In this work; a response surface methodology (RSM) was implemented to investigate the process variables in a hydrogen production system. The effects of five independent variables; namely the temperature (X₁); the flow rate (X₂); the catalyst weight (X₃); the catalyst loading (X₄) and the glycerol-water molar ratio (X₅) on the H₂ yield (Y₁) and the conversion of glycerol to gaseous products (Y₂) were explored. Using multiple regression analysis; the experimental results of the H₂ yield and the glycerol conversion to gases were fit to quadratic polynomial models. The proposed mathematical models have correlated the dependent factors well within the limits that were being examined. The best values of the process variables were a temperature of approximately 600 °C; a feed flow rate of 0.05 mL/min; a catalyst weight of 0.2 g; a catalyst loading of 20% and a glycerol-water molar ratio of approximately 12; where the H₂ yield was predicted to be 57.6% and the conversion of glycerol was predicted to be 75%. To validate the proposed models; statistical analysis using a two-sample t-test was performed; and the results showed that the models could predict the responses satisfactorily within the limits of the variables that were studied.
Propylene is one type of plastic that is widely used in our everyday life. This study focuses on the identification and justification of the optimum process parameters for polypropylene production in a novel pilot plant based fluidized bed reactor. This first-of-its-kind statistical modeling with experimental validation for the process parameters of polypropylene production was conducted by applying ANNOVA (Analysis of variance) method to Response Surface Methodology (RSM). Three important process variables i.e., reaction temperature, system pressure and hydrogen percentage were considered as the important input factors for the polypropylene production in the analysis performed. In order to examine the effect of process parameters and their interactions, the ANOVA method was utilized among a range of other statistical diagnostic tools such as the correlation between actual and predicted values, the residuals and predicted response, outlier t plot, 3D response surface and contour analysis plots. The statistical analysis showed that the proposed quadratic model had a good fit with the experimental results. At optimum conditions with temperature of 75 °C, system pressure of 25 bar and hydrogen percentage of 2%, the highest polypropylene production obtained is 5.82% per pass. Hence it is concluded that the developed experimental design and proposed model can be successfully employed with over a 95% confidence level for optimum polypropylene production in a fluidized bed catalytic reactor (FBCR).
This study examines the feasibility of catalytically pretreated biochar derived from the dried exocarp or fruit peel of mangostene with Group I alkali metal hydroxide (KOH). The pretreated char was activated in the presence of carbon dioxide gas flow at high temperature to upgrade its physiochemical properties for the removal of copper, Cu(II) cations in single solute system. The effect of three independent variables, including temperature, agitation time and concentration, on sorption performance were carried out. Reaction kinetics parameters were determined by using linear regression analysis of the pseudo first, pseudo second, Elovich and intra-particle diffusion models. The regression co-efficient, R² values were best for the pseudo second order kinetic model for all the concentration ranges under investigation. This implied that Cu(II) cations were adsorbed mainly by chemical interactions with the surface active sites of the activated biochar. Langmuir, Freundlich and Temkin isotherm models were used to interpret the equilibrium data at different temperature. Thermodynamic studies revealed that the sorption process was spontaneous and endothermic. The surface area of the activated sample was 367.10 m²/g, whereas before base activation, it was only 1.22 m²/g. The results elucidated that the base pretreatment was efficient enough to yield porous carbon with an enlarged surface area, which can successfully eliminate Cu(II) cations from waste water.
In this work, batch adsorption experiments were carried out to investigate the suitability of prepared acid activated carbons in removing heavy metal ions such as nickel(II), lead(II) and chromium(VI). Acid activated carbons were obtained from oil palm and coconut shells using phosphoric acid under similar activation process while the differences lie either in impregnation condition or in both pretreatment and impregnation conditions. Prepared activated carbons were modified by dispersing hydrated iron oxide. The adsorption equilibrium data for nickel(II) and lead(II) were obtained from adsorption by the prepared and commercial activated carbons. Langmuir and Freundlich models fit the data well. Prepared activated carbons showed higher adsorption capacity for nickel(II) and lead(II). The removal of chromium(VI) was studied by the prepared acid activated, modified and commercial activated carbons at different pH. The isotherms studies reveal that the prepared activated carbon performs better in low concentration region while the commercial ones in the high concentration region. Thus, a complete adsorption is expected in low concentration by the prepared activated carbon. The kinetics data for Ni(II), Pb(II) and Cr(VI) by the best selected activated carbon fitted very well to the pseudo-second-order kinetic model.
Two different ionic liquid-based biopolymer electrolyte systems were prepared using a solution casting technique. Corn starch and lithium hexafluorophosphate (LiPF₆) were employed as polymer and salt, respectively. Additionally, two different counteranions of ionic liquids, viz. 1-butyl-3-methylimidazolium hexafluorophosphate (BmImPF₆) and 1-butyl-3-methylimidazolium trifluoromethanesulfonate (also known as 1-butyl-3-methylimidazolium triflate) (BmImTf) were used and studied in this present work. The maximum ionic conductivities of (1.47 ± 0.02) × 10(-4) and (3.21 ± 0.01) × 10(-4) S∙cm(-1) were achieved with adulteration of 50 wt% of BmImPF₆ and 80 wt% of BmImTf, respectively at ambient temperature. Activated carbon-based electrodes were prepared and used in supercapacitor fabrication. Supercapacitors were then assembled using the most conducting polymer electrolyte from each system. The electrochemical properties of the supercapacitors were then analyzed. The supercapacitor containing the triflate-based biopolymer electrolyte depicted a higher specific capacitance with a wider electrochemical stability window compared to that of the hexafluorophosphate system.
A new coumarin derivative, N,N'-((2E,2'E)-2,2'-(1,4-phenylenebis (methanylylidene))bis(hydrazinecarbonothioyl))bis(2-oxo-2H-chromene-3-carboxamide) PMBH, was synthesized and its chemical structure was elucidated and confirmed using spectroscopic techniques (Infrared spectroscopy IR, Proton nuclear magnetic resonance, (1)H-NMR and carbon-13 nuclear magnetic resonance (13)C-NMR). The corrosion inhibition effect of PMBH on mild steel in 1.0 M HCl was investigated using corrosion potential (ECORR), potentiodynamic polarization, electrochemical impedance spectroscopy (EIS), and electrochemical frequency modulation (EFM) measurements. The obtained results indicated that PMBH has promising inhibitive effects on the corrosion of mild steel in 1.0 M HCl across all of the conditions examined. Scanning electron microscopy (SEM) was used to investigate the morphology of the mild steel before and after immersion in 1.0 M HCl solution containing 0.5 mM of PMBH. Surface analysis revealed improvement of corrosion resistance in presence of PMBH.
Multi-component nanohybrids comprising of organo-modified montmorillonite (MMT) and immiscible biopolymer blends of poly(3-hydroxybutyrate) (PHB) and epoxidized natural rubber (ENR-50) were prepared by solvent casting technique. The one and three dimensional morphology of PHB/ENR-50/MMT systems were studied using Polarizing Optical Microscopy (POM) and Scanning Electron Microscopy (SEM). Differential scanning calorimetry (DSC) technique was used to evaluate the thermal properties of the nanohybrids. The melting temperature (Tm) and enthalpy of melting (ΔHm) of PHB decrease with respect to the increase in ENR-50 as well as MMT content. The non-isothermal decomposition of the nanohybrids was studied using thermogravimetric (TG-DTG) analysis. FTIR-ATR spectra supported ring opening of the epoxide group via reaction with carboxyl group of PHB and amines of organic modifier. The reaction mechanism towards the formation of the nanohybrids is proposed.
This paper investigates the effect of driving voltage on the attachment force of an electroadhesion actuator, as the existing literature on the saturation of the adhesive force at a higher electric field is incomplete. A new type of electroadhesion actuator using normally available materials, such as aluminum foil, PVC tape and a silicone rubber sheet used for keyboard protection, has been developed with a simple layered structure that is capable of developing adhesive force consistently. The developed actuator is subjected to the experiment for the evaluation of various test surfaces; aluminum, brick, ceramic, concrete and glass. The driving high voltage is varied in steps to determine the characteristics of the output holding force. Results show a quadratic relation between F (adhesion force) and V (driving voltage) within the 2 kV range. After this range, the F-V responses consistently show a saturation trend at high electric fields. Next, the concept of the leakage current that can occur in the dielectric material and the corona discharge through air has been introduced. Results show that the voltage level, which corresponds to the beginning of the supply current, matches well with the beginning of the force saturation. With the confirmation of this hypothesis, a working model for electroadhesion actuation is proposed. Based on the experimental results, it is proposed that such a kind of actuator can be driven within a range of optimum high voltage to remain electrically efficient. This practice is recommended for the future design, development and characterization of electroadhesion actuators for robotic applications.
This paper presents the design and analysis of a novel split-H-shaped metamaterial unit cell structure that is applicable in a multi-band frequency range and that exhibits negative permeability and permittivity in those frequency bands. In the basic design, the separate split-square resonators are joined by a metal link to form an H-shaped unit structure. Moreover, an analysis and a comparison of the 1 × 1 array and 2 × 2 array structures and the 1 × 1 and 2 × 2 unit cell configurations were performed. All of these configurations demonstrate multi-band operating frequencies (S-band, C-band, X-band and Ku-band) with double-negative characteristics. The equivalent circuit model and measured result for each unit cell are presented to validate the resonant behavior. The commercially available finite-difference time-domain (FDTD)-based simulation software, Computer Simulation Technology (CST) Microwave Studio, was used to obtain the reflection and transmission parameters of each unit cell. This is a novel and promising design in the electromagnetic paradigm for its simplicity, scalability, double-negative characteristics and multi-band operation.
50 years ago, Karl Ziegler and Giulio Natta were awarded the Nobel Prize for their discovery of the catalytic polymerization of ethylene and propylene using titanium compounds and aluminum-alkyls as co-catalysts. Polyolefins have grown to become one of the biggest of all produced polymers. New metallocene/methylaluminoxane (MAO) catalysts open the possibility to synthesize polymers with highly defined microstructure, tacticity, and steroregularity, as well as long-chain branched, or blocky copolymers with excellent properties. This improvement in polymerization is possible due to the single active sites available on the metallocene catalysts in contrast to their traditional counterparts. Moreover, these catalysts, half titanocenes/MAO, zirconocenes, and other single site catalysts can control various important parameters, such as co-monomer distribution, molecular weight, molecular weight distribution, molecular architecture, stereo-specificity, degree of linearity, and branching of the polymer. However, in most cases research in this area has reduced academia as olefin polymerization has seen significant advancements in the industries. Therefore, this paper aims to further motivate interest in polyolefin research in academia by highlighting promising and open areas for the future.
A synthesis of acrylonitrile (AN)/butyl acrylate (BA)/fumaronitrile (FN) and AN/EHA (ethyl hexyl acrylate)/FN terpolymers was carried out by redox polymerization using sodium bisulfite (SBS) and potassium persulphate (KPS) as initiator at 40 °C. The effect of comonomers, BA and EHA and termonomer, FN on the glass transition temperature (Tg) and stabilization temperature was studied using Differential Scanning Calorimetry (DSC). The degradation behavior and char yield were obtained by Thermogravimetric Analysis. The conversions of AN, comonomers (BA and EHA) and FN were 55%-71%, 85%-91% and 76%-79%, respectively. It was found that with the same comonomer feed (10%), the Tg of AN/EHA copolymer was lower at 63 °C compared to AN/BA copolymer (70 °C). AN/EHA/FN terpolymer also exhibited a lower Tg at 63 °C when compared to that of the AN/BA/FN terpolymer (67 °C). By incorporating BA and EHA into a PAN system, the char yield was reduced to ~38.0% compared to that of AN (~47.7%). It was found that FN reduced the initial cyclization temperature of AN/BA/FN and AN/EHA/FN terpolymers to 228 and 221 °C, respectively, in comparison to that of AN/BA and AN/EHA copolymers (~260 °C). In addition, FN reduced the heat liberation per unit time during the stabilization process that consequently reduced the emission of volatile group during this process. As a result, the char yields of AN/BA/FN and AN/EHA/FN terpolymers are higher at ~45.1% and ~43.9%, respectively, as compared to those of AN/BA copolymer (37.1%) and AN/EHA copolymer (38.0%).
The upgrade recycling of cast-iron scrap chips towards β-FeSi₂ thermoelectric materials is proposed as an eco-friendly and cost-effective production process. By using scrap waste from the machining process of cast-iron components, the material cost to fabricate β-FeSi₂ is reduced and the industrial waste is recycled. In this study, β-FeSi₂ specimens obtained from cast iron scrap chips were prepared both in the undoped form and doped with Al and Co elements. The maximum figure of merit (ZT) indicated a thermoelectric performance of approximately 70% in p-type samples and nearly 90% in n-type samples compared to β-FeSi₂ prepared from pure Fe and other published studies. The use of cast iron scrap chips to produce β-FeSi₂ shows promise as an eco-friendly and cost-effective production process for thermoelectric materials.
Hydrolyzing the amorphous region while keeping the crystalline region unaltered is the key technology for producing nanocellulose. This study investigated if the dissolution properties of the amorphous region of microcrystalline cellulose can be enhanced in the presence of Fe(3+) salt in acidic medium. The process parameters, including temperature, time and the concentration of metal chloride catalyst (FeCl₃), were optimized by using the response surface methodology (RSM). The experimental observation demonstrated that temperature and time play vital roles in hydrolyzing the amorphous sections of cellulose. This would yield hydrocellulose with higher crystallinity. The factors that were varied for the production of hydrocellulose were the temperature (x₁), time (x₂) and FeCl₃ catalyst concentration (x₃). Responses were measured in terms of percentage of crystallinity (y₁) and the yield (y₂) of the prepared hydrocellulose. Relevant mathematical models were developed. Analysis of variance (ANOVA) was carried out to obtain the most significant factors influencing the responses of the percentage of crystallinity and yield. Under optimum conditions, the percentage of crystallinity and yield were 83.46% and 86.98% respectively, at 90.95 °C, 6 h, with a catalyst concentration of 1 M. The physiochemical characteristics of the prepared hydrocellulose were determined in terms of XRD, SEM, TGA and FTIR analyses. The addition of FeCl₃ salt in acid hydrolyzing medium is a novel technique for substantially increasing crystallinity with a significant morphological change.
The significant increase in metal costs has forced the electronics industry to provide new materials and methods to reduce costs, while maintaining customers' high-quality expectations. This paper considers the problem of most electronic industries in reducing costly materials, by introducing a solder paste with alloy composition tin 98.3%, silver 0.3%, and copper 0.7%, used for the construction of the surface mount fine-pitch component on a Printing Wiring Board (PWB). The reliability of the solder joint between electronic components and PWB is evaluated through the dynamic characteristic test, thermal shock test, and Taguchi method after the printing process. After experimenting with the dynamic characteristic test and thermal shock test with 20 boards, the solder paste was still able to provide a high-quality solder joint. In particular, the Taguchi method is used to determine the optimal control parameters and noise factors of the Solder Printer (SP) machine, that affects solder volume and solder height. The control parameters include table separation distance, squeegee speed, squeegee pressure, and table speed of the SP machine. The result shows that the most significant parameter for the solder volume is squeegee pressure (2.0 mm), and the solder height is the table speed of the SP machine (2.5 mm/s).
Porous structured silicon or porous silicon (PS) powder was prepared by chemical etching of silicon powder in an etchant solution of HF: HNO₃: H₂O (1:3:5 v/v). An immersion time of 4 min was sufficient for depositing Cu metal from an aqueous solution of CuSO₄ in the presence of HF. Scanning electron microscopy (SEM) analysis revealed that the Cu particles aggregated upon an increase in metal content from 3.3 wt% to 9.8 wt%. H₂-temperature programmed reduction (H₂-TPR) profiles reveal that re-oxidation of the Cu particles occurs after deposition. Furthermore, the profiles denote the existence of various sizes of Cu metal on the PS. The Cu-PS powders show excellent catalytic reduction on the p-nitrophenol regardless of the Cu loadings.
Recently, as a supplement of cement, the utilization of pozzolanic materials in cement and concrete manufacturing has increased significantly. This study investigates the scope to use pozzolanic wastes (slag, palm oil fuel ash and rice husk ash) as an alkali activated binder (AAB) that can be used as an alternative to cement. To activate these materials, sodium hydroxide solution was used at 1.0, 2.5 and 5.0 molar concentration added into the mortar, separately. The required solution was used to maintain the flow of mortar at 110% ± 5%. The consistency and setting time of the AAB-paste were determined. Mortar was tested for its flow, compressive strength, porosity, water absorption and thermal resistance (heating at 700 °C) and investigated by scanning electron microscopy. The experimental results reveal that AAB-mortar exhibits less flow than that of ordinary Portland cement (OPC). Surprisingly, AAB-mortars (with 2.5 molar solution) achieved a compressive strength of 34.3 MPa at 28 days, while OPC shows that of 43.9 MPa under the same conditions. Although water absorption and porosity of the AAB-mortar are slightly high, it shows excellent thermal resistance compared to OPC. Therefore, based on the test results, it can be concluded that in the presence of a chemical activator, the aforementioned pozzolans can be used as an alternative material for cement.
A new design and analysis of a wide-band double-negative metamaterial, considering a frequency range of 0.5 to 7 GHz, is presented in this paper. Four different unit cells with varying design parameters are analyzed to evaluate the effects of the unit-cell size on the resonance frequencies of the metamaterial. Moreover, open and interconnected 2 × 2 array structures of unit cells are analyzed. The finite-difference time-domain (FDTD) method, based on the Computer Simulation Technology (CST) Microwave Studio, is utilized in the majority of this investigation. The experimental portion of the study was performed in a semi-anechoic chamber. Good agreement is observed between the simulated and measured S parameters of the developed unit cell and array. The designed unit cell exhibits negative permittivity and permeability simultaneously at S-band (2.95 GHz to 4.00 GHz) microwave frequencies. In addition, the designed unit cell can also operate as a double-negative medium throughout the C band (4.00 GHz to 4.95 GHz and 5.00 GHz to 5.57 GHz). At a number of other frequencies, it exhibits a single negative value. The two array configurations cause a slight shift in the resonance frequencies of the metamaterial and hence lead to a slight shift of the single- and double-negative frequency ranges of the metamaterial.
The performance of advance photocatalytic degradation of 4-chlorophenoxyacetic acid (4-CPA) strongly depends on photocatalyst dosage, initial concentration and initial pH. In the present study, a simple response surface methodology (RSM) was applied to investigate the interaction between these three independent factors. Thus, the photocatalytic degradation of 4-CPA in aqueous medium assisted by ultraviolet-active ZnO photocatalyst was systematically investigated. This study aims to determine the optimum processing parameters to maximize 4-CPA degradation. Based on the results obtained, it was found that a maximum of 91% of 4-CPA was successfully degraded under optimal conditions (0.02 g ZnO dosage, 20.00 mg/L of 4-CPA and pH 7.71). All the experimental data showed good agreement with the predicted results obtained from statistical analysis.
A miniaturized antenna employing a negative index metamaterial with modified split-ring resonator (SRR) and capacitance-loaded strip (CLS) unit cells is presented for Ultra wideband (UWB) microwave imaging applications. Four left-handed (LH) metamaterial (MTM) unit cells are located along one axis of the antenna as the radiating element. Each left-handed metamaterial unit cell combines a modified split-ring resonator (SRR) with a capacitance-loaded strip (CLS) to obtain a design architecture that simultaneously exhibits both negative permittivity and negative permeability, which ensures a stable negative refractive index to improve the antenna performance for microwave imaging. The antenna structure, with dimension of 16 × 21 × 1.6 mm³, is printed on a low dielectric FR4 material with a slotted ground plane and a microstrip feed. The measured reflection coefficient demonstrates that this antenna attains 114.5% bandwidth covering the frequency band of 3.4-12.5 GHz for a voltage standing wave ratio of less than 2 with a maximum gain of 5.16 dBi at 10.15 GHz. There is a stable harmony between the simulated and measured results that indicate improved nearly omni-directional radiation characteristics within the operational frequency band. The stable surface current distribution, negative refractive index characteristic, considerable gain and radiation properties make this proposed negative index metamaterial antenna optimal for UWB microwave imaging applications.
Foamed mortar with a density of 1300 kg/m³ was prepared. In the initial laboratory trials, water-to-cement (w/c) ratios ranging from 0.54 to 0.64 were tested to determine the optimal value for foamed mortar corresponding to the highest compressive strength without compromising its fresh state properties. With the obtained optimal w/c ratio of 0.56, two types of foamed mortar were prepared, namely cement-foamed mortar (CFM) and slag-foamed mortar (SFM, 50% cement was replaced by slag weight). Four different curing conditions were adopted for both types of foamed mortar to assess their compressive strength, ultrasonic pulse velocity (UPV) and thermal insulation performance. The test results indicated that utilizing 50% of slag as cement replacement in the production of foamed mortar improved the compressive strength, UPV and thermal insulation properties. Additionally, the initial water curing of seven days gained higher compressive strength and increased UPV values as compared to the air cured and natural weather curing samples. However, this positive effect was more pronounced in the case of compressive strength than in the UPV and thermal conductivity of foamed mortar.