Search results for: thermogravimetric

Authors: M. A. Karakassides, M. Baikousi, A. Kouloumpis, D. Gournis

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Nanocomposites of Carbon Nanorods (CNRs) with Polystyrene (PS), have been synthesized successfully by means of in situ polymerization process and characterized. Firstly, carbon nanorods with graphitic structure were prepared by the standard synthetic procedure of CMK-3 using MCM-41 as template, instead of SBA-15, and sucrose as carbon source. In order to create an organophilic surface on CNRs, two parts of modification were realized: surface chemical oxidation (CNRs-ox) according to the Staudenmaier’s method and the attachment of octadecylamine molecules on the functional groups of CNRs-ox (CNRs-ODA The nanocomposite materials of polystyrene with CNRs-ODA, were prepared by a solution-precipitation method at three nanoadditive to polymer loadings (1, 3 and 5 wt. %). The as derived nanocomposites were studied with a combination of characterization and analytical techniques. Especially, Fourier-transform infrared (FT-IR) and Raman spectroscopies were used for the chemical and structural characterization of the pristine materials and the derived nanocomposites while the morphology of nanocomposites and the dispersion of the carbon nanorods were analyzed by atomic force and scanning electron microscopy techniques. Tensile testing and thermogravimetric analysis (TGA) along with differential scanning calorimetry (DSC) were also used to examine the mechanical properties and thermal stability -glass transition temperature of PS after the incorporation of CNRs-ODA nanorods. The results showed that the thermal and mechanical properties of the PS/ CNRs-ODA nanocomposites gradually improved with increasing of CNRs-ODA loading.

Keywords: nanocomposites, polystyrene, carbon, nanorods

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Authors: Seyfullah Madakbas, Emrah Cakmakci

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Polyaniline (PANI), the most studied member of the conductive polymers, has a wide range of uses from several electronic devices to various conductive high-technology applications. Boron nitride (BN) is a boron and nitrogen containing compound with superior chemical and thermal resistance and thermal conductivity. Even though several composites of PANI was prepared in literature, the preparation of h-BN/PANI composites is rare. In this work PANI was polymerized in the presence of different amounts of h-BN (1, 3 and 5% with respect to PANI) by using 0.1 M solution of NH4S2O8 in HCl as the oxidizing agent and conductive composites were prepared. Composites were structurally characterized with FTIR spectroscopy and X-Ray Diffraction (XRD). Thermal properties of conductive composites were determined by thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). Dielectric measurements were performed in the frequency range of 106–108 Hz at room temperature. The corresponding bands for the benzenoid and quinoid rings at around 1593 and 1496 cm-1 in the FTIR spectra of the composites proved the formation of polyaniline. Together with the FTIR spectra, XRD analysis also revealed the existence of the interactions between PANI and h-BN. Glass transition temperatures (Tg) of the composites increased with the increasing amount of PANI (from 87 to 101). TGA revealed that the char yield of the composites increased as the amount of h-BN was increased in the composites. Finally the dielectric permittivity of 3 wt.%h-BN-containing composite was measured and found as approximately 17. This work was supported by Marmara University, Commission of Scientific Research Project.

Keywords: dielectric permittivity, h-BN, PANI, thermal analysis

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Authors: Gamze Karanfil Celep, Kevser Dincer

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The effects of polymer concentration and electrospinning process parameters on the average diameters of electrospun polyacrylonitrile (PAN) nanofibers were experimentally investigated. Besides, mechanical and thermal properties of PAN nanofibers were examined by tensile test and thermogravimetric analysis (TGA), respectively. For this purpose, the polymer concentration, solution feed rate, supply voltage and tip-to-collector distance were determined as the control factors. To succeed these aims, Taguchi’s L16 orthogonal design (4 parameters, 4 level) was employed for the experimental design. Optimal electrospinning conditions were defined using the signal-to-noise (S/N) ratio that was calculated from diameters of the electrospun PAN nanofibers according to "the-smaller-the-better" approachment. In addition, analysis of variance (ANOVA) was evaluated to conclude the statistical significance of the process parameters. The smallest diameter of PAN nanofibers was observed. According to the S/N ratio response results, the most effective parameter on finding out of nanofiber diameter was determined. Finally, the Taguchi design of experiments method has been found to be an effective method to statistically optimize the critical electrospinning parameters used in nanofiber production. After determining the optimum process parameters of nanofiber production, electrical conductivity and fuel cell performance of electrospun PAN nanofibers on the carbon papers will be evaluated.

Keywords: nanofiber, electrospinning, polyacrylonitrile, Taguchi method

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Authors: Kwangwon Seo, Haksoo Han

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Al-Si was synthesized and introduced in poly 2,2’-m-(phenylene)-5,5’-bibenzimidazole (PBI). As a result, a series of five Al-Si/PBI composite (ASPBI) membranes (0, 3, 6, 9, and 12 wt.%) were developed and characterized for application in high temperature polymer electrolyte membrane fuel cells (HT-PEMFCs). The chemical and morphological structure of ASPBI membranes were analyzed by Fourier transform infrared spectroscopy, X-ray diffractometer and scanning electron microscopy. According to the doping level test and thermogravimetric analysis, as the concentration of Al-Si increased, the doping level increased up to 475%. Moreover, the proton conductivity, current density at 0.6V, and maximum power density of ASPBI membranes increased up to 0.31 Scm-1, 0.320 Acm-2, and 0.370 Wcm-2, respectively, because the increased concentration of Al-Si allows the membranes to hold more PA. Alternatively, as the amount of Al-Si increased, the tensile strength of PA-doped and -undoped membranes decreased. This was resulted by both excess PA and aggregation, which can cause serious degradation of the membrane and induce cracks. Moreover, the PA-doped and -undoped ASPBI12 had the lowest tensile strength. The improved performances of ASPBI membranes imply that ASPBI membranes are possible candidates for HT-PEMFC applications. However, further studies searching to improve the compatibility between PBI matrix and inorganic and optimize the loading of Al-Si should be performed.

Keywords: composite membrane, high temperature polymer electrolyte membrane fuel cell, membrane electrode assembly, polybenzimidazole, polymer electrolyte membrane, proton conductivity

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Authors: M. A. Hannan, N. Matthias Neisius

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Organophosphorus compound diethyloxymethyl-9-oxa-10-phosphaphenanthrene-10-oxide (DOPAC) was applied on cotton cellulose to impart eco-friendly flame retardant property to it. Here acetal linkage was introduced rather than conventionally used ester linkage to rescue from the undurability problem of flame retardant compound. Some acidic catalysts, sodium dihydrogen phosphate (NaH2PO4), ammonium dihydrogen phosphate (NH4H2PO4) and phosphoric acid (H3PO4) were successfully used to form acetal linkage between the base material and flame retardant compound. Inspiring limiting oxygen index (LOI) value of 22.4 was found after exclusive washing treatment. A good outcome of total heat of combustion (THC) 6.05 KJ/g was found possible during pyrolysis combustion flow calorimetry (PCFC) test of the treated sample. Low temperature dehydration with sufficient amount of char residue (14.89%) was experienced in case of treated sample. In addition, the temperature of peak heat release rate (TPHRR) 343.061°C supported the expected low temperature pyrolysis in condensed phase mechanism. With the consequence of pyrolysis effects, thermogravimetric analysis (TGA) also reported inspiring weight retention% of the treated samples.

Keywords: acetal linkage, char residue, cotton cellulose, flame retardant, loi, low temperature pyrolysis, organophosphorus, THC, THRR

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Authors: Alireza Khaloo, Asghar Gholizadeh-Vayghan

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The present work focuses on the characterization of the physicochemical properties of kaolinitic clays in both raw and calcined (i.e., dehydroxylated) states. The properties investigated included the dehydroxylation temperature, chemical composition and crystalline phases, band types, kaolinite content, vitreous phase, and reactive and unreactive silica and alumina. The thermogravimetric analysis, X-ray diffractometry and infrared spectroscopy results suggest that full dehydroxylation takes place at 639°C, converting kaolinite to reactive metakaolinite (Si₂Al₂O₇). Application of higher temperatures up to 800 °C leads to complete decarbonation of the calcite phase, and the kaolinite converts to mullite at temperatures exceeding 957 °C. Calcination at 639°C was found to cause a 50% increase in the vitreous content of kaolin. Statistically meaningful increases in the reactivity of silica, alumina, calcite and sodium carbonate in kaolin were detected as a result of such thermal treatment. Such increases were found to be 11%, 47%, 240% and 10%, respectively. The ferrite phase, however, showed a 36% decline in reactivity. The proposed approach can be used as an analytical method to determine the viability of the source of kaolinite and proper physical and chemical modifications needed to enhance its suitability for geopolymer production.

Keywords: physicochemical properties, dehydroxylation, kaolinitic clays, kaolinite content, vitreous phase, reactivity

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Authors: Christian C. Vaso, Rinlee Butch M. Cervera

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One of the most promising anode materials for solid oxide electrolysis cell (SOEC) application is the Sr-doped LaMnO₃ (LSM) which is known to have a high electronic conductivity but low ionic conductivity. To increase the ionic conductivity or diffusion of ions through the anode, Yttria-stabilized Zirconia (YSZ), which has good ionic conductivity, is proposed to be combined with LSM to create a composite electrode and to obtain a high mixed ionic and electronic conducting anode. In this study, composite of lanthanum strontium manganite and YSZ oxide, La_0.8Sr_0.2MnO₃/Zr_0.92Y_0.08O₂ (LSM/YSZ), with different wt.% compositions of LSM and YSZ were synthesized using solid-state reaction. The obtained prepared composite samples of 60, 50, and 40 wt.% LSM with remaining wt.% of 40, 50, and 60, respectively for YSZ were fully characterized for its microstructure by using powder X-ray diffraction (XRD), Thermogravimetric analysis (TGA), Fourier transform infrared (FTIR), and Scanning electron microscope/Energy dispersive spectroscopy (SEM/EDS) analyses. Surface morphology of the samples via SEM analysis revealed a well-sintered and densified pure LSM, while a more porous composite sample of LSM/YSZ was obtained. Electrochemical impedance measurements at intermediate temperature range (500-700 °C) of the synthesized samples were also performed which revealed that the 50 wt.% LSM with 50 wt.% YSZ (L50Y50) sample showed the highest total conductivity of 8.27x10^-1 S/cm at 600 ^oC with 0.22 eV activation energy.

Keywords: ceramics, microstructure, fuel cells, electrochemical impedance spectroscopy

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Authors: Emmanuel Chinagorom Nwadike, Joseph Tagbo Nwabanne, Matthew Ndubuisi Abonyi, Onyemazu Andrew Azaka

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This research focused on the modeling of the convective drying of aerial yam using finite element methods. The thermo-gravimetric analyzer was used to determine the thermal stability of the sample. An aerial yam sample of size 30 x 20 x 4 mm was cut with a mold designed for the purpose and dried in a convective dryer set at 4m/s fan speed and temperatures of 68.58 and 60.56°C. The volume shrinkage of the resultant dried sample was determined by immersing the sample in a toluene solution. The finite element analysis was done with PDE tools in Matlab 2015. Seven kinetic models were employed to model the drying process. The result obtained revealed three regions in the thermogravimetric analysis (TGA) profile of aerial yam. The maximum thermal degradation rates of the sample occurred at 432.7°C. The effective thermal diffusivity of the sample increased as the temperature increased from 60.56°C to 68.58°C. The finite element prediction of moisture content of aerial yam at an air temperature of 68.58°C and 60.56°C shows R² of 0.9663 and 0.9155, respectively. There was a good agreement between the finite element predicted moisture content and the measured moisture content, which is indicative of a highly reliable finite element model developed. The result also shows that the best kinetic model for the aerial yam under the given drying conditions was the Logarithmic model with a correlation coefficient of 0.9991.

Keywords: aerial yam, finite element, convective, effective, diffusivity

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Authors: Rana Th. A. Al-Rubaye, Arthur A. Garforth

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This work details the generation of thin films of structured zeolite catalysts (ZSM–5 and Y) onto the surface of a metal substrate (FeCrAlloy) using in-situ hydrothermal synthesis. In addition, the zeolite Y is post-synthetically modified by acidified ammonium ion exchange to generate US-Y. Finally the catalytic activity of the structured ZSM-5 catalyst films (Si/Al = 11, thickness 146 µm) and structured US–Y catalyst film (Si/Al = 8, thickness 23µm) were compared with the pelleted powder form of ZSM–5 and USY catalysts of similar Si/Al ratios. The structured catalyst films have been characterised using a range of techniques, including X-ray diffraction (XRD), Electron microscopy (SEM), Energy Dispersive X–ray analysis (EDX) and Thermogravimetric Analysis (TGA). The transition from oxide-on-alloy wires to hydrothermally synthesised uniformly zeolite coated surfaces was followed using SEM and XRD. In addition, the robustness of the prepared coating was confirmed by subjecting these to thermal cycling (ambient to 550°C). The cracking of n–heptane over the pellets and structured catalysts for both ZSM–5 and Y zeolite showed very similar product selectivities for similar amounts of catalyst with an apparent activation energy of around 60 kJ mol-1. This paper demonstrates that structured catalysts can be manufactured with excellent zeolite adherence and when suitably activated/modified give comparable cracking results to the pelleted powder forms. These structured catalysts will improve temperature distribution in highly exothermic and endothermic catalysed processes.

Keywords: FeCrAlloy, structured catalyst, zeolite Y, zeolite ZSM-5

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Authors: Ana Jurkeviciute, Larisa Grigorieva, Ksenia Moskvinа

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Oil shale alkylresorcinols are formed as a by-product in oil shale processing. They are unique raw material for chemical industry. Polycondensation resins obtaining is one of the worthwhile directions of oil shale alkylresorcinols use. These resins are widely applied in many branches of industry such as wood-working, metallurgic, tire, rubber products, construction etc. Possibility of resins obtaining using overall alkylresorcinols will allow to cheapen finished products on their base and to widen the range of resins offered on the market. Synthesis of polycondensation resins on the basis of alkylresorcinols was conducted by several methods in the process of investigations. In the formulations a part of resorcinol was replaced by fractions of oil shale alkylresorcinols containing different amount of 5-methylresorcinol (40-80 mass %). Some resins were modified by aromatic alkene at the stage of synthesis. Thermal stability and degradation behavior of resins were investigated by thermogravimetric analysis (TGA) method both in an inert nitrogen environment and in an oxidative environment of air. TGA integral curves were obtained and processed in dynamic mode for interval of temperatures from 25 to 830 °C. Rate of temperature rise was 5°C/min, gas flow rate - 50 ml/min. Resins power for carbonization was evaluated by carbon residue. Physical-chemical parameters of the resins were determined. Content of resorcinol and 5-methylresorcinol not reacted in the process of synthesis were determined by gas chromatography method.

Keywords: resorcinol, oil shale alkylresorcinols, aromatic alkene, polycondensation resins, modified resins

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Authors: Marcelle Muriel Domkam Tchunkam, Rolin Feudjio

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This work investigates the ultrastructure, physicochemical and thermal properties evaluation of Palm Kernel Shells (PKS). PKS Tenera waste samples were obtained from a palm oil mill in Dizangué Sub-Division, Littoral region of Cameroon, while PKS Dura waste samples were collected from the Institute of Agricultural Research for Development (IRAD) of Mbongo. A sodium hydroxide solution was used to wash the shells. They were then rinsed by demineralised water and dried in an oven at 70 °C during 72 hours. They were then grounded and sieved to obtained powders from 0.04 mm to 0.45 mm in size. Transmission Electron Microscopy (TEM) and Surface Electron Microscopy (SEM) were used to characterized powder samples. Chemical compounds and elemental constituents, as well as thermal performance were evaluated by Van Soest Method, TEM/EDXA and SEM/EDS techniques. Thermal characterization was also performed using Differential Scanning Calorimetry (DSC) and Thermogravimetric Analysis (TGA). Our results from microstructural analysis revealed that most of the PKS material is made of particles with irregular morphology, mainly amorphous phases of carbon/oxygen with small amounts of Ca, K, and Mg. The DSC data enabled the derivation of the materials’ thermal transition phases and the relevant characteristic temperatures and physical properties. Overall, our data show that PKS have nanopores and show potential in 3D printing and membrane filtration applications.

Keywords: DSC, EDXA, palm kernel shells, SEM, TEM

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Authors: Sandra C. L. Dorea, Joann K. Whalen, Yixin Shao, Oumarou Savadogo

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The major challenge for industries that rely on fossil fuels in manufacturing processes or to provide goods and services is to lower their CO2 emissions, as the case for the manufacture of Portland cement. Feasible materials for this purpose can include agro-industrial or agricultural wastes, which are termed 'biosilica' since the silica was contained in a biological matrix (biomass). Corn cob (CC) has some characteristics that make it a good candidate as biosilica source: 1) it is an abundant grain crop produced around the world; 2) more production means more available residues is left in the field to be used. This work aims to evaluate the CC collected from different farms in Canada during the corn harvest in order to see if they can be used together as a biosilica source. The characterization of the raw CC was made in the physical, chemical, and thermal way. The moisture content, the granulometry, and the morphology were also analyzed. The ash content measured was 2,1%. The Thermogravimetric Analysis (TGA) and its Derivative (DTG) evaluated of CC as a function of weight loss with temperature variation ranging between 30°C and 800°C in an atmosphere of N2. The chemical composition and the presence of silica revealed that the different sources of the CC do not interfere in its basic chemical composition, which means that this kind of waste can be used together as a source of biosilica no matter where they come from. Then, this biosilica can partially replace the cement Portland making sustainable cementitious mixtures and contributing to reduce the CO2 emissions.

Keywords: biosilica, characterization, corn cob, sustainable cementitious materials

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Authors: Umran Kurtan, Hamide Aydin, Sevim Unugur Celik, Ayhan Bozkurt

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In the present work, novel hBN/polyacrylonitrile composite nanofibers were produced via electrospinning approach and loaded with the electrolyte for rechargeable lithium-ion battery applications. The electrospun nanofibers comprising various hBN contents were characterized by using Fourier transform infrared spectroscopy (FT-IR), thermogravimetric analysis (TGA), X-ray diffraction (XRD) and scanning electron microscopy (SEM) techniques. The influence of hBN/PAN ratios onto the properties of the porous composite system, such as fiber diameter, porosity, and the liquid electrolyte uptake capability were systematically studied. Ionic conductivities and electrochemical characterizations were evaluated after loading electrospun hBN/PAN composite nanofiber with liquid electrolyte, i.e., 1 M lithium hexafluorophosphate (LiPF6) in ethylene carbonate (EC)/ethyl methyl carbonate (EMC) (1:1 vol). The electrolyte loaded nanofiber has a highest ionic conductivity of 10−3 S cm⁻¹ at room temperature. According to cyclic voltammetry (CV) results it exhibited a high electrochemical stability window up to 4.7 V versus Li+/Li. Li//10 wt% hBN/PAN//LiCO₂ cell was produced which delivered high discharge capacity of 144 mAhg⁻¹ and capacity retention of 92.4%. Considering high safety and low cost properties of the resulting hBN/PAN fiber electrolytes, these materials can be suggested as potential separator materials for lithium-ion batteries.

Keywords: hexagonal boron nitride, polyacrylonitrile, electrospinning, lithium ion battery

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Authors: Seyfullah Madakbaş, Ferhat Şen, Memet Vezir Kahraman

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The aim of this study was to improve thermal stability, mechanical and surface properties of thermoplastic polyurethane (TPU) with the addition of BaTiO3. The TPU/ BaTiO3 composites having various ratios of TPU and BaTiO3 were prepared. The chemical structure of the prepared composites was investigated by FT-IR. FT-IR spectra of TPU/ barium titanate composites show that they successfully were prepared. Thermal stability of the samples was evaluated by thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). The prepared composites showed high thermal stability, and the char yield increased as barium titanate content increased. The glass transition temperatures of the composites rise with the addition of barium titanate. Mechanical properties of the samples were characterized with stress-strain test. The mechanical properties of the TPU were increased with the contribution of the contribution of the barium titanate it increased. Hydrophobicity of the samples was determined by the contact angle measurements. The contact angles have the tendency to increase the hydrophobic behavior on the surface, when barium titanate was added into TPU. Moreover, the surface morphology of the samples was investigated by a scanning electron microscopy (SEM). SEM-EDS mapping images showed that barium titanate particles were dispersed homogeneously. Finally, the obtained results prove that the prepared composites have good thermal, mechanical and surface properties and that they can be used in many applications such as the electronic devices, materials engineering and other emergent.

Keywords: barium titanate, composites, thermoplastic polyurethane, scanning electron microscopy

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Authors: Ljerka Kratofil Krehula, Martina Perlog, Jasmina Stjepanović, Vanja Gilja, Marijana Kraljić Roković, Zlata Hrnjak-Murgić

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The composite preparation of titanium dioxide and zinc oxide photocatalysts with the conductive polymers gives the opportunity to carry out the catalysis reactions not only under UV light but also under visible light. Such processes may efficiently use sunlight in degradation of different organic pollutants and present new design for wastewater treatment. The paper presents the preparation procedure, material characteristics and photocatalytic efficiency of polypyrrole/titanium dioxide and polypyrrole/zinc oxide composites (PPy/TiO2 and PPy/ZnO). The obtained composite samples were characterized by Fourier transform infrared spectroscopy (FTIR), UV-Vis spectroscopy and thermogravimetric analysis (TGA). The photocatalytic efficiency of the samples was determined following the decomposition of Acid Blue 25 dye (AB 25) under UV and visible light by UV/Vis spectroscopy. The efficiency of degradation is determined by total organic carbon content (TOC) after photocatalysis processes. The results show enhanced photocatalytic efficiency of the samples under visible light, so the prepared composite samples are recognized as efficient catalysts in degradation process of AB 25 dye. It can be concluded that the preparation of TiO2 or ZnO composites with PPy can serve as a very efficient method for the improvement of TiO2 and ZnO photocatalytic performance under visible light.

Keywords: composite, photocatalysis, polypyrrole, titanium dioxide, zinc oxide

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Authors: Anastasia Stamatiou, Melissa Obermeyer, Ludger J. Fischer, Philipp Schuetz, Jörg Worlitschek

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This study evaluates unbranched, saturated carboxylic esters with respect to their suitability to be used as storage media for latent heat storage applications. Important thermophysical properties are gathered both by means of literature research as well as by experimental measurements. Additionally, esters are critically evaluated against other common phase-change materials in terms of their environmental impact and their economic potential. The experimental investigations are performed for eleven selected ester samples with a focus on the determination of their melting temperature and their enthalpy of fusion using differential scanning calorimetry. Transient Hot Bridge was used to determine the thermal conductivity of the liquid samples while thermogravimetric analysis was employed for the evaluation of the 5% weight loss temperature as well as of the decomposition temperature of the non-volatile samples. Both experimental results and literature data reveal the high potential of esters as phase-change materials. Their good thermal and environmental properties as well as the possibility for production from natural sources (e.g. vegetable oils) render esters as very promising for future storage applications. A particularly high short term application potential of esters could lie in low temperature storage applications where the main alternative is using salt hydrates as phase-change material.

Keywords: esters, phase-change materials, thermal properties, latent heat storage

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Authors: Marcia Silva, Jayme Kolarik, Brennon Garthwait, William Lee, Hai-Feng Zhang

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Adsorption of lead by a natural porous material was studied to establish a baseline for the removal of heavy metals from drinking and waste water. Samples were examined under different conditions such as solution pH, solution concentration, solution temperature, and exposure time. New materials with potentially enhanced adsorption properties were developed by functionalizing the surface of the natural porous material to fabricate graphene based coated and sulfide based treated porous material. The functionalized materials were characterized with Fourier Transform Infrared Spectroscopy (FTIR), Raman, Thermogravimetric Analysis (TGA) and Scanning Electron Microscopy (SEM) and Energy Dispersive Spectroscopy (EDS) techniques. Solution pH effect on removal efficiency has been investigated in acidic (pH = 4), neutral (pH = 6) and basic (pH = 10) pH levels. All adsorbent materials showed highest adsorption capacities at neutral pH levels. Batch experiment was employed to assess the efficacy for the removal of lead with the sorption kinetics and the adsorption isotherms being determined for the natural and treated porous materials. The addition of graphene-based and sulfide-based materials increased the lead removal capacity of the natural clean porous material. Theoretical calculations confirmed pseudo-second order model as kinetic mechanism for lead adsorption for all adsorbents.

Keywords: heavy metals, ion exchange, adsorption, water remediation

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Authors: Maíra O. Palm, Cintia Marangoni, Ozair Souza, Noeli Sellin

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Wastes from a vegetal extracts industry (cocoa, oak, Guarana and mate) were characterized by particle size, proximate and ultimate analysis, lignocellulosic fractions, high heating value, thermal analysis (Thermogravimetric analysis – TGA, and Differential thermal analysis - DTA) and energy density to evaluate their potential as biomass in the form of briquettes for power generation. All wastes presented adequate particle sizes to briquettes production. The wastes showed high moisture content, requiring previous drying for use as briquettes. Cocoa and oak wastes had the highest volatile matter contents with maximum mass loss at 310 ºC and 450 ºC, respectively. The solvents used in the aroma extraction process influenced in the moisture content of the wastes, which was higher for mate due to water has been used as solvent. All wastes showed an insignificant loss mass after 565 °C, hence resulting in low ash content. High carbon and hydrogen contents and low sulfur and nitrogen contents were observed ensuring a low generation of sulfur and nitrous oxides. Mate and cocoa exhibited the highest carbon and lignin content, and high heating value. The dried wastes had high heating value, from 17.1 MJ/kg to 20.8 MJ/kg. The results indicate the energy potential of wastes for use as fuel in power generation.

Keywords: agro-industrial waste, biomass, briquettes, combustion

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Authors: Hati̇ce Bi̇rtane, Asli Beyler Çi̇ği̇l, Memet Vezi̇r Kahraman

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Polyimide (PI) is one of the most important super-engineering materials because of its mechanical properties and its thermal stability. Electronic industry is the typical extensive applications of polyimides including interlayer insulation films, buffer coating, films, alpha-ray shielding films, and alignment films for liquid crystal displays. The mechanical and thermal properties of polymers are generally improved by the addition of inorganic additives. The challenges in this area of high-performance organic/inorganic hybrid materials are to obtain significant improvements in the interfacial adhesion between the polymer matrix and the reinforcing material since the organic matrix is relatively incompatible with the inorganic phase. In this study, modified nanodiamond was prepared from the reaction of nanodiamond and (3-Mercaptopropyl)trimethoxysilane. Poly(amic acid) was prepared from the reaction of 3,3',4,4'-Benzophenonetetracarboxylic dianhydride (BTDA) and 4,4'-Oxydianiline (ODA). Polyimide/modified nanodiamond hybrids were prepared by blending of poly(amic acid) and organically modified nanodiamond. The morphology of the Polyimide/ modified nanodiamond hybrids was characterized by scanning electron microscopy (SEM). Chemical structure of polyimide and Polyimide/modified nanodiamond hybrids was characterized by FTIR. FTIR results showed that the Polyimide/modified nanodiamond hybrids were successfully prepared. A thermal property of the Polyimide/modified nanodiamond hybrids was characterized by thermogravimetric analysis (TGA).

Keywords: hybrid materials, nanodiamond, polyimide, polymer

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Authors: Rezzouq Asiya, Bouftou Abderrahim, Belfadil Doha, Taoufyk Azzeddine, El Bouchti Mehdi, Zyade Souad, Cherkaoui Omar, Majid Sanaa

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Plastic packaging is widely used, but its pollution is a major environmental problem. Solutions require new sustainable technologies, environmental management, and the use of bio-based polymers as sustainable packaging. Cellulose acetate (CA) is a biobased polymer used in a variety of applications such as the manufacture of plastic films, textiles, and filters. However, it has limitations in terms of thermal stability and rigidity, which necessitates the addition of plasticizers to optimize its use in packaging. Plasticizers are molecules that increase the flexibility of polymers, but their influence on the chemical and physical properties of films (CA) has not been studied in detail. Some studies have focused on mechanical and thermal properties. However, an in-depth analysis is needed to understand the interactions between the additives and the polymer matrix. In this study, the aim is to examine the effect of two types of plasticizers, glycerol (a conventional plasticizer) and an ionic liquid, on the transparency, mechanical, thermal and barrier properties of cellulose acetate (CA) films prepared by the solution-casting method . Various analytical techniques were used to characterize these films, including infrared spectroscopy (FT-IR), X-ray diffraction (XRD), thermogravimetric analysis (TGA), water vapor permeability (WVP), oxygen permeability, scanning electron microscopy (SEM), opacity, transmission analysis and mechanical tests.

Keywords: cellulose acetate, plasticizers, biopolymers, ionic liquid, glycerol.

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Authors: Sajid Shah, Yoshimitsu Uemura, Katsuki Kusakabe

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Sol-gel derived hydrophobic silica membranes with pore sizes less than 1 nm are quite attractive for gas separation in a wide range of temperatures. A nano-structured hydrophobic membrane was prepared by sol-gel technique on a porous α–Al₂O₃ tubular support with yttria stabilized zirconia (YSZ) as an intermediate layer. Bistriethoxysilylethane (BTESE) derived sol was modified by adding phenyltriethoxysilylethane (PhTES) as an organic template. Six times dip coated modified silica membrane having a thickness of about 782 nm was characterized by field emission scanning electron microscopy. Thermogravimetric analysis, together along contact angle and Fourier transform infrared spectroscopy, showed that hydrophobic properties were improved by increasing the PhTES content. The contact angle of water droplet increased from 37° for pure to 111.5° for the modified membrane. The permeance of single gas H₂ was higher than H₂:CO₂ ratio of 75:25 binary feed mixtures. However, the permeance of H₂ for 60:40 H₂:CO₂ was found lower than single and binary mixture 75:25 H₂:CO₂. The binary selectivity values for 75:25 H₂:CO₂ were 24.75, 44, and 57, respectively. Selectivity had an inverse relation with PhTES content. Hydrophobicity properties were improved by increasing PhTES content in the silica matrix. The system exhibits proper three layers adhesion or integration, and smoothness. Membrane system suitable in steam environment and high-temperature separation. It was concluded that the hydrophobic silica membrane is highly promising for the separation of H₂/CO₂ mixture from various H₂-containing process streams.

Keywords: gas separation, hydrophobic properties, silica membrane, sol–gel method

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Authors: Mohammad H. Al-Sayah, Khalid Jarrah, Soleiman Hisaindee

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Hydrophobic sorbents are usually used to remove oil spills from water surfaces. In this study, the hydrophilic fibers of natural cotton were chemically modified with a solvent-free process to modify them into hydrophobic fibers that can remove oil from water surfaces. The cellulose-based fibers of cotton were reacted with trichlorosilanes through gas-solid reaction in a dry chamber. Cotton fibers were exposed to vapors of four different chloroalkylsilanes at room temperature for 24 hours. The chlorosilanes were namely trichloromethylsilane, dichlorodimethyl silane, butyltrichlorosilane, and trichloro (3,3,3-trifluoropropyl) silane. The modified cotton fibers were characterized by IR-spectroscopy, thermogravimetric analysis (TGA) and Scanning Electron Microscopy/Energy Dispersive X-Ray Spectroscopy (SEM-EDS). The degree of substitution for each of the grafted alkyl groups was in the range between 0.1 and 0.3 per glucose residue. As a result of sialylation, the cotton fibers became hydrophobic; this was reflected by water contact-angle measurements of the fibers which increased from zero for the unmodified cotton to above 100 degrees for the modified fibers. In addition, the adsorption capacity of the fibers for oil from water surfaces increased by about five times that of the unmodified cotton reaching 18 g oil/g of cotton modified by dimethyl substituted silyl ethers. The optimal fiber-oil contact time and temperature for adsorption were 10 mins at 25°C, respectively. Therefore, the efficacy of cotton fibers to remove oil spills from contaminated water surfaces was significantly enhanced by using a simple solvent-free and environment-friendly process.

Keywords: gas-solid silyl reaction, modified cellulose, solvent-free, oil pollution, cotton

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Authors: Noureddine Ramdani

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In recent years, extensive attention has been given to the study of conductive nanocomposites due to their unique properties, which are dependent on their size and shape. The potential applications of these materials include electromagnetic interference shielding, energy storage, photovoltaics, and others. These outstanding properties have led to increased interest and research in this field. In this work, a conductive poly benzoxazine nanocomposite, PBZ/Gr-Cu, was synthesized through a compression molding technique to achieve a high-performance material suitable for electromagnetic interference (EMI) shielding applications. The microstructure of the nanocomposites was analyzed using scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR). The thermal stability, electrical conductivity, and EMI shielding properties of the nanocomposites were evaluated using thermogravimetric analysis, a four-point probe, and a VNA analyzer, respectively. The TGA results revealed that the thermal stability and electrical conductivity of the nanocomposites were significantly enhanced by the incorporation of Gr/Cu nanoparticles. The nanocomposites exhibited a low percolation threshold of about 3.5 wt.% and an increase in carrier concentration and mobility of the carriers with increasing hybrid nanofiller content, causing the composites to behave as n-type semiconductors. These nanocomposites also displayed a high dielectric constant and a high dissipation factor in the frequency range of 8-12 GHz, resulting in higher EMI shielding effectiveness (SE) of 25-44 dB. These characteristics make them promising candidates for lightweight EMI shielding materials in aerospace and radar evasion applications.

Keywords: polybenzoxazine matrix, conductive nanocomposites, electrical conductivity, EMI shielding

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Authors: Jibril Mohammed, Usman Dadum Hamza, Abdulsalam Surajudeen, Baba Yahya Danjuma

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Considerable concerns have been raised over the presence of volatile organic compounds (VOCs) in water. In this study, coconut shell based activated carbon was produced through chemical activation with potassium acetate (PAAC) for adsorption of benzene and toluene. The porous carbons were characterized using Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), scanning electron microscopy (SEM), proximate analysis, and ultimate analysis and nitrogen adsorption tests. Adsorption of benzene and toluene on the porous carbons were conducted at varying concentrations (50-250 mg/l). The high BET surface area of 622 m2/g and highly heteroporous adsorbent prepared gave good removal efficiencies of 79 and 82% for benzene and toluene respectively, with 32% yield. Equilibrium data were fitted to Langmuir, Freundlich and Temkin isotherms with all the models having R2 > 0.94. The equilibrium data were best represented by the Langmuir isotherm, with maximum adsorption capacity of 192 mg/g and 227 mg/g for benzene and toluene respectively. The Webber and Chakkravorti equilibrium parameter (RL) values are between 0 and 1 confirming the favourability of the Langmuir model. The adsorption kinetics was found to follow the pseudo-second-order kinetic model. The PAAC produced can be used effectively to salvage environmental pollution problems posed by VOCs through a sustainable process.

Keywords: adsorption, equilibrium and kinetics studies, potassium acetate, water treatment

Procedia PDF Downloads 190

Authors: Asli Beyler Çi̇ği̇l, Memet Vezi̇r Kahraman

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Organic–inorganic hybrids have become an effective source of advanced materials because they combine the advantages of both the organic moiety such as flexibility, low dielectric constant, and processability, and inorganic moiety as rigidity, strength, durability, and thermal stability. By incorporating cross-linkable side chains, the hybrid materials can be made photosensitive and UV curable, which offers many advantages including low processing temperature, low equipment cost and compatibility. In this study, uv-curable organic-inorganic hybrid material, which was contained surface modified polyaniline particles (PANI), was prepared. PANI surface photografted with hydroxy ethyl methacrylate (HEMA) to produce hydroxyl groups. Hydroxyl functionalized PANI/HEMA was acrylated using isocyanato ethyl methacrylate (IEM) in order to improve the dispersion and interfacial interaction in composites. UV-curable formulation was prepared by mixing the surface modified PANI, polyethylene glycol diacrylate (PEGDA), trimethylolpropane triacrylate (TMPTA), hydrolized 3- methacryloxypropyltrimethoxysilane (hyd. MEMO) and photoinitiator. Chemical structure of nano-hybrid material was characterized by FTIR. FTIR spectra showed that the photografting of PANI was prepared successfully. Thermal properties of the nano-hybrid material were determined by thermogravimetric analysis (TGA). The morphology of the nano-hybrid material was performed by scanning electron microscopy (SEM).

Keywords: polyaniline, photograft, sol-gel, uv-curable polymer

Procedia PDF Downloads 269

Authors: Carolin Lutz, Jörg Matthes, Patrick Waibel, Ulrich Precht, Krassimir Garbev, Günter Beuchle, Uwe Schweike, Peter Stemmermann, Hubert B. Keller

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Online measurement of the product quality is a challenging task in cement production, especially in the production of Celitement, a novel environmentally friendly hydraulic binder. The mineralogy and chemical composition of clinker in ordinary Portland cement production is measured by X-ray diffraction (XRD) and X ray fluorescence (XRF), where only crystalline constituents can be detected. But only a small part of the Celitement components can be measured via XRD, because most constituents have an amorphous structure. This paper describes the development of algorithms suitable for an on-line monitoring of the final processing step of Celitement based on NIR-data. For calibration intermediate products were dried at different temperatures and ground for variable durations. The products were analyzed using XRD and thermogravimetric analyses together with NIR-spectroscopy to investigate the dependency between the drying and the milling processes on one and the NIR-signal on the other side. As a result, different characteristic parameters have been defined. A short overview of the Celitement process and the challenging tasks of the online measurement and evaluation of the product quality will be presented. Subsequently, methods for systematic development of near-infrared calibration models and the determination of the final calibration model will be introduced. The application of the model on experimental data illustrates that NIR-spectroscopy allows for a quick and sufficiently exact determination of crucial process parameters.

Keywords: calibration model, celitement, cementitious material, NIR spectroscopy

Procedia PDF Downloads 467

Authors: Ogunniran Kehinde Olurotimi, Adekoya Joseph, Ehi-Eromosele Cyril, Mehdi Shihab, Mesubi Adediran, Tadigoppula Narender

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Nicotinic acid hydrazide and 2,4-dihydoxylbenzaldehyde were condensed at 20°C to form an acylhydrazone (H3L) with ONO coordination pattern. The structure of the acylhydrazone was elucidated by using CHN analyzer, ESI mass spectrometry, IR, 1H NMR, 13C NMR and 2D NMR such as COSY and HSQC. Thereafter, five novel metal complexes [Mn(II), Fe(II), Pt(II) Zn(II) and Pd(II)] of the hydrazone ligand were synthesized and their structural characterization were achieved by several physicochemical methods, namely elemental analysis, electronic spectra, infrared, EPR, molar conductivity and powder X-ray diffraction studies. Structural geometries of some of the compounds were supported by using Hyper Chem-8 program for the molecular mechanics and semi-empirical calculations. The stability energy (E) and electron potentials (eV) for the frontier molecules were calculated by using PM3 method. An octahedral geometry was suggested for both Pd(II) and Zn(II) complexes while both Mn(II) and Fe(II) complexes conformed with tetrahedral pyramidal. However, Pt(II) complex agreed with tetrahedral geometry. In vitro antitubercular activity study of the ligand and the metal complexes were evaluated against Mycobacterium tuberculosis, H37Rv, by using micro-diluted method. The results obtained revealed that (PtL1) (MIC = 0.56 µg/mL), (ZnL1) (MIC = 0.61 µg/mL), (MnL1) (MIC = 0.71 µg/mL) and (FeL1) (MIC = 0.82 µg/mL), exhibited a significant activity when compared with first line drugs such as isoniazid (INH) (MIC = 0.9 µg/mL). H3L1 exhibited lesser antitubercular activity with MIC value of 1.02 µg/mL. However, the metal complexes displayed higher cytoxicity but were found to be non-significant different (P ˂ 0.05) to isoniazid drug.

Keywords: hydrazones, electron spin resonance, thermogravimetric, powder X-ray diffraction, antitubercular agents

Procedia PDF Downloads 236

Authors: H. K. G. K. D. K. Hapuhinna, R. D. Gunaratne, H. M. J. C. Pitawala

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Hydroxyapatite is a bioceramic which can be used for applications in orthopedics and dentistry due to its structural similarity with the mineral phase of mammalian bones and teeth. In this study, it was synthesized, chemically changing natural Eppawala chloroapatite mineral as a value-added product. Sol-gel approach and solid state sintering were used to synthesize products using diluted nitric acid, ethanol and calcium hydroxide under different conditions. Synthesized Eppawala hydroxyapatite powder was characterized using X-ray Fluorescence (XRF), X-ray Powder Diffraction (XRD), Fourier-transform Infrared Spectroscopy (FTIR), Scanning Electron Microscopy (SEM), Thermogravimetric Analysis (TGA) and Differential Scanning Calorimetry (DSC) in order to find out its composition, crystallinity, presence of functional groups, bonding type, surface morphology, microstructural features, and thermal dependence and stability, respectively. The XRD results reflected the formation of a hexagonal crystal structure of hydroxyapatite. Elementary composition and microstructural features of products were discussed based on the XRF and SEM results of the synthesized hydroxyapatite powder. TGA and DSC results of synthesized products showed high thermal stability and good material stability in nature. Also, FTIR spectroscopy results confirmed the formation of hydroxyapatite from apatite via the presence of hydroxyl groups. Those results coincided with the FTIR results of mammalian bones including human bones. The study concludes that there is a possibility of producing hydroxyapatite using commercially available Eppawala chloroapatite in Sri Lanka.

Keywords: dentistry, Eppawala chlorapatite, hydroxyapatite, orthopedics

Procedia PDF Downloads 214

Authors: Saja M. Nabat Al-Ajrash, Charles Browning, Rose Eckerle, Li Cao, Robyn L. Bradford, Donald Klosterman

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An additive manufacturing process and subsequent pyrolysis cycle were used to fabricate SiC matrix/carbon fiber hybrid composites. The matrix was fabricated using a mixture of preceramic polymer and acrylate monomers, while polyacrylonitrile (PAN) precursor was used to fabricate fibers via electrospinning. The precursor matrix and reinforcing fibers at 0, 2, 5, or 10 wt% were printed using digital light processing, and both were simultaneously pyrolyzed to yield the final ceramic matrix composite structure. After pyrolysis, XRD and SEAD analysis proved the existence of SiC nanocrystals and turbostratic carbon structure in the matrix, while the reinforcement phase was shown to have a turbostratic carbon structure similar to commercial carbon fibers. Thermogravimetric analysis (TGA) in the air up to 1400 °C was used to evaluate the oxidation resistance of this material. TGA results showed some weight loss due to oxidation of SiC and/or carbon up to about 900 °C, followed by weight gain to about 1200 °C due to the formation of a protective SiO2 layer. Although increasing carbon fiber content negatively impacted the total mass loss for the first heating cycle, exposure of the composite to second-run air revealed negligible weight chance. This is explained by SiO2 layer formation, which acts as a protective film that prevents oxygen diffusion. Oxidation of SiC and the formation of a glassy layer has been proven to protect the sample from further oxidation, as well as provide healing of surface cracks and defects, as revealed by SEM analysis.

Keywords: silicon carbide, carbon fibers, additive manufacturing, composite

Procedia PDF Downloads 45

Authors: Salwa M. Elmesallamy, Ahmed A. Farag, Magd M. Badr, Dalia S. Fathy, Ahmed Bakry, Mona A. El-Etre

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The term green environment is an international trend. It is become imperative to treat the corrosion of steel with a green coating to protect the environment. From the potential adverse effects of the traditional materials.A series of polybenzoxazine/henna composites (PBZ/henna), with different weight percent (3,5, and 7 wt % (of henna), were prepared for corrosion protection of carbon steel. The structures of the prepared composites were verified using FTIR analysis. The mechanical properties of the resins, such as adhesion, hardness, binding, and tensile strength, were also measured. It was found that the tensile strength increases by henna loading up to 25% higher than the tidy resin. The thermal stability was investigated by thermogravimetric analysis (TGA) the loading of lawsone (henna) molecules into the PBZ matrix increases the thermal stability of the composite. UV stability was tested by the UV weathering accelerator to examine the possibility that henna can also act as an aging UV stabilizer. The effect of henna content on the corrosion resistance of composite coatings was tested using potentiostatic polarization and electrochemical spectroscopy. The presence of henna in the coating matrix enhances the protection efficiency of polybenzoxazine coats. Increasing henna concentration increases the protection efficiency of composites. The quantum chemical calculations for polybenzoxazine/henna composites have resulted that the highest corrosion inhibition efficiency, has the highest EHOMO and lowest ELUMO; which is in good agreement with results obtained from experiments.

Keywords: polybenzoxazine, corrosion, green chemistry, carbon steel

Procedia PDF Downloads 64