Search results for: Microscopy

Authors: Zainudin Kornain, Azman Jalar, Rozaidi Rasid, Fong Chee Seng

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Void formation in underfill is considered as failure in flip chip manufacturing process. Void formation possibly caused by several factors such as poor soldering and flux residue during die attach process, void entrapment due moisture contamination, dispense pattern process and setting up the curing process. This paper presents the comparison of single step and two steps curing profile towards the void and black dots formation in underfill for Hi-CTE Flip Chip Ceramic Ball Grid Array Package (FC-CBGA). Statistic analysis was conducted to analyze how different factors such as wafer lot, sawing technique, underfill fillet height and curing profile recipe were affected the formation of voids and black dots. A C-Mode Scanning Aqoustic Microscopy (C-SAM) was used to scan the total count of voids and black dots. It was shown that the 2 steps curing profile provided solution for void elimination and black dots in underfill after curing process.

Keywords: black dots formation, curing profile, FC-CBGA, underfill, void formation,

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Authors: Bruno Bacci Fernandes, Stephan Mändl, Ataíde Ribeiro da Silva Junior, José Osvaldo Rossi, Mário Ueda

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Nitrogen implantation in aluminum and its alloys is acquainted for the difficulties in obtaining modified layers deeper than 200 nm. The present work addresses a new method to overcome such a problem; although, the coating with nitrogen and oxygen obtained by plasma immersion ion implantation (PIII) into a 7075 aluminum alloy surface was too shallow. This alloy is commonly used for structural parts in aerospace applications. Such a layer was characterized by secondary ion mass spectroscopy, electron microscopy, and nanoindentation experiments reciprocating wear tests. From the results, one can assume that the wear of this aluminum alloy starts presenting severe abrasive wear followed by an additional adhesive mechanism. PIII produced a slight difference, as shown in all characterizations carried out in this work. The results shown here can be used as the scientific basis for further nitrogen PIII experiments in aluminum alloys which have the goal to produce thicker modified layers or to improve their surface properties.

Keywords: Aluminum alloys, plasma immersion ion implantation, tribological properties, hardness, nanofatigue.

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Authors: Tsung-Yen Tsai, Naveen Bunekar, Ming Hsuan Chang, Wen-Kuang Wang, Satoshi Onda

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The structure-property relationship and initiator effect on bulk polymerized poly(methyl methacrylate) (PMMA)–oragnomodified layered silicate nanocomposites was investigated. In this study, we used 2, 2'-azobis (4-methoxy-2,4-dimethyl valeronitrile and benzoyl peroxide initiators for bulk polymerization. The bulk polymerized nanocomposites’ morphology was investigated by X-ray diffraction and transmission electron microscopy. The type of initiator strongly influences the physiochemical properties of the polymer nanocomposite. The thermal degradation of PMMA in the presence of nanofiller was studied. 5 wt% weight loss temperature (T5d) increased as compared to pure PMMA. The peak degradation temperature increased for the nanocomposites. Differential scanning calorimetry and dynamic mechanical analysis were performed to investigate the glass transition temperature and the nature of the constrained region as the reinforcement mechanism respectively. Furthermore, the optical properties such as UV-Vis and Total Luminous Transmission of nanocomposites are examined.

Keywords: Initiator, bulk polymerization, layered silicates, methyl methacrylate.

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Authors: C. Photiphitak, P. Rakkwamsuk, P. Muthitamongkol, C. Thanachayanont

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TiO2/MgO composite films were prepared by coating the magnesium acetate solution in the pores of mesoporous TiO2 films using a dip coating method. Concentrations of magnesium acetate solution were varied in a range of 1x10-4 – 1x10-1 M. The TiO2/MgO composite films were characterized by scanning electron microscopy (SEM), transmission electron microscropy (TEM), electrochemical impedance spectroscopy(EIS) , transient voltage decay and I-V test. The TiO2 films and TiO2/MgO composite films were immersed in a 0.3 mM N719 dye solution. The Dye-sensitized solar cells with the TiO2/MgO/N719 structure showed an optimal concentration of magnesium acetate solution of 1x10-3 M resulting in the MgO film estimated thickness of 0.0963 nm and giving the maximum efficiency of 4.85%. The improved efficiency of dyesensitized solar cell was due to the magnesium oxide film as the wide band gap coating decays the electron back transfer to the triiodide electrolyte and reduce charge recombination.

Keywords: Magnesium oxide thin film, TiO2/MgO composite films, Electrochemical Impedance Spectrum, Transient voltage decay

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Authors: Lina Paola Orozco-Marín, Yuliet Montoya, John Bustamante

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Ischemic events can culminate in acute myocardial infarction with irreversible cardiac lesions that cannot be restored due to the limited regenerative capacity of the heart. Tissue engineering proposes therapeutic alternatives by using biomaterials to resemble the native extracellular medium combined with healthy and functional cells. This research focused on developing a natural thermosensitive hydrogel, its physical-chemical characterization and in vitro biocompatibility determination. Hydrogels’ morphological characterization was carried out through scanning electron microscopy and its chemical characterization by employing Infrared Spectroscopy technic. In addition, the biocompatibility was determined using fetal human ventricular cardiomyocytes cell line RL-14 and the MTT cytotoxicity test according to the ISO 10993-5 standard. Four biocompatible and thermosensitive hydrogels were obtained with a three-dimensional internal structure and two gelation times. The results show the potential of the hydrogel to increase the cell survival rate to the cardiac cell therapies under investigation and lay the foundations to continue with its characterization and biological evaluation both in vitro and in vivo models.

Keywords: cardiac cell therapy, cardiac ischemia, natural polymers, thermosensitive hydrogel

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Authors: Uma Batra, Seema Kapoor

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Commercial hydroxyapatite (HA) was reinforced by adding 2, 5, and 10 wt % of 28.5%CaO-28.5%P2O5-38%Na2 O- 5%CaF2 based glass and then sintered. Although HA shows good biocompatibility with the human body, its applications are limited to non load-bearing areas and coatings due to its poor mechanical properties. These mechanical properties can be improved substantially with addition of glass ceramics by sintering. In this study, the effects of sintering hydroxyapatite with above specified phosphate glass additions are quantified. Each composition was sintered over a range of temperatures. Scanning electron microscopy and x-ray diffraction were used to characterize the microstructure and phases of the composites. The density, microhardness, and compressive strength were measured using Archimedes Principle, Vickers Microhardness Tester (at 0.98 N), and Instron Universal Testing Machine (cross speed of 0.5 mm/min) respectively. These results were used to indicate which composition provided suitable material for use in hard tissue replacement. Composites containing 10 wt % glass additions formed dense HA/TCP (tricalcium phosphate) composite materials possessing good compressive strength and hardness than HA. In-vitro bioactivity was assessed by evaluating changes in pH and Ca2+ ion concentration of SBF-simulated body fluid on immersion of these composites in it for two weeks.

Keywords: Bioglass, Composite, Hydroxyapatite, Sintering.

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Authors: Su-Ling Li, Qun-Yu Gao

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Mung bean starches were subjected to heat-moisture treatment (HMT) by different moisture contents (15%, 20%, 25%, 30% and 35%) at 120Ôäâ for 12h. The impact on the yields of resistant starch (RS), microstructure, physicochemical and functional properties was investigated. Compared to native starch, the RS content of heat-moisture treated starches increased significantly. The RS level of HMT-20 was the highest of all the starches. Birefringence was displayed clear at the center of native starch. For HMT starches, pronounced birefringence was exhibited on the periphery of starch granules; however, birefringence disappeared at the centre of some starch granules. The shape of HMT starches hadn-t been changed and the integrity of starch granules was preserved for all the conditions. Concavity could be observed on HMT starches under scanning electronic microscopy. After HMT, apparent amylose contents were increased and starch macromolecule was degraded in comparison with those of native starch. There was a reduction in swelling power on HMT starches, but the solubility of HMT starches was higher than that of native starch. Both of native and HMT starches showed A-type X-ray diffraction pattern. Furthermore, there is a higher intensity at the peak of 15.0 and 22.9 Å than those of native starch.

Keywords: Resistant starch, mung bean (Phaseolus radiatus) starch, heat-moisture treatment, physicochemical properties.

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Authors: Bintao Wu, Xiangfang Xu, Yugang Miao, Duanfeng Han

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Joining of 1mm thick aluminum 6061 to titanium TC4 was conducted using Bypass-current MIG welding-brazed, and stable welding process and good bead appearance were obtained. The Joint profile and microstructure of Ti/Al joints were observed by optical microscopy and SEM and then the structure of the interfacial reaction layers were analyzed in details. It was found that the intermetallic compound layer at the interfacial top is in the form of columnar crystal, which is in short and dense state. A mount of AlTi were observed at the interfacial layer near the Ti base metal while intermetallic compound like Al3Ti, TiSi3 were formed near the Al base metal, and the Al11Ti5 transition phase was found in the center of the interface layer due to the uneven distribution inside the weld pool during the welding process. Tensile test results show that the average tensile strength of joints is up to 182.6 MPa, which reaches about 97.6% of aluminum base metal. Fracture is prone to occur in the base metal with a certain amount of necking.

Keywords: Bypass-current MIG welding-brazed, Al alloy, Ti alloy, joint characteristics, mechanical properties.

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Authors: Md. Ashikur Rahman Khan, M. M. Rahman

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Electrical discharge machining (EDM) is a relatively modern machining process having distinct advantages over other machining processes and can machine Ti-alloys effectively. The present study emphasizes the features of the development of regression equation based on response surface methodology (RSM) for correlating the interactive and higher-order influences of machining parameters on surface finish of Titanium alloy Ti-6Al-4V. The process parameters selected in this study are discharge current, pulse on time, pulse off time and servo voltage. Machining has been accomplished using negative polarity of Graphite electrode. Analysis of variance is employed to ascertain the adequacy of the developed regression model. Experiments based on central composite of response surface method are carried out. Scanning electron microscopy (SEM) analysis was performed to investigate the surface topography of the EDMed job. The results evidence that the proposed regression equation can predict the surface roughness effectively. The lower ampere and short pulse on time yield better surface finish.

Keywords: Graphite electrode, regression model, response surface methodology, surface roughness.

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Authors: Y.K. Kim, Y.S. Jang, H.H. Park, J.H. Ji, I.S. Park, T.S. Bae, M.H. Lee

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Magnesium is used implant material potentially for non-toxicity to the human body. Due to the excellent bio-compatibility, Mg alloys is applied to implants avoiding removal second surgery. However, it is found commercial magnesium alloys including aluminum has low corrosion resistance, resulting subcutaneous gas bubbles and consequently the approach as permanent bio-materials. Generally, Aluminum is known to pollution substance, and it raises toxicity to nervous system. Therefore especially Mg-35Zn-3Ca alloy is prepared for new biodegradable materials in this study. And the pulsed power is used in constant-current mode of DC power kinds of anodization. Based on the aforementioned study, it examines corrosion resistance and biocompatibility by effect of current and frequency variation. The surface properties and thickness were compared using scanning electronic microscopy. Corrosion resistance was assessed via potentiodynamic polarization and the effect of oxide layer on the body was assessed cell viability. Anodized Mg-35Zn-3Ca alloy has good biocompatibility in vitro by current and frequency variation.

Keywords: Biodegradable material, Mg, anodization, osteoblast cell, pulse power.

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Authors: Farid Amidi-Fazli, Neda Amidi-Fazli

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Replacement of plastics used in the food industry seems to be a serious issue to overcome mainly the environmental problems in recent years. This study investigates the hydrophilicity and permeability properties of starch biopolymer which ethylene vinyl alcohol (EVOH) (0-10%) and nanocrystalline cellulose (NCC) (1-15%) were used to enhance its properties. Starch -EVOH nanocomposites were prepared by casting method in different formulations. NCC production by acid hydrolysis was confirmed by scanning electron microscopy. Solubility, water vapor permeability, water vapor transmission rate and moisture absorbance were measured on each of the nanocomposites. The results were analyzed by SAS software. The lowest moisture absorbance was measured in pure starch nanocomposite containing 8% NCC. The lowest permeability to water vapor belongs to starch nanocomposite containing 8% NCC and the sample containing 7.8% EVOH and 13% NCC. Also the lowest solubility was observed in the composite contains the highest amount of EVOH. Applied Process resulted in production of bio films which have good resistance to water vapor permeability and solubility in water. The use of NCC and EVOH leads to reduced moisture absorbance property of the biofilms.

Keywords: Starch, EVOH, nanocrystalline cellulose, Hydrophilicity.

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Authors: Ella C. Linganiso, Bonex W. Mwakikunga, Trilock Singh, Sanjay Mathur, Odireleng M. Ntwaeaborwa

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The use of nanostructured semiconducting material to catalyze degradation of environmental pollutants still receives much attention to date. One of the desired characteristics for pollutant degradation under ultra-violet visible light is the materials with extended carrier charge separation that allows for electronic transfer between the catalyst and the pollutants. In this work, zinc oxide n-type semiconductor vertically aligned structures were fabricated on silicon (100) substrates using the chemical bath deposition method. The as-synthesized structures were treated with nickel and sulphur. X-ray diffraction, scanning electron microscopy, energy dispersive X-ray spectroscopy were used to characterize the phase purity, structural dimensions and elemental composition of the obtained structures respectively. Photoluminescence emission measurements showed a decrease in both the near band edge emission as well as the defect band emission upon addition of nickel and sulphur with different concentrations. This was attributed to increased charger-carrier-separation due to the presence of Ni-S material on ZnO surface, which is linked to improved charge transfer during photocatalytic reactions.

Keywords: Carrier-charge-separation, nickel, sulphur, zinc oxide, photoluminescence.

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Authors: Said Nurdin, Fatimah A. Misebah, Rosli M. Yunus, Mohd S. Mahmud, Ahmad Z. Sulaiman

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The discarded clam shell waste, fossil and edible oil as biolubricant feedstocks create environmental impacts and food chain dilemma, thus this work aims to circumvent these issues by using activated saltwater clam shell waste (SCSW) as solid catalyst for conversion of Jatropha curcas oil as non-edible sources to ester biolubricant. The characterization of solid catalyst was done by Differential Thermal Analysis-Thermo Gravimetric Analysis (DTATGA), X-Ray Fluorescence (XRF), X-Ray Diffraction (XRD), Brunauer-Emmett-Teller (BET), Field Emission Scanning Electron Microscopy (FESEM) and Fourier Transformed Infrared Spectroscopy (FTIR) analysis. The calcined catalyst was used in the transesterification of Jatropha oil to methyl ester as the first step, and the second stage was involved the reaction of Jatropha methyl ester (JME) with trimethylolpropane (TMP) based on the various process parameters. The formated biolubricant was analyzed using the capillary column (DB-5HT) equipped Gas Chromatography (GC). The conversion results of Jatropha oil to ester biolubricant can be found nearly 96.66%, and the maximum distribution composition mainly contains 72.3% of triester (TE).

Keywords: Conversion, ester biolubricant, Jatropha curcas oil, solid catalyst.

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Authors: Olga Długosz, Jolanta Pulit-Prociak, Marcin Banach

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The paper presents a process to obtain glutathione-modified titanium oxide nanoparticles. The processes were carried out in a microwave radiation field. The influence of the molar ratio of glutathione to titanium oxide and the effect of the fold of NaOH vs. stoichiometric amount on the size of the formed TiO2 nanoparticles was determined. The physicochemical properties of the obtained products were evaluated using dynamic light scattering (DLS), transmission electron microscope- energy-dispersive X-ray spectroscopy (TEM-EDS), low-temperature nitrogen adsorption method (BET), X-Ray Diffraction (XRD) and Fourier-transform infrared spectroscopy (FTIR) microscopy methods. The size of TiO2 nanoparticles was characterized from 30 nm to 336 nm. The release of titanium ions from the prepared products was evaluated. These studies were carried out using different media in which the powders were incubated for a specific time. These were: water, SBF and Ringer's solution. The release of titanium ions from modified products is weaker compared to unmodified titanium oxide nanoparticles. The reduced release of titanium ions may allow the use of such modified materials as substances in drug delivery systems.

Keywords: titanium dioxide, nanoparticles, drug carrier, glutathione

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Authors: Seifollah Bahramikia

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Amyloid aggregation of polypeptides is related to a growing number of pathologic states known as amyloid disorders. In recent years, blocking or reversing amyloid aggregation via the use of small compounds are considered as two useful approaches in hampering the development of these diseases. In this research, we have compared the ability of several manganese-salen derivatives, as synthetic compounds, and apigenin, as a natural flavonoid, to inhibit of hen egg-white lysozyme (HEWL) aggregation, as an in vitro model system. Different spectroscopic analyses such as Thioflavin T (ThT) and Anilinonaphthalene-8-sulfonic acid (ANS) fluorescence, Congo red (CR) absorbance along with transmission electron microscopy were used in this work to monitor the HEWL aggregation kinetic and inhibition. Our results demonstrated that both type of compounds were capable to prevent the formation of lysozyme amyloid aggregation in vitro. In addition, our data indicated that synthetic compounds had higher activity to inhibit of the β-sheet structures relative to natural compound. Regarding the higher antioxidant activities of the salen derivatives, it can be concluded that in addition to aromatic rings of each of the compounds, the potent antioxidant properties of salen derivatives contributes to lower lysozyme fibril accumulation.

Keywords: Aggregation, anti-amyloidogenic, apigenin, hen egg white lysozyme, salen derivatives.

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Authors: Mehran Bakhshi, Mohammad Raouf Hosseini, Mohammadhosein Rahimi

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The cadmium sulfide nanoparticles were synthesized from the nickel-cadmium cake of a hydrometallurgical zinc producing plant and sodium sulfide as Cd²⁺ and S^-2 sources, respectively. Also, the synthesis process was performed by using the secretions of Bacillus licheniformis as bio-surfactant. Initially, in order to obtain a cadmium rich solution, two following steps were carried out: 1) Alkaline leaching for the removal of zinc oxide from the cake, and 2) acidic leaching to dissolve cadmium from the remained solid residue. Afterward, the obtained CdSO₄ solution was used for the nanoparticle biosynthesis. Nanoparticles were characterized by the energy dispersive spectroscopy (EDS) and X-ray diffraction (XRD) to confirm the formation of CdS crystals with cubic structure. Also, transmission electron microscopy (TEM) was applied to determine the particle sizes which were in 2-10 nm range. Moreover, the presence of the protein containing bio-surfactants was approved by using infrared analysis (FTIR). In addition, the absorbance below 400 nm confirms quantum particles’ size. Finally, it was shown that valuable CdS quantum dots could be obtained from the industrial waste products via environment-friendly biological approaches.

Keywords: Biosynthesis, cadmium cake, cadmium sulfide, nanoparticle, zinc smelter.

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Authors: S. Al-Enezi, J. Samuel, A. Al-Banna

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Polymer based membranes are one of the low-cost technologies available for the gas separation. Three major elements required for a commercial gas separating membrane are high permeability, high selectivity, and good mechanical strength. Poly(vinylidene fluoride) (PVDF) is a commercially available fluoropolymer and a widely used membrane material in gas separation devices since it possesses remarkable thermal, chemical stability, and excellent mechanical strength. The PVDF membrane was chemically modified by soaking in different ionic liquids and dried. The thermal behavior of modified membranes was investigated by differential scanning calorimetry (DSC), and thermogravimetry (TGA), and the results clearly show the best affinity between the ionic liquid and the polymer support. The porous structure of the PVDF membranes was clearly seen in the scanning electron microscopy (SEM) images. The CO₂ permeability of blended membranes was explored in comparison with the unmodified matrix. The ionic liquid immobilized in the hydrophobic PVDF support exhibited good performance for separations of CO₂/N₂. The improved permeability of modified membrane (PVDF-IL) is attributed to the high concentration of nitrogen rich imidazolium moieties.

Keywords: PVDF, gas permeability, polymer membrane, ionic liquid.

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Authors: Sh. Sousani, Z. Shadrokh, M. Hofbauerová, J. Kollár, M. Jergel, V. Nádaždy, M. Omastová, E. Majková

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In this paper, we discuss the preparation and impact of post-treatment procedures, including purification, passivation, and ligand exchange, on the formation and stability of halide perovskite quantum dots (PQDs). CsPbBr3 quantum dots were synthesized via the conventional hot-injection method using cesium oleate, PbBr2, and oleylamine (OAm) & oleic acid (OA) and didodecyldimethylammonium bromide (DDAB) as ligands. Characterization by scanning transmission electron microscopy (STEM) confirms the QDs' cubic shape and monodispersity with an average size of 10-14 nm. The photoluminescent (PL) properties of perovskite quantum dots/CH3NH3PbI3 perovskite (PQDs/MAPI)  bilayers with OAm&OA and DDAB ligands spin coated on Indium Tin Oxide (ITO) substrate were explored. The impact of ligand type and oxygen plasma treatment on linear optical behaviour and PQDs/MAPI interface formation in ITO/PQDs/MAPI perovskite structures was examined. The obtained results have direct implications for selection of suitable ligands and processes for photovoltaic applications and enhancing their stability.

Keywords: Perovskite quantum dots, ligand exchange, photoluminescence, O3 plasma.

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Authors: Ezgi Dündar-Tekkaya, Nilgün Karatepe

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Carbon nanotubes (CNTs) with their high mechanical, electrical, thermal and chemical properties are regarded as promising materials for many different potential applications. Having unique properties they can be used in a wide range of fields such as electronic devices, electrodes, drug delivery systems, hydrogen storage, textile etc. Catalytic chemical vapor deposition (CCVD) is a common method for CNT production especially for mass production. Catalysts impregnated on a suitable substrate are important for production with chemical vapor deposition (CVD) method. Iron catalyst and MgO substrate is one of most common catalyst-substrate combination used for CNT. In this study, CNTs were produced by CCVD of acetylene (C2H2) on magnesium oxide (MgO) powder substrate impregnated by iron nitrate (Fe(NO3)3•9H2O) solution. The CNT synthesis conditions were as follows: at synthesis temperatures of 500 and 800°C multiwall and single wall CNTs were produced respectively. Iron (Fe) catalysts were prepared by with Fe:MgO ratio of 1:100, 5:100 and 10:100. The duration of syntheses were 30 and 60 minutes for all temperatures and catalyst percentages. The synthesized materials were characterized by thermal gravimetric analysis (TGA), transmission electron microscopy (TEM) and Raman spectroscopy.

Keywords: Carbon nanotube, catalyst, catalytic chemical vapordeposition, iron

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Authors: Hendriëtte van der Walt, Lesley Chown, Richard Harris, Ndabenhle Sosibo, Robert Tshikhudo

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The use of magnetic and magnetic/gold core/shell nanoparticles in biotechnology or medicine has shown good promise due to their hybrid nature which possesses superior magnetic and optical properties. Some of these potential applications include hyperthermia treatment, bio-separations, diagnostics, drug delivery and toxin removal. Synthesis refinement to control geometric and magnetic/optical properties, and finding functional surfactants for biomolecular attachment, are requirements to meet application specifics. Various high-temperature preparative methods were used for the synthesis of iron oxide and gold-coated iron oxide nanoparticles. Different surface functionalities, such as 11-aminoundecanoic and 11-mercaptoundecanoic acid, were introduced on the surface of the particles to facilitate further attachment of biomolecular functionality and drug-like molecules. Nanoparticle thermal stability, composition, state of aggregation, size and morphology were investigated and the results from techniques such as Fourier Transform-Infra Red spectroscopy (FT-IR), Ultraviolet visible spectroscopy (UV-vis), Transmission Electron Microscopy (TEM) and thermal analysis are discussed.

Keywords: Core/shell, Iron oxide, Gold coating, Nanoparticles.

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Authors: Amaneh Javid, Shahin Ahmadian, Ali A. Saboury, Saeed Rezaei-Zarchi

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This study determines the effect of naked and heparinbased super-paramagnetic iron oxide nanoparticles on the human cancer cell lines of A2780. Doxorubicin was used as the anticancer drug, entrapped in the SPIO-NPs. This study aimed to decorate nanoparticles with heparin, a molecular ligand for 'active' targeting of cancerous cells and the application of modified-nanoparticles in cancer treatment. The nanoparticles containing the anticancer drug DOX were prepared by a solvent evaporation and emulsification cross-linking method. The physicochemical properties of the nanoparticles were characterized by various techniques, and uniform nanoparticles with an average particle size of 110±15 nm with high encapsulation efficiencies (EE) were obtained. Additionally, a sustained release of DOX from the SPIO-NPs was successful. Cytotoxicity tests showed that the SPIO-DOX-HP had higher cell toxicity than the individual HP and confocal microscopy analysis confirmed excellent cellular uptake efficiency. These results indicate that HP based SPIO-NPs have potential uses as anticancer drug carriers and also have an enhanced anticancer effect.

Keywords: Heparin, A2780 cells, ovarian cancer, nanoparticles, doxorubicin.

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Authors: A. M. Metak, T. T. Ajaal

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Commercial nanocomposite food packaging type nano-silver containers were characterised using scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDX). The presence of nanoparticles consistent with the incorporation of 1% nano-silver (Ag) and 0.1% titanium dioxide (TiO₂) nanoparticle into polymeric materials formed into food containers was confirmed. Both nanomaterials used in this type of packaging appear to be embedded in a layered configuration within the bulk polymer. The dimensions of the incorporated nanoparticles were investigated using X-ray diffraction (XRD) and determined by calculation using the Scherrer Formula; these were consistent with Ag and TiO₂ nanoparticles in the size range 20-70nm both were spherical shape nanoparticles. Antimicrobial assessment of the nanocomposite container has also been performed and the results confirm the antimicrobial activity of Ag and TiO₂ nanoparticles in food packaging containers. Migration assessments were performed in a wide range of food matrices to determine the migration of nanoparticles from the packages. The analysis was based upon the relevant European safety Directives and involved the application of inductively coupled plasma mass spectrometry (ICP-MS) to identify the range of migration risk. The data pertain to insignificance levels of migration of Ag and TiO₂ nanoparticles into the selected food matrices.

Keywords: Nano-silver, antimicrobial food packaging, migration, titanium dioxide.

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Authors: L. Major, J. M. Lackner, M. Dyner, B. Major

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Development of new generation bio-tribological, multilayer coatings opens an avenue for fabrication of future hightech functional surfaces. In the presented work, nano-composite, Cr/CrN+[Cr/ a-C:H implanted by metallic nanocrystals] multilayer coatings have been developed for surface protection of medical tools. Thin films were fabricated by a hybrid Pulsed Laser Deposition technique. Complex microstructure analysis of nanomultilayer coatings, subjected to mechanical and biological tests, were performed by means of transmission electron microscopy (TEM). Microstructure characterization revealed the layered arrangement of Cr23C6 nanoparticles in multilayer structure. Influence of deposition conditions on bio-tribological properties of the coatings was studied. The bio-tests were used as a screening tool for the analyzed nanomultilayer coatings before they could be deposited on medical tools. Bio-medical tests were done using fibroblasts. The mechanical properties of the coatings were investigated by means of a ball-ondisc mechanical test. The micro hardness was done using Berkovich indenter. The scratch adhesion test was done using Rockwell indenter. From the bio-tribological point of view, the optimal properties had the C106_1 material.

Keywords: Bio-tribological coatings, cell-material interaction, hybrid PLD, tribology.

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Authors: C. S. Paglia

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The deformation and the crystallization in a 7075-T651 friction stir weld, in particular for regions directly in contact with the mechanical action of the rotating probe, have been investigated by means of optical microscopy. The investigation enabled to identify regions of the weld differently affected by the deformation caused by the welding process. The highly deformed grains in the horizontal direction close to the plate margin were indicative of shear movements along the horizontal plane, while highly deformed grains along the plate margin in the vertical direction were indicative of vertical shear movements of opposite directions, which superimposed the shear movement along the horizontal plane. The vertical shear movements were not homogeneous through the plate thickness. The microstructure indicated that after the probe passes, the grain growth may take place under static conditions. The small grains microstructure of the nugget region, formed after the main dynamic recrystallization process, develops to an equiaxed microstructure. A material transport influenced by the rotating shoulder was also observed from the trailing to the advancing side of the weld.

Keywords: AA7075-T651, friction stir welding, deformation, crystallization.

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Authors: M. J. Shivaram, Shashi Bhushan Arya, Jagannath Nayak, Bharat Bhooshan Panigrahi

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Titanium and its alloys have become more significant implant materials due to their mechanical properties, excellent biocompatibility and high corrosion resistance. Biomaterials can be produce by using the powder metallurgy (PM) methods and required properties can tailored by varying the processing parameters, such as ball milling time, space holder particles, and sintering temperature. The desired properties such as, structural and mechanical properties can be obtained by powder metallurgy method.  In the present study, deals with fabrication of solid and porous Ti-20Nb-5Ag alloy using high energy ball milling for different times (5 and 20 h). The resultant powder particles were used to fabricate solid and porous Ti-20Nb-5Ag alloy by adding space holder particles (NH₄HCO₃). The resultant powder particles, fabricated solid and porous samples were characterized by scanning electron microscopy (SEM). The compressive strength, elastic modulus and microhardness properties were investigated. Solid and porous Ti-20Nb-5Ag alloy samples showed good mechanical properties for 20 h ball milling time as compare to 5 h ball milling.

Keywords: Ball Milling, compressive strengths, microstructure, porous Titanium alloy.

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Authors: C. Sinescu, M. Negrutiu, M. Romînu, C. Haiduc, E. Petrescu, M. Leretter, A.G. Podoleanu

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Optical Coherence Tomography (OCT) combined with the Confocal Microscopy, as a noninvasive method, permits the determinations of materials defects in the ceramic layers depth. For this study 256 anterior and posterior metal and integral ceramic fixed partial dentures were used, made with Empress (Ivoclar), Wollceram and CAD/CAM (Wieland) technology. For each investigate area 350 slices were obtain and a 3D reconstruction was perform from each stuck. The Optical Coherent Tomography, as a noninvasive method, can be used as a control technique in integral ceramic technology, before placing those fixed partial dentures in the oral cavity. The purpose of this study is to evaluate the capability of En face Optical Coherence Tomography (OCT) combined with a fluorescent method in detection and analysis of possible material defects in metalceramic and integral ceramic fixed partial dentures. As a conclusion, it is important to have a non invasive method to investigate fixed partial prostheses before their insertion in the oral cavity in order to satisfy the high stress requirements and the esthetic function.

Keywords: Ceramic Fixed Partial Dentures, Material Defects, En face Optical Coherence Tomography, Fluorescence.

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Authors: Harald Rojacz, Markus Varga, Horst Winkelmann

Abstract:

Within this work High Temperature Single Impact Studies were performed to evaluate deformation mechanisms at different energy and momentum levels. To show the influence of different microstructures and hardness levels and their response to single impacts four different materials were tested at various temperatures up to 700°C. One carbide reinforced NiCrBSi based Metal Matrix Composite and three different steels were tested. The aim of this work is to determine critical energies for fracture appearance and the materials response at different energy and momenta levels. Critical impact loadings were examined at elevated temperatures to limit operating conditions in impact dominated regimes at elevated temperatures. The investigations on the mechanisms were performed using different means of microscopy at the surface and in metallographic cross sections. Results indicate temperature dependence of the occurrence of cracks in hardphase rich materials, such as Metal Matrix Composites High Speed Steels and the influence of different impact momenta at constant energies on the deformation of different steels.

Keywords: Deformation, High Temperature, Metal Matrix Composite, Single Impact Test, Steel.

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Authors: Dionisios Panagiotaras, Dimitrios Papoulis, Elias Stathatos

Abstract:

Microfibrous palygorskite and tubular halloysite clay mineral combined with nanocrystalline TiO₂ are incorporating in the preparation of nanocomposite films on glass substrates via sol-gel route at 450^oC. The synthesis is employing nonionic surfactant molecule as pore directing agent along with acetic acid-based sol-gel route without addition of water molecules. Drying and thermal treatment of composite films ensure elimination of organic material lead to the formation of TiO₂ nanoparticles homogeneously distributed on the palygorskite or halloysite surfaces. Nanocomposite films without cracks of active anatase crystal phase on palygorskite and halloysite surfaces are characterized by microscopy techniques, UV-Vis spectroscopy, and porosimetry methods in order to examine their structural properties.

The composite palygorskite-TiO₂ and halloysite-TiO₂ films with variable quantities of palygorskite and halloysite were tested as photocatalysts in the photo-oxidation of Basic Blue 41 azo dye in water. These nanocomposite films proved to be most promising photocatalysts and highly effective to dye’s decoloration in spite of small amount of palygorskite-TiO₂ or halloysite-TiO₂ catalyst immobilized onto glass substrates mainly due to the high surface area and uniform distribution of TiO₂ on clay minerals avoiding aggregation.

Keywords: Halloysite, Palygorskite, Photocatalysis, Titanium Dioxide.

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Authors: Megha Rao, Søren H. Jensen, Xiufu Sun, Anke Hagen, Mogens B. Mogensen

Abstract:

Solid oxide electrolysis cells have an immense potential in converting CO₂ and H₂O into syngas during co-electrolysis operation. The produced syngas can be further converted into hydrocarbons. This kind of technology is called power-to-gas or power-to-liquid. To produce hydrocarbons via this route, durability of the cells is still a challenge, which needs to be further investigated in order to improve the cells. In this work, various nickel-yttria stabilized zirconia (Ni-YSZ) fuel electrode supported or YSZ electrolyte supported cells, cerium gadolinium oxide (CGO) barrier layer, and an oxygen electrode are investigated for durability under co-electrolysis conditions in both galvanostatic and potentiostatic conditions. While changing the gas on the oxygen electrode, keeping the fuel electrode gas composition constant, a change in the gas concentration arc was observed by impedance spectroscopy. Measurements of open circuit potential revealed the presence of leaks in the setup. It is speculated that the change in concentration impedance may be related to the leaks. Furthermore, the cells were also tested under pressurized conditions to find an inter-play between the leak rate and the pressure. A mathematical modeling together with electrochemical and microscopy analysis is presented.

Keywords: Co-electrolysis, solid oxide electrolysis cells, leaks, durability, gas concentration.

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Authors: A. Srion, W. Thepsuwan, N. Monmaturapoj

Abstract:

Two Lithium Disilicate (LD) glass ceramics based on SiO2-Li2O-K2O-Al2O3 system were prepared through a glass melting method. The glass rods were then fabricated into dental crowns via a hot pressing at 900˚C and 850˚C in order to study the effect of the pressing temperatures on the phase formation and microstructure of the glasses. Different samples of as cast glass and heat treated samples (600˚C and 700˚C) were used to press for investigating the effect of an initial microstructure on the hot pressing technique. Xray diffraction (XRD) and scanning electron microscopy (SEM) were performed to determine the phase formation and microstructure of the samples, respectively. XRD results show that the main crystalline structure was Li2Si2O5 by having Li3PO4, Li0.6Al0.6Si2O6, Li2SiO3, Ca5 (PO4)3F and SiO2 as minor phases. Glass compositions with different heat treatment temperatures exhibited a difference phase formations but have less effect during pressing. SEM micrographs showed the microstructure of Li2Si2O5 as lath-like shape in all glasses. With increasing the initial heat treatment temperature, the longer the lath-like crystals of lithium disilicate were increased especially when using glass heat treatment at 700˚C followed by pressing at 900˚C. This could be suggested that LD1 heat treatment at 700˚C which pressing at 900˚C presented the best formation by the hot pressing and compiled microstructure.

Keywords: Lithium disilicate, Hot pressing, Dental crown, Microstructure.

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