Search results for: electron beam

Authors: Nabil Al-Zaqri

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Semiconductor photocatalysts with surface defects display incredible light absorption bandwidth, and these defects function as highly active sites for oxidation processes by interacting with the surface band structure. Accordingly, engineering the photocatalyst with surface oxygen vacancies will enhance the semiconductor nanostructure's photocatalytic efficiency. Herein, a CeO2₋ₓ nanostructure is designed under the influence of low-frequency ultrasonic waves to create surface oxygen vacancies. This approach enhances the photocatalytic efficiency compared to many heterostructures while keeping the intrinsiccrystal structure intact. Ultrasonic waves induce the acoustic cavitation effect leading to the dissemination of active elements on the surface, which results in vacancy formation in conjunction with larger surface area and smaller particle size. The structural analysis of CeO₂₋ₓ revealed higher crystallinity, as well as morphological optimization, and the presence of oxygen vacancies is verified through Raman, X-rayphotoelectron spectroscopy, temperature-programmed reduction, photoluminescence, and electron spinresonance analyses. Oxygen vacancies accelerate the redox cycle between Ce₄+ and Ce₃+ by prolongingphotogenerated charge recombination. The ultrasound-treated pristine CeO₂ sample achieved excellenthydrogen production showing a quantum efficiency of 1.125% and efficient organic degradation. Ourpromising findings demonstrated that ultrasonic treatment causes the formation of surface oxygenvacancies and improves photocatalytic hydrogen evolution and pollution degradation. Conclusion: Defect engineering of the ceria nanoparticles with oxygen vacancies was achieved for the first time using low-frequency ultrasound treatment. The U-CeO₂₋ₓsample showed high crystallinity, and morphological changes were observed. Due to the acoustic cavitation effect, a larger surface area and small particle size were observed. The ultrasound treatment causes particle aggregation and surface defects leading to oxygen vacancy formation. The XPS, Raman spectroscopy, PL spectroscopy, and ESR results confirm the presence of oxygen vacancies. The ultrasound-treated sample was also examined for pollutant degradation, where 1O₂was found to be the major active species. Hence, the ultrasound treatment influences efficient photocatalysts for superior hydrogen evolution and an excellent photocatalytic degradation of contaminants. The prepared nanostructure showed excellent stability and recyclability. This work could pave the way for a unique post-synthesis strategy intended for efficient photocatalytic nanostructures.

Keywords: surface defect, CeO₂₋ₓ, photocatalytic, water treatment, H₂ production

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Authors: Adrian Niewiadomski, Barbara Surma, Katarzyna Kolodziejak, Dorota A. Pawlak

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Oxide-oxide eutectic is attracting increasing interest of scientific community because of their unique properties and numerous potential applications. Some of the most interesting examples of applications are metamaterials, glucose sensors, photoactive materials, thermoelectric materials, and photocatalysts. Their unique properties result from the fact that composite materials consist of two or more phases. As a result, these materials have additive and product properties. Additive properties originate from particular phases while product properties originate from the interaction between phases. MnTiO3-TiO2 eutectic is one of such materials. TiO2 is a well-known semiconductor, and it is used as a photocatalyst. Moreover, it may be used to produce solar cells, in a gas sensing devices and in electrochemistry. MnTiO3 is a semiconductor and antiferromagnetic. Therefore it has potential application in integrated circuits devices, and as a gas and humidity sensor, in non-linear optics and as a visible-light activated photocatalyst. The above facts indicate that eutectic MnTiO3-TiO2 constitutes an extremely promising material that should be studied. Despite that Raman spectroscopy is a powerful method to characterize materials, to our knowledge Raman studies of eutectics are very limited, and there are no studies of the MnTiO3-TiO2 eutectic. While to our knowledge the papers regarding this material are scarce. The MnTiO3-TiO2 eutectic, as well as TiO2 and MnTiO3 single crystals, were grown by the micro-pulling-down method at the Institute of Electronic Materials Technology in Warsaw, Poland. A nitrogen atmosphere was maintained during whole crystal growth process. The as-grown samples of MnTiO3-TiO2 eutectic, as well as TiO2 and MnTiO3 single crystals, are black and opaque. Samples were cut perpendicular to the growth direction. Cross sections were examined with scanning electron microscopy (SEM) and with Raman spectroscopy. The present studies showed that maintaining nitrogen atmosphere during crystal growth process may result in obtaining black TiO2 crystals. SEM and Raman experiments showed that studied eutectic consists of three distinct regions. Furthermore, two of these regions correspond with MnTiO3, while the third region corresponds with the TiO2-xNx phase. Raman studies pointed out that TiO2-xNx phase crystallizes in rutile structure. The studies show that Raman experiments may be successfully used to characterize eutectic materials. The MnTiO3-TiO2 eutectic was grown by the micro-pulling-down method. SEM and micro-Raman experiments were used to establish phase composition of studied eutectic. The studies revealed that the TiO2 phase had been doped with nitrogen. Therefore the TiO2 phase is, in fact, a solid solution with TiO2-xNx composition. The remaining two phases exhibit Raman lines of both rutile TiO2 and MnTiO3. This points out to some kind of coexistence of these phases in studied eutectic.

Keywords: compound materials, eutectic growth and characterization, Raman spectroscopy, rutile TiO₂

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Authors: Y. Roumila, D. Meziani, R. Bagtache, K. Abdmeziem, M. Trari

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Heterogeneous photocatalysis over semiconductors has proved its effectiveness in the treatment of wastewaters since it works under soft conditions. It has emerged as a promising technique, giving rise to less toxic effluents and offering the opportunity of using sunlight as a sustainable and renewable source of energy. Many compounds have been used as photocatalysts. Though synthesized ones are intensively used, they remain expensive, and their synthesis involves special conditions. We thus thought of implementing a natural material, a phosphate ore, due to its low cost and great availability. Our work is devoted to the removal of hazardous organic pollutants, which cause several environmental problems and health risks. Among them, dye pollutants occupy a large place. This work relates to the study of the photodegradation of methyl violet (MV) and rhodamine B (RhB), in single and binary systems, under UV light and sunlight irradiation. Methyl violet is a triarylmethane dye, while RhB is a heteropolyaromatic dye belonging to the Xanthene family. In the first part of this work, the natural compound was characterized using several physicochemical and photo-electrochemical (PEC) techniques: X-Ray diffraction, chemical, and thermal analyses scanning electron microscopy, UV-Vis diffuse reflectance measurements, and FTIR spectroscopy. The electrochemical and photoelectrochemical studies were performed with a Voltalab PGZ 301 potentiostat/galvanostat at room temperature. The structure of the phosphate material was well characterized. The photo-electrochemical (PEC) properties are crucial for drawing the energy band diagram, in order to suggest the formation of radicals and the reactions involved in the dyes photo-oxidation mechanism. The PEC characterization of the natural phosphate was investigated in neutral solution (Na₂SO₄, 0.5 M). The study revealed the semiconducting behavior of the phosphate rock. Indeed, the thermal evolution of the electrical conductivity was well fitted by an exponential type law, and the electrical conductivity increases with raising the temperature. The Mott–Schottky plot and current-potential J(V) curves recorded in the dark and under illumination clearly indicate n-type behavior. From the results of photocatalysis, in single solutions, the changes in MV and RhB absorbance in the function of time show that practically all of the MV was removed after 240 mn irradiation. For RhB, the complete degradation was achieved after 330 mn. This is due to its complex and resistant structure. In binary systems, it is only after 120 mn that RhB begins to be slowly removed, while about 60% of MV is already degraded. Once nearly all of the content of MV in the solution has disappeared (after about 250 mn), the remaining RhB is degraded rapidly. This behaviour is different from that observed in single solutions where both dyes are degraded since the first minutes of irradiation.

Keywords: environment, organic pollutant, phosphate ore, photodegradation

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Authors: Swati Tomar, Sunil Kumar Gupta

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Anammox is a novel and promising technology that has changed the traditional concept of biological nitrogen removal. The process facilitates direct oxidation of ammonical nitrogen under anaerobic conditions with nitrite as an electron acceptor without the addition of external carbon sources. The present study investigated the feasibility of anammox hybrid reactor (AHR) combining the dual advantages of suspended and attached growth media for biodegradation of ammonical nitrogen in wastewater. The experimental unit consisted of 4 nos. of 5L capacity AHR inoculated with mixed seed culture containing anoxic and activated sludge (1:1). The process was established by feeding the reactors with synthetic wastewater containing NH4-H and NO2-N in the ratio 1:1 at HRT (hydraulic retention time) of 1 day. The reactors were gradually acclimated to higher ammonium concentration till it attained pseudo steady state removal at a total nitrogen concentration of 1200 mg/l. During this period, the performance of the AHR was monitored at twelve different HRTs varying from 0.25-3.0 d with increasing NLR from 0.4 to 4.8 kg N/m3d. AHR demonstrated significantly higher nitrogen removal (95.1%) at optimal HRT of 1 day. Filter media in AHR contributed an additional 27.2% ammonium removal in addition to 72% reduction in the sludge washout rate. This may be attributed to the functional mechanism of filter media which acts as a mechanical sieve and reduces the sludge washout rate many folds. This enhances the biomass retention capacity of the reactor by 25%, which is the key parameter for successful operation of high rate bioreactors. The effluent nitrate concentration, which is one of the bottlenecks of anammox process was also minimised significantly (42.3-52.3 mg/L). Process kinetics was evaluated using first order and Grau-second order models. The first-order substrate removal rate constant was found as 13.0 d-1. Model validation revealed that Grau second order model was more precise and predicted effluent nitrogen concentration with least error (1.84±10%). A new mathematical model based on mass balance was developed to predict N2 gas in AHR. The mass balance model derived from total nitrogen dictated significantly higher correlation (R2=0.986) and predicted N2 gas with least error of precision (0.12±8.49%). SEM study of biomass indicated the presence of the heterogeneous population of cocci and rod shaped bacteria of average diameter varying from 1.2-1.5 mm. Owing to enhanced NRE coupled with meagre production of effluent nitrate and its ability to retain high biomass, AHR proved to be the most competitive reactor configuration for dealing with nitrogen laden wastewater.

Keywords: anammox, filter media, kinetics, nitrogen removal

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Authors: Soad Abubakr Abdelgalil, Gaber Attia Abo-Zaid, Mohamed Mohamed Yousri Kaddah

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Background: The Environmental Protection Agency has listed eggshell waste as the 15th most significant food industry pollution hazard. The utilization of eggshell waste as a source of renewable energy has been a hot topic in recent years. Therefore, finding a sustainable solution for the recycling and valorization of eggshell waste by investigating its potential to produce acid phosphatase (ACP) and organic acids by the newly-discovered B. sonorensis was the target of the current investigation. Results: The most potent ACP-producing B. sonorensis strain ACP2 was identified as a local bacterial strain obtained from the effluent of paper and pulp industries on basis of molecular and morphological characterization. The use of consecutive statistical experimental approaches of Plackett-Burman Design (PBD), and Orthogonal Central Composite Design (OCCD), followed by pH-uncontrolled cultivation conditions in a 7 L bench-top bioreactor, revealed an innovative medium formulation that substantially improved ACP production, reaching 216 U L⁻¹ with ACP yield coefficient Yp/x of 18.2 and a specific growth rate (µ) of 0.1 h⁻¹. The metals Ag+, Sn+, and Cr+ were the most efficiently released from eggshells during the solubilization process by B. sonorensis. The uncontrolled pH culture condition is the most suited and favored setting for improving the ACP and organic acids production simultaneously. Quantitative and qualitative analyses of produced organic acids were carried out using liquid chromatography-tandem mass spectrometry (LC-MS/MS). Lactic acid, citric acid, and hydroxybenzoic acid isomer were the most common organic acids produced throughout the cultivation process. The findings of thermogravimetric analysis (TGA), differential scan calorimeter (DSC), scanning electron microscope (SEM), energy-dispersive spectroscopy (EDS), Fourier-Transform Infrared Spectroscopy (FTIR), and X-Ray Diffraction (XRD) analysis emphasize the significant influence of organic acids and ACP activity on the solubilization of eggshells particles. Conclusions: This study emphasized robust microbial engineering approaches for the large-scale production of a newly discovered acid phosphatase accompanied by organic acids production from B. sonorensis. The biovalorization of the eggshell waste and the production of cost-effective ACP and organic acids were integrated into the current study, and this was done through the implementation of a unique and innovative medium formulation design for eggshell waste management, as well as scaling up ACP production on a bench-top scale.

Keywords: chicken eggshells waste, bioremediation, statistical experimental design, batch fermentation

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Authors: Karolina Ordon, Sandrine Coste, Malgorzata Makowska-Janusik, Abdelhadi Kassiba

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Photocatalytic processes play key role in the production of a new source of energy (as hydrogen), design of self-cleaning surfaces or for the environment preservation. The most challenging task deals with the purification of water distinguished by high efficiency. In the mentioned process, organic pollutants in solutions are decomposed to the simple, non-toxic compounds as H2O and CO2. The most known photocatalytic materials are ZnO, CdS and TiO2 semiconductors with a particular involvement of TiO2 as an efficient photocatalysts even with a high band gap equal to 3.2 eV which exploit only UV radiation from solar emitted spectrum. However, promising material with visible light induced photoactivity was searched through the monoclinic polytype of BiVO4 which has energy gap about 2.4 eV. As required in heterogeneous photocatalysis, the high contact surface is required. Also, BiVO4 as photocatalyst can be optimized by increasing its surface area by achieving the mesoporous structure synthesize. The main goal of the present work consists in the synthesis and characterization of BiVO4 mesoporous thin film. The synthesis method based on sol-gel was carried out using a standard surfactants such as P123 and F127. The thin film was deposited by spin and dip coating method. Then, the structural analysis of the obtained material was performed thanks to X-ray diffraction (XRD) and Raman spectroscopy. The surface of resulting structure was investigated using a scanning electron microscopy (SEM). The computer simulations based on modeling the optical and electronic properties of bulk BiVO4 by using DFT (density functional theory) methodology were carried out. The semiempirical parameterized method PM6 was used to compute the physical properties of BiVO4 nanostructures. The Raman and IR absorption spectra were also measured for synthesized mesoporous material, and the results were compared with the theoretical predictions. The simulations of nanostructured BiVO4 have pointed out the occurrence of quantum confinement for nanosized clusters leading to widening of the band gap. This result overcame the relevance of nanosized objects to harvest wide part of the solar spectrum. Also, a balance was searched experimentally through the mesoporous nature of the films devoted to enhancing the contact surface as required for heterogeneous catalysis without to lower the nanocrystallite size under some critical sizes inducing an increased band gap. The present contribution will discuss the relevant features of the mesoporous films with respect to their photocatalytic responses.

Keywords: bismuth vanadate, photocatalysis, thin film, quantum-chemical calculations

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Authors: Cécile Dufloux, Klaus Böttcher, Heike Oppermann, Jürgen Wollweber

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Hexagonal aluminum nitride (AlN) is a promising candidate for several wide band gap semiconductor compound applications such as deep UV light emitting diodes (UVC LED) and fast power transistors (HEMTs). To date, bulk AlN single crystals are still commonly grown from the physical vapor transport (PVT). Single crystalline AlN wafers obtained from this process could offer suitable substrates for a defect-free growth of ultimately active AlGaN layers, however, these wafers still lack from small sizes, limited delivery quantities and high prices so far.Although there is already an increasing interest in the commercial availability of AlN wafers, comparatively cheap Si, SiC or sapphire are still predominantly used as substrate material for the deposition of active AlGaN layers. Nevertheless, due to a lattice mismatch up to 20%, the obtained material shows high defect densities and is, therefore, less suitable for high power devices as described above. Therefore, the use of AlN with specially adapted properties for optical and sensor applications could be promising for mass market products which seem to fulfill fewer requirements. To respond to the demand of suitable AlN target material for the growth of AlGaN layers, we have designed an innovative technology based on reactive plasma spraying. The goal is to produce coarse grained AlN boules with N-terminated columnar structure and high purity. In this process, aluminum is injected into a microwave stimulated nitrogen plasma. AlN, as the product of the reaction between aluminum powder and the plasma activated N2, is deposited onto the target. We used an aluminum filament as the initial material to minimize oxygen contamination during the process. The material was guided through the nitrogen plasma so that the mass turnover was 10g/h. To avoid any impurity contamination by an erosion of the electrodes, an electrode-less discharge was used for the plasma ignition. The pressure was maintained at 600-700 mbar, so the plasma reached a temperature high enough to vaporize the aluminum which subsequently was reacting with the surrounding plasma. The obtained products consist of thick polycrystalline AlN layers with a diameter of 2-3 cm. The crystallinity was determined by X-ray crystallography. The grain structure was systematically investigated by optical and scanning electron microscopy. Furthermore, we performed a Raman spectroscopy to provide evidence of stress in the layers. This paper will discuss the effects of process parameters such as microwave power and deposition geometry (specimen holder, radiation shields, ...) on the topography, crystallinity, and stress distribution of AlN.

Keywords: aluminum nitride, polycrystal, reactive plasma spraying, semiconductor

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Authors: A. J. Cobley, L. Krishnan

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The demand for multi-functional lightweight materials in sectors such as automotive, aerospace, electronics is growing, and for this reason fibre-reinforced, epoxy polymer composites are being widely utilized. The fibre reinforcing material is mainly responsible for the strength and stiffness of the composites whilst the main role of the epoxy polymer matrix is to enhance the load distribution applied on the fibres as well as to protect the fibres from the effect of harmful environmental conditions. The superior properties of the fibre-reinforced composites are achieved by the best properties of both of the constituents. Although factors such as the chemical nature of the epoxy and how it is cured will have a strong influence on the properties of the epoxy matrix, the method of mixing and degassing of the resin can also have a significant impact. The production of a fibre-reinforced epoxy polymer composite will usually begin with the mixing of the epoxy pre-polymer with a hardener and accelerator. Mechanical methods of mixing are often employed for this stage but such processes naturally introduce air into the mixture, which, if it becomes entrapped, will lead to voids in the subsequent cured polymer. Therefore, degassing is normally utilised after mixing and this is often achieved by placing the epoxy resin mixture in a vacuum chamber. Although this is reasonably effective, it is another process stage and if a method of mixing could be found that, at the same time, degassed the resin mixture this would lead to shorter production times, more effective degassing and less voids in the final polymer. In this study the effect of four different methods for mixing and degassing of the pre-polymer with hardener and accelerator were investigated. The first two methods were manual stirring and magnetic stirring which were both followed by vacuum degassing. The other two techniques were ultrasonic mixing/degassing using a 40 kHz ultrasonic bath and a 20 kHz ultrasonic probe. The cured cast resin samples were examined under scanning electron microscope (SEM), optical microscope, and Image J analysis software to study morphological changes, void content and void distribution. Three point bending test and differential scanning calorimetry (DSC) were also performed to determine the thermal and mechanical properties of the cured resin. It was found that the use of the 20 kHz ultrasonic probe for mixing/degassing gave the lowest percentage voids of all the mixing methods in the study. In addition, the percentage voids found when employing a 40 kHz ultrasonic bath to mix/degas the epoxy polymer mixture was only slightly higher than when magnetic stirrer mixing followed by vacuum degassing was utilized. The effect of ultrasonic mixing/degassing on the thermal and mechanical properties of the cured resin will also be reported. The results suggest that low frequency ultrasound is an effective means of mixing/degassing a pre-polymer mixture and could enable a significant reduction in production times.

Keywords: degassing, low frequency ultrasound, polymer composites, voids

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Authors: Franciele L. Bernard, Felipe Dalla Vecchia, Barbara B. Polesso, Jose A. Donato, Marcus Seferin, Rosane Ligabue, Jailton F. do Nascimento, Sandra Einloft

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The increasing level of carbon dioxide concentration in the atmosphere related to fossil fuels processing and utilization are contributing to global warming phenomena considerably. Carbon capture and storage (CCS) technologies appear as one of the key technologies to reduce CO2 emissions mitigating the effects of climate change. Absorption using amines solutions as solvents have been extensively studied and used in industry for decades. However, solvent degradation and equipment corrosion are two of the main problems in this process. Poly (ionic liquid) (PIL) is considered as a promising material for CCS technology, potentially more environmentally friendly and lesser energy demanding than traditional material. PILs possess a unique combination of ionic liquids (ILs) features, such as affinity for CO2, thermal and chemical stability and adjustable properties, coupled with the intrinsic properties of the polymer. This study investigated new Poly (ionic liquid) (PIL) based on polyurethanes with different ionic liquids cations and its potential for CO2 capture. The PILs were synthesized by the addition of diisocyante to a difunctional polyol, followed by an exchange reaction with the ionic Liquids 1-butyl-3-methylimidazolium chloride (BMIM Cl); tetrabutylammonium bromide (TBAB) and tetrabutylphosphonium bromide (TBPB). These materials were characterized by Fourier transform infrared spectroscopy (FTIR), Proton Nuclear Magnetic Resonance (1H-NMR), Atomic force microscopy (AFM), Tensile strength analysis, Field emission scanning electron microscopy (FESEM), Thermogravimetric analysis (TGA), Differential scanning calorimetry (DSC). The PILs CO2 sorption capacity were gravimetrically assessed in a Magnetic Suspension Balance (MSB). It was found that the ionic liquids cation influences in the compounds properties as well as in the CO2 sorption. The best result for CO2 sorption (123 mgCO2/g at 30 bar) was obtained for the PIL (PUPT-TBA). The higher CO2 sorption in PUPT-TBA is probably linked to the fact that the tetraalkylammonium cation having a higher positive density charge can have a stronger interaction with CO2, while the imidazolium charge is delocalized. The comparative CO2 sorption values of the PUPT-TBA with different ionic liquids showed that this material has greater capacity for capturing CO2 when compared to the ILs even at higher temperature. This behavior highlights the importance of this study, as the poly (urethane) based PILs are cheap and versatile materials.

Keywords: capture, CO2, ionic liquids, ionic poly(urethane)

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Authors: Pantea Salehizadeh, Martin P. Bucknall, Robert Driscoll, Jayashree Arcot, George Srzednicki

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Banana is one of the most important crops produced in large quantities in tropical and sub-tropical countries. Of the total plant material grown, approximately 40% is considered waste and left in the field to decay. This practice allows fungal diseases such as Sigatoka Leaf Spot to develop, limiting plant growth and spreading spores in the air that can cause respiratory problems in the surrounding population. The pseudostem is considered a waste residue of production (60 to 80 tonnes/ha/year), although it is a good source of dietary fiber and volatile organic compounds (VOC’s). Strategies to process banana pseudostem into palatable, nutritious and marketable food materials could provide significant social and economic benefits. Extraction of VOC’s with desirable odor from dried and fresh pseudostem could improve the smell of products from the confectionary and bakery industries. Incorporation of banana pseudostem flour into bakery products could provide cost savings and improve nutritional value. The aim of this study was to determine the effects of drying methods and different banana species on the profile of volatile aroma compounds in dried banana pseudostem. The banana species analyzed were Musa acuminata and Musa balbisiana. Fresh banana pseudostem samples were processed by either freeze-drying (FD) or heat pump drying (HPD). The extraction of VOC’s was performed at ambient temperature using vacuum distillation and the resulting, mostly aqueous, distillates were analyzed using headspace solid phase microextraction (SPME) gas chromatography – mass spectrometry (GC-MS). Optimal SPME adsorption conditions were 50 °C for 60 min using a Supelco 65 μm PDMS/DVB Stableflex fiber1. Compounds were identified by comparison of their electron impact mass spectra with those from the Wiley 9 / NIST 2011 combined mass spectral library. The results showed that the two species have notably different VOC profiles. Both species contained VOC’s that have been established in literature to have pleasant appetizing aromas. These included l-Menthone, D-Limonene, trans-linlool oxide, 1-Nonanol, CIS 6 Nonen-1ol, 2,6 Nonadien-1-ol, Benzenemethanol, 4-methyl, 1-Butanol, 3-methyl, hexanal, 1-Propanol, 2-methyl- acid، 2-Methyl-2-butanol. Results show banana pseudostem VOC’s are better preserved by FD than by HPD. This study is still in progress and should lead to the optimization of processing techniques that would promote the utilization of banana pseudostem in the food industry.

Keywords: heat pump drying, freeze drying, SPME, vacuum distillation, VOC analysis

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Authors: Hyohun Kim, Dongwha Shin, Yeonseok Kim, Ji-Su Ahn, Kensuke Nakamura, Dongeun Choi, Byung-Woo Hong

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Artefacts are commonly encountered in the imaging process of clinical computed tomography (CT) where the artefact refers to any systematic discrepancy between the reconstructed observation and the true attenuation coefficient of the object. It is known that CT images are inherently more prone to artefacts due to its image formation process where a large number of independent detectors are involved, and they are assumed to yield consistent measurements. There are a number of different artefact types including noise, beam hardening, scatter, pseudo-enhancement, motion, helical, ring, and metal artefacts, which cause serious difficulties in reading images. Thus, it is desired to remove nuisance factors from the degraded image leaving the fundamental intrinsic information that can provide better interpretation of the anatomical and pathological characteristics. However, it is considered as a difficult task due to the high dimensionality and variability of data to be recovered, which naturally motivates the use of machine learning techniques. We propose an image restoration algorithm based on the deep neural network framework where the denoising auto-encoders are stacked building multiple layers. The denoising auto-encoder is a variant of a classical auto-encoder that takes an input data and maps it to a hidden representation through a deterministic mapping using a non-linear activation function. The latent representation is then mapped back into a reconstruction the size of which is the same as the size of the input data. The reconstruction error can be measured by the traditional squared error assuming the residual follows a normal distribution. In addition to the designed loss function, an effective regularization scheme using residual-driven dropout determined based on the gradient at each layer. The optimal weights are computed by the classical stochastic gradient descent algorithm combined with the back-propagation algorithm. In our algorithm, we initially decompose an input image into its intrinsic representation and the nuisance factors including artefacts based on the classical Total Variation problem that can be efficiently optimized by the convex optimization algorithm such as primal-dual method. The intrinsic forms of the input images are provided to the deep denosing auto-encoders with their original forms in the training phase. In the testing phase, a given image is first decomposed into the intrinsic form and then provided to the trained network to obtain its reconstruction. We apply our algorithm to the restoration of the corrupted CT images by the artefacts. It is shown that our algorithm improves the readability and enhances the anatomical and pathological properties of the object. The quantitative evaluation is performed in terms of the PSNR, and the qualitative evaluation provides significant improvement in reading images despite degrading artefacts. The experimental results indicate the potential of our algorithm as a prior solution to the image interpretation tasks in a variety of medical imaging applications. This work was supported by the MISP(Ministry of Science and ICT), Korea, under the National Program for Excellence in SW (20170001000011001) supervised by the IITP(Institute for Information and Communications Technology Promotion).

Keywords: auto-encoder neural network, CT image artefact, deep learning, intrinsic image representation, noise reduction, total variation

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Authors: Chen Yuan, Nick Green, Stuart Blackburn

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The investment casting process offers a great freedom of design combined with the economic advantage of near net shape manufacturing. It is widely used for the production of high value precision cast parts in particularly in the aerospace sector. Various combinations of materials have been used to produce the ceramic moulds, but most investment foundries use a silica based binder system in conjunction with fused silica, zircon, and alumino-silicate refractories as both filler and coarse stucco materials. However, in the context of advancing alloy technologies, silica based systems are struggling to keep pace, especially when net-shape casting titanium alloys. Study has shown that the casting of titanium based alloys presents considerable problems, including the extensive interactions between the metal and refractory, and the majority of metal-mould interaction is due to reduction of silica, present as binder and filler phases, by titanium in the molten state. Cleaner, more refractory systems are being devised to accommodate these changes. Although yttria has excellent chemical inertness to titanium alloy, it is not very practical in a production environment combining high material cost, short slurry life, and poor sintering properties. There needs to be a cost effective solution to these issues. With limited options for using pure oxides, in this work, a silica-free magnesia spinel MgAl₂O₄ was used as a primary coat filler and alumina as a binder material to produce facecoat in the investment casting mould. A comparison system was also studied with a fraction of the rare earth oxide Y₂O₃ adding into the filler to increase the inertness. The stability of the MgAl₂O₄/Al₂O₃ and MgAl₂O₄/Y₂O₃/Al₂O₃ slurries was assessed by tests, including pH, viscosity, zeta-potential and plate weight measurement, and mould properties such as friability were also measured. The interaction between the face coat and titanium alloy was studied by both a flash re-melting technique and a centrifugal investment casting method. The interaction products between metal and mould were characterized using x-ray diffraction (XRD), scanning electron microscopy (SEM) and Energy Dispersive X-Ray Spectroscopy (EDS). The depth of the oxygen hardened layer was evaluated by micro hardness measurement. Results reveal that introducing a fraction of Y₂O₃ into magnesia spinel can significantly increase the slurry life and reduce the thickness of hardened layer during centrifugal casting.

Keywords: titanium alloy, mould, MgAl₂O₄, Y₂O₃, interaction, investment casting

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Authors: Kristina Zuzek, Xuan Xu, Awais Ikram, Richard Sheridan, Allan Walton, Saso Sturm

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Recycling of end-of-life REEs based Nd-Fe-B magnets is an important strategy for reducing the environmental dangers associated with rare-earth mining and overcoming the well-documented supply risks related to the REEs. However, challenges on their reprocessing still remain. We report on the possibility of direct electrochemical recycling and reprocessing of Nd-Fe(B)-based magnets. In this investigation, we were able first to electrochemically leach the end-of-life NdFeB magnet and to electrodeposit Nd–Fe using a 1-ethyl-3-methyl imidazolium dicyanamide ([EMIM][DCA]) ionic liquid-based electrolyte. We observed that Nd(III) could not be reduced independently. However, it can be co-deposited on a substrate with the addition of Fe(II). Using advanced TEM techniques of electron-energy-loss spectroscopy (EELS) it was shown that Nd(III) is reduced to Nd(0) during the electrodeposition process. This gave a new insight into determining the Nd oxidation state, as X-ray photoelectron spectroscopy (XPS) has certain limitations. This is because the binding energies of metallic Nd (Nd0) and neodymium oxide (Nd₂O₃) are very close, i. e., 980.5-981.5 eV and 981.7-982.3 eV, respectively, making it almost impossible to differentiate between the two states. These new insights into the electrodeposition process represent an important step closer to efficient recycling of rare piles of earth in metallic form at mild temperatures, thus providing an alternative to high-temperature molten-salt electrolysis and a step closer to deposit Nd-Fe-based magnetic materials. Further, we propose a new concept of recycling the sintered Nd-Fe-B magnets by direct recovering the 2:14:1 matrix phase. Via an electrochemical etching method, we are able to recover pure individual 2:14:1 grains that can be re-used for new types of magnet production. In the frame of physical reprocessing, we have successfully synthesized new magnets out of hydrogen (HDDR)-recycled stocks with a contemporary technique of pulsed electric current sintering (PECS). The optimal PECS conditions yielded fully dense Nd-Fe-B magnets with the coercivity Hc = 1060 kA/m, which was boosted to 1160 kA/m after the post-PECS thermal treatment. The Br and Hc were tackled further and increased applied pressures of 100 – 150 MPa resulted in Br = 1.01 T. We showed that with a fine tune of the PECS and post-annealing it is possible to revitalize the Nd-Fe-B end-of-life magnets. By applying advanced TEM, i.e. atomic-scale Z-contrast STEM combined with EDXS and EELS, the resulting magnetic properties were critically assessed against various types of structural and compositional discontinuities down to atomic-scale, which we believe control the microstructure evolution during the PECS processing route.

Keywords: electrochemistry, Nd-Fe-B, pulsed electric current sintering, recycling, reprocessing

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Authors: Majid Farsadrouh Rashti, Amir Shafiee Kisomi, Parisa Jahani

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The direct ethanol fuel cells (DEFCs) are contemplated as a promising energy source because, In addition to being used in portable electronic devices, it is also used for electric vehicles. The synthesis of bimetallic nanostructures due to their novel optical, catalytic and electronic characteristic which is precisely in contrast to their monometallic counterparts is attracting extensive attention. Galvanic replacement (sometimes is named to as cementation or immersion plating) is an uncomplicated and effective technique for making nanostructures (such as core-shell) of different metals, semiconductors, and their application in DEFCs. The replacement of galvanic does not need any external power supply compared to electrodeposition. In addition, it is different from electroless deposition because there is no need for a reducing agent to replace galvanizing. In this paper, a fast method for the palladium (Pd) wire nanostructures synthesis with the great surface area through galvanic replacement reaction utilizing copper nanowires (CuNWS) as a template by the assistance of ultrasound under room temperature condition is proposed. To evaluate the morphology and composition of Pd@ Copper nanowires/MultiWalled Carbon nanotubes-Chitosan, emission scanning electron microscopy, energy dispersive X-ray spectroscopy were applied. In order to measure the phase structure of the electrocatalysts were performed via room temperature X-ray powder diffraction (XRD) applying an X-ray diffractometer. Various electrochemical techniques including chronoamperometry and cyclic voltammetry were utilized for the electrocatalytic activity of ethanol electrooxidation and durability in basic solution. Pd@ Copper nanowires/MultiWalled Carbon nanotubes-Chitosan catalyst demonstrated substantially enhanced performance and long-term stability for ethanol electrooxidation in the basic solution in comparison to commercial Pd/C that demonstrated the potential in utilizing Pd@ Copper nanowires/MultiWalled Carbon nanotubes-Chitosan as efficient catalysts towards ethanol oxidation. Noticeably, the Pd@ Copper nanowires/MultiWalled Carbon nanotubes-Chitosan presented excellent catalytic activities with a peak current density of 320.73 mAcm² which was 9.5 times more than in comparison to Pd/C (34.2133 mAcm²). Additionally, activation energy thermodynamic and kinetic evaluations revealed that the Pd@ Copper nanowires/MultiWalled Carbon nanotubes-Chitosan catalyst has lower compared to Pd/C which leads to a lower energy barrier and an excellent charge transfer rate towards ethanol oxidation.

Keywords: core-shell structure, electrocatalyst, ethanol oxidation, galvanic replacement reaction

Procedia PDF Downloads 118

Authors: Maksudur Rahman Khan, Kar Min Chan, Huei Ruey Ong, Chin Kui Cheng, Wasikur Rahman

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Microbial fuel cells (MFCs) represent a promising technology for simultaneous bioelectricity generation and wastewater treatment. Catalysts are significant portions of the cost of microbial fuel cell cathodes. Many materials have been tested as aqueous cathodes, but air-cathodes are needed to avoid energy demands for water aeration. The sluggish oxygen reduction reaction (ORR) rate at air cathode necessitates efficient electrocatalyst such as carbon supported platinum catalyst (Pt/C) which is very costly. Manganese oxide (MnO2) was a representative metal oxide which has been studied as a promising alternative electrocatalyst for ORR and has been tested in air-cathode MFCs. However, the single MnO2 has poor electric conductivity and low stability. In the present work, the MnO2 catalyst has been modified by doping Pt nanoparticle. The goal of the work was to improve the performance of the MFC with minimum Pt loading. MnO2 and Pt nanoparticles were prepared by hydrothermal and sol-gel methods, respectively. Wet impregnation method was used to synthesize Pt/MnO2 catalyst. The catalysts were further used as cathode catalysts in air-cathode cubic MFCs, in which anaerobic sludge was inoculated as biocatalysts and palm oil mill effluent (POME) was used as the substrate in the anode chamber. The as-prepared Pt/MnO2 was characterized comprehensively through field emission scanning electron microscope (FESEM), X-Ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and cyclic voltammetry (CV) where its surface morphology, crystallinity, oxidation state and electrochemical activity were examined, respectively. XPS revealed Mn (IV) oxidation state and Pt (0) nanoparticle metal, indicating the presence of MnO2 and Pt. Morphology of Pt/MnO2 observed from FESEM shows that the doping of Pt did not cause change in needle-like shape of MnO2 which provides large contacting surface area. The electrochemical active area of the Pt/MnO2 catalysts has been increased from 276 to 617 m2/g with the increase in Pt loading from 0.2 to 0.8 wt%. The CV results in O2 saturated neutral Na2SO4 solution showed that MnO2 and Pt/MnO2 catalysts could catalyze ORR with different catalytic activities. MFC with Pt/MnO2 (0.4 wt% Pt) as air cathode catalyst generates a maximum power density of 165 mW/m3, which is higher than that of MFC with MnO2 catalyst (95 mW/m3). The open circuit voltage (OCV) of the MFC operated with MnO2 cathode gradually decreased during 14 days of operation, whereas the MFC with Pt/MnO2 cathode remained almost constant throughout the operation suggesting the higher stability of the Pt/MnO2 catalyst. Therefore, Pt/MnO2 with 0.4 wt% Pt successfully demonstrated as an efficient and low cost electrocatalyst for ORR in air cathode MFC with higher electrochemical activity, stability and hence enhanced performance.

Keywords: microbial fuel cell, oxygen reduction reaction, Pt/MnO2, palm oil mill effluent, polarization curve

Procedia PDF Downloads 532

Authors: Rio Hirakawa, Christian Gundlach, Sven Hartwig

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Aluminium has been used in a wide range of industrial applications due to its numerous advantages, including excellent specific strength, thermal conductivity, corrosion resistance, workability and recyclability. The automotive industry is increasingly adopting multi-materials, including aluminium in structures and components to improve the mechanical usability and performance of individual components. A common method for assembling dissimilar materials is mechanical joining, but mechanical joining requires multiple manufacturing steps, affects the mechanical properties of the base material and increases the weight due to additional metal parts. Fusion bonding is being used in more and more industries as a way of avoiding the above drawbacks. Infusion bonding, and surface pre-treatment of the base material is essential to ensure the long-life durability of the joint. Laser surface treatment of aluminium has been shown to improve the durability of the joint by forming a passive oxide film and roughening the substrate surface. Infusion bonding, the polymer bonds directly to the metal instead of the adhesive, but the sensitivity to interfacial contamination is higher due to the chemical activity and molecular size of the polymer. Laser-treated surfaces are expected to absorb impurities from the storage atmosphere over time, but the effect of such changes in the treated surface over time on the durability of fusion-bonded joints has not yet been fully investigated. In this paper, the effect of the ageing of laser-treated surfaces of aluminum alloys on the corrosion resistance of fusion-bonded joints is therefore investigated. AlMg3 of 1.5 mm thickness was cut using a water-jet cutting machine, cleaned and degreased with isopropanol and surface pre-treated with a pulsed fiber laser at a wavelength of 1060 nm, maximum power of 70 W and repetition rate of 55 kHz. The aluminum surfaces were then stored in air for various periods of time and their corrosion resistance was assessed by cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). For the aluminum joints, induction heating was employed as the fusion bonding method and single-lap shear specimens were prepared. The corrosion resistance of the joints was assessed by measuring the lap shear strength before and after neutral salt spray. Cross-sectional observations by scanning electron microscopy (SEM) were also carried out to investigate changes in the microstructure of the bonded interface. Finally, the corrosion resistance of the surface and the joint were compared and the differences in the mechanisms of corrosion resistance enhancement between the two were discussed.

Keywords: laser surface treatment, pre-treatment, bonding, corrosion, durability, interface, automotive, aluminium alloys, joint, fusion bonding

Procedia PDF Downloads 49

Authors: Asad Hanif, Pavithra Parthasarathy, Zongjin Li

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Thermal insulating composites help to reduce the total power consumption in a building by creating a barrier between external and internal environment. Such composites can be used in the roofing tiles or wall panels for exterior surfaces. This study purposes to develop lightweight cement-based composites for thermal insulating applications. Waste materials like silica fume (an industrial by-product) and fly ash cenosphere (FAC) (hollow micro-spherical shells obtained as a waste residue from coal fired power plants) were used as partial replacement of cement and lightweight filler, respectively. Moreover, aerogel, a nano-porous material made of silica, was also used in different dosages for improved thermal insulating behavior, while poly vinyl alcohol (PVA) fibers were added for enhanced toughness. The raw materials including binders and fillers were characterized by X-Ray Diffraction (XRD), X-Ray Fluorescence spectroscopy (XRF), and Brunauer–Emmett–Teller (BET) analysis techniques in which various physical and chemical properties of the raw materials were evaluated like specific surface area, chemical composition (oxide form), and pore size distribution (if any). Ultra-lightweight cementitious composites were developed by varying the amounts of FAC and aerogel with 28-day unit weight ranging from 1551.28 kg/m³ to 1027.85 kg/m³. Excellent mechanical and thermal insulating properties of the resulting composites were obtained ranging from 53.62 MPa to 8.66 MPa compressive strength, 9.77 MPa to 3.98 MPa flexural strength, and 0.3025 W/m-K to 0.2009 W/m-K as thermal conductivity coefficient (QTM-500). The composites were also tested for peak temperature difference between outer and inner surfaces when subjected to heating (in a specially designed experimental set-up) by a 275W infrared lamp. The temperature difference up to 16.78 ^oC was achieved, which indicated outstanding properties of the developed composites to act as a thermal barrier for building envelopes. Microstructural studies were carried out by Scanning Electron Microscopy (SEM) and Energy Dispersive X-ray Spectroscopy (EDS) for characterizing the inner structure of the composite specimen. Also, the hydration products were quantified using the surface area mapping and line scale technique in EDS. The microstructural analyses indicated excellent bonding of FAC and aerogel in the cementitious system. Also, selective reactivity of FAC was ascertained from the SEM imagery where the partially consumed FAC shells were observed. All in all, the lightweight fillers, FAC, and aerogel helped to produce the lightweight composites due to their physical characteristics, while exceptional mechanical properties, owing to FAC partial reactivity, were achieved.

Keywords: aerogel, cement-based, composite, fly ash cenosphere, lightweight, sustainable development, thermal conductivity

Procedia PDF Downloads 195

Authors: Martin Alexander Eder, Sergei Semenov

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Many glass-epoxy composite structures, such as large utility wind turbine rotor blades (WTBs), comprise of adhesive joints with typically thick bond lines used to connect the different components during assembly. Performance optimization of rotor blades to increase power output by simultaneously maintaining high stiffness-to-low-mass ratios entails intricate geometries in conjunction with complex anisotropic material behavior. Consequently, adhesive joints in WTBs are subject to multiaxial stress states with significant stress gradients depending on the local joint geometry. Moreover, the dynamic aero-elastic interaction of the WTB with the airflow generates non-proportional, variable amplitude stress histories in the material. Empiricism shows that a prominent failure type in WTBs is high cycle fatigue failure of adhesive bond line interfaces, which in fact over time developed into a design driver as WTB sizes increase rapidly. Structural optimization employed at an early design stage, therefore, sets high demands on computationally efficient interface fatigue models capable of predicting the critical locations prone for interface failure. The numerical stress-based interface fatigue model presented in this work uses the Drucker-Prager criterion to compute three different damage indices corresponding to the two interface shear tractions and the outward normal traction. The two-parameter Drucker-Prager model was chosen because of its ability to consider shear strength enhancement under compression and shear strength reduction under tension. The governing interface damage index is taken as the maximum of the triple. The damage indices are computed through the well-known linear Palmgren-Miner rule after separate rain flow-counting of the equivalent shear stress history and the equivalent pure normal stress history. The equivalent stress signals are obtained by self-similar scaling of the Drucker-Prager surface whose shape is defined by the uniaxial tensile strength and the shear strength such that it intersects with the stress point at every time step. This approach implicitly assumes that the damage caused by the prevailing multiaxial stress state is the same as the damage caused by an amplified equivalent uniaxial stress state in the three interface directions. The model was implemented as Python plug-in for the commercially available finite element code Abaqus for its use with solid elements. The model was used to predict the interface damage of an adhesively bonded, tapered glass-epoxy composite cantilever I-beam tested by LM Wind Power under constant amplitude compression-compression tip load in the high cycle fatigue regime. Results show that the model was able to predict the location of debonding in the adhesive interface between the webfoot and the cap. Moreover, with a set of two different constant life diagrams namely in shear and tension, it was possible to predict both the fatigue lifetime and the failure mode of the sub-component with reasonable accuracy. It can be concluded that the fidelity, robustness and computational efficiency of the proposed model make it especially suitable for rapid fatigue damage screening of large 3D finite element models subject to complex dynamic load histories.

Keywords: adhesive, fatigue, interface, multiaxial stress

Procedia PDF Downloads 142

Authors: Sudhir Kumar, V. R. Sinha

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Background: The topical and systemic toxicity associated with present nonmelanoma skin cancer (NMSC) treatment therapy using 5-Fluorouracil (5-FU) make it necessary to develop a novel delivery system having lesser toxicity and better control over drug release. Solid lipid nanoparticles offer many advantages like: controlled and localized release of entrapped actives, nontoxicity, and better tolerance. Aim:-To investigate safety and efficacy of 5-FU loaded solid lipid nanoparticles as a topical delivery system for the treatment of nonmelanoma skin cancer. Method: Topical solid lipid nanoparticles of 5-FU were prepared using Compritol 888 ATO (Glyceryl behenate) as lipid component and pluronic F68 (Poloxamer 188), Tween 80 (Polysorbate 80), Tyloxapol (4-(1,1,3,3-Tetramethylbutyl) phenol polymer with formaldehyde and oxirane) as surfactants. The SLNs were prepared with emulsification method. Different formulation parameters viz. type and ratio of surfactant, ratio of lipid and ratio of surfactant:lipid were investigated on particle size and drug entrapment efficiency. Results: Characterization of SLNs like–Transmission Electron Microscopy (TEM), Differential Scannig calorimetry (DSC), Fourier transform infrared spectroscopy (FTIR), Particle size determination, Polydispersity index, Entrapment efficiency, Drug loading, ex vivo skin permeation and skin retention studies, skin irritation and histopathology studies were performed. TEM results showed that shape of SLNs was spherical with size range 200-500nm. Higher encapsulation efficiency was obtained for batches having higher concentration of surfactant and lipid. It was found maximum 64.3% for SLN-6 batch with size of 400.1±9.22 nm and PDI 0.221±0.031. Optimized SLN batches and marketed 5-FU cream were compared for flux across rat skin and skin drug retention. The lesser flux and higher skin retention was obtained for SLN formulation in comparison to topical 5-FU cream, which ensures less systemic toxicity and better control of drug release across skin. Chronic skin irritation studies lacks serious erythema or inflammation and histopathology studies showed no significant change in physiology of epidermal layers of rat skin. So, these studies suggest that the optimized SLN formulation is efficient then marketed cream and safer for long term NMSC treatment regimens. Conclusion: Topical and systemic toxicity associated with long-term use of 5-FU, in the treatment of NMSC, can be minimized with its controlled release with significant drug retention with minimal flux across skin. The study may provide a better alternate for effective NMSC treatment.

Keywords: 5-FU, topical formulation, solid lipid nanoparticles, non melanoma skin cancer

Procedia PDF Downloads 486

Authors: Augustus K. Lebechi, Kenneth I. Ozoemena

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

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

Procedia PDF Downloads 33

Authors: Gómez S. Jennifer, Méndez V. Camila, Moncayo M. Diana, Vega M. Lizeth

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The cape gooseberry is a climacteric fruit; Colombia is one of the principal exporters in the world. The environmental condition of temperature and relative moisture decreases the titratable acidity and pH. These conditions and fruit maturation result in the fungal proliferation of Botrytis cinerea disease. Plastic packaging for fresh cape gooseberries was used for mechanical damage protection but created a suitable atmosphere for fungal growth. Beta-cyclodextrins are currently implemented as coatings for the encapsulation of hydrophobic compounds, for example, with bioactive compounds from essential oils such as cinnamaldehyde, which has a high antimicrobial capacity. However, it is a volatile substance. In this article, the casting method was used to obtain a polylactic acid (PLA) polymer film containing the beta-cyclodextrin-cinnamaldehyde inclusion complex, generating an insert that allowed the controlled release of the antifungal substance in packed cape gooseberries to decrease contamination by Botrytis cinerea in a latent state during storage. For the encapsulation technique, three ratios for the cinnamaldehyde: beta-cyclodextrin inclusion complex were proposed: (25:75), (40:60), and (50:50). Spectrophotometry, colorimetry in L*a*b* coordinate space and scanning electron microscopy (SEM) were made for the complex characterization. Subsequently, two ratios of tween and water (40:60) and (50:50) were used to obtain the polylactic acid (PLA) film. To determine mechanical and physical parameters of colourimetry in L*a*b* coordinate space, atomic force microscopy and stereoscopy were done to determine the transparency and flexibility of the film; for both cases, Statgraphics software was used to determine the best ratio in each of the proposed phases, where for encapsulation it was (50:50) with an encapsulation efficiency of 65,92%, and for casting the ratio (40:60) obtained greater transparency and flexibility that permitted its incorporation into the polymeric packaging. A liberation assay was also developed under ambient temperature conditions to evaluate the concentration of cinnamaldehyde inside the packaging through gas chromatography for three weeks. It was found that the insert had a controlled release. Nevertheless, a higher cinnamaldehyde concentration is needed to obtain the minimum inhibitory concentration for the fungus Botrytis cinerea (0.2g/L). The homogeneity of the cinnamaldehyde gas phase inside the packaging can be improved by considering other insert configurations. This development aims to impact emerging food preservation technologies with the controlled release of antifungals to reduce the affectation of the physico-chemical and sensory properties of the fruit as a result of contamination by microorganisms in the postharvest stage.

Keywords: antifungal, casting, encapsulation, postharvest

Procedia PDF Downloads 48

Authors: Alan N. A. Heberle, Salatiel W. Da Silva, Valentin Perez-Herranz, Andrea M. Bernardes

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Contaminants of emerging concern are substances widely used, such as pharmaceutical products. These compounds represent risk for both wild and human life since they are not completely removed from wastewater by conventional wastewater treatment plants. In the environment, they can be harm even in low concentration (µ or ng/L), causing bacterial resistance, endocrine disruption, cancer, among other harmful effects. One of the most common taken medicine to treat cardiocirculatory diseases is the Atenolol (ATL), a β-Blocker, which is toxic to aquatic life. In this way, it is necessary to implement a methodology, which is capable to promote the degradation of the ATL, to avoid the environmental detriment. A very promising technology is the advanced electrochemical oxidation (AEO), which mechanisms are based on the electrogeneration of reactive radicals (mediated oxidation) and/or on the direct substance discharge by electron transfer from contaminant to electrode surface (direct oxidation). The hydroxyl (HO•) and sulfate (SO₄•⁻) radicals can be generated, depending on the reactional medium. Besides that, at some condition, the peroxydisulfate (S₂O₈²⁻) ion is also generated from the SO₄• reaction in pairs. Both radicals, ion, and the direct contaminant discharge can break down the molecule, resulting in the degradation and/or mineralization. However, ATL molecule and byproducts can still remain in the treated solution. On this wise, some efforts can be done to implement the AEO process, being one of them the use of a cationic membrane to separate the cathodic (reduction) from the anodic (oxidation) reactor compartment. The aim of this study is investigate the influence of the implementation of a cationic membrane (Nafion®-117) to separate both cathodic and anodic, AEO reactor compartments. The studied reactor was a filter-press, with bath recirculation mode, flow 60 L/h. The anode was an Nb/BDD2500 and the cathode a stainless steel, both bidimensional, geometric surface area 100 cm². The solution feeding the anodic compartment was prepared with ATL 100 mg/L using Na₂SO₄ 4 g/L as support electrolyte. In the cathodic compartment, it was used a solution containing Na₂SO₄ 71 g/L. Between both solutions was placed the membrane. The applied currents densities (iₐₚₚ) of 5, 20 and 40 mA/cm² were studied over 240 minutes treatment time. Besides that, the ATL decay was analyzed by ultraviolet spectroscopy (UV/Vis). The mineralization was determined performing total organic carbon (TOC) in TOC-L CPH Shimadzu. In the cases without membrane, the iₐₚₚ 5, 20 and 40 mA/cm² resulted in 55, 87 and 98 % ATL degradation at the end of treatment time, respectively. However, with membrane, the degradation, for the same iₐₚₚ, was 90, 100 and 100 %, spending 240, 120, 40 min for the maximum degradation, respectively. The mineralization, without membrane, for the same studied iₐₚₚ, was 40, 55 and 72 %, respectively at 240 min, but with membrane, all tested iₐₚₚ reached 80 % of mineralization, differing only in the time spent, 240, 150 and 120 min, for the maximum mineralization, respectively. The membrane increased the ATL oxidation, probably due to avoid oxidant ions (S₂O₈²⁻) reduction on the cathode surface.

Keywords: contaminants of emerging concern, advanced electrochemical oxidation, atenolol, cationic membrane, double compartment reactor

Procedia PDF Downloads 110

Authors: Sankha Chakrabortty, Biswajit Ruj, Parimal Pal

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

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

Procedia PDF Downloads 89

Authors: Patrícia Severino, Luciana Nalone, Daniele Martins, Marco Chaud, Classius Ferreira, Cristiane Bani, Ricardo Albuquerque

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Hydrogels produced with polymers have been used in the development of dressings for wound treatment and tissue revitalization. Our study on polymer nanocomposites containing silver nanoparticles shows antimicrobial activity and applications in wound healing. The effects are linked with the slow oxidation and Ag⁺ liberation to the biological environment. Furthermore, bacterial cell membrane penetration and metabolic disruption through cell cycle disarrangement also contribute to microbial cell death. The silver antimicrobial activity has been known for many years, and previous reports show that low silver concentrations are safe for human use. This work aims to develop a hydrogel using natural polymers (sodium alginate and gelatin) combined with silver nanoparticles for wound healing and with antimicrobial properties in cutaneous lesions. The hydrogel development utilized different sodium alginate and gelatin proportions (20:80, 50:50 and 80:20). The silver nanoparticles incorporation was evaluated at the concentrations of 1.0, 2.0 and 4.0 mM. The physico-chemical properties of the formulation were evaluated using ultraviolet-visible (UV-Vis) absorption spectroscopy, Fourier transform infrared (FTIR) spectroscopy, differential scanning calorimetry (DSC), and thermogravimetric (TG) analysis. The morphological characterization was made using transmission electron microscopy (TEM). Human fibroblast (L2929) viability assay was performed with a minimum inhibitory concentration (MIC) assessment as well as an in vivo cicatrizant test. The results suggested that sodium alginate and gelatin in the (80:20) proportion with 4 mM of AgNO₃ in the (UV-Vis) exhibited a better hydrogel formulation. The nanoparticle absorption spectra of this analysis showed a maximum band around 430 - 450 nm, which suggests a spheroidal form. The TG curve exhibited two weight loss events. DSC indicated one endothermic peak at 230-250 °C, due to sample fusion. The polymers acted as stabilizers of a nanoparticle, defining their size and shape. Human fibroblast viability assay L929 gave 105 % cell viability with a negative control, while gelatin presented 96% viability, alginate: gelatin (80:20) 96.66 %, and alginate 100.33 % viability. The sodium alginate:gelatin (80:20) exhibited significant antimicrobial activity, with minimal bacterial growth at a ratio of 1.06 mg.mL⁻¹ in Pseudomonas aeruginosa and 0.53 mg.mL⁻¹ in Staphylococcus aureus. The in vivo results showed a significant reduction in wound surface area. On the seventh day, the hydrogel-nanoparticle formulation reduced the total area of injury by 81.14 %, while control reached a 45.66 % reduction. The results suggest that silver-hydrogel nanoformulation exhibits potential for wound dressing therapeutics.

Keywords: nanocomposite, wound healing, hydrogel, silver nanoparticle

Procedia PDF Downloads 81

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

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During their lifetime, industrial machines are often subjected to chemical, mechanical and thermal extreme conditions. In some cases, the loss of efficiency comes from the degradation of the surface as a result of its exposition to abrasive environments that can cause wear. This is a common problem to be solved in industries of diverse nature such as food, paper or concrete industries, among others. For this reason, a good selection of the material is of high importance. In the machine design context, stainless steels such as AISI 304 and 316 are widely used. However, the severity of the external conditions can require additional protection for the steel and sometimes coating solutions are demanded in order to extend the lifespan of these materials. Therefore, the development of effective coatings with high wear resistance is of utmost technological relevance. In this research, bilayer coatings made of Titanium-Tantalum, Titanium-Niobium, Titanium-Hafnium, and Titanium-Zirconium have been developed using magnetron sputtering configuration by PVD (Physical Vapor Deposition) technology. Their tribological behavior has been measured and evaluated under different environmental conditions. Two kinds of steels were used as substrates: AISI 304, AISI 316. For the comparison with these materials, titanium alloy substrate was also employed. Regarding the characterization, wear rate and friction coefficient were evaluated by a tribo-tester, using a pin-on-ball configuration with different lubricants such as tomato sauce, wine, olive oil, wet compost, a mix of sand and concrete with water and NaCl to approximate the results to real extreme conditions. In addition, topographical images of the wear tracks were obtained in order to get more insight of the wear behavior and scanning electron microscope (SEM) images were taken to evaluate the adhesion and quality of the coating. The characterization was completed with the measurement of nanoindentation hardness and elastic modulus. Concerning the results, thicknesses of the samples varied from 100 nm (Ti-Zr layer) to 1.4 µm (Ti-Hf layer) and SEM images confirmed that the addition of the Ti layer improved the adhesion of the coatings. Moreover, results have pointed out that these coatings have increased the wear resistance in comparison with the original substrates under environments of different severity. Furthermore, nanoindentation hardness results showed an improvement of the elastic strain to failure and a high modulus of elasticity (approximately 200 GPa). As a conclusion, Ti-Ta, Ti-Zr, Ti-Nb, and Ti-Hf are very promising and effective coatings in terms of tribological behavior, improving considerably the wear resistance and friction coefficient of typically used machine materials.

Keywords: coating, stainless steel, tribology, wear

Procedia PDF Downloads 126

Authors: Precious Ehiomogue, Ifechukwude Israel Ahuchaogu, Isiguzo Edwin Ahaneku

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Vermicompost is the product of the decomposition process using various species of worms, to create a mixture of decomposing vegetable or food waste, bedding materials, and vemicast. This process is called vermicomposting, while the rearing of worms for this purpose is called vermiculture. Several works have verified the adsorption of toxic metals using vermicompost but the application is still scarce for the retention of organic compounds. This research brings to knowledge the effectiveness of earthworm waste (vermicompost) for the remediation of crude oil contaminated soils. The remediation methods adopted in this study were two soil washing methods namely, batch and column process which represent laboratory and in-situ remediation. Characterization of the vermicompost and crude oil contaminated soil were performed before and after the soil washing using Fourier transform infrared (FTIR), scanning electron microscopy (SEM), X-ray fluorescence (XRF), X-ray diffraction (XRD) and Atomic adsorption spectrometry (AAS). The optimization of washing parameters, using response surface methodology (RSM) based on Box-Behnken Design was performed on the response from the laboratory experimental results. This study also investigated the application of machine learning models [Artificial neural network (ANN), Adaptive neuro fuzzy inference system (ANFIS). ANN and ANFIS were evaluated using the coefficient of determination (R²) and mean square error (MSE)]. Removal efficiency obtained from the Box-Behnken design experiment ranged from 29% to 98.9% for batch process remediation. Optimization of the experimental factors carried out using numerical optimization techniques by applying desirability function method of the response surface methodology (RSM) produce the highest removal efficiency of 98.9% at absorbent dosage of 34.53 grams, adsorbate concentration of 69.11 (g/ml), contact time of 25.96 (min), and pH value of 7.71, respectively. Removal efficiency obtained from the multilevel general factorial design experiment ranged from 56% to 92% for column process remediation. The coefficient of determination (R²) for ANN was (0.9974) and (0.9852) for batch and column process, respectively, showing the agreement between experimental and predicted results. For batch and column precess, respectively, the coefficient of determination (R²) for RSM was (0.9712) and (0.9614), which also demonstrates agreement between experimental and projected findings. For the batch and column processes, the ANFIS coefficient of determination was (0.7115) and (0.9978), respectively. It can be concluded that machine learning models can predict the removal of crude oil from polluted soil using vermicompost. Therefore, it is recommended to use machines learning models to predict the removal of crude oil from contaminated soil using vermicompost.

Keywords: ANFIS, ANN, crude-oil, contaminated soil, remediation and vermicompost

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Authors: Mohammed Fayez Al Rez

Abstract:

Nowadays, there is an unmet clinical need for new small-diameter vascular grafts to overcome the drawbacks of traditional methods used for treatment of widespread cardiovascular diseases. Vascular tissue engineering (VTE) is a promising approach that can be utilized to develop viable vascular grafts by in vitro seeding of functional cells onto a scaffold allowing them to attach, proliferate and differentiate. To achieve this purpose, the scaffold should provide cells with the initial necessary extracellular matrix environment and structure until being able to reconstruct the required vascular tissue. Therefore, producing scaffolds with suitable features is crucial for guiding cells properly to develop the desired tissue-engineered vascular grafts for clinical applications. The main objective of this work is fabrication and characterization of tubular small-diameter ( < 6 mm) bilayered scaffolds for VTE. The scaffolds were prepared via mixing electrospinning approach of biodegradable poly(ε-caprolactone) (PCL) polymer – due to its favorable physicochemical properties – to mimic the natural environment-extracellular matrix. Firstly, tubular nanofibrous construct with inner diameter of 3, 4 or 5 mm was electrospun as inner layer, and secondly, microfibrous construct was electrospun as outer layer directly on the first produced inner layer. To improve the biological properties of PCL, a group of the electrospun scaffolds was immersed in type-1 collagen solution. The morphology and structure of the resulting fibrous scaffolds were investigated by scanning electron microscope. The electrospun nanofibrous inner layer contained fibers measuring 219±35 nm in diameter, while the electrospun microfibrous outer layer contained fibers measuring 1011 ± 150 nm. Furthermore, mechanical, thermal and physical tests were conducted with both electrospun bilayered scaffold types where revealed improved properties. Biological investigations using endothelial, smooth muscle and fibroblast cell line showed good biocompatibility of both tested electrospun scaffolds. Better attachment and proliferation were obviously found when cells were cultured on the scaffolds immersed with collagen due to increasing the hydrophilicity of the PCL. The easy, inexpensive and versatile electrospinning approach used in this work was able to successfully produce double layered tubular elastic structures containing both nanofibers and microfibers to imitate the native vascular structure. The PCL – as a suitable and approved biomaterial for many biomedical and tissue engineering applications – can ensure favorable mechanical properties of scaffolds used for VTE. The VTE approach using electrospun bilayered scaffolds offers optimal solutions and holds significant promises for treatment of many cardiovascular diseases.

Keywords: electrospinning, poly(ε-caprolactone) (PCL), tissue-engineered vascular graft, tubular bilayered scaffolds, vascular cells

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Authors: Ghada Al-Kafaji, Mohamed Sabry

Abstract:

Mitochondria are the site of cellular respiration and produce energy in the form of adenosine triphosphate (ATP) via oxidative phosphorylation. They are the major source of intracellular reactive oxygen species (ROS) and are also direct target to ROS attack. Oxidative stress and ROS-mediated disruptions of mitochondrial function are major components involved in the pathogenicity of diabetic complications. In this work, the changes in mitochondrial DNA (mtDNA) copy number, biogenesis, gene expression of mtDNA-encoded subunits of electron transport chain (ETC) complexes, and mitochondrial function in response to hyperglycemia-induced ROS and the effect of direct inhibition of ROS on mitochondria were investigated in an in vitro model of diabetic nephropathy using human renal mesangial cells. The cells were exposed to normoglycemic and hyperglycemic conditions in the presence and absence of Mn(III)tetrakis(4-benzoic acid) porphyrin chloride (MnTBAP) or catalase for 1, 4 and 7 days. ROS production was assessed by the confocal microscope and flow cytometry. mtDNA copy number and PGC-1a, NRF-1, and TFAM, as well as ND2, CYTB, COI, and ATPase 6 transcripts, were all analyzed by real-time PCR. PGC-1a, NRF-1, and TFAM, as well as ND2, CYTB, COI, and ATPase 6 proteins, were analyzed by Western blotting. Mitochondrial function was determined by assessing mitochondrial membrane potential and adenosine triphosphate (ATP) levels. Hyperglycemia-induced a significant increase in the production of mitochondrial superoxide and hydrogen peroxide at day 1 (P < 0.05), and this increase remained significantly elevated at days 4 and 7 (P < 0.05). The copy number of mtDNA and expression of PGC-1a, NRF-1, and TFAM as well as ND2, CYTB, CO1 and ATPase 6 increased after one day of hyperglycemia (P < 0.05), with a significant reduction in all those parameters at 4 and 7 days (P < 0.05). The mitochondrial membrane potential decreased progressively at 1 to 7 days of hyperglycemia with the parallel progressive reduction in ATP levels over time (P < 0.05). MnTBAP and catalase treatment of cells cultured under hyperglycemic conditions attenuated ROS production reversed renal mitochondrial oxidative stress and improved mtDNA, mitochondrial biogenesis, and function. These results show that hyperglycemia-induced ROS caused an early increase in mtDNA copy number, mitochondrial biogenesis and mtDNA-encoded gene expression of the ETC subunits in human mesangial cells as a compensatory response to the decline in mitochondrial function, which precede the mtDNA defect and mitochondrial dysfunction with a progressive oxidative response. Protection from ROS-mediated damage to renal mitochondria induced by hyperglycemia may be a novel therapeutic approach for the prevention/treatment of DN.

Keywords: diabetic nephropathy, hyperglycemia, reactive oxygen species, oxidative stress, mtDNA, mitochondrial dysfunction, manganese superoxide dismutase, catalase

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Authors: Chien-Chun Huang, P. W. Yuan

Abstract:

Banana is one of the important fruits which constitute a valuable source of energy, vitamins and minerals and an important food component throughout the world. The fruit ripening and maturity standards vary from country to country depending on the expected shelf life of market. During ripening there are changes in appearance, texture and chemical composition of banana. The changes of component of banana during ethylene-induced ripening are categorized as nutritive values and commercial utilization. The objectives of this study were to investigate the changes of chemical composition and physicochemical properties of banana during ethylene-induced ripening. Green bananas were harvested and ripened by ethylene gas at low temperature (15℃) for seven stages. At each stage, banana was sliced and freeze-dried for banana flour preparation. The changes of total starch, resistant starch, chemical compositions, physicochemical properties, activity of amylase, polyphenolic oxidase (PPO) and phenylalanine ammonia lyase (PAL) of banana were analyzed each stage during ripening. The banana starch was isolated and analyzed for gelatinization properties, pasting properties and microscopic appearance each stage of ripening. The results indicated that the highest total starch and resistant starch content of green banana were 76.2% and 34.6%, respectively at the harvest stage. Both total starch and resistant starch content were significantly declined to 25.3% and 8.8%, respectively at the seventh stage. Soluble sugars content of banana increased from 1.21% at harvest stage to 37.72% at seventh stage during ethylene-induced ripening. Swelling power of banana flour decreased with the progress of ripening stage, but solubility increased. These results strongly related with the decreases of starch content of banana flour during ethylene-induced ripening. Both water insoluble and alcohol insoluble solids of banana flour decreased with the progress of ripening stage. Both activity of PPO and PAL increased, but the total free phenolics content decreased, with the increases of ripening stages. As ripening stage extended, the gelatinization enthalpy of banana starch significantly decreased from 15.31 J/g at the harvest stage to 10.55 J/g at the seventh stage. The peak viscosity and setback increased with the progress of ripening stages in the pasting properties of banana starch. The highest final viscosity, 5701 RVU, of banana starch slurry was found at the seventh stage. The scanning electron micrograph of banana starch showed the shapes of banana starch appeared to be round and elongated forms, ranging in 10-50 μm at the harvest stage. As the banana closed to ripe status, some parallel striations were observed on the surface of banana starch granular which could be caused by enzyme reaction during ripening. These results inferred that the highest resistant starch was found in the green banana could be considered as a potential application of healthy foods. The changes of chemical composition and physicochemical properties of banana could be caused by the hydrolysis of enzymes during the ethylene-induced ripening treatment.

Keywords: maturation of banana, appearance, texture, soluble sugars, resistant starch, enzyme activities, physicochemical properties of banana starch

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Authors: Abid Hussain, Binay Kumar

Abstract:

Environment-friendly lead-free Na₀.₅₂K₀.₄₄Li₀.₀₄Nb₀.₈₄Ta₀.₁₀Sb₀.₀₆O₃ (NKLNTS) ceramic was synthesized by solid-state reaction method in search of a potential candidate to replace lead-based ceramics such as PbZrO₃-PbTiO₃ (PZT), Pb(Mg₁/₃Nb₂/₃)O₃-PbTiO₃ (PMN-PT) etc., for various applications. The ceramic was calcined at temperature 850 ᵒC and sintered at 1090 ᵒC. The powder X-Ray Diffraction (XRD) pattern revealed the formation of pure perovskite phase having tetragonal symmetry with space group P4mm of the synthesized ceramic. The surface morphology of the ceramic was studied using Field Emission Scanning Electron Microscopy (FESEM) technique. The well-defined grains with homogeneous microstructure were observed. The average grain size was found to be ~ 0.6 µm. A very large value of piezoelectric charge coefficient (d₃₃ ~ 754 pm/V) was obtained for the synthesized ceramic which indicated its potential for use in transducers and actuators. In dielectric measurements, a high value of ferroelectric to paraelectric phase transition temperature (Tm~305 ᵒC), a high value of maximum dielectric permittivity ~ 2110 (at 1 kHz) and a very small value of dielectric loss ( < 0.6) were obtained which suggested the utility of NKLNTS ceramic in high-temperature ferroelectric devices. Also, the degree of diffuseness (γ) was found to be 1.61 which confirmed a relaxor ferroelectric behavior in NKLNTS ceramic. P-E hysteresis loop was traced and the value of spontaneous polarization was found to be ~11μC/cm² at room temperature. The pyroelectric coefficient was obtained to be very high (p ∼ 1870 μCm⁻² ᵒC⁻¹) for the present case indicating its applicability in pyroelectric detector applications including fire and burglar alarms, infrared imaging, etc. NKLNTS ceramic showed fatigue free behavior over 107 switching cycles. Remanent hysteresis task was performed to determine the true-remanent (or intrinsic) polarization of NKLNTS ceramic by eliminating non-switchable components which showed that a major portion (83.10 %) of the remanent polarization (Pr) is switchable in the sample which makes NKLNTS ceramic a suitable material for memory switching devices applications. Time-Dependent Compensated (TDC) hysteresis task was carried out which revealed resistive leakage free nature of the ceramic. The performance of NKLNTS ceramic was found to be superior to many lead based piezoceramics and hence can effectively replace them for use in piezoelectric, pyroelectric and long duration ferroelectric applications.

Keywords: dielectric properties, ferroelectric properties , lead free ceramic, piezoelectric property, solid state reaction, true-remanent polarization

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