Search results for: mesoporous siliceous

Authors: Azeem Ur Rehman, Asma Tayyaba

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This article deals with the promotional effects of CeO2 on PtPd/CeO2-OMC electro catalysts. The synthesized catalysts are characterized using different physico chemical techniques and evaluated in a formic acid oxidation fuel cell. N2 adsorption/desorption analysis shows that CeO2 modification increases the surface area of OMC from 1005 m2/g to 1119 m2/g. SEM, XRD and TEM analysis reveal that the presence of CeO2 enhances the active metal(s) dispersion on the CeO2-OMC surface. The average particle size of the dispersed metal decreases with the increase of Pt/Pd ratio on CeO2-OMC support. Cyclic voltametry measurement of Pd/CeO2-OMC gives 12 % higher anodic current activity with 83 mV negative shift of the peak potential as compared to unmodified Pd/OMC. In bimetallic catalysts, the addition of Pt improves the activity and stability of the catalysts significantly. Among the bimetallic samples, Pd3Pt1/CeO2-OMC displays superior current density (74.6 mA/cm2), which is 28.3 times higher than that of Pt/CeO2-OMC. It also shows higher stability in extended period of runs with least indication of CO poisoning effects.

Keywords: CeO2, ordered mesoporous carbon (OMC), electro catalyst, formic acid fuel cell

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Authors: Charmaine Lamiel, Van Hoa Nguyen, Marjorie Baynosa, Jae-Jin Shim

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Electrochemical supercapacitors have attracted considerable attention because of their high potential as an efficient energy storage system. The combination of carbon-based material and transition metal oxides/sulfides are studied because they have long and improved cycle life as well as high energy and power densities. In this study, a hierarchical mesoporous carbon sphere/nickel cobalt sulfide (CS/Ni-Co-S) core/shell structure was synthesized using a facile hydrothermal method without any further sulfurization or post-heat treatment. The CS/Ni-Co-S core/shell microstructures exhibited a high capacitance of 724 F g−1 at 2 A g−1 in a 6 M KOH electrolyte. After 2000 charge-discharge cycles, it retained 86.1% of its original capacitance, with high Coulombic efficiency of 97.9%. The electrode exhibited a high energy density of 58.0 Wh kg−1 at an energy density of 1440 W kg−1, and high power density of 7200 W kg−1 at an energy density of 34.2 Wh kg−1. The successful synthesis was considered to be simple and cost-effective which supports the viability of this composite as an alternative activated material for high performance supercapacitors.

Keywords: carbon sphere, electrochemical, hydrothermal, nickel cobalt sulfide, supercapacitor

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Authors: Su-Ning Wang, Yao-Qiang Chen

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The CeO2-ZrO2-La2O3-Al2O3 composite oxides are synthesized using co-precipitation method by two different reactors (i.e. continuous stirred-tank reactor and batch reactor), and the corresponding Rh-only three-way catalysts are obtained by wet-impregnation approach. The textural, structural, morphology and redox properties of the support materials, as well as the catalytic performance of the Rh-only catalyst are investigated systematically. The results reveal that the materials (CZLA-C) synthesized by continuous stirred-tank reactor have a better physic-chemical properties than the counterpart material (CZLA-B) prepared by batch reactor. After aging treatment at 1000 ℃ for 5 h, the BET surface area and pore volume of S1 reach up to 76 m2 g-1 and 0.36 mL/g, respectively, which is higher than that of S2. The XRD and Raman results demonstrate that a high structural stability is obtained by S1 because of the negligible lattice variation and the slight grain growth after aging treatment. The SEM and TEM images display that the morphology of S1 is assembled by many homogeneous primary nanoparticles (about 6.12 nm) that are connected to form mesoporous structure The TPR measurement shows that S1 possesses a higher reduction ability than S2. Compared with the catalyst supported on the CZLA-B, the as-prepared CZLA-C demonstrates an improved three-way catalytic activity both before and after aging treatment.

Keywords: composite oxides, reactor, catalysis, catalytic performance

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Authors: Snehal L. Kadam, Shriniwas B. Kulkarni

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Flexible electrode material with high surface area and good electrochemical properties is the current trend captivating the researchers across globe for application in the next generation energy storage field. In the present work, crumpled sheet like reduced graphene oxide grown on carbon cloth by the hydrothermal method with a series of different deposition temperatures at fixed time. The influence of the deposition temperature on the structural, morphological, optical and supercapacitive properties of the electrode material was investigated by XRD, RAMAN, XPS, TEM, FE-SEM, UV-VISIBLE and electrochemical characterization techniques.The results show that the hydrothermally synthesized reduced graphene oxide on carbon cloth has sheet like mesoporous structure. The reduced graphene oxide material at 160°C exhibits the best supercapacitor performance, with a specific capacitance of 443 F/g at scan rate 5mV/sec. Moreover, stability studies show 97% capacitance retention over 1000 CV cycles. This result shows that hydrothermally synthesized RGO on carbon cloth is the potential electrode material and would be used in the next-generation wearable energy storage systems. The detailed analysis and results will be presented at the conference.

Keywords: graphene oxide, reduced graphene oxide, carbon cloth, deposition temperature, supercapacitor

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Authors: Hu-Cheng Weng, Jhen-Ting Huang, Chia-Chia Chang, An-Ya Lo

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In this study, carbon mesoporous material, CMK-3, was adopted as supporting material for electroactive polymerspolyaniline (PANI), polyaniline, for supercapacitor application, where hydroquinone (HQ) was integrated to enhance the redox reaction of PANI. The results show that the addition of PANI improves the capacitance of electrode from 89 F/g (CMK-3) to 337 F/g (PANI/CMK-3), the addition of HQ furtherly improves the capacitance to 463 F/g (PANI/CMK-3/HQ). The PANI provides higher energy density and also acts as binder of the electrode; the CMK-3 provides higher electron double layer capacitance EDLC and stabilize the polyaniline by its highly porosity. With the addition of HQ, the capacitance of PANI/CMK-3 was further enhanced. In-situ analyses including cyclic voltammetry (CV), chronopotentiometry (CP), electron impedance spectrum (EIS) analyses were applied for electrode performance examination. For materials characterization, the crystal structure, morphology, microstructure, and porosity were examined by X-ray diffraction (XRD), scanning electron microscope (SEM), and transmission electron microscopy (TEM), and 77K N2 adsorption/desorption analyses, respectively. The effects of electrolyte pH value, PANI polymerization time, HQ concentration, and PANI/CMK-3 ratio on capacitance were discussed. The durability was also studied by long-term operation test. The results show that PANI/CMK-3/HQ with great potential for supercapacitor application. Finally, the potential of all-solid PANI/CMK-3/HQ based supercapacitor was successfully demonstrated.

Keywords: CMK3, PANI, redox electrolyte, solid supercapacitor

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Authors: Seid Yimer Abate, Ding-Chi Huang, Yu-Tai Tao

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In this study, charge extraction characteristics at the perovskite/TiO2 interface in the conventional perovskite solar cell is studied by interface engineering. Self-assembled monolayers of phosphonic acids with different chain length and terminal functional group were used to modify mesoporous TiO2 surface to modulate the surface property and interfacial energy barrier to investigate their effect on charge extraction and transport from the perovskite to the mp-TiO2 and then the electrode. The chain length introduces a tunnelling distance and the end group modulate the energy level alignment at the mp-TiO2 and perovskite interface. The work function of these SAM-modified mp-TiO2 varied from −3.89 eV to −4.61 eV, with that of the pristine mp-TiO2 at −4.19 eV. A correlation of charge extraction and transport with respect to the modification was attempted. The study serves as a guide to engineer ETL interfaces with simple SAMs to improve the charge extraction, carrier balance and device long term stability. In this study, a maximum PCE of ~16.09% with insignificant hysteresis was obtained, which is 17% higher than the standard device.

Keywords: Energy level alignment, Interface engineering, Perovskite solar cells, Phosphonic acid monolayer, Tunnelling distance

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Authors: Saji George, Eng Khuan Seng, Christof Luda

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Nanotechnology has been recognized as an important tool for modern agriculture and has the potential to overcome some of the pressing challenges faced by aquaculture industry. A strategy for optimizing nanotechnology-based therapeutic delivery platform for immunizing farmed fish was developed. Accordingly, a compositional library of nanomaterials of natural chemistry (Halloysite (clay), Chitosan, Hydroxyapatite, Mesoporous Silica and a composite material of clay-chitosan) was screened for their toxicity and efficiency in delivering models antigens in cellular and zebrafish embryo models using high throughput screening platforms. Through multi-parametric optimization, chitosan modified halloysite (clay) nanomaterial was identified as an optimal vaccine delivery platform. Further, studies conducted in juvenile seabass showed the potential of clay-chitosan in delivering outer membrane protein of Tenacibaculum maritimum- TIMA (pathogenic bacteria) to and its efficiency in eliciting immune responses in fish. In short, as exemplified by this work, the strategy of using compositional nanomaterial libraries and their biological profiling using high-throughput screening platform could fasten the discovery process of nanomaterials with potential applications in food and agriculture.

Keywords: nanotechnology, fish-vaccine, drug-delivery, halloysite-chitosan

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Authors: Ifeyinwa Orakwe, Ngozi Nwogu, Edward Gobina

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This work presents experimental results relating to the structural characterization of a commercially available alumina membrane. A γ-alumina mesoporous tubular membrane has been used. Nitrogen adsorption-desorption, scanning electron microscopy and gas permeability test has been carried out on the alumina membrane to characterize its structural features. Scanning electron microscopy (SEM) was used to determine the pore size distribution of the membrane. Pore size, specific surface area and pore size distribution were also determined with the use of the Nitrogen adsorption-desorption instrument. Gas permeation tests were carried out on the membrane using a variety of single and mixed gases. The permeabilities at different pressure between 0.05-1 bar and temperature range of 25-200oC were used for the single and mixed gases: nitrogen (N2), helium (He), oxygen (O2), carbon dioxide (CO2), 14%CO₂/N₂, 60%CO₂/N₂, 30%CO₂/CH4 and 21%O₂/N₂. Plots of flow rate verses pressure were obtained. Results got showed the effect of temperature on the permeation rate of the various gases. At 0.5 bar for example, the flow rate for N2 was relatively constant before decreasing with an increase in temperature, while for O2, it continuously decreased with an increase in temperature. In the case of 30%CO₂/CH4 and 14%CO₂/N₂, the flow rate showed an increase then a decrease with increase in temperature. The effect of temperature on the membrane performance of the various gases is presented and the influence of the trans membrane pressure drop will be discussed in this paper.

Keywords: alumina membrane, Nitrogen adsorption-desorption, scanning electron microscopy, gas permeation, temperature

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Authors: Bhargav Baruah, Ali Shemsedin Reshad, Pankaj Tiwari

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This work presents a detailed study on the thermal degradation kinetics of co-pyrolysis of oil shale of Upper Assam, India with rubber seed shell, and lab-scale pyrolysis to investigate the influence of pyrolysis parameters on product yield and composition of products. The physicochemical characteristics of oil shale and rubber seed shell were studied by proximate analysis, elemental analysis, Fourier transform infrared spectroscopy and X-ray diffraction. The physicochemical study showed the mixture to be of low moisture, high ash, siliceous, sour with the presence of aliphatic, aromatic, and phenolic compounds. The thermal decomposition of the oil shale with rubber seed shell was studied using thermogravimetric analysis at heating rates of 5, 10, 20, 30, and 50 °C/min. The kinetic study of the oil shale pyrolysis process was performed on the thermogravimetric (TGA) data using three model-free isoconversional methods viz. Friedman, Flynn Wall Ozawa (FWO), and Kissinger Akahira Sunnose (KAS). The reaction mechanisms were determined using the Criado master plot. The understanding of the composition of Indian oil shale and rubber seed shell and pyrolysis process kinetics can help to establish the experimental parameters for the extraction of valuable products from the mixture. Response surface methodology (RSM) was employed usinf central composite design (CCD) model to setup the lab-scale experiment using TGA data, and optimization of process parameters viz. heating rate, temperature, and particle size. The samples were pre-dried at 115°C for 24 hours prior to pyrolysis. The pyrolysis temperatures were set from 450 to 650 °C, at heating rates of 2 to 20°C/min. The retention time was set between 2 to 8 hours. The optimum oil yield was observed at 5°C/min and 550°C with a retention time of 5 hours. The pyrolytic oil and gas obtained at optimum conditions were subjected to characterization using Fourier transform infrared spectroscopy (FT-IR) gas chromatography and mass spectrometry (GC-MS) and nuclear magnetic resonance spectroscopy (NMR).

Keywords: Indian oil shale, rubber seed shell, co-pyrolysis, isoconversional methods, gas chromatography, nuclear magnetic resonance, Fourier transform infrared spectroscopy

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Authors: Kusum Kumari, Ramesh Banoth, V. S. Reddy Channu

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Organic-inorganic perovskite solar cells (PrSCs) have emerged as a promising solar photovoltaic technology in terms of realizing high power conversion efficiency (PCE). However, their limited lifetime and poor device stability limits their commercialization in future. In this regard, interface engineering of the electron transport layer (ETL) using 2D materials have been currently used owing to their high carrier mobility, high thermal stability and tunable work function, which in turn enormously impact the charge carrier dynamics. In this work, we report an easy and effective way of simultaneously enhancing the efficiency of PrSCs along with the long-term stability through interface engineering via the incorporation of 2D-Molybdenum disulfide (2D-MoS₂, few layered nanoflakes) in mesoporous-Titanium dioxide (mp-TiO₂)scaffold electron transport buffer layer, and using poly 3-hexytheophene (P3HT) as hole transport layers. The PSCs were fabricated in ambient air conditions in device configuration, FTO/c-TiO₂/mp-TiO₂:2D-MoS₂/CH3NH3PbI3/P3HT/Au, with an active area of 0.16 cm². The best device using c-TiO₂/mp-TiO₂:2D-MoS₂ (0.5wt.%) ETL exhibited a substantial increase in PCE ~13.04% as compared to PCE ~8.75% realized in reference device fabricated without incorporating MoS₂ in mp-TiO₂ buffer layer. The incorporation of MoS₂ nanoflakes in mp-TiO₂ ETL not only enhances the PCE to ~49% but also leads to better device stability in ambient air conditions without encapsulation (retaining PCE ~86% of its initial value up to 500 hrs), as compared to ETLs without MoS₂.

Keywords: perovskite solar cells, MoS₂, nanoflakes, electron transport layer

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Authors: Josef Novák, Alena Kohoutková

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The performance of concrete structures in fire depends on several factors which include, among others, the change in material properties due to the fire. Today, fiber reinforced concrete (FRC) belongs to materials which have been widely used for various structures and elements. While the knowledge and experience with FRC behavior under ambient temperature is well-known, the effect of elevated temperature on its behavior has to be deeply investigated. This paper deals with an experimental investigation and stress‑strain relations for hybrid fiber reinforced concrete (HFRC) which contains siliceous aggregates, polypropylene and steel fibers. The main objective of the experimental investigation is to enhance a database of mechanical properties of concrete composites with addition of fibers subject to elevated temperature as well as to validate existing stress-strain relations for HFRC. Within the investigation, a unique heat transport test, compressive test and splitting tensile test were performed on 150 mm cubes heated up to 200, 400, and 600 °C with the aim to determine a time period for uniform heat distribution in test specimens and the mechanical properties of the investigated concrete composite, respectively. Both findings obtained from the presented experimental test as well as experimental data collected from scientific papers so far served for validating the computational accuracy of investigated stress-strain relations for HFRC which have been developed during last few years. Owing to the presence of steel and polypropylene fibers, HFRC becomes a unique material whose structural performance differs from conventional plain concrete when exposed to elevated temperature. Polypropylene fibers in HFRC lower the risk of concrete spalling as the fibers burn out shortly with increasing temperature due to low ignition point and as a consequence pore pressure decreases. On the contrary, the increase in the concrete porosity might affect the mechanical properties of the material. To validate this thought requires enhancing the existing result database which is very limited and does not contain enough data. As a result of the poor database, only few stress-strain relations have been developed so far to describe the structural performance of HFRC at elevated temperature. Moreover, many of them are inconsistent and need to be refined. Most of them also do not take into account the effect of both a fiber type and fiber content. Such approach might be vague especially when high amount of polypropylene fibers are used. Therefore, the existing relations should be validated in detail based on other experimental results.

Keywords: elevated temperature, fiber reinforced concrete, mechanical properties, stress strain relation

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Authors: Xin Li, Zhenxue Jiang, Zhuo Li

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Generally, shale gas is trapped within shale systems with low porosity and ultralow permeability as free and adsorbing states. Its production is controlled by properties, in terms of occurrence phases, gas contents, and percolation characteristics. These properties are all influenced by porous features. In this paper, porosity differences of marine shales were explored between Lower Cambrian shale and Lower Silurian shale of Sichuan Basin, South China. Both the two shales were marine shales with abundant oil-prone kerogen and rich siliceous minerals. Whereas Lower Cambrian shale (3.56% Ro) possessed a higher thermal degree than that of Lower Silurian shale (2.31% Ro). Samples were measured by a combination of organic-chemistry geology measurement, organic matter (OM) isolation, X-ray diffraction (XRD), N2 adsorption, and focused ion beam milling and scanning electron microscopy (FIB-SEM). Lower Cambrian shale presented relatively low pore properties, with averaging 0.008ml/g pore volume (PV), averaging 7.99m²/g pore surface area (PSA) and averaging 5.94nm average pore diameter (APD). Lower Silurian shale showed as relatively high pore properties, with averaging 0.015ml/g PV, averaging 10.53m²/g PSA and averaging 18.60nm APD. Additionally, fractal analysis indicated that the two shales presented discrepant pore morphologies, mainly caused by differences in the combination of pore types between the two shales. More specifically, OM-hosted pores with pin-hole shape and dissolved pores with dead-end openings were the main types in Lower Cambrian shale, while OM-hosted pore with a cellular structure was the main type in Lower Silurian shale. Moreover, porous characteristics of isolated OM suggested that OM of Lower Silurian shale was more capable than that of Lower Cambrian shale in the aspect of pore contribution. PV of isolated OM in Lower Silurian shale was almost 6.6 times higher than that in Lower Cambrian shale, and PSA of isolated OM in Lower Silurian shale was almost 4.3 times higher than that in Lower Cambrian shale. However, no apparent differences existed among samples with various matrix compositions. At late diagenetic or metamorphic epoch, extensive diagenesis overprints the effects of minerals on pore properties and OM plays the dominant role in pore developments. Hence, differences of porous features between the two marine shales highlight the effect of diagenetic degree on OM-hosted pore development. Consequently, distinctive pore characteristics may be caused by the different degrees of diagenetic evolution, even with similar matrix basics.

Keywords: marine shale, lower Cambrian, lower Silurian, om isolation, pore properties, om-hosted pore

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Authors: Eszter Kulcsar, Agnes Takacs, Gabriella B. Kiss, Peter Prakfalvi

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The Karancs Mountain is part of the Miocene Inner Carpathian Volcanic Belt and is located in N-NE Hungary, along the Hungarian-Slovakian border. The 14 Ma old andesitic-dacitic units are surrounded by Oligocene sedimentary units (sandstone, siltstone). The host rocks of the mineralisation are siliceous and/or argillaceous volcanic units, quartz veins, hydrothermal breccia, and strongly silicified vuggy rocks, found in the various altered volcanic units. The hydrothermal breccia consists of highly silicified vuggy quartz clasts in quartz matrix. The hydrothermal alteration of the host units shows structural control at the deeper levels. The main ore minerals are galena, pyrite, marcasite, sphalerite, hematite, magnetite, arsenopyrite, anglesite and argentite The mineralisation was first mentioned in 1944 and the first exploration took place between 1961 and 1962 in the area. The first ore geological studies were performed between 1984-1985. The exploration programme was limited only to surface sampling; no drilling programme was performed. Petrographical and preliminary fluid inclusion studies were performed on calcite samples from a galena-bearing vein. Despite the early discovery of the mineralisation, no detailed description is available, thus its size, characteristics, and origin have remained unknown. The aim of this study is to examine the mineralisation, describe the characteristics in detail and to test the possible gold content of the various quartz veins and breccias. Finally, we also investigate the potential relation of the hydrothermal mineralisation to the surrounding similar mineralisations with similar ages (e.g. W-Mátra Mountains in Hungary, Banska Bystrica, Banska Stiavnica in Slovakia) in order to place the mineralisation within the volcanic-hydrothermal evolution of the Miocene Inner Carpathian Belt. As first steps, the study includes field mapping, traditional petrological and ore microscopy; X-ray diffraction analysis; SEM-EDS and EMPA studies on ore minerals, to obtain mineral chemical information. Fluid inclusion petrography and microthermometry and micro-Raman-spectroscopy studies are also planned on quartz-hosted inclusions to investigate the physical and chemical properties of the ore-forming fluid.

Keywords: epithermal, Karancs Mountain, Hungary, Miocene Inner Carpathian volcanic belt, polimetallic ore deposit

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Authors: Andile Mkhohlakali, Tien-Chien Jen, James Tshilongo, Happy Mabowa

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Among different parameters, oxygen is one of the most important analytes of interest, dissolved oxygen (DO) concentration is very crucial and significant for various areas of physical, chemical, and environmental monitoring. Herein we report oxygen-sensitive luminophores -based lanthanum(III) trifluoromethanesulfonate), [La]³⁺ was encapsulated into SiO₂-based xerogel matrix. The nanosensor is composed of organically modified silica nanoparticles, doped with the luminescent oxygen–sensitive lanthanum(III) trifluoromethanesulfonate complex. The precursor materials used for sensing film were triethyl ethoxy silane (TEOS) and (3-Mercaptopropyltriethoxysilane) (MPTMS- TEOS) used for SiO2-baed matrices. Brunauer–Emmett–Teller (BET), and BJH indicate that the SiO₂ transformed from microporous to mesoporous upon the addition of La³⁺ luminophore with increased surface area (SBET). The typical amorphous SiO₂ based xerogels were revealed with X-Ray diffraction (XRD) and Selected Area Electron Diffraction (SAED) analysis. Scanning electron microscope- (SEM) and transmission electron microscope (TEM) showed the porous morphology and reduced particle for SiO₂ and La-SiO₂ xerogels respectively. The existence of elements, siloxane networks, and thermal stability of xerogel was confirmed by energy dispersive spectroscopy (EDS), Fourier-transform infrared spectroscopy (FTIR), and Thermographic analysis (TGA). UV-Vis spectroscopy and photoluminescence (PL) have been used to characterize the optical properties of xerogels. La-SiO₂ demonstrates promising characteristic features of an active sensing film for dissolved oxygen in the water. Keywords: Sol-gel, ORMOSILs, encapsulation, Luminophores quenching, O₂-sensing

Keywords: sol-gel, ORMOSILs, luminophores quenching, O₂-sensing

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Authors: Y. J. Lin, Y. F. Lin

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CO2 is the primary greenhouse gas which causes global warming in recent years. As the carbon capture and storage (CCS) getting maturing, the reuse of carbon dioxide which made from CCS is the important issue. In this way, the most common method is the synthesis of cyclic carbonate chemicals from the cycloaddition reaction of carbon dioxide and epoxide. The catalyst plays an important role in the CO2/epoxide cycloaddition reactions. The Lewis acid and base sites are both needed on the catalyst surface for the help of epoxide ring opening, leading to the synthesis of cyclic carbonate. Furthermore, the larger specific surface area and more active site of the catalyst are also needed to enhance the efficiency of the CO2/epoxide cycloaddition reactions. Aerogel is a mesoporous nanomaterial (pore size between 2~50 nm) with high specific surface area and porosity (at least 90%) and low density. In this study, the ternary metal oxide aerogels, Mg-doped Al2O3 aerogels, with higher specific surface area and Lewis acid and base sites on the aerogel surface are successfully prepared by using a facile sol-gel reaction. The as-prepared Mg-doped Al2O3 aerogels are also served as heterogenous catalyst for the CO2/propylene- oxide cycloaddition reaction. Compared to the pristine Al2O3 aerogels, the Mg-doped Al2O3 aerogels possessed both Lewis acid and base sites on the surface are able to enhance the efficiency of the CO2/propylene oxide cycloaddition reactions. As a result, the as-prepared Mg-doped Al2O3 aerogels are a promising and novel catalyst for the CO2/epoxide cycloaddition reactions.

Keywords: ternary, metal oxide aerogel, CO2 reuse, cycloaddition, propylene oxide

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Authors: Chia-Chia Chang, Jhen-Ting Huang, Hu-Cheng Weng, An-Ya Lo

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This study developed a simple hierarchical porous carbon (HPC) synthesis process and used for supercapacitor application. In which, mesopore provides huge specific surface area, meanwhile, macropore provides excellent mass transfer. Thus the hierarchical porous electrode improves the charge-discharge performance. On the other hand, cerium oxide (CeO2) have also got a lot research attention owing to its rich in content, low in price, environmentally friendly, good catalytic properties, and easy preparation. Besides, a rapid redox reaction occurs between trivalent cerium and tetravalent cerium releases oxygen atom and increase the conductivity. In order to prevent CeO2 from disintegration under long-term charge-discharge operation, the CeO2 carbon porous materials were was integrated as composite material in this study. For in the ex-situ analysis, scanning electron microscope (SEM), X-ray diffraction (XRD), transmission electron microscope (TEM) analysis were adopted to identify the surface morphology, crystal structure, and microstructure of the composite. 77K Nitrogen adsorption-desorption analysis was used to analyze the porosity of each specimen. For the in-situ test, cyclic voltammetry (CV) and chronopotentiometry (CP) were conducted by potentiostat to understand the charge and discharge properties. Ragone plot was drawn to further analyze the resistance properties. Based on above analyses, the effect of macropores/mespores and the CeO2/HPC ratios on charge-discharge performance were investigated. As a result, the capacitance can be greatly enhanced by 2.6 times higher than pristine mesoporous carbon electrode.

Keywords: hierarchical porous carbon, cerium oxide, supercapacitor

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Authors: Sony, Ashok N. Bhaskarwar

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Production of hydrogen from a renewable raw material without any co-synthesis of harmful greenhouse gases is the current need for sustainable energy solutions. The sulfur-iodine (SI) thermochemical cycle, using intermediate chemicals, is an efficient process for producing hydrogen at a much lower temperature than that required for the direct splitting of water. No net byproduct forms in the cycle. Hydrogen iodide (HI) decomposition is a crucial reaction in this cycle, as the product, hydrogen, forms only in this step. It is an endothermic, reversible, and equilibrium-limited reaction. The theoretical equilibrium conversion at 550°C is just a meagre of 24%. There is a growing interest, therefore, in enhancing the HI conversion to near-equilibrium values at lower reaction temperatures and by possibly improving the rate. The reaction is relatively slow without a catalyst, and hence catalytic decomposition of HI has gained much significance. Bi-metallic Ni-Co, Ni-Mn, Co-Mn, and tri-metallic Ni-Co-Mn catalysts over zirconia support were tested for HI decomposition reaction. The catalysts were synthesized via a sol-gel process wherein Ni was 3wt% in all the samples, and Co and Mn had equal weight ratios in the Co-Mn catalyst. Powdered X-ray diffraction and Brunauer-Emmett-Teller surface area characterizations indicated the polycrystalline nature and well-developed mesoporous structure of all the samples. The experiments were performed in a vertical laboratory-scale packed bed reactor made of quartz, and HI (55 wt%) was fed along with nitrogen at a WHSV of 12.9 hr⁻¹. Blank experiments at 500°C for HI decomposition suggested conversion of less than 5%. The activities of all the different catalysts were checked at 550°C, and the highest conversion of 23.9% was obtained with the tri-metallic 3Ni-Co-Mn-ZrO₂ catalyst. The decreasing order of the performance of catalysts could be expressed as: 3Ni-Co-Mn-ZrO₂ > 3Ni-2Co-ZrO₂ > 3Ni-2Mn-ZrO₂ > 2.5Co-2.5Mn-ZrO₂. The tri-metallic catalyst remained active till 360 mins at 550°C without any observable drop in its activity/stability. Among the explored catalyst compositions, the tri-metallic catalyst certainly has a better performance for HI conversion when compared to the bi-metallic ones. Owing to their low costs and ease of preparation, these trimetallic catalysts could be used for large-scale hydrogen production.

Keywords: sulfur-iodine cycle, hydrogen production, hydrogen iodide decomposition, bi-, and tri-metallic catalysts

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Authors: Paolo Boscaro, Vasile Hulea, François Fajula, Francis Luck, Anne Galarneau

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TiO2 based monoliths with hierarchical macropores and mesopores have been synthesized following a novel one pot sol-gel synthesis method. Taking advantage of spinodal separation that occurs between titanium isopropoxide and an acidic solution in presence of polyethylene oxide polymer, monoliths with homogeneous interconnected macropres of 3 μm in diameter and mesopores of ca. 6 nm (surface area 150 m2/g) are obtained. Furthermore, these monoliths present some carbon and nitrogen (as shown by XPS and elemental analysis), which considerably reduce titanium oxide energy gap and enable light to be absorbed up to 700 nm wavelength. XRD shows that anatase is the dominant phase with a small amount of brookite. Enhanced light absorption and high porosity of the monoliths are responsible for a remarkable photocatalytic activity. Wastewater treatment has been performed in closed reactor under sunlight using orange G dye as target molecule. Glass reactors guarantee that most of UV radiations (to almost 300 nm) of solar spectrum are excluded. TiO2 nanoparticles P25 (usually used in photocatalysis under UV) and un-doped TiO2 monoliths with similar porosity were used as comparison. C,N-doped TiO2 monolith allowed a complete colorant degradation in less than 1 hour, whereas 10 h are necessary for 40% colorant degradation with P25 and un-doped monolith. Experiment performed in the dark shows that only 3% of molecules have been adsorbed in the C,N-doped TiO2 monolith within 1 hour. The much higher efficiency of C,N-doped TiO2 monolith in comparison to P25 and un-doped monolith, proves that doping TiO2 is an essential issue and that nitrogen and carbon are effective dopants. Monoliths offer multiples advantages in respect to nanometric powders: sample can be easily removed from batch (no needs to filter or to centrifuge). Moreover flow reactions can be set up with cylindrical or flat monoliths by simple sheathing or by locking them with O-rings.

Keywords: C-N doped, sunlight photocatalytic activity, TiO2 monolith, visible absorbance

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Authors: Dina Kon Mushid, Sage Ngoie, Tshimbalanga Madiba, Kabutakapua Kakanda

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Slope stability assessment is still the biggest challenge in mining activities and civil engineering structures. The slope in an opencast mine frequently reaches multiple weak layers that lead to the instability of the pit. Faults and soft layers throughout the rock would increase weathering and erosion rates. Therefore, it is essential to investigate the stability of the complex strata to figure out how stable they are. In the Dikuluwe-Mashamba (DIMA) area, the lithology of the stratum is a set of metamorphic rocks whose parent rocks are sedimentary rocks with a low degree of metamorphism. Thus, due to the composition and metamorphism of the parent rock, the rock formation is different in hardness and softness, which means that when the content of dolomitic and siliceous is high, the rock is hard. It is softer when the content of argillaceous and sandy is high. Therefore, from the vertical direction, it appears as a weak and hard layer, and from the horizontal direction, it seems like a smooth and hard layer in the same rock layer. From the structural point of view, the main structures in the mining area are the Dikuluwe dipping syncline and the Mashamba dipping anticline, and the occurrence of rock formations varies greatly. During the folding process of the rock formation, the stress will concentrate on the soft layer, causing the weak layer to be broken. At the same time, the phenomenon of interlayer dislocation occurs. This article aimed to evaluate the stability of metasedimentary rocks of the Dikuluwe-Mashamba (DIMA) open-pit mine using limit equilibrium and stereographic methods Based on the presence of statistical structural planes, the stereographic projection was used to study the slope's stability and examine the discontinuity orientation data to identify failure zones along the mine. The results revealed that the slope angle is too steep, and it is easy to induce landslides. The numerical method's sensitivity analysis showed that the slope angle and groundwater significantly impact the slope safety factor. The increase in the groundwater level substantially reduces the stability of the slope. Among the factors affecting the variation in the rate of the safety factor, the bulk density of soil is greater than that of rock mass, the cohesion of soil mass is smaller than that of rock mass, and the friction angle in the rock mass is much larger than that in the soil mass. The analysis showed that the rock mass structure types are mostly scattered and fragmented; the stratum changes considerably, and the variation of rock and soil mechanics parameters is significant.

Keywords: slope stability, weak layer, safety factor, limit equilibrium method, stereography method

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Authors: Irakli Gamkrelidze, David Shengelia, Tamara Tsutsunava, Giorgi Chichinadze, Giorgi Beridze, Ketevan Tedliashvili, Tamara Tsamalashvili

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The Loki crystalline massif crops out in the Caucasian region and the geological retrospective represent the northern marginal part of the Baiburt-Sevanian terrain (island arc), bordering with the Paleotethys oceanic basin in the north. The pre-Alpine basement of the massif is built up of Lower-Middle Paleozoic metamorphic complex (metasedimentary and metabasite rocks), Upper Devonian quartz-diorites and Late Variscan granites. Earlier metamorphic complex was considered as an indivisible set including suites with different degree of metamorphism. Systematic geologic, petrologic and geochemical investigations of the massif’s rocks suggest the different conception on composition, structure and formation conditions of the massif. In particular, there are two main rock types in the Loki massif: the oldest autochthonous series of gneissic quartz-diorites and cutting them granites. The massif is flanked on its western side by a volcano-sedimentary sequence, metamorphosed to low-T facies. Petrologic, metamorphic and structural differences in this sequence prove the existence of a number of discrete units (overthrust sheets). One of them, the metabasic sheet represents the fragment of ophiolite complex. It comprises transition types of the second and third layers of the Paleooceanic crust: the upper noncumulated part of the third layer gabbro component and the following lowest part of the parallel diabase dykes of the second layer. The ophiolites are represented by metagabbros, metagabbro-diabases, metadiabases and amphibolite schists. According to the content of petrogenic components and additive elements in metabasites is stated that the protolith of metabasites belongs to petrochemical type of tholeiitic series of basalts. The parental magma of metaophiolites is of E-MORB composition, and by petrochemical parameters, it is very close to the composition of intraplate basalts. The dykes of hypabissal leucocratic siliceous and medium magmatic rocks associated with the metaophiolite sheet form the separate complex. They are granitoids with the extremely low content of CaO and quartz-diorite porphyries. According to various petrochemical parameters, these rocks have mixed characteristics. Their formation took place in spreading conditions or in the areas of manifestation of plumes most likely of island arc type. The metamorphism degree of the metaophiolites corresponds to a very low stage of green schist facies. The rocks of the metaophiolite complex are obducted from the Paleotethys Ocean. Geological and paleomagnetic data show that the primary location of the ocean is supposed to be to the north of the Loki crystalline massif.

Keywords: the Caucasus, crystalline massif, ophiolites, tectonic sheet

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Authors: Asim Laeeq Khan, Mazhar Amjad Gilani, Tayub Raza

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The use of fossil fuels for energy generation leads to the emission of greenhouse gases particularly CO2 into the atmosphere. To date, several techniques have been proposed for the efficient removal of CO2 from flue gas mixtures. Membrane technology is a promising choice due to its several inherent advantages such as low capital cost, high energy efficiency, and low ecological footprint. One of the goals in the development of membranes is to achieve high permeability and selectivity. Mixed matrix membranes comprising of inorganic fillers embedded in polymer matrix are a class of membranes that have showed improved separation properties. One of the biggest challenges in the commercialization if mixed matrix membranes are the removal of non-selective voids existing at the polymer-filler interface. In this work, mixed matrix membranes were prepared using polysulfone as polymer matrix and ordered mesoporous MCM-41 as filler materials. A new approach to removing the interfacial voids was developed by introducing room temperature ionic (RTIL) at the polymer-filler interface. The results showed that the imidazolium based RTIL not only provided wettability characteristics but also helped in further improving the separation properties. The removal of interfacial voids and good contact between polymer and filler was verified by SEM measurement. The synthesized membranes were tested in a custom built gas permeation set-up for the measurement of gas permeability and ideal gas selectivity. The results showed that the mixed matrix membranes showed significantly higher CO2 permeability in comparison to the pristine membrane. In order to have further insight into the role of fillers, diffusion and solubility measurements were carried out. The results showed that the presence of highly porous fillers resulted in increasing the diffusion coefficient while the solubility showed a slight drop. The RTIL filled membranes showed higher CO2/CH4 and CO2/N2 selectivity than unfilled membranes while the permeability dropped slightly. The increase in selectivity was due to the highly selective RTIL used in this work. The study revealed that RTIL filled mixed matrix membranes are an interesting candidate for gas separation membranes.

Keywords: ionic liquids, CO2 separation, membranes, mixed matrix membranes

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Authors: Masome Moeni, Roya Abedizadeh, Elham Aram, Hamid Sadeghi-Abandansari, Davood Sabour, Robert Menzel, Ali Hassanpour

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Significant number of studies and preclinical research in formulation of cancer nano-pharmaceutics have led to an improvement in cancer care. Nonetheless, the antineoplastic agents have ‘failed to live up to its promise’ since their clinical performance is moderately low. For almost ninety years, iron oxide nanoparticles (IONPS) have managed to keep its reputation in clinical application due to their low toxicity, versatility and multi-modal capabilities. Drug Administration approved utilization of IONPs for diagnosis of cancer as contrast media in magnetic resonance imaging, as heat mediator in magnetic hyperthermia and for the treatment of iron deficiency. Furthermore, IONPs have high drug-loading capacity, which makes them good candidates as therapeutic agent transporters. There are yet challenges to overcome for successful clinical application of IONPs, including stability of drug and poor delivery, which might lead to (i) drug resistance, (ii) shorter blood circulation time, and (iii) rapid elimination and adverse side effects from the system. In this study, highly stable and super paramagnetic IONPs were prepared for efficient and targeted drug delivery in cancer treatment. The synthesis procedure was briefly involved the production of IONPs via co-precipitation followed by coating with tetraethyl orthosilicate and 3-aminopropylethoxysilane and grafting with folic acid for stability targeted purposes and controlled drug release. Physiochemical and morphological properties of modified IONPs were characterised using different analytical techniques. The resultant IONPs exhibited clusters of 10 nm spherical shape crystals with less than 100 nm size suitable for drug delivery. The functionalized IONP showed mesoporous features, high stability, dispersibility and crystallinity. Subsequently, the functionalized IONPs were successfully loaded with oxaliplatin, a chemotherapeutic agent, for a controlled drug release in an actively targeting cancer cells. FT-IR observations confirmed presence of oxaliplatin functional groups, while ICP-MS results verified the drug loading was ~ 1.3%.

Keywords: cancer treatment, chemotherapeutic agent, drug delivery, iron oxide, multi-functional nanoparticle

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Authors: Agnieszka Feliczak-Guzik, Paulina Szczyglewska, Izabela Nowak

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A catalyst-assisted oxidation reaction is one of the key reactions exploited by various industries. Their conductivity yields essential compounds and intermediates, such as alcohols, epoxides, aldehydes, ketones, and organic acids. Researchers are devoting more and more attention to developing active and selective materials that find application in many catalytic reactions, such as cyclohexene epoxidation. This reaction yields 1,2-epoxycyclohexane and 1,2-diols as the main products. These compounds are widely used as intermediates in the perfume industry and synthesizing drugs and lubricants. Hence, our research aimed to use hierarchical zeolites modified with transition metal ions, e.g., Nb, V, and Ta, in the epoxidation reaction of cyclohexene using microwaveheating. Hierarchical zeolites are materials with secondary porosity, mainly in the mesoporous range, compared to microporous zeolites. In the course of the research, materials based on two commercial zeolites, with Faujasite (FAU) and Zeolite Socony Mobil-5 (ZSM-5) structures, were synthesized and characterized by various techniques, such as X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), and low-temperature nitrogen adsorption/desorption isotherms. The materials obtained were then used in a cyclohexene epoxidation reaction, which was carried out as follows: catalyst (0.02 g), cyclohexene (0.1 cm3), acetonitrile (5 cm3) and dihydrogen peroxide (0.085 cm3) were placed in a suitable glass reaction vessel with a magnetic stirrer inside in a microwave reactor. Reactions were carried out at 45° C for 6 h (samples were taken every 1 h). The reaction mixtures were filtered to separate the liquid products from the solid catalyst and then transferred to 1.5 cm3 vials for chromatographic analysis. The test techniques confirmed the acquisition of additional secondary porosity while preserving the structure of the commercial zeolite (XRD and low-temperature nitrogen adsorption/desorption isotherms). The results of the activity of the hierarchical catalyst modified with niobium in the cyclohexene epoxidation reaction indicate that the conversion of cyclohexene, after 6 h of running the process, is about 70%. As the main product of the reaction, 2-cyclohexanediol was obtained (selectivity > 80%). In addition to the mentioned product, adipic acid, cyclohexanol, cyclohex-2-en-1-one, and 1,2-epoxycyclohexane were also obtained. Furthermore, in a blank test, no cyclohexene conversion was obtained after 6 h of reaction. Acknowledgments The work was carried out within the project “Advanced biocomposites for tomorrow’s economy BIOG-NET,” funded by the Foundation for Polish Science from the European Regional Development Fund (POIR.04.04.00-00-1792/18-00.

Keywords: epoxidation, oxidation reactions, hierarchical zeolites, synthesis

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Authors: Lucero Gonzalez, Salvador Alfaro

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Carbon dioxide (CO2) and methane (CH4) are considered as the compounds with higher abundance among the greenhouse gases (CO2, NOx, SOx, CxHx, etc.), due to its higher concentration, this two gases have a greater impact in the environment pollution and provokes global warming. So, recovery, disposal and subsequent reuse, are of great interest, especially from the ecological and health perspective. By one hand, porous inorganic materials are good candidates to capture gases, because these type of materials are higher stability from the point view of thermal, chemical and mechanical under adsorption gas processes. By another hand, during the design and the synthetic preparation of the porous materials is possible add other intrinsic properties (physicochemical and structural) by adding chemical compounds as dopants or using structured directed agents or surfactants to improve the porous structure, the above features allow to have alternative materials for separation, capture and storage of greenhouse gases. In this work, ordered mesoporous materials base silica were prepared using Surfynol as surfactant. The surfactant micelles are commonly used as self-assembly templates for the development of new structure porous silica’s, adding a variety of textures and structures. By another hand, the Surfynol is a commercial surfactant, is non-ionic, for that is necessary determine its critical micelles concentration (cmc) by the pyrene I1/I3 ratio method, before to prepare silica particles. One time known the CMC, a precursor gel was prepared via sol-gel process at room temperature using TEOS as silica precursor, NH4OH as catalyst, Surfynol as template and H2O as solvent. Then, the gel precursor was treatment hydrothermally in a Teflon-lined stainless steel autoclave with a volume of 100 mL and kept at 100 ºC for 24 h under static conditions in a convection oven. After that, the porous silica particles obtained were impregnated with lithium to improve the CO2 adsorption capacity. Then the silica particles were characterized physicochemical, morphology and structurally, by XRD, FTIR, BET and SEM techniques. The thermal stability and the CO2 adsorption capacity was evaluated by thermogravimetric analysis (TGA). According the results, we found that the Surfynol is a good candidate to prepare silica particles with an ordered structure. Also the TGA analysis shown that the particles has a good thermal stability in the range of 250 °C and 800 °C. The best materials had, the capacity to adsorbing 70 and 90 mg per gram of silica particles and its CO2 adsorption capacity depends on the way to thermal pretreatment of the porous silica before of the adsorption experiments and of the concentration of surfactant used during the synthesis of silica particles. Acknowledgments: This work was supported by SIP-IPN through project SIP-20161862.

Keywords: CO2 adsorption, lithium as dopant, porous silica, surfynol as surfactant, thermogravimetric analysis

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Authors: Ala’a H. Al-Muhtaseb, Farrukh Jamil, Sandeep K. Saxena

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The fast growth rate of energy consumption along with world population expected to demand 50% more energy by 2030 than nowadays. At present, the energy demand is mostly provided by limited fossil fuel sources such as oil, natural gas, and coal that are resulting in dramatic increase in CO2 emissions from combustion of fossil fuels. The growth of the biodiesel industry over the last decade has resulted in a price drop because glycerol is obtained as a by-product during transesterification of vegetable oil or animal fats, which accounts for one tenth of every gallon of biodiesel produced. The production of oxygenates from glycerol gains much importance due to the excellent diesel-blending property of the oxygenates that not only improve the quality of the fuel but also increases the overall yield of the biodiesel in helping to meet the target for energy production from renewable sources for transport in the energy utilization directives. The reaction of bio-glycerol with bio-acetone was carried out in a magnetically stirred two necked round bottom flaskS. Condensation of bio-glycerol with acetone in the presence of various modified forms of beta zeolite has been done for synthesizing solketal (AB-2 modified with nitric acid, AB-3 modified with oxalic acid). Among all modified forms of beta zeolite, AB-2 showed the best performance for maximum glycerol conversion 94.26 % with 94.21 % solketal selectivity and minimum acetal formation 0.05 %. The physiochemical properties of parent beta zeolite and all its modified forms were analyzed by XRD, SEM, TEM, BET, FTIR and TPD. It has been revealed that AB-2 catalysts with high pore volume and surface area gave high glycerol conversion with maximum solketal selectivity. Despite this, the crystallinity of AB-3 was lower than AB-2 which helps to provide the shorter path length for reactants and product but due high pore volume AB-2 was preferred which gave maximum bio-glycerol conversion. Temperature does matter the glycerol conversion and selectivity of solketal, as it increases from 40 ºC to 60 ºC the conversion of glycerol rises from 80.04 % to 94.26 % and selectivity of solketal from 80.0 % to 94.21 % but further increase in temperature to 100 ºC glycerol conversion reduced to 93.06 % and solketal selectivity to 92.08 %. AB-2 was found to be highly stable as up to 4 repeated experimental runs there was less than 10% decrease in its activity. This process offers an attractive route for converting bio-glycerol, the main by-product of biodiesel to solketal with bio-acetone; a value-added green product with potential industrial applications as a valuable green fuel additive or combustion promoter for gasoline/diesel engines.

Keywords: beta-zeolite, bio-glycerol, catalyst, solketal

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Authors: Qing Zhang, Janak L. Pathak, Macro N. Helder, Richard T. Jaspers, Yin Xiao

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Introduction: Nanomaterial-based bone regeneration is greatly influenced by the immune microenvironment. Tissue-engineered nanomaterials mediate the inflammatory response of macrophages to regulate bone regeneration. Silica nanoparticles have been widely used in tissue engineering-related preclinical studies. However, the effect of topological features on the surface of silica nanoparticles on the immune response of macrophages remains unknown. Purposes: The aims of this research are to compare the influences of normal and pollen-like silica nano-surface topography on macrophage immune responses and to obtain insight into their potential regulatory mechanisms. Method: Macrophages (RAW 264.7 cells) were exposed to mesoporous silica nanoparticles with normal morphology (MSNs) and pollen-like morphology (PMSNs). RNA-seq, RT-qPCR, and LSCM were used to assess the changes in expression levels of immune response-related genes and proteins. SEM and TEM were executed to evaluate the contact and adherence of silica nanoparticles by macrophages. For the assessment of the immunomodulation-mediated osteogenic potential, BMSCs were cultured with conditioned medium (CM) from LPS pre-stimulated macrophage cultures treated with MSNs or PMSNs. Osteoimmunomodulatory potential of MSNs and PMSNs in vivo was tested in a mouse cranial bone osteolysis model. Results: The results of the RNA-seq, RT-qPCR, and LSCM assays showed that PMSNs inhibited the expression of pro-inflammatory genes and proteins in macrophages. SEM images showed distinct macrophage membrane surface binding patterns of MSNs and PMSNs. MSNs were more evenly dispersed across the macrophage cell membrane, while PMSNs were aggregated. PMSNs-induced macrophage anti-inflammatory response was associated with upregulation of the cell surface receptor CD28 and inhibition of ERK phosphorylation. TEM images showed that both MSNs and PMSNs could be phagocytosed by macrophages, and inhibiting nanoparticle phagocytosis did not affect the expression of anti-inflammatory genes and proteins. Moreover, PMSNs-induced conditioned medium from macrophages enhanced BMP-2 expression and osteogenic differentiation mBMSCs. Similarly, PMSNs prevented LPS-induced bone resorption via downregulation of inflammatory reaction. Conclusions: PMSNs can promote bone regeneration by modulating osteoimmunological processes through surface topography. The study offers insights into how surface physical contact cues can modulate the regulation of osteoimmunology and provides a basis for the application of nanoparticles with pollen-like morphology to affect immunomodulation in bone tissue engineering and regeneration.

Keywords: physical contact, osteoimmunology, macrophages, silica nanoparticles, surface morphology, membrane receptor, osteogenesis, inflammation

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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: María Canal-Rodríguez, María Arnaiz, Natalia Rey-Raap, Ana Arenillas, Jon Ajuria

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The constant demand of electrical energy, as well as the increase in environmental concern, lead to the necessity of investing in clean and eco-friendly energy sources that implies the development of enhanced energy storage devices. Li-ion batteries (LIBs) and Electrical double layer capacitors (EDLCs) are the most widespread energy systems. Batteries are able to storage high energy densities contrary to capacitors, which main strength is the high-power density supply and the long cycle life. The combination of both technologies gave rise to Li-ion capacitors (LICs), which offers all these advantages in a single device. This is achieved combining a capacitive, supercapacitor-like positive electrode with a faradaic, battery-like negative electrode. Due to the abundance and affordability, dual carbon-based LICs are nowadays the common technology. Normally, an Active Carbon (AC) is used as the EDLC like electrode, while graphite is the material commonly employed as anode. LICs are potential systems to be used in applications in which high energy and power densities are required, such us kinetic energy recovery systems. Although these devices are already in the market, some drawbacks like the limited power delivered by graphite or the energy limiting nature of AC must be solved to trigger their used. Focusing on the anode, one possibility could be to replace graphite with Hard Carbon (HC). The better rate capability of the latter increases the power performance of the device. Moreover, the disordered carbonaceous structure of HCs enables storage twice the theoretical capacity of graphite. With respect to the cathode, the ACs are characterized for their high volume of micropores, in which the charge is storage. Nevertheless, they normally do not show mesoporous, which are really important mainly at high C-rates as they act as transport channels for the ions to reach the micropores. Usually, the porosity of ACs cannot be tailored, as it strongly depends on the precursor employed to get the final carbon. Moreover, they are not characterized for having a high electrical conductivity, which is an important characteristic to get a good performance in energy storage applications. A possible candidate to substitute ACs are carbon aerogels (CAs). CAs are materials that combine a high porosity with great electrical conductivity, opposite characteristics in carbon materials. Furthermore, its porous properties can be tailored quite accurately according to with the requirements of the application. In the present study, CAs with controlled porosity were obtained from polymerization of resorcinol and formaldehyde by microwave heating. Varying the synthesis conditions, mainly the amount of precursors and pH of the precursor solution, carbons with different textural properties were obtained. The way the porous characteristics affect the performance of the cathode was studied by means of a half-cell configuration. The material with the best performance was evaluated as cathode in a LIC versus a hard carbon as anode. An analogous full LIC made by a high microporous commercial cathode was also assembled for comparison purposes.

Keywords: li-ion capacitors, energy storage, tailored porosity, carbon aerogels

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Authors: R. P. Naik, A. K. Rakshit

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In recent years, with the rapid development in science and technology, people have increasing requirements on uses of clothing for new functions, which contributes to opportunities for further development and incorporation of new technologies along with novel materials. In this context, textiles are of fast decalescence or fast heat radiation media as per as comfort accountability of textile articles are concern. The microstructure and texture of textiles play a vital role in determining the heat-moisture comfort level of the human body because clothing serves as a barrier to the outside environment and a transporter of heat and moisture from the body to the surrounding environment to keep thermal balance between body heat produced and body heat loss. The main bottleneck which is associated with textile materials to be successful as thermal insulation materials can be enumerated as; firstly, high loft or bulkiness of material so as to provide predetermined amount of insulation by ensuring sufficient trapping of air. Secondly, the insulation depends on forced convection; such convective heat loss cannot be prevented by textile material. Third is that the textile alone cannot reach the level of thermal conductivity lower than 0.025 W/ m.k of air. Perhaps, nano-fibers can do so, but still, mass production and cost-effectiveness is a problem. Finally, such high loft materials for thermal insulation becomes heavier and uneasy to manage especially when required to carry over a body. The proposed works aim at developing lightweight effective thermal insulation textiles in combination with nanoporous silica-gel which provides the fundamental basis for the optimization of material properties to achieve good performance of the clothing system. This flexible nonwoven silica-gel composites fabric in intact monolith was successfully developed by reinforcing SiO2-gel in thermal bonded nonwoven fabric via sol-gel processing. Ambient Pressure Drying method is opted for silica gel preparation for cost-effective manufacturing. The formed structure of the nonwoven / SiO₂ -gel composites were analyzed, and the transfer properties were measured. The effects of structure and fibre on the thermal properties of the SiO₂-gel composites were evaluated. Samples are then tested against untreated samples of same GSM in order to study the effect of SiO₂-gel application on various properties of nonwoven fabric. The nonwoven fabric composites reinforced with aerogel showed intact monolith structure were also analyzed for their surface structure, functional group present, microscopic images. Developed product reveals a significant reduction in pores' size and air permeability than the conventional nonwoven fabric. Composite made from polyester fibre with lower GSM shows lowest thermal conductivity. Results obtained were statistically analyzed by using STATISTICA-6 software for their level of significance. Univariate tests of significance for various parameters are practiced which gives the P value for analyzing significance level along with that regression summary for dependent variable are also studied to obtain correlation coefficient.

Keywords: silica-gel, heat insulation, nonwoven fabric, thermal barrier clothing

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Authors: Ayman Hijazi, Witold Kwapinski, J. J. Leahy

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Finding a sustainable alternative energy to fossil fuel is an urgent need as various environmental challenges in the world arise. Therefore, formic acid (FA) decomposition has been an attractive field that lies at the center of biomass platform, comprising a potential pool of hydrogen energy that stands as a new energy vector. Liquid FA features considerable volumetric energy density of 6.4 MJ/L and a specific energy density of 5.3 MJ/Kg that qualifies it in the prime seat as an energy source for transportation infrastructure. Additionally, the increasing research interest in FA decomposition is driven by the need of in-situ H2 production, which plays a key role in the hydrogenation reactions of biomass into higher value components. It is reported elsewhere in literature that catalytic decomposition of FA is usually performed in poorly designed setup using simple glassware under magnetic stirring, thus demanding further energy investment to retain the used catalyst. it work suggests an approach that integrates designing a novel catalyst featuring magnetic property with a robust setup that minimizes experimental & measurement discrepancies. One of the most prominent active species for dehydrogenation/hydrogenation of biomass compounds is palladium. Accordingly, we investigate the potential of engrafting palladium metal onto functionalized magnetic nanoparticles as a heterogeneous catalyst to favor the production of CO-free H2 gas from FA. Using ordinary magnet to collect the spent catalyst renders core-shell magnetic nanoparticles as the backbone of the process. Catalytic experiments were performed in a jacketed batch reactor equipped with an overhead stirrer under inert medium. Through a novel approach, FA is charged into the reactor via high-pressure positive displacement pump at steady state conditions. The produced gas (H2+CO2) was measured by connecting the gas outlet to a measuring system based on the amount of the displaced water. The novelty of this work lies in designing a very responsive catalyst, pumping consistent amount of FA into a sealed reactor running at steady state mild temperatures, and continuous gas measurement, along with collecting the used catalyst without the need for centrifugation. Catalyst characterization using TEM, XRD, SEM, and CHN elemental analyzer provided us with details of catalyst preparation and facilitated new venues to alter the nanostructure of the catalyst framework. Consequently, the introduction of amine groups has led to appreciable improvements in terms of dispersion of the doped metals and eventually attaining nearly complete conversion (100%) of FA after 7 hours. The relative importance of the process parameters such as temperature (35-85°C), stirring speed (150-450rpm), catalyst loading (50-200mgr.), and Pd doping ratio (0.75-1.80wt.%) on gas yield was assessed by a Taguchi design-of-experiment based model. Experimental results showed that operating at lower temperature range (35-50°C) yielded more gas while the catalyst loading and Pd doping wt.% were found to be the most significant factors with a P-values 0.026 & 0.031, respectively.

Keywords: formic acid decomposition, green catalysis, hydrogen, mesoporous silica, process optimization, nanoparticles

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