Commenced in January 2007
Frequency: Monthly
Edition: International
Paper Count: 26

Thermal Stability Related Abstracts

26 Investigation of Microstructure, Mechanical Properties and Anti-Corrosive Behavior of Al2O3/Cr2O3 Nanocomposite on Zn Rich Bath

Authors: N. Malatji, A. P. I. Popoola


Zn-Al2O3 and Cr2O3 nanocomposite coatings were successfully produced by electrodeposition technique from chloride acidic bath. Particle loading of Al2O3 (50nm) particles were varied from 5-10 g/L and for Cr2O3(100nm) was 10-20 g/L. Scanning electron microscope (SEM) affixed with energy dispersive spectrometry was used to study the surface morphology and content of the nanoparticles incorporated into the coatings. Microhardness, thermal stability, wear and corrosion behavior of the coatings were also evaluated to study the effect of these nanoparticles on these properties. Zn-Al2O3 nanocomposite was found to exhibit good surface properties especially corrosion resistance. On the other side, Cr2O3 incorporation resulted in the improvement of only mechanical properties. Therefore, Zn-Al2O3 proved to be a better coating for most industrial applications where both chemical and mechanical properties are required.

Keywords: Corrosion, Tribology, Thermal Stability, Nanocomposite Coatings, electrodeposition

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25 Mechanical Properties of Kenaf Reinforced Composite with Different Fiber Orientation

Authors: Y. C. Ching, K. H. Chong


The increasing of environmental awareness has led to grow interest in the expansion of materials with eco-friendly attributes. In this study, a 3 ply sandwich layer of kenaf fiber reinforced unsaturated polyester with various fiber orientations was developed. The effect of the fiber orientation on mechanical and thermal stability properties of polyester was studied. Unsaturated polyester as a face sheets and kenaf fibers as a core was fabricated with combination of hand lay-up process and cold compression method. Tested result parameters like tensile, flexural, impact strength, melting point, and crystallization point were compared and recorded based on different fiber orientation. The failure mechanism and property changes associated with directional change of fiber to polyester composite were discussed.

Keywords: Thermal Stability, tensile, kenaf fiber, polyester

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24 Economic Viability of Using Guar Gum as a Viscofier in Water Based Drilling Fluids

Authors: Devesh Motwani, Amey Kashyap


Interest in cost effective drilling has increased substantially in the past years. Economics associated with drilling fluids is needed to be considered seriously for lesser cost per foot in planning and drilling of a wellbore and the various environmental concerns imposed by international communities related with the constituents of the drilling fluid. Viscofier such as Guar Gum is a high molecular weight polysaccharide from Guar plants, is used to increase viscosity in water-based and brine-based drilling fluids thus enabling more efficient cleaning of the bore. Other applications of this Viscofier are to reduce fluid loss by giving a better colloidal solution, decrease fluid friction and so minimising power requirements and used in hydraulic fracturing to increase the recovery of oil and gas. Guar gum is also used as a surfactant, synthetic polymer and defoamer. This paper presents experimental results to verifying the properties of guar gum as a viscofier and filtrate retainer as well as observing the impact of different quantities of guar gum and Carboxymethyl cellulose (CMC) in a standard sample of water based bentonite mud solution. This is in attempt to make a drilling fluid which contains half of the quantity of drilling mud used and yet is equally viscous to the standardised mud sample. Thus we can see that mud economics will be greatly affected by this approach. However guar gum is thermally stable till 60-65°C thus limited to be used in drilling shallow wells and for a wider thermal range, suitable chrome free additives are required.

Keywords: Economics, Thermal Stability, CMC, guargum, viscofier

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23 Nanocrystalline Cellulose from Oil Palm Fiber

Authors: Ridzuan Ramli, Rosli M. Yunus, Mohammad Dalour Beg, Zianor Azrina Zianon Abdin


Nanocrystalline cellulose (NCC) were produced by using the ultrasound assisted acid hydrolysis from oil palm empty fruit bunch (EFB) pulp with different hydrolysis time then were analyzed by using FESEM and TGA as in comparison with EFB fiber and EFB pulp. Based on the FESEM analysis, it was found that NCC has a rod like shaped under the acid hydrolysis with an assistant of ultrasound. According to thermal stability, the NCC obtained show remarkable sign of high thermal stability compared to EFB fiber and EFB pulp. However, as the hydrolysis time increase, the thermal stability of NCC was deceased. As in conclusion, the NCC can be prepared by using ultrasound assisted acid hydrolysis. The NCC obtained have good thermal stability and have a great potential as the reinforcement in composite materials.

Keywords: Morphology, Thermal Stability, empty fruit bunch (EFB), Nanocrystalline cellulose, ultrasound assisted acid hydrolysis

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22 Thermal Expansion Coefficient and Young’s Modulus of Silica-Reinforced Epoxy Composite

Authors: Gyo Woo Lee, Hyu Sang Jo


In this study, the evaluation of thermal stability of the micrometer-sized silica particle reinforced epoxy composite was carried out through the measurement of thermal expansion coefficient and Young’s modulus of the specimens. For all the specimens in this study from the baseline to those containing 50 wt% silica filler, the thermal expansion coefficients and the Young’s moduli were gradually decreased down to 20% and increased up to 41%, respectively. The experimental results were compared with filler-volume-based simple empirical relations. The experimental results of thermal expansion coefficients correspond with those of Thomas’s model which is modified from the rule of mixture. However, the measured result for Young’s modulus tends to be increased slightly. The differences in increments of the moduli between experimental and numerical model data are quite large.

Keywords: Thermal Stability, silica-reinforced, epoxy composite, coefficient of thermal expansion, empirical model

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21 Microwave Assisted Synthesis and Metal Complexes of Some Copolymers Based on Itaconic Acid

Authors: Mohamed H. El-Newehy, Sameh M. Osman, Moamen S. Refat, Salem S. Al-Deyab, Ayman El-Faham


The two copolymers itaconic acid-methyl methacrylate and itaconic acid-acrylamide have been prepared in different ratio by radical copolymerization in the presence of azobisisobutyronitrile (AIBN) as initiator and using 2-butanone as reaction medium using microwave irradiation. The microwave technique is safe, fast, and gives high yield of the products with high purity in an optimum time, comparing to the traditional conventional heating. All the prepared copolymers were characterized by FT-IR, thermal analysis and elemental microanalysis. The itaconic acid-based copolymers showed a good sensitivity in alkaline media for scavenging Cu (II) and Pb (II). The chelation behavior of both Cu (II) and Pb (II) complexes were checked using FT-IR, thermogravimetric analysis (TGA), and differential scanning calorimetery (DSC). The infrared data are in a good agreement with the coordination through carboxylate-to-metal, in which the copolymers acting as a bidentate ligand.

Keywords: Thermal Stability, microwave synthesis, itaconic acid, copolymerization, scavenging

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20 Properties of Poly(Amide-Imide) with Low Residual Stress for Electronic Material

Authors: Kwangin Kim, Taewon Yoo, Haksoo Han


Polyimide is a superior polymer in the electronics industry, and we conducted a study to synthesize poly(amide-imide) at low temperatures. Poly(amide-imide) was synthesized at low-temperature curing to offer a thermal stable membrane with low residual stress and good processability. As a result, the low crack polymer with good processability could be used to various applications such as semiconductors, integrated circuits, coating materials, membranes, and display. The synthesis of poly(amide-imide) at low temperatures was confirmed by Fourier transform infrared spectroscopy (FT-IR). Thermal stabilities of the polymer was confirmed by thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC).

Keywords: Thermal Stability, Residual Stress, poly(amide-imide)

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19 Sintered Phosphate Cement for HLW Encapsulation

Authors: S. M. M. Nelwamondo, W. C. M. H. Meyer, H. Krieg


The presence of volatile radionuclides in high level waste (HLW) in the nuclear industry limits the use of high temperature encapsulation technologies (glass and ceramic). Chemically bonded phosphate cement (CBPC) matrixes can be used for encapsulation of low level waste. This waste form is however not suitable for high level waste due to the radiolysis of water in these matrixes. In this research, the sintering behavior of the magnesium potassium phosphate cement waste forms was investigated. The addition of sintering aids resulted in the sintering of these phosphate cement matrixes into dense monoliths containing no water. Experimental evidence will be presented that this waste form can now be considered as a waste form for volatile radionuclides and high level waste as radiation studies indicated no chemical phase transition or physical degradation of this waste form.

Keywords: Thermal Stability, radiation stability, chemically bonded phosphate cements, HLW encapsulation

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18 Preparation and Flame-Retardant Properties of Epoxy Resins Containing Organophosphorus Compounds

Authors: Tachita Vlad-Bubulac, Ionela-Daniela Carja, Diana Serbezeanu, Corneliu Hamciuc, Vicente Javier Forrat Perez


The present work describes the preparation of new organophosphorus compounds with high content of phosphorus followed by the incorporation of these compounds into epoxy resin systems in order to investigate the phosphorus effect in terms of thermal stability, flame-retardant and mechanical properties of modified epoxy resins. Thus, two new organophosphorus compounds have been synthesized and fully characterized. 6-Oxido-6H-dibenz[c,e][1,2]oxaphosphorinyl-phenylcarbinol has been prepared by the addition reaction of P–H group of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide to carbonyl group of benzaldehyde. By treating the phenylcarbinol derivative with POCl3 a new phosphorus compound was obtained, having a content of 12.227% P. The organophosphorus compounds have been purified by recrystallization while their chemical structures have been confirmed by melting point measurements, FTIR and HNMR spectroscopies. In the next step various flame-retardant epoxy resins with different content of phosphorus have been prepared starting from a commercial epoxy resin and using dicyandiamide (DICY) as a latent curing agent in the presence of an accelerator. Differential scanning calorimetry (DSC) has been applied to investigate the behavior and kinetics of curing process of thermosetting systems. The results showed that the best curing characteristic and glass transition temperature are obtained at a ratio of epoxy resin: DICY: accelerator equal to 94:5:1. The thermal stability of the phosphorus-containing epoxy resins was investigated by thermogravimetric analysis in nitrogen and air, DSC, SEM and LOI test measurements.

Keywords: Thermal Stability, epoxy resins, flame retardant properties, phosphorus-containing compounds

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17 Advanced Phosphorus-Containing Polymer Materials towards Eco-Friendly Flame Retardant Epoxy Thermosets

Authors: Tachita Vlad-Bubulac, Ionela-Daniela Carja, Diana Serbezeanu, Corneliu Hamciuc


Nowadays, epoxy materials are extensively used in ever more areas and under ever more demanding environmental conditions due to their remarkable combination of properties, light weight and ease of processing. However, these materials greatly increase the fire risk due to their flammability and possible release of toxic by-products as a result of their chemical composition which consists mainly from carbon and hydrogen atoms. Therefore, improving the fire retardant behaviour to prevent the loss of life and property is of particular concern among government regulatory bodies, consumers and manufacturers alike. Modification of epoxy resins with organophosphorus compounds, as reactive flame retardants or additives, is the key to achieving non-flammable advanced epoxy materials. Herein, a detailed characterization of fire behaviour for a series of phosphorus-containing epoxy thermosets is reported. A carefully designed phosphorus flame retardant additive was simply blended with a bifunctional bisphenol-A based epoxy resin. Further thermal cross-linking in the presence of various aminic hardeners led to eco-friendly flame retardant epoxy resins. The type of hardener, concentration of flame retardant additive, compatibility between the components of the mixture, char formation and morphology, thermal stability, flame retardant mechanisms were investigated. It was found that even a very low content of phosphorus introduced into the epoxy matrix increased the limiting oxygen index value to about 30%. In addition, the peak of the heat release rate value decreased up to 45% as compared to the one of the neat epoxy system. The main flame retardant mechanism was the condensed-phase one as revealed by SEM and XPS measurements.

Keywords: Thermal Stability, epoxy resin, condensed-phase mechanism, eco-friendly phosphorus flame retardant

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16 Organic Thin-Film Transistors with High Thermal Stability

Authors: Sibani Bisoyi, Ute Zschieschang, Alexander Hoyer, Hagen Klauk


Abstract— Organic thin-film transistors (TFTs) have great potential to be used for various applications such as flexible displays or sensors. For some of these applications, the TFTs must be able to withstand temperatures in excess of 100 °C, for example to permit the integration with devices or components that require high process temperatures, or to make it possible that the devices can be subjected to the standard sterilization protocols required for biomedical applications. In this work, we have investigated how the thermal stability of low-voltage small-molecule semiconductor dinaphtho[2,3-b:2’,3’-f]thieno[3,2-b]thiophene (DNTT) TFTs is affected by the encapsulation of the TFTs and by the ambient in which the thermal stress is performed. We also studied to which extent the thermal stability of the TFTs depends on the channel length. Some of the TFTs were encapsulated with a layer of vacuum-deposited Teflon, while others were left without encapsulation, and the thermal stress was performed either in nitrogen or in air. We found that the encapsulation with Teflon has virtually no effect on the thermal stability of our TFTs. In contrast, the ambient in which the thermal stress is conducted was found to have a measurable effect, but in a surprising way: When the thermal stress is carried out in nitrogen, the mobility drops to 70% of its initial value at a temperature of 160 °C and to close to zero at 170 °C, whereas when the stress is performed in air, the mobility remains at 75% of its initial value up to a temperature of 160 °C and at 60% up to 180 °C. To understand this behavior, we studied the effect of the thermal stress on the semiconductor thin-film morphology by scanning electron microscopy. While the DNTT films remain continuous and conducting when the heating is carried out in air, the semiconductor morphology undergoes a dramatic change, including the formation of large, thick crystals of DNTT and a complete loss of percolation, when the heating is conducted in nitrogen. We also found that when the TFTs are heated to a temperature of 200 °C in air, all TFTs with a channel length greater than 50 µm are destroyed, while TFTs with a channel length of less than 50 µm survive, whereas when the TFTs are heated to the same temperature (200 °C) in nitrogen, only the TFTs with a channel smaller than 8 µm survive. This result is also linked to the thermally induced changes in the semiconductor morphology.

Keywords: encapsulation, Thermal Stability, organic thin-film transistors, thin-film morphology

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15 QSAR Study on Diverse Compounds for Effects on Thermal Stability of a Monoclonal Antibody

Authors: Olubukayo-Opeyemi Oyetayo, Oscar Mendez-Lucio, Andreas Bender, Hans Kiefer


The thermal melting curve of a protein provides information on its conformational stability and could provide cues on its aggregation behavior. Naturally-occurring osmolytes have been shown to improve the thermal stability of most proteins in a concentration-dependent manner. They are therefore commonly employed as additives in therapeutic protein purification and formulation. A number of intertwined and seemingly conflicting mechanisms have been put forward to explain the observed stabilizing effects, the most prominent being the preferential exclusion mechanism. We attempted to probe and summarize molecular mechanisms for thermal stabilization of a monoclonal antibody (mAb) by developing quantitative structure-activity relationships using a rationally-selected library of 120 osmolyte-like compounds in the polyhydric alcohols, amino acids and methylamines classes. Thermal stabilization potencies were experimentally determined by thermal shift assays based on differential scanning fluorimetry. The cross-validated QSAR model was developed by partial least squares regression using descriptors generated from Molecular Operating Environment software. Careful evaluation of the results with the use of variable importance in projection parameter (VIP) and regression coefficients guided the selection of the most relevant descriptors influencing mAb thermal stability. For the mAb studied and at pH 7, the thermal stabilization effects of tested compounds correlated positively with their fractional polar surface area and inversely with their fractional hydrophobic surface area. We cannot claim that the observed trends are universal for osmolyte-protein interactions because of protein-specific effects, however this approach should guide the quick selection of (de)stabilizing compounds for a protein from a chemical library. Further work with a large variety of proteins and at different pH values would help the derivation of a solid explanation as to the nature of favorable osmolyte-protein interactions for improved thermal stability. This approach may be beneficial in the design of novel protein stabilizers with optimal property values, especially when the influence of solution conditions like the pH and buffer species and the protein properties are factored in.

Keywords: Monoclonal Antibodies, Thermal Stability, osmolytes, quantitative structure-activity relationships

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14 3D Interpenetrated Network Based on 1,3-Benzenedicarboxylate and 1,2-Bis(4-Pyridyl) Ethane

Authors: Laura Bravo-García, Gotzone Barandika, Begoña Bazán, M. Karmele Urtiaga, Luis M. Lezama, María I. Arriortua


Solid coordination networks (SCNs) are materials consisting of metal ions or clusters that are linked by polyfunctional organic ligands and can be designed to form tridimensional frameworks. Their structural features, as for example high surface areas, thermal stability, and in other cases large cavities, have opened a wide range of applications in fields like drug delivery, host-guest chemistry, biomedical imaging, chemical sensing, heterogeneous catalysis and others referred to greenhouse gases storage or even separation. In this sense, the use of polycarboxylate anions and dipyridyl ligands is an effective strategy to produce extended structures with the needed characteristics for these applications. In this context, a novel compound, [Cu4(m-BDC)4(bpa)2DMF]•DMF has been obtained by microwave synthesis, where m-BDC is 1,3-benzenedicarboxylate and bpa 1,2-bis(4-pyridyl)ethane. The crystal structure can be described as a three dimensional framework formed by two equal, interpenetrated networks. Each network consists of two different CuII dimers. Dimer 1 have two coppers with a square pyramidal coordination, and dimer 2 have one with a square pyramidal coordination and other with octahedral one, the last dimer is unique in literature. Therefore, the combination of both type of dimers is unprecedented. Thus, benzenedicarboxylate ligands form sinusoidal chains between the same type of dimers, and also connect both chains forming these layers in the (100) plane. These layers are connected along the [100] direction through the bpa ligand, giving rise to a 3D network with 10 Å2 voids in average. However, the fact that there are two interpenetrated networks results in a significant reduction of the available volume. Structural analysis was carried out by means of single crystal X-ray diffraction and IR spectroscopy. Thermal and magnetic properties have been measured by means of thermogravimetry (TG), X-ray thermodiffractometry (TDX), and electron paramagnetic resonance (EPR). Additionally, CO2 and CH4 high pressure adsorption measurements have been carried out for this compound.

Keywords: Thermal Stability, Magnetic Measurements, gas adsorption, interpenetrated networks, solid coordination network (SCN)

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13 Simultaneous Measurement of Pressure and Temperature Profile of Lubricating Oil-Film along Orthogonally Displaced Non-Circular Journal Bearing: An Experimental Study

Authors: Amit Chauhan, Amit Singla


The non-circular journal bearings provide better thermal stability and lesser oil-film temperature rise as compared to circular journal bearings. Experimentation on simultaneous measurement of pressure and temperature of lubricated oil-film along the profile of the bearing will help the designer to design journal bearings. In this paper, pressure and temperature of oil-film along orthogonally displaced non-circular journal bearing have been measured on a designed journal bearing test rig. The orthogonal non-circular journal bearing has been fabricated by displacing two circular halves away from the centers in the orthogonal direction. The data acquisition for oil film pressure and temperature has been carried out at journal speed=3000 rpm and by increasing the static radial load from 500 N to 2000 N in steps of 500 N using three different grades of oil (ISOVG 32, 68, and 150) named as oil-1, oil-2, and oil-3 respectively. The results show that the oil-film pressure and temperature increases with increase in radial load and change of lubricating oil towards increasing viscosity. Further, two lobes in the pressure and temperature profiles have been obtained which accounts for better thermal stability as it reduces cavitation zone inside the bearing.

Keywords: cavitation, Thermal Stability, non-circular journal bearing, orthogonally displaced

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12 Synthesis and Characterization of Poly (N-(Pyridin-2-Ylmethylidene)Pyridin-2-Amine: Thermal and Conductivity Properties

Authors: Nuray Yılmaz Baran


The conjugated Schiff base polymers which are also called as polyazomethines are promising materials for various applications due to their good thermal resistance semiconductive, liquid crystal, fiber forming, nonlinear optical outstanding photo- and electroluminescence and antimicrobial properties. In recent years, polyazomethines have attracted intense attention of researchers especially due to optoelectronic properties which have made its usage possible in organic light emitting diodes (OLEDs), solar cells (SCs), organic field effect transistors (OFETs), and photorefractive holographic materials (PRHMs). In this study, N-(pyridin-2-ylmethylidene)pyridin-2-amine Schiff base was synthesized from condensation reaction of 2-aminopyridine with 2-pyridine carbaldehyde. Polymerization of Schiff base was achieved by polycondensation reaction using NaOCl oxidant in methanol medium at various time and temperatures. The synthesized Schiff base monomer and polymer (Poly(N-(pyridin-2-ylmethylidene)pyridin-2-amine)) was characterized by UV-vis, FT-IR, 1H-NMR, XRD techniques. Molecular weight distribution and the surface morphology of the polymer was determined by GPC and SEM-EDAX techniques. Thermal behaviour of the monomer and polymer was investigated by TG/DTG, DTA and DSC techniques.

Keywords: Thermal Stability, polyazomethines, polycondensation reaction, Schiff base polymers

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11 Synthesis and Characterization of Poly(2-[[4-(Dimethylamino)Benzylidene] Amino]Phenol) in Organic Medium: Investigation of Thermal Stability, Conductivity, and Antimicrobial Properties

Authors: Mehmet Saçak, Nuray Yilmaz Baran


Schiff base polymers are one class of conjugated polymers, also called as poly(azomethines). They have drawn the attention of researchers in recent years due to their some properties such as, optoelectronic, semiconductive, and photovoltaic, antimicrobial activities and high thermal stability. In this study, Poly(2-[[4-(dimethylamino)benzylidene]amino] phenol) P(2-DBAP), which is a Schiff base polymer, was synthesized by an oxidative polycondensation reaction of -[[4-(dimethylamino)benzylidene]amino]phenol (2-DBAP) with oxidants NaOCl, H₂O₂ and O₂ in various organic medium. At the end of the polymerizations carried out at various temperatures and time, maximum conversion of the monomer to the polymer could be obtained as around 93.7 %. The structures of the monomer and polymer were characterized by UV-Vis, FTIR and ¹HNMR techniques. Thermal analysis of the polymer was identified by TG-DTG and DTA techniques, and the thermal degradation behavior was supported by Thermo-IR spectra recorded in the temperature range of 25-800 °C. The number average molecular weight (Mn), weight average molecular weight (Mw) and polydispersity index (PDI) of the polymer were found to be 26337, 9860 g/mol 2.67, respectively. The change of electrical conductivity value of the P(2-DBAP) doped with iodine vapor at different temperatures and time was investigated its maximum was measured by increasing 10¹⁰ fold as 2 x10⁻⁴ Scm⁻¹ after doping for 48 h at 60 °C. Antibacterial and antifungal activities of P(2-DBAP) Schiff base and its polymer were also investigated against Sarcina lutea, Enterobacter aerogenes, Escherichia coli, Enterococcus Faecalis, Klebsiella pneumoniae, Bacillus subtilis, and Candida albicans, Saccharomyces cerevisiae, respectively.

Keywords: Thermal Stability, polyazomethines, polycondensation reaction, Schiff base polymers, conductive properties

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10 Topographic and Thermal Analysis of Plasma Polymer Coated Hybrid Fibers for Composite Applications

Authors: Hande Yavuz, Grégory Girard, Jinbo Bai


Manufacturing of hybrid composites requires particular attention to overcome various critical weaknesses that are originated from poor interfacial compatibility. A large number of parameters have to be considered to optimize the interfacial bond strength either to avoid flaw sensitivity or delamination that occurs in composites. For this reason, surface characterization of reinforcement phase is needed in order to provide necessary data to drive an assessment of fiber-matrix interfacial compatibility prior to fabrication of composite structures. Compared to conventional plasma polymerization processes such as radiofrequency and microwave, dielectric barrier discharge assisted plasma polymerization is a promising process that can be utilized to modify the surface properties of carbon fibers in a continuous manner. Finding the most suitable conditions (e.g., plasma power, plasma duration, precursor proportion) for plasma polymerization of pyrrole in post-discharge region either in the presence or in the absence of p-toluene sulfonic acid monohydrate as well as the characterization of plasma polypyrrole coated fibers are the important aspects of this work. Throughout the current investigation, atomic force microscopy (AFM) and thermogravimetric analysis (TGA) are used to characterize plasma treated hybrid fibers (CNT-grafted Toray T700-12K carbon fibers, referred as T700/CNT). TGA results show the trend in the change of decomposition process of deposited polymer on fibers as a function of temperature up to 900 °C. Within the same period of time, all plasma pyrrole treated samples began to lose weight with relatively fast rate up to 400 °C which suggests the loss of polymeric structures. The weight loss between 300 and 600 °C is attributed to evolution of CO2 due to decomposition of functional groups (e.g. carboxyl compounds). With keeping in mind the surface chemical structure, the higher the amount of carbonyl, alcohols, and ether compounds, the lower the stability of deposited polymer. Thus, the highest weight loss is observed in 1400 W 45 s pyrrole+pTSA.H2O plasma treated sample probably because of the presence of less stable polymer than that of other plasma treated samples. Comparison of the AFM images for untreated and plasma treated samples shows that the surface topography may change on a microscopic scale. The AFM image of 1800 W 45 s treated T700/CNT fiber possesses the most significant increase in roughening compared to untreated T700/CNT fiber. Namely, the fiber surface became rougher with ~3.6 fold that of the T700/CNT fiber. The increase observed in surface roughness compared to untreated T700/CNT fiber may provide more contact points between fiber and matrix due to increased surface area. It is believed to be beneficial for their application as reinforcement in composites.

Keywords: Thermal Stability, surface roughness, hybrid fibers, surface characterization

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9 Effect of Manganese Doping on Ferrroelectric Properties of (K0.485Na0.5Li0.015)(Nb0.98V0.02)O3 Lead-Free Piezoceramic

Authors: K. Chandramani Singh, Chongtham Jiten, Radhapiyari Laishram


Alkaline niobate (Na0.5K0.5)NbO3 ceramic system has attracted major attention in view of its potential for replacing the highly toxic but superior lead zirconate titanate (PZT) system for piezoelectric applications. Recently, a more detailed study of this system reveals that the ferroelectric and piezoelectric properties are optimized in the Li- and V-modified system having the composition (K0.485Na0.5Li0.015)(Nb0.98V0.02)O3. In the present work, we further study the pyroelectric behaviour of this composition along with another doped with Mn4+. So, (K0.485Na0.5Li0.015)(Nb0.98V0.02)O3 + x MnO2 (x = 0, and 0.01 wt. %) ceramic compositions were synthesized by conventional ceramic processing route. X-ray diffraction study reveals that both the undoped and Mn4+-doped ceramic samples prepared crystallize into a perovskite structure having orthorhombic symmetry. Dielectric study indicates that Mn4+ doping has little effect on both the Curie temperature (Tc) and tetragonal-orthorhombic phase transition temperature (Tot). The bulk density, room-temperature dielectric constant (εRT), and room-c The room-temperature coercive field (Ec) is observed to be lower in Mn4+ doped sample. The detailed analysis of the P-E hysteresis loops over the range of temperature from about room temperature to Tot points out that enhanced ferroelectric properties exist in this temperature range with better thermal stability for the Mn4+ doped ceramic. The study reveals that small traces of Mn4+ can modify (K0.485Na0.5Li0.015)(Nb0.98V0.02)O3 system so as to improve its ferroelectric properties with good thermal stability over a wide range of temperature.

Keywords: sintering, Ceramics, Thermal Stability, dielectric properties, ferroelectric properties, lead-free

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8 Fabrication of Titanium Diboride-Based High Emissive Paint Coating Using Economical Dip Coating Method for High Temperature Applications

Authors: Atasi Dan, Kamanio Chattopadhyay, Bikramjit Basu


A cost-effective titanium diboride (TiB2) paint coating has been developed on stainless steel substrate using commercially available polyvinylpyrrolidone as a binder by convenient dip-coating technique. The emittance of the coating has been explored by tailoring various process parameters to obtain highest thermal radiation. The optimized coating has achieved a high thermal emittance of 0.85. In addition, the coating exhibited an excellent thermal stability while heat-treated at 500 °C in air. Along with the emittance, the structural and physical properties of the As-deposited and heat-treated coatings have been investigated systematically. The high temperature annealing has not affected the emittance, chemical composition and morphology of the coating significantly. Hence, the fabricated paint coating is expected to open up new possibilities for using it as a low-cost, thermally stable emitter in high temperature applications.

Keywords: Thermal Stability, paint coating, titanium diboride, emittance

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7 Hazardous Effects of Metal Ions on the Thermal Stability of Hydroxylammonium Nitrate

Authors: Shweta Hoyani, Charlie Oommen


HAN-based liquid propellants are perceived as potential substitute for hydrazine in space propulsion. Storage stability for long service life in orbit is one of the key concerns for HAN-based monopropellants because of its reactivity with metallic and non-metallic impurities which could entrain from the surface of fuel tanks and the tubes. The end result of this reactivity directly affects the handling, performance and storability of the liquid propellant. Gaseous products resulting from the decomposition of the propellant can lead to deleterious pressure build up in storage vessels. The partial loss of an energetic component can change the ignition and the combustion behavior and alter the performance of the thruster. The effect of largely plausible metals- iron, copper, chromium, nickel, manganese, molybdenum, zinc, titanium and cadmium on the thermal decomposition mechanism of HAN has been investigated in this context. Studies involving different concentrations of metal ions and HAN at different preheat temperatures have been carried out. Effect of metal ions on the decomposition behavior of HAN has been studied earlier in the context of use of HAN as gun propellant. However the current investigation pertains to the decomposition mechanism of HAN in the context of use of HAN as monopropellant for space propulsion. Decomposition onset temperature, rate of weight loss, heat of reaction were studied using DTA- TGA and total pressure rise and rate of pressure rise during decomposition were evaluated using an in-house built constant volume batch reactor. Besides, reaction mechanism and product profile were studied using TGA-FTIR setup. Iron and copper displayed the maximum reaction. Initial results indicate that iron and copper shows sensitizing effect at concentrations as low as 50 ppm with 60% HAN solution at 80°C. On the other hand 50 ppm zinc does not display any effect on the thermal decomposition of even 90% HAN solution at 80°C.

Keywords: Thermal Stability, hydroxylammonium nitrate, monopropellant, reaction mechanism

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6 Stability of Porous SiC Based Materials under Relevant Conditions of Radiation and Temperature

Authors: Marta Malo, Carlota Soto, Carmen García-Rosales, Teresa Hernández


SiC based composites are candidates for possible use as structural and functional materials in the future fusion reactors, the main role is intended for the blanket modules. In the blanket, the neutrons produced in the fusion reaction slow down and their energy is transformed into heat in order to finally generate electrical power. In the blanket design named Dual Coolant Lead Lithium (DCLL), a PbLi alloy for power conversion and tritium breeding circulates inside hollow channels called Flow Channel Inserts (FCIs). These FCI must protect the steel structures against the highly corrosive PbLi liquid and the high temperatures, but also provide electrical insulation in order to minimize magnetohydrodynamic interactions of the flowing liquid metal with the high magnetic field present in a magnetically confined fusion environment. Due to their nominally high temperature and radiation stability as well as corrosion resistance, SiC is the main choice for the flow channel inserts. The significantly lower manufacturing cost presents porous SiC (dense coating is required in order to assure protection against corrosion and as a tritium barrier) as a firm alternative to SiC/SiC composites for this purpose. This application requires the materials to be exposed to high radiation levels and extreme temperatures, conditions for which previous studies have shown noticeable changes in both the microstructure and the electrical properties of different types of silicon carbide. Both initial properties and radiation/temperature induced damage strongly depend on the crystal structure, polytype, impurities/additives that are determined by the fabrication process, so the development of a suitable material requires full control of these variables. For this work, several SiC samples with different percentage of porosity and sintering additives have been manufactured by the so-called sacrificial template method at the Ceit-IK4 Technology Center (San Sebastián, Spain), and characterized at Ciemat (Madrid, Spain). Electrical conductivity was measured as a function of temperature before and after irradiation with 1.8 MeV electrons in the Ciemat HVEC Van de Graaff accelerator up to 140 MGy (~ 2·10 -5 dpa). Radiation-induced conductivity (RIC) was also examined during irradiation at 550 ºC for different dose rates (from 0.5 to 5 kGy/s). Although no significant RIC was found in general for any of the samples, electrical conductivity increase with irradiation dose was observed to occur for some compositions with a linear tendency. However, first results indicate enhanced radiation resistance for coated samples. Preliminary thermogravimetric tests of selected samples, together with posterior XRD analysis allowed interpret radiation-induced modification of the electrical conductivity in terms of changes in the SiC crystalline structure. Further analysis is needed in order to confirm this.

Keywords: Radiation Damage, Electrical Conductivity, Thermal Stability, flow channel insert, DCLL blanket, porous SiC

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5 In situ High Temperature Characterization of Diamond-Like Carbon Films

Authors: M. Rouhani, F. C. N. Hong, Y. R. Jeng


The tribological performance of DLC films is limited by graphitization at elevated temperatures. Despite of numerous studies on the thermal stability of DLC films, a comprehensive in-situ characterization at elevated temperature is still lacking. In this study, DLC films were deposited using filtered cathodic arc vacuum method. Thermal stability of the films was characterized in-situally using a synchronized technique integrating Raman spectroscopy and depth-sensing measurements. Tests were performed in a high temperature chamber coupled with feedback control to make it possible to study the temperature effects in the range of 21 – 450 ̊C. Co-located SPM and Raman microscopy maps at different temperature over a specific area on the surface of the film were prepared. The results show that the thermal stability of the DLC films depends on their sp3 content. Films with lower sp3 content endure graphitization during the temperature-course used in this study. The graphitization is accompanied with significant changes in surface roughness and Raman spectrum of the film. Surface roughness of the films start to change even before graphitization transformation could be detected using Raman spectroscopy. Depth-sensing tests (nanoindentation, nano-scratch and wear) endorse the surface roughness change seen before graphitization occurrence. This in-situ study showed that the surface of the films is more sensitive to temperature rise compared to the bulk. We presume the changes observed in films hardness, surface roughness and scratch resistance with temperature rise, before graphitization occurrence, is due to surface relaxation.

Keywords: Raman spectroscopy, Thermal Stability, Nanoindentation, DLC film

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4 Influence of Controlled Retting on the Quality of the Hemp Fibres Harvested at the Seed Maturity by Using a Designed Lab-Scale Pilot Unit

Authors: Brahim Mazian, Anne Bergeret, Jean-Charles Benezet, Sandrine Bayle, Luc Malhautier


Hemp fibers are increasingly used as reinforcements in polymer matrix composites due to their competitive performance (low density, mechanical properties and biodegradability) compared to conventional fibres such as glass fibers. However, the huge variation of their biochemical, physical and mechanical properties limits the use of these natural fibres in structural applications when high consistency and homogeneity are required. In the hemp industry, traditional processes termed field retting are commonly used to facilitate the extraction and separation of stem fibers. This retting treatment consists to spread out the stems on the ground for a duration ranging from a few days to several weeks. Microorganisms (fungi and bacteria) grow on the stem surface and produce enzymes that degrade pectinolytic substances in the middle lamellae surrounding the fibers. This operation depends on the weather conditions and is currently carried out very empirically in the fields so that a large variability in the hemp fibers quality (mechanical properties, color, morphology, chemical composition…) is resulting. Nonetheless, if controlled, retting might be favorable for good properties of hemp fibers and then of hemp fibers reinforced composites. Therefore, the present study aims to investigate the influence of controlled retting within a designed environmental chamber (lab-scale pilot unit) on the quality of the hemp fibres harvested at the seed maturity growth stage. Various assessments were applied directly on fibers: color observations, morphological (optical microscope), surface (ESEM), biochemical (gravimetry) analysis, spectrocolorimetric measurements (pectins content), thermogravimetric analysis (TGA) and tensile testing. The results reveal that controlled retting leads to a rapid change of color from yellow to dark grey due to development of microbial communities (fungi and bacteria) at the stem surface. An increase of thermal stability of fibres due to the removal of non-cellulosic components along retting is also observed. A separation of bast fibers to elementary fibers occurred with an evolution of chemical composition (degradation of pectins) and a rapid decrease in tensile properties (380MPa to 170MPa after 3 weeks) due to accelerated retting process. The influence of controlled retting on the biocomposite material (PP / hemp fibers) properties is under investigation.

Keywords: Mechanical Properties, Thermal Stability, controlled retting, hemp fibre

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3 Dependence of Free Fatty Acid and Chlorophyll Content on Thermal Stability of Extra Virgin Olive Oil

Authors: Yongjun Ahn, Sung Gyu Choi, Seung-Yeop Kwak


Selective removal of free fatty acid (FFA) and chlorophyll in extra virgin olive oil (EVOO) is necessary to enhance the thermal stability in the condition of the deep frying. In this work, we demonstrated improving the thermal stability of EVOO by selective removal of free fatty acid and chlorophyll using (3-Aminopropyl)trimethoxysilane (APTMS) functionalized mesoporous silica with controlled pore size. The adsorption kinetics of free fatty acid and chlorophyll into the mesoporous silica were quantitatively analyzed by Freundlich and Langmuir model. The highest chlorophyll adsorption efficiency was shown in the pore size at 5 nm, suggesting that the interaction between the silica and the chlorophyll could be optimized at this point. The amino-functionalized mesoporous silica showed drastically improved removal efficiency of FFA than the bare silica. Moreover, beneficial compounds like tocopherol and phenolic compounds maintained even after adsorptive removal. Extra virgin olive oil treated by aminopropyl-functionalized silica had a smoke point high enough to be used as commercial frying oil. Based on these results, it is expected to attract the considerable amount of interest toward facile adsorptive refining process of EVOO using pore size controlled and amino-functionalized mesoporous silica.

Keywords: Thermal Stability, mesoporous silica, extra virgin olive oil, selective adsorption

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2 Effects of Small Amount of Poly(D-Lactic Acid) on the Properties of Poly(L-Lactic Acid)/Microcrystalline Cellulose/Poly(D-Lactic Acid) Blends

Authors: Md. Hafezur Rahaman, Md. Sagor Hosen, Md. Abdul Gafur, Rasel Habib


This research is a systematic study of effects of poly(D-lactic acid) (PDLA) on the properties of poly(L-lactic acid)(PLLA)/microcrystalline cellulose (MCC)/PDLA blends by stereo complex crystallization. Blends were prepared with constant percentage of (3 percent) MCC and different percentage of PDLA by solution casting methods. These blends were characterized by Fourier Transform Infrared Spectroscopy (FTIR) for the confirmation of blends compatibility, Wide-Angle X-ray Scattering (WAXS) and scanning electron microscope (SEM) for the analysis of morphology, thermo-gravimetric analysis (TGA) and differential thermal analysis (DTA) for thermal properties measurement. FTIR Analysis results confirm no new characteristic absorption peaks appeared in the spectrum instead shifting of peaks due to hydrogen bonding help to have compatibility of blends component. Development of three new peaks from XRD analysis indicates strongly the formation of stereo complex crystallinity in the PLLA structure with the addition of PDLA. TGA and DTG results indicate that PDLA can improve the heat resistivity of the PLLA/MCC blends by increasing its degradation temperature. Comparison of DTA peaks also ensure developed thermal properties. Image of SEM shows the improvement of surface morphology.

Keywords: Thermal Stability, microcrystalline cellulose, poly(L-lactic acid), stereocomplex crystallization

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1 Improvement of Thermal Stability in Ethylene Methyl Acrylate Composites for Gasket Application

Authors: Manit Nithitanakul, Pitt Supaphol, Pemika Ketsuwan


A typical used of ethylene methyl acrylate (EMA) gasket is in the manufacture of optical lens, and often, they are deteriorated rapidly due to high temperature during the process. The objective of this project is to improve the thermal stability of the EMA copolymer gasket by preparing EMA with cellulose and silica composites. Hydroxy propyl methyl cellulose (HPMC) and Carboxy methyl cellulose (CMC) were used in preparing of EMA/cellulose composites and fumed silica (SiO2) was used in preparing EMA/silica composites with different amounts of filler (3, 5, 7, 10, 15 wt.%), using a twin screw extruder at 160 °C and the test specimens were prepared by the injection molding machine. The morphology and dispersion of fillers in the EMA matrix were investigated by field emission scanning electron microscopy (FESEM). The thermal stability of the composite was determined by thermal gravimetric analysis (TGA), and differential scanning calorimeter (DSC). Mechanical properties were evaluated by tensile testing. The developed composites were found to enhance thermal and mechanical properties when compared to that of the EMA copolymer alone.

Keywords: Thermal Stability, HPMC, silica, ethylene methyl acrylate

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