-visible spectroscopy, TEM and X Ray-Photoelectron Spectroscopy. The aim was to determine the influence of the composition and the preparation method of the catalysts on the conversion and selectivity in the nitrate reduction, as well as going through an overall and better understanding of the process. Nanocatalysts synthesis: For the mono and bimetallic catalysts preparation, wise-drop wetness impregnation of the precursors (AgNO3, H2PtCl6, K2PtCl6) followed by a reduction step (NaBH4) was used to obtain the metal colloids. Results and conclusions: Denitration experiments were performed in a 350 mL PTFE batch reactor under inert standard operational conditions, ultraviolet irradiations (λ=254 nm (UV-C); λ=365 nm (UV-A)), and presence/absence of hydrogen gas as a reducing agent, contrary to most studies using oxalic or formic acid. Samples were analyzed by Ionic Chromatography. Blank experiments using respectively P25 (dark conditions), hydrogen only and UV irradiations without hydrogen demonstrated a clear influence of the presence of hydrogen on nitrate reduction. Also, they demonstrated that UV irradiation increased the selectivity to N2. Interestingly, the best activity was obtained under ultraviolet lamps, especially at a closer wavelength to visible light irradiation (λ = 365 nm) and H2. 2% Ag/P25 leaded to the highest NO3- conversion among the monometallic catalysts. However, nitrite quantities have to be diminished. On the other hand, practically no nitrate conversion was observed with the monometallics based on Pt/P25. Therefore, the amount of 2% Ag was chosen for the bimetallic catalysts. Regarding the bimetallic catalysts, it is observed that the metal impregnation order, amount and Pt precursor highly affects the results. Higher selectivity to the desirable N2 gas is obtained when Pt was firstly added, especially with K2PtCl6 as Pt precursor. This suggests that when Pt is secondly added, it covers the Ag particles, which are the most active in this reaction. It could be concluded that Ag allows the nitrate reduction step to nitrite, and Pt the nitrite reduction step toward the desirable N2 gas.

Keywords: heterogeneous catalysis, hydrogenation, nanocatalyst, nitrate removal, photocatalysis

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Authors: Sankha Chakrabortty, Biswajit Ruj, Parimal Pal

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Methanol is one of the most important chemical products and intermediates. It can be used as a solvent, intermediate or raw material for a number of higher valued products, fuels or additives. From the last one decay, the total global demand of methanol has increased drastically which forces the scientists to produce a large amount of methanol from a renewable source to meet the global demand with a sustainable way. Different types of non-renewable based raw materials have been used for the synthesis of methanol on a large scale which makes the process unsustainable. In this circumstances, photocatalytic conversion of CO₂ into methanol under solar/UV excitation becomes a viable approach to give a sustainable production approach which not only meets the environmental crisis by recycling CO₂ to fuels but also reduces CO₂ amount from the atmosphere. Development of such sustainable production approach for CO₂ conversion into methanol still remains a major challenge in the current research comparing with conventional energy expensive processes. In this backdrop, the development of environmentally friendly materials, like photocatalyst has taken a great perspective for methanol synthesis. Scientists in this field are always concerned about finding an improved photocatalyst to enhance the photocatalytic performance. Graphene-based hybrid and composite materials with improved properties could be a better nanomaterial for the selective conversion of CO₂ to methanol under visible light (solar energy) or UV light. The present invention relates to synthesis an improved heterogeneous graphene-based photocatalyst with improved catalytic activity and surface area. Graphene with enhanced surface area is used as coupled material of copper-loaded titanium oxide to improve the electron capture and transport properties which substantially increase the photoinduced charge transfer and extend the lifetime of photogenerated charge carriers. A fast reduction method through H₂ purging has been adopted to synthesis improved graphene whereas ultrasonication based sol-gel method has been applied for the preparation of graphene coupled copper loaded titanium oxide with some enhanced properties. Prepared photocatalysts were exhaustively characterized using different characterization techniques. Effects of catalyst dose, CO₂ flow rate, reaction temperature and stirring time on the efficacy of the system in terms of methanol yield and productivity have been studied in the present study. The study shown that the newly synthesized photocatalyst with an enhanced surface resulting in a sustained productivity and yield of methanol 0.14 g/Lh, and 0.04 g/gcat respectively, after 3 h of illumination under UV (250W) at an optimum catalyst dosage of 10 g/L having 1:2:3 (Graphene: TiO₂: Cu) weight ratio.

Keywords: renewable energy, CO₂ capture, photocatalytic conversion, methanol

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Authors: Prateek Goyal, Archini Paruthi, Superb K. Misra

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Contamination of water resources has been a major concern, which has drawn attention to the need to develop new material models for treatment of effluents. Existing conventional waste water treatment methods remain ineffective sometimes and uneconomical in terms of remediating contaminants like heavy metal ions (mercury, arsenic, lead, cadmium and chromium); organic matter (dyes, chlorinated solvents) and high salt concentration, which makes water unfit for consumption. We believe that nanotechnology based strategy, where we use nanoparticles as a tool to remediate a class of pollutants would prove to be effective due to its property of high surface area to volume ratio, higher selectivity, sensitivity and affinity. In recent years, scientific advancement has been made to study the application of photocatalytic (ZnO, TiO2 etc.) nanomaterials and magnetic nanomaterials in remediating contaminants (like heavy metals and organic dyes) from water/wastewater. Our study focuses on the synthesis and monitoring remediation efficiency of ZnO, Fe3O4 and Fe3O4 coated ZnO nanoparticulate system for the removal of heavy metals and dyes simultaneously. Multitude of ZnO nanostructures (spheres, rods and flowers) using multiple routes (microwave & hydrothermal approach) offers a wide range of light active photo catalytic property. The phase purity, morphology, size distribution, zeta potential, surface area and porosity in addition to the magnetic susceptibility of the particles were characterized by XRD, TEM, CPS, DLS, BET and VSM measurements respectively. Further on, the introduction of crystalline defects into ZnO nanostructures can also assist in light activation for improved dye degradation. Band gap of a material and its absorbance is a concrete indicator for photocatalytic activity of the material. Due to high surface area, high porosity and affinity towards metal ions and availability of active surface sites, iron oxide nanoparticles show promising application in adsorption of heavy metal ions. An additional advantage of having magnetic based nanocomposite is, it offers magnetic field responsive separation and recovery of the catalyst. Therefore, we believe that ZnO linked Fe3O4 nanosystem would be efficient and reusable. Improved photocatalytic efficiency in addition to adsorption for environmental remediation has been a long standing challenge, and the nano-composite system offers the best of features which the two individual metal oxides provide for nanoremediation.

Keywords: adsorption, nanocomposite, nanoremediation, photocatalysis

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Authors: Yohann R. J. Thomas, Sébastien Solan

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Conventional battery technology includes the assembly of electrode/separator/electrode by standard techniques such as stacking or winding, depending on the format size. In that type of batteries, coating or pasting techniques are only used for the electrode process. The processes are suited for large scale production of batteries and perfectly adapted to plenty of application requirements. Nevertheless, as the demand for both easier and cost-efficient production modes, flexible, custom-shaped and efficient small sized batteries is rising. Thin-film, printable batteries are one of the key areas for printed electronics. In the frame of European BASMATI project, we are investigating the feasibility of a new design of lithium-ion battery: interdigitated planar core design. Polymer substrate is used to produce bendable and flexible rechargeable accumulators. Direct fully printed batteries lead to interconnect the accumulator with other electronic functions for example organic solar cells (harvesting function), printed sensors (autonomous sensors) or RFID (communication function) on a common substrate to produce fully integrated, thin and flexible new devices. To fulfill those specifications, a high resolution printing process have been selected: Aerosol jet printing. In order to fit with this process parameters, we worked on nanomaterials formulation for current collectors and electrodes. In addition, an advanced printed polymer-electrolyte is developed to be implemented directly in the printing process in order to avoid the liquid electrolyte filling step and to improve safety and flexibility. Results: Three different current collectors has been studied and printed successfully. An ink of commercial copper nanoparticles has been formulated and printed, then a flash sintering was applied to the interdigitated design. A gold ink was also printed, the resulting material was partially self-sintered and did not require any high temperature post treatment. Finally, carbon nanotubes were also printed with a high resolution and well defined patterns. Different electrode materials were formulated and printed according to the interdigitated design. For cathodes, NMC and LFP were efficaciously printed. For anodes, LTO and graphite have shown to be good candidates for the fully printed battery. The electrochemical performances of those materials have been evaluated in a standard coin cell with lithium-metal counter electrode and the results are similar with those of a traditional ink formulation and process. A jellified plastic crystal solid state electrolyte has been developed and showed comparable performances to classical liquid carbonate electrolytes with two different materials. In our future developments, focus will be put on several tasks. In a first place, we will synthesize and formulate new specific nano-materials based on metal-oxyde. Then a fully printed device will be produced and its electrochemical performance will be evaluated.

Keywords: high resolution digital printing, lithium-ion battery, nanomaterials, solid-state electrolytes

Procedia PDF Downloads 223

Authors: Mayoorika Shukla, Pramila Jakhar, Tejendra Dixit, I. A. Palani, Vipul Singh

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Biosensors are analytical devices with wide range of applications in biological, chemical, environmental and clinical analysis. It comprises of bio-recognition layer which has biomolecules (enzymes, antibodies, DNA, etc.) immobilized over it for detection of analyte and transducer which converts the biological signal into the electrical signal. The performance of biosensor primarily the depends on the bio-recognition layer and therefore it has to be chosen wisely. In this regard, nanostructures of metal oxides such as ZnO, SnO2, V2O5, and TiO2, etc. have been explored extensively as bio-recognition layer. Recently, ZnO has the attracted attention of researchers due to its unique properties like high iso-electric point, biocompatibility, stability, high electron mobility and high electron binding energy, etc. Although there have been many reports on usage of ZnO as bio-recognition layer but to the authors’ knowledge, none has ever observed correlation between optical properties like defect suppression and biosensing capability of the sensor. Here, ZnO nanorods (ZNR) have been synthesized by a low cost, simple and low-temperature hydrothermal growth process, over Platinum (Pt) coated glass substrate. The ZNR have been synthesized in two steps viz. initially a seed layer was coated over substrate (Pt coated glass) followed by immersion of it into nutrient solution of Zinc nitrate and Hexamethylenetetramine (HMTA) with in situ addition of KMnO4. The addition of KMnO4 was observed to have a profound effect over the growth rate anisotropy of ZnO nanostructures. Clustered and powdery growth of ZnO was observed without addition of KMnO4, although by addition of it during the growth, uniform and crystalline ZNR were found to be grown over the substrate. Moreover, the same has resulted in suppression of defects as observed by Normalized Photoluminescence (PL) spectra since KMnO4 is a strong oxidizing agent which provides an oxygen rich growth environment. Further, to explore the correlation between defect suppression and biosensing capability of the ZNR Glucose oxidase (Gox) was immobilized over it, using physical adsorption technique followed by drop casting of nafion. Here the main objective of the work was to analyze effect of defect suppression over biosensing capability, and therefore Gox has been chosen as model enzyme, and electrochemical amperometric glucose detection was performed. The incorporation of KMnO4 during growth has resulted in variation of optical and charge transfer properties of ZNR which in turn were observed to have deep impact on biosensor figure of merits. The sensitivity of biosensor was found to increase by 12-18 times, due to variations introduced by addition of KMnO4 during growth. The amperometric detection of glucose in continuously stirred buffer solution was performed. Interestingly, defect suppression has been observed to contribute towards the improvement of biosensor performance. The detailed mechanism of growth of ZNR along with the overall influence of defect suppression on the sensing capabilities of the resulting enzymatic electrochemical biosensor and different figure of merits of the biosensor (Glass/Pt/ZNR/Gox/Nafion) will be discussed during the conference.

Keywords: biosensors, defects, KMnO4, ZnO nanorods

Procedia PDF Downloads 252

Authors: Francisco Pereira, António Augusto Vicente, Filipe Vaz, Joel Borges, Pedro Geada

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Light is a growth-limiting factor in microalgae cultivation, where factors like spectral components, intensity, and duration, often characterized by its wavelength, are well-reported to have a substantial impact on cell growth rates and, consequently, photosynthetic performance and mitigation of CO2, one of the most significant greenhouse gases (GHGs). Photobioreactors (PBRs) are commonly used to grow microalgae under controlled conditions, but they often fail to provide an even light distribution to the cultures. For this reason, there is a pressing need for innovations aiming at enhancing the efficient utilization of light. So, one potential approach to address this issue is by implementing plasmonic films, such as the localized surface plasmon resonance (LSPR). LSPR is an optical phenomenon connected to the interaction of light with metallic nanostructures. LSPR excitation is characterized by the oscillation of unbound conduction electrons of the nanoparticles coupled with the electromagnetic field from incident light. As a result of this excitation, highly energetic electrons and a strong electromagnetic field are generated. These effects lead to an amplification of light scattering, absorption, and extinction of specific wavelengths, contingent on the nature of the employed nanoparticle. Thus, microalgae might benefit from this biotechnology as it enables the selective filtration of inhibitory wavelengths and harnesses the electromagnetic fields produced, which could lead to enhancements in both biomass and metabolite productivity. This study aimed at implementing and evaluating a “plasmon-enhanced PBR”. The goal was to utilize LSPR thin films to enhance the growth and CO2 bio-fixation rate of Chlorella vulgaris. The internal/external walls of the PBRs were coated with a TiO2 matrix containing different nanoparticles (Au, Ag, and Au-Ag) in order to evaluate the impact of this approach on microalgae’s performance. Plasmonic films with distinct compositions resulted in different Chlorella vulgaris growth, ranging from 4.85 to 6.13 g.L-1. The highest cell concentrations were obtained with the metallic Ag films, demonstrating a 14% increase compared to the control condition. Moreover, it appeared to be no differences in growth between PBRs with inner and outer wall coatings. In terms of CO2 bio-fixation, distinct rates were obtained depending on the coating applied, ranging from 0.42 to 0.53 gCO2L-1d-1. Ag coating was demonstrated to be the most effective condition for carbon fixation by C. vulgaris. The impact of LSPR films on the biochemical characteristics of biomass (e.g., proteins, lipids, pigments) was analysed as well. Interestingly, Au coating yielded the most significant enhancements in protein content and total pigments, with increments of 15 % and 173 %, respectively, when compared to the PBR without any coating (control condition). Overall, the incorporation of plasmonic films in PBRs seems to have the potential to improve the performance and efficiency of microalgae cultivation, thereby representing an interesting approach to increase both biomass production and GHGs bio-mitigation.

Keywords: CO₂ bio-fixation, plasmonic effect, photobioreactor, photosynthetic microalgae

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Authors: Cristina Diaz, Lucia Perez, Simone Visigalli, Giuseppe Di Florio, Gonzalo Fuentes, Roberto Canziani, Paolo Gronchi

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During the last 50 years, the selection of materials is one of the main decisions in machine design for different industrial applications. It is due to numerous physical, chemical, mechanical and technological factors to consider in it. Corrosion effects are related with all of these factors and impact in the life cycle, machine incidences and the costs for the life of the machine. Corrosion affects the deterioration or destruction of metals due to the reaction with the environment, generally wet. In food industry, dewatering industry, concrete industry, paper industry, etc. corrosion is an unsolved problem and it might introduce some alterations of some characteristics in the final product. Nowadays, depending on the selected metal, its surface and its environment of work, corrosion prevention might be a change of metal, use a coating, cathodic protection, use of corrosion inhibitors, etc. In the vast majority of the situations, use of a corrosion resistant material or in its defect, a corrosion protection coating is the solution. Stainless steels are widely used in machine design, because of their strength, easily cleaned capacity, corrosion resistance and appearance. Typical used are AISI 304 and AISI 316. However, their benefits don’t fit every application, and some coatings are required against corrosion such as some paintings, galvanizing, chrome plating, SiO₂, TiO₂ or ZrO₂ coatings, etc. In this work, some coatings based in a bilayer made of Titanium-Tantalum, Titanium-Niobium, Titanium-Hafnium or Titanium-Zirconium, have been developed used magnetron sputtering configuration by PVD (Physical Vapor Deposition) technology, for trying to reduce corrosion effects on AISI 304, AISI 316 and comparing it with Titanium alloy substrates. Ti alloy display exceptional corrosion resistance to chlorides, sour and oxidising acidic media and seawater. In this study, Ti alloy (99%) has been included for comparison with coated AISI 304 and AISI 316 stainless steel. Corrosion tests were conducted by a Gamry Instrument under ASTM G5-94 standard, using different electrolytes such as tomato salsa, wine, olive oil, wet compost, a mix of sand and concrete with water and NaCl for testing corrosion in different industrial environments. In general, in all tested environments, the results showed an improvement of corrosion resistance of all coated AISI 304 and AISI 316 stainless steel substrates when they were compared to uncoated stainless steel substrates. After that, comparing these results with corrosion studies on uncoated Ti alloy substrate, it was observed that in some cases, coated stainless steel substrates, reached similar current density that uncoated Ti alloy. Moreover, Titanium-Zirconium and Titanium-Tantalum coatings showed for all substrates in study including coated Ti alloy substrates, a reduction in current density more than two order in magnitude. As conclusion, Ti-Ta, Ti-Zr, Ti-Nb and Ti-Hf coatings have been developed for improving corrosion resistance of AISI 304 and AISI 316 materials. After corrosion tests in several industry environments, substrates have shown improvements on corrosion resistance. Similar processes have been carried out in Ti alloy (99%) substrates. Coated AISI 304 and AISI 316 stainless steel, might reach similar corrosion protection on the surface than uncoated Ti alloy (99%). Moreover, coated Ti Alloy (99%) might increase its corrosion resistance using these coatings.

Keywords: coatings, corrosion, PVD, stainless steel

Procedia PDF Downloads 122

Authors: Mingqian Zhang

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Tip-enhanced Raman spectroscopy (TERS) is a scanning probe technique for individual objects and structured surfaces investigation that provides a wealth of enhanced spectral information with nanoscale spatial resolution and high detection sensitivity. It has become a powerful and promising chemical and physical information detection method in the nanometer scale. The TERS technique uses a sharp metallic tip regulated in the near-field of a sample surface, which is illuminated with a certain incident beam meeting the excitation conditions of the wave-vector matching. The local electric field, and, consequently, the Raman scattering, from the sample in the vicinity of the tip apex are both greatly tip-enhanced owning to the excitation of localized surface plasmons and the lightning-rod effect. Typically, a TERS setup is composed of a scanning probe microscope, excitation and collection optical configurations, and a Raman spectroscope. In the illumination configuration, an objective lens or a parabolic mirror is always used as the most important component, in order to focus the incident beam on the tip apex for excitation. In this research, a novel TERS setup was built up by introducing a plasmonic lens to the excitation optics as a focusing device. A plasmonic lens with symmetry breaking semi-annular slits corrugated on gold film was designed for the purpose of generating concentrated sub-wavelength light spots with strong longitudinal electric field. Compared to conventional far-field optical components, the designed plasmonic lens not only focuses an incident beam to a sub-wavelength light spot, but also realizes a strong z-component that dominants the electric field illumination, which is ideal for the excitation of tip-enhancement. Therefore, using a PL in the illumination configuration of TERS contributes to improve the detection sensitivity by both reducing the far-field background and effectively exciting the localized electric field enhancement. The FDTD method was employed to investigate the optical near-field distribution resulting from the light-nanostructure interaction. And the optical field distribution was characterized using an scattering-type scanning near-field optical microscope to demonstrate the focusing performance of the lens. The experimental result is in agreement with the theoretically calculated one. It verifies the focusing performance of the plasmonic lens. The optical field distribution shows a bright elliptic spot in the lens center and several arc-like side-lobes on both sides. After the focusing performance was experimentally verified, the designed plasmonic lens was used as a focusing component in the excitation configuration of TERS setup to concentrate incident energy and generate a longitudinal optical field. A collimated linearly polarized laser beam, with along x-axis polarization, was incident from the bottom glass side on the plasmonic lens. The incident light focused by the plasmonic lens interacted with the silver-coated tip apex and enhanced the Raman signal of the sample locally. The scattered Raman signal was gathered by a parabolic mirror and detected with a Raman spectroscopy. Then, the plasmonic lens based setup was employed to investigate carbon nanotubes and TERS experiment was performed. Experimental results indicate that the Raman signal is considerably enhanced which proves that the novel TERS configuration is feasible and promising.

Keywords: longitudinal electric field, plasmonics, raman spectroscopy, tip-enhancement

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Authors: Şeyma Dombaycıoğlu, Hilal Köse, Ali Osman Aydın, Hatem Akbulut

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Rechargeable lithium ion batteries (LIBs) have been considered as one of the most attractive energy storage choices for laptop computers, electric vehicles and cellular phones owing to their high energy and power density. Compared with conventional carbonaceous materials, transition metal oxides (TMOs) have attracted great interests and stand out among versatile novel anode materials due to their high theoretical specific capacity, wide availability and good safety performance. ZnO, as an anode material for LIBs, has a high theoretical capacity of 978 mAh g-1, much higher than that of the conventional graphite anode (∼370 mAhg-1). However, several major problems such as poor cycleability, resulting from the severe volume expansion and contraction during the alloying-dealloying cycles with Li+ ions and the associated charge transfer process, the pulverization and the agglomeration of individual particles, which drastically reduces the total entrance/exit sites available for Li+ ions still hinder the practical use of ZnO powders as an anode material for LIBs. Therefore, a great deal of effort has been devoted to overcome these problems, and many methods have been developed. In most of these methods, it is claimed that carbon nanotubes (CNTs) will radically improve the performance of batteries, because their unique structure may especially enhance the kinetic properties of the electrodes and result in an extremely high specific charge compared with the theoretical limits of graphitic carbon. Due to outstanding properties of CNTs, MWCNT buckypaper substrate is considered a buffer material to prevent mechanical disintegration of anode material during the battery applications. As the bridge connecting the positive and negative electrodes, the electrolyte plays a critical role affecting the overall electrochemical performance of the cell including rate, capacity, durability and safety. Commercial electrolytes for Li-ion batteries normally consist of certain lithium salts and mixed organic linear and cyclic carbonate solvents. Most commonly, LiPF6 is attributed to its remarkable features including high solubility, good ionic conductivity, high dissociation constant and satisfactory electrochemical stability for commercial fabrication. Besides LiPF6, LiBF4 is well known as a conducting salt for LIBs. LiBF4 shows a better temperature stability in organic carbonate based solutions and less moisture sensitivity compared to LiPF6. In this work, free standing zinc oxide (ZnO) and multiwalled carbon nanotube (MWCNT) nanocomposite materials were prepared by a sol gel technique giving a high capacity anode material for lithium ion batteries. Electrolyte solutions (including 1 m Li+ ion) were prepared with different Li salts in glove box. For this purpose, LiPF6 and LiBF4 salts and also mixed of these salts were solved in EC:DMC solvents (1:1, w/w). CR2016 cells were assembled by using these prepared electrolyte solutions, the ZnO/MWCNT buckypaper nanocomposites as working electrodes, metallic lithium as cathode and polypropylene (PP) as separator. For investigating the effect of different Li salts on the electrochemical performance of ZnO/MWCNT nanocomposite anode material electrochemical tests were performed at room temperature.

Keywords: anode, electrolyte, Li-ion battery, ZnO/MWCNT

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Authors: Noor S. Nasri, Eric C. A. Tatt, Usman D. Hamza, Jibril Mohammed, Husna M. Zain

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Climate change has becoming a global environmental issue that may trigger irreversible changes in the environment with catastrophic consequences for human, animals and plants on our planet. Methane, carbon dioxide and nitrous oxide are the greenhouse gases (GHG) and as the main factor that significantly contributes to the global warming. Mainly carbon dioxide be produced and released to atmosphere by thermal industrial and power generation sectors. Methane is dominant component of natural gas releases significant of thermal heat, and the gaseous pollutants when homogeneous thermal combustion takes place at high temperature. Heterogeneous catalytic Combustion (HCC) principle is promising technologies towards environmental friendly energy production should be developed to ensure higher yields with lower pollutants gaseous emissions and perform complete combustion oxidation at moderate temperature condition as comparing to homogeneous high thermal combustion. Hence the principle has become a very interesting alternative total oxidation for the treatment of pollutants gaseous emission especially NOX product formation. Noble metals are dispersed on a support-porous HCC such as γ- Al2O3, TiO2 and ThO2 to increase thermal stability of catalyst and to increase to effectiveness of catalytic combustion. Support-porous HCC material to be selected based on factors of the surface area, porosity, thermal stability, thermal conductivity, reactivity with reactants or products, chemical stability, catalytic activity, and catalyst life. γ- Al2O3 with high catalytic activity and can last longer life of catalyst, is commonly used as the support for Pd catalyst at low temperatures. Sustainable and renewable support-material of bio-mass char was derived from agro-industrial waste material and used to compare with those the conventional support-porous material. The abundant of biomass wastes generated in palm oil industries is one potential source to convert the wastes into sustainable material as replacement of support material for catalysts. Objective of this study was to compare the kinetic rate of reaction the combustion of methane on Palladium (Pd) based catalyst with Al2O3 support and bio-char (Bc) support derived from shell kernel. The 2wt% Pd was prepared using incipient wetness impregnation method and the HCC performance was accomplished using tubular quartz reactor with gas mixture ratio of 3% methane and 97% air. Material characterization was determined using TGA, SEM, and BET surface area. The methane porous-HCC conversion was carried out by online gas analyzer connected to the reactor that performed porous-HCC. BET surface area for prepared 2 wt% Pd/Bc is smaller than prepared 2wt% Pd/ Al2O3 due to its low porosity between particles. The order of catalyst activity based on kinetic rate on reaction of catalysts in low temperature is prepared 2wt% Pd/Bc > calcined 2wt% Pd/ Al2O3 > prepared 2wt% Pd/ Al2O3 > calcined 2wt% Pd/Bc. Hence the usage of agro-industrial bio-mass waste material can enhance the sustainability principle.

Keywords: catalytic-combustion, environmental, support-bio-char material, sustainable and renewable material

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Authors: Vladimir Smirnov, Roman Tominov, Vadim Avilov, Oleg Ageev

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The creation of a new generation micro- and nanoelectronics elements opens up unlimited possibilities for electronic devices parameters improving, as well as developing neuromorphic computing systems. Interest in the latter is growing up every year, which is explained by the need to solve problems related to the unstructured classification of data, the construction of self-adaptive systems, and pattern recognition. However, for its technical implementation, it is necessary to fulfill a number of conditions for the basic parameters of electronic memory, such as the presence of non-volatility, the presence of multi-bitness, high integration density, and low power consumption. Several types of memory are presented in the electronics industry (MRAM, FeRAM, PRAM, ReRAM), among which non-volatile resistive memory (ReRAM) is especially distinguished due to the presence of multi-bit property, which is necessary for neuromorphic systems manufacturing. ReRAM is based on the effect of resistive switching – a change in the resistance of the oxide film between low-resistance state (LRS) and high-resistance state (HRS) under an applied electric field. One of the methods for the technical implementation of neuromorphic systems is cross-bar structures, which are ReRAM cells, interconnected by cross data buses. Such a structure imitates the architecture of the biological brain, which contains a low power computing elements - neurons, connected by special channels - synapses. The choice of the ReRAM oxide film material is an important task that determines the characteristics of the future neuromorphic system. An analysis of literature showed that many metal oxides (TiO2, ZnO, NiO, ZrO2, HfO2) have a resistive switching effect. It is worth noting that the manufacture of nanocomposites based on these materials allows highlighting the advantages and hiding the disadvantages of each material. Therefore, as a basis for the neuromorphic structures manufacturing, it was decided to use ZnₓTiᵧHfzOᵢ nanocomposite. It is also worth noting that the ZnₓTiᵧHfzOᵢ nanocomposite does not need an electroforming, which degrades the parameters of the formed ReRAM elements. Currently, this material is not well studied, therefore, the study of the effect of resistive switching in forming-free ZnₓTiᵧHfzOᵢ nanocomposite is an important task and the goal of this work. Forming-free nanocomposite ZnₓTiᵧHfzOᵢ thin film was grown by pulsed laser deposition (Pioneer 180, Neocera Co., USA) on the SiO2/TiN (40 nm) substrate. Electrical measurements were carried out using a semiconductor characterization system (Keithley 4200-SCS, USA) with W probes. During measurements, TiN film was grounded. The analysis of the obtained current-voltage characteristics showed a resistive switching from HRS to LRS resistance states at +1.87±0.12 V, and from LRS to HRS at -2.71±0.28 V. Endurance test shown that HRS was 283.21±32.12 kΩ, LRS was 1.32±0.21 kΩ during 100 measurements. It was shown that HRS/LRS ratio was about 214.55 at reading voltage of 0.6 V. The results can be useful for forming-free nanocomposite ZnₓTiᵧHfzOᵢ films in neuromorphic systems manufacturing. This work was supported by RFBR, according to the research project № 19-29-03041 mk. The results were obtained using the equipment of the Research and Education Center «Nanotechnologies» of Southern Federal University.

Keywords: nanotechnology, nanocomposites, neuromorphic systems, RRAM, pulsed laser deposition, resistive switching effect

Procedia PDF Downloads 100

Authors: Alfonso Sepulveda, Brecht Put, Nouha Labyedh, Philippe M. Vereecken

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High energy and power density are the main requirements of today’s high demanding applications in consumer electronics. Lithium ion batteries (LIB) have the highest energy density of all known systems and are thus the best choice for rechargeable micro-batteries. Liquid electrolyte LIBs present limitations in safety, size and design, thus thin film all-solid state batteries are predominantly considered to overcome these restrictions in small devices. Although planar all-solid state thin film LIBs are at present commercially available they have low capacity (<1mAh/cm2) which limits their application scenario. By using micro-or nanostructured surfaces (i.e. 3D batteries) and appropriate conformal coating technology (i.e. electrochemical deposition, ALD) the capacity can be increased while still keeping a high rate performance. The main challenges in the introduction of solid-state LIBs are low ionic conductance and limited cycle life time due to mechanical stress and shearing interfaces. Novel materials and innovative nanostructures have to be explored in order to overcome these limitations. Thin film 3D compatible materials need to provide with the necessary requirements for functional and viable thin-film stacks. Thin film electrodes offer shorter Li-diffusion paths and high gravimetric and volumetric energy densities which allow them to be used at ultra-fast charging rates while keeping their complete capacities. Thin film electrolytes with intrinsically high ion conductivity (~10-3 S.cm) do exist, but are not electrochemically stable. On the other hand, electronically insulating electrolytes with a large electrochemical window and good chemical stability are known, but typically have intrinsically low ionic conductivities (<10-6 S cm). In addition, there is the need for conformal deposition techniques which can offer pinhole-free coverage over large surface areas with large aspect ratio features for electrode, electrolyte and buffer layers. To tackle the scaling of electrodes and the conformal deposition requirements on future 3D batteries we study LiMn2O4 (LMO) and Li4Ti5O12 (LTO). These materials are among the most interesting electrode candidates for thin film batteries offering low cost, low toxicity, high voltage and high capacity. LMO and LTO are considered 3D compatible materials since they can be prepared through conformal deposition techniques. Here, we show the scaling effects on rate performance and cycle stability of thin film cathode layers of LMO created by RF-sputtering. Planar LMO thin films below 100 nm have been electrochemically characterized. The thinnest films show the highest volumetric capacity and the best cycling stability. The increased stability of the films below 50 nm allows cycling in both the 4 and 3V potential region, resulting in a high volumetric capacity of 1.2Ah/cm3. Also, the creation of LTO anode layers through a post-lithiation process of TiO2 is demonstrated here. Planar LTO thin films below 100 nm have been electrochemically characterized. A 70 nm film retains 85% of its original capacity after 100 (dis)charging cycles at 10C. These layers can be implemented into a high aspect ratio structures. IMEC develops high aspect Si pillars arrays which is the base for the advance of 3D thin film all-solid state batteries of future technologies.

Keywords: Li-ion rechargeable batteries, thin film, nanostructures, rate performance, 3D batteries, all-solid state

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Authors: Mazaher Yarmohamadi-Vasel, Ali Reza Modarresi-Alama, Sahar Shabzendedara

Abstract:

Purpose/Objectives: The first purpose was synthesize Poly(N-(sulfophenyl)aniline) nanoflowers (PSANFLs) and Poly(N-(sulfophenyl)aniline) nanofibers/titanium dioxide nanoparticles ((PSANFs/TiO2NPs) by a solid-state mechano-chemical reaction and template-free method and use them in hybrid solar cell. Also, our second aim was to increase the solubility and the processability of conjugated nanomaterials in water through polar functionalized materials. poly[N-(4-sulfophenyl)aniline] is easily soluble in water because of the presence of polar groups of sulfonic acid in the polymer chain. Materials/Methods: Iron (III) chloride hexahydrate (FeCl3∙6H2O) were bought from Merck Millipore Company. Titanium oxide nanoparticles (TiO2, <20 nm, anatase) and Sodium diphenylamine-4-sulfonate (99%) were bought from Sigma-Aldrich Company. Titanium dioxide nanoparticles paste (PST-20T) was prepared from Sharifsolar Co. Conductive glasses coated with indium tin oxide (ITO) were bought from Xinyan Technology Co (China). For the first time we used the solid-state mechano-chemical reaction and template-free method to synthesize Poly(N-(sulfophenyl)aniline) nanoflowers. Moreover, for the first time we used the same technique to synthesize nanocomposite of Poly(N-(sulfophenyl)aniline) nanofibers and titanium dioxide nanoparticles (PSANFs/TiO2NPs) also for the first time this nanocomposite was synthesized. Examining the results of electrochemical calculations energy gap obtained by CV curves and UV–vis spectra demonstrate that PSANFs/TiO2NPs nanocomposite is a p-n type material that can be used in photovoltaic cells. Doctor blade method was used to creat films for three kinds of hybrid solar cells in terms of different patterns like ITO│TiO2NPs│Semiconductor sample│Al. In the following, hybrid photovoltaic cells in bilayer and bulk heterojunction structures were fabricated as ITO│TiO2NPs│PSANFLs│Al and ITO│TiO2NPs│PSANFs /TiO2NPs│Al, respectively. Fourier-transform infrared spectra, field emission scanning electron microscopy (FE-SEM), ultraviolet-visible spectra, cyclic voltammetry (CV) and electrical conductivity were the analysis that used to characterize the synthesized samples. Results and Conclusions: FE-SEM images clearly demonstrate that the morphology of the synthesized samples are nanostructured (nanoflowers and nanofibers). Electrochemical calculations of band gap from CV curves demonstrated that the forbidden band gap of the PSANFLs and PSANFs/TiO2NPs nanocomposite are 2.95 and 2.23 eV, respectively. I–V characteristics of hybrid solar cells and their power conversion efficiency (PCE) under 100 mWcm−2 irradiation (AM 1.5 global conditions) were measured that The PCE of the samples were 0.30 and 0.62%, respectively. At the end, all the results of solar cell analysis were discussed. To sum up, PSANFLs and PSANFLs/TiO2NPs were successfully synthesized by an affordable and straightforward mechanochemical reaction in solid-state under the green condition. The solubility and processability of the synthesized compounds have been improved compared to the previous work. We successfully fabricated hybrid photovoltaic cells of synthesized semiconductor nanostructured polymers and TiO2NPs as different architectures. We believe that the synthesized compounds can open inventive pathways for the development of other Poly(N-(sulfophenyl)aniline based hybrid materials (nanocomposites) proper for preparing new generation solar cells.

Keywords: mechanochemical synthesis, PSANFLs, PSANFs/TiO2NPs, solar cell

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Authors: Atabaev I. G., Fayziev Sh. A., Irmatova Sh. K.

Abstract:

Raw materials with high content of Kalium oxide widely used in ceramic technology for prevention or decreasing of deformation of ceramic goods during drying process and under thermal annealing. Becouse to low melting temperature it is also used to decreasing of the temperature of thermal annealing during fabrication of ceramic goods [1,2]. So called “Porceline or China stones” - quartz-sericite (muscovite) minerals is also can be used for prevention of deformation as the content of Kalium oxide in muscovite is rather high (SiO2, + KAl2[AlSi3O10](OH)2). [3] . To estimation of possibility of use of this mineral for ceramic manufacture, in the presented article the influence of thermal processing on phase and a chemical content of this raw material is investigated. As well as to other ceramic raw materials (kaoline, white burning clays) the basic requirements of the industry to quality of "a porcelain stone» are following: small size of particles, relative high uniformity of disrtribution of components and phase, white color after burning, small content of colorant oxides or chromophores (Fe2O3, FeO, TiO2, etc) [4,5]. In the presented work natural minerale from the Boynaksay deposit (Uzbekistan) is investigated. The samples was mechanically polished for investigation by Scanning Electron Microscope. Powder with size of particle up to 63 μm was used to X-ray diffractometry and chemical analysis. The annealing of samples was performed at 900, 1120, 1350oC during 1 hour. Chemical composition of Boynaksay raw material according to chemical analysis presented in the table 1. For comparison the composition of raw materials from Russia and USA are also presented. In the Boynaksay quartz – sericite the average parity of quartz and sericite makes 55-60 and 30-35 % accordingly. The distribution of quartz and sericite phases in raw material was investigated using electron probe scanning electronic microscope «JEOL» JXA-8800R. In the figure 1 the scanning electron microscope (SEM) micrograps of the surface and the distributions of Al, Si and K atoms in the sample are presented. As it seen small granular, white and dense mineral includes quartz, sericite and small content of impurity minerals. Basically, crystals of quartz have the sizes from 80 up to 500 μm. Between quartz crystals the sericite inclusions having a tablet form with radiant structure are located. The size of sericite crystals is ~ 40-250 μm. Using data on interplanar distance [6,7] and ASTM Powder X-ray Diffraction Data it is shown that natural «a porcelain stone» quartz – sericite consists the quartz SiO2, sericite (muscovite type) KAl2[AlSi3O10](OH)2 and kaolinite Al203SiO22Н2О (See Figure 2 and Table 2). As it seen in the figure 3 and table 3a after annealing at 900oC the quartz – sericite contains quartz – SiO2 and muscovite - KAl2[AlSi3O10](OH)2, the peaks related with Kaolinite are absent. After annealing at 1120oC the full disintegration of muscovite and formation of mullite phase Al203 SiO2 is observed (the weak peaks of mullite appears in fig 3b and table 3b). After annealing at 1350oC the samples contains crystal phase of quartz and mullite (figure 3c and table 3с). Well known Mullite gives to ceramics high density, abrasive and chemical stability. Thus the obtained experimental data on formation of various phases during thermal annealing can be used for development of fabrication technology of advanced materials. Conclusion: The influence of thermal annealing in the interval 900-1350oC on phase composition and structure of quartz-sericite minerale is investigated. It is shown that during annealing the phase content of raw material is changed. After annealing at 1350oC the samples contains crystal phase of quartz and mullite (which gives gives to ceramics high density, abrasive and chemical stability).

Keywords: quartz-sericite, kaolinite, mullite, thermal processing

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Authors: Ching-Sung Lee, Wei-Chou Hsu, Han-Yin Liu, Hung-Hsi Huang, Si-Fu Chen, Yun-Jung Yang, Bo-Chun Chiang, Yu-Chuang Chen, Shen-Tin Yang

Abstract:

AlGaN/GaN high electron mobility transistors (HEMTs) have been intensively studied due to their intrinsic advantages of high breakdown electric field, high electron saturation velocity, and excellent chemical stability. They are also suitable for ultra-violet (UV) photodetection due to the corresponding wavelengths of GaN bandgap. To improve the optical responsivity by decreasing the dark current due to gate leakage problems and limited Schottky barrier heights in GaN-based HEMT devices, various metal-oxide-semiconductor HEMTs (MOS-HEMTs) have been devised by using atomic layer deposition (ALD), molecular beam epitaxy (MBE), metal-organic chemical vapor deposition (MOCVD), liquid phase deposition (LPD), and RF sputtering. The gate dielectrics include MgO, HfO2, Al2O3, La2O3, and TiO2. In order to provide complementary circuit operation, enhancement-mode (E-mode) devices have been lately studied using techniques of fluorine treatment, p-type capper, piezoneutralization layer, and MOS-gate structure. This work reports an Al2O3-dielectric Al0.25Ga0.75N/GaN E-mode MOS-HEMT design by using a cost-effective ozone water oxidization technique. The present ozone oxidization method advantages of low cost processing facility, processing simplicity, compatibility to device fabrication, and room-temperature operation under atmospheric pressure. It can further reduce the gate-to-channel distance and improve the transocnductance (gm) gain for a specific oxide thickness, since the formation of the Al2O3 will consume part of the AlGaN barrier at the same time. The epitaxial structure of the studied devices was grown by using the MOCVD technique. On a Si substrate, the layer structures include a 3.9 m C-doped GaN buffer, a 300 nm GaN channel layer, and a 5 nm Al0.25Ga0.75N barrier layer. Mesa etching was performed to provide electrical isolation by using an inductively coupled-plasma reactive ion etcher (ICP-RIE). Ti/Al/Au were thermally evaporated and annealed to form the source and drain ohmic contacts. The device was immersed into the H2O2 solution pumped with ozone gas generated by using an OW-K2 ozone generator. Ni/Au were deposited as the gate electrode to complete device fabrication of MOS-HEMT. The formed Al2O3 oxide thickness 7 nm and the remained AlGaN barrier thickness is 2 nm. A reference HEMT device has also been fabricated in comparison on the same epitaxial structure. The gate dimensions are 1.2 × 100 µm 2 with a source-to-drain spacing of 5 μm for both devices. The dielectric constant (k) of Al2O3 was characterized to be 9.2 by using C-V measurement. Reduced interface state density after oxidization has been verified by the low-frequency noise spectra, Hooge coefficients, and pulse I-V measurement. Improved device characteristics at temperatures of 300 K-450 K have been achieved for the present MOS-HEMT design. Consequently, Al2O3-dielectric Al0.25Ga0.75N/GaN E-mode MOS-HEMTs by using the ozone water oxidization method are reported. In comparison with a conventional Schottky-gate HEMT, the MOS-HEMT design has demonstrated excellent enhancements of 138% (176%) in gm, max, 118% (139%) in IDS, max, 53% (62%) in BVGD, 3 (2)-order reduction in IG leakage at VGD = -60 V at 300 (450) K. This work is promising for millimeter-wave integrated circuit (MMIC) and three-terminal active UV photodetector applications.

Keywords: MOS-HEMT, enhancement mode, AlGaN/GaN, passivation, ozone water oxidation, gate leakage

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