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Showing papers in "Journal of Thermal Analysis and Calorimetry in 2011"


Journal ArticleDOI
TL;DR: In this paper, the thermal degradation pathway of poly(N-vinyl pyrrolidone) using Thermogravimetry coupled with Fourier Transform Infrared Spectroscopy (TG-FTIR) in addition to IR and 1H NMR spectroscopic studies of the partially degraded samples was investigated.
Abstract: The aim of this study was to gain some fundamental knowledge on the thermal degradation pathways of poly(N-vinyl pyrrolidone) using Thermogravimetry coupled with Fourier Transform Infrared Spectroscopy (TG–FTIR) in addition to IR and 1H NMR spectroscopic studies of the partially degraded samples. It was found that the vinyl pyrrolidone is the main volatile products of the thermal degradation of PVP which implies that the predominant mechanism during thermal degradation of this polymer is the depolymerization to monomer of the polymeric main chain; however, it is evident that simultaneous reactions may be involved yielding oligomers. FTIR and 1H NMR spectra of partially degraded samples of PVP exhibited very similar characteristics to that observed for undegraded samples although the 1H NMR spectra suggest the presence of simultaneous reactions as the fragmentation of polymeric main chain.

195 citations


Journal ArticleDOI
TL;DR: In this paper, the thermal decomposition of citric acid, trans-and cis-aconitic acid has been studied using the TG-MS, TG-FTIR and DSC techniques.
Abstract: Thermal decomposition of citric acid, trans- and cis-aconitic acid has been studied using the TG-MS, TG-FTIR and DSC techniques. The measurements were carried out in an argon atmosphere over a temperature range of 293–673 K. The influence of the acid structures and configurational geometry on stability of the transition products and pathways of thermal transformations of the studied compounds studied is discussed.

181 citations


Journal ArticleDOI
TL;DR: In this article, the decomposition behavior of kaolin samples has been carried out by simultaneous TG-DTA experiments and new layer-structure formation during the calcination process was found, and metakaolin compound was detected between 600 and 900 °C.
Abstract: The decomposition behavior of kaolin samples has been carried out by simultaneous TG–DTA experiments. New layer-structure formation during the calcination process was found, and metakaolin compound was detected between 600 and 900 °C. The thermal stability of kaolin samples was then identified by TG–DTA, and the results are confirmed by characterization of X-ray powder diffraction (XRD), N2 adsorption (Brunauer-Emmet-Teller model, BET), and scanning electron microscopy (SEM).

143 citations


Journal ArticleDOI
TL;DR: In this paper, the effect of ZnO nanoparticles particles on the mechanical properties and the curing behavior of an epoxy nanocomposite was studied using different loadings of pre-dispersed ZnOs having an average size of 40 nm.
Abstract: Effect of ZnO nanoparticles particles on the mechanical properties and the curing behavior of an epoxy nanocomposite were studied. Nanocomposites were prepared using different loadings of pre-dispersed ZnO nanoparticles having an average size of 40 nm. The surface topography and morphology of the nanocomposites were studied using atomic force microscope (AFM). The mechanical properties of nanocomposites were studied using analytical techniques including dynamic mechanical thermal analysis and micro-Vickers hardness. Effects of ZnO nanoparticles on the curing behavior of these nanocomposites were investigated utilizing isothermal and non-isothermal differential scanning calorimeter techniques. In addition, chemical compositions of coatings containing different ZnO nanoparticles contents were studied using a Fourier transform inferred. It was found that, ZnO nanoparticles can effectively influence the mechanical properties of epoxy coating. In addition, lower curing degrees, and therefore crosslinking density of epoxy coating including higher ZnO nanoparticles were obtained. This effect was completely different at low and high loadings of the particles.

111 citations



Journal ArticleDOI
TL;DR: In this paper, the thermal stability of pure urea-formaldehyde resin (PR) and modified ureaformaldehyde (UF) resins with hexamethylenetetetramine-HMTA (Resin 1), melamine-M(Resin 2), and ethylene urea (EU, Resin 3) including nano-SiO2 was investigated by non-isothermal thermo-gravimetric analysis (TG), differential thermal gravimetry (DTG), and differential thermal analysis (DTA) supported by data from IR spectrosc
Abstract: The thermal stability of pure urea–formaldehyde resin (PR) and modified urea–formaldehyde (UF) resins with hexamethylenetetramine-HMTA (Resin 1), melamine-M (Resin 2), and ethylene urea (EU, Resin 3) including nano-SiO2 was investigated by non-isothermal thermo-gravimetric analysis (TG), differential thermal gravimetry (DTG), and differential thermal analysis (DTA) supported by data from IR spectroscopy. Possibility of combining inorganic filler in a form of silicon dioxide with UF resins was found investigated and percentage of free formaldehyde was determined. The shift of DTG peaks to a high temperature indicates the increase of thermal stability of modified UF resin with EU (Resin 3) which is confirmed by data obtained from the FTIR study. The minimum percentage (6%) of free formaldehyde was obtained in Resin 3.

95 citations


Journal ArticleDOI
TL;DR: In this paper, the optimal heating conditions when electrospun organic/inorganic composite fibers are annealed to get ceramic nanofibers in appropriate quality (crystal structure, composition, and morphology) and to avoid their disintegration were discussed.
Abstract: This article demonstrates how important it is to find the optimal heating conditions when electrospun organic/inorganic composite fibers are annealed to get ceramic nanofibers in appropriate quality (crystal structure, composition, and morphology) and to avoid their disintegration. Polyvinylpyrrolidone [PVP, (C6H9NO) n ] and ammonium metatungstate [AMT, (NH4)6[H2W12O40]·nH2O] nanofibers were prepared by electrospinning aqueous solutions of PVP and AMT. The as-spun fibers and their annealing were characterized by TG/DTA-MS, XRD, SEM, Raman, and FTIR measurements. The 400–600 nm thick and tens of micrometer long PVP/AMT fibers decomposed thermally in air in four steps, and pure monoclinic WO3 nanofibers formed between 500 and 600 °C. When a too high heating rate and heating temperature (10 °C min−1, 600 °C) were used, the WO3 nanofibers completely disintegrated. At lower heating rate but too high temperature (1 °C min−1, 600 °C), the fibers broke into rods. If the heating rate was adequate, but the annealing temperature was too low (1 °C min−1, 500 °C), the nanofiber morphology was excellent, but the sample was less crystalline. When the optimal heating rate and temperature (1 °C min−1, 550 °C) were applied, WO3 nanofibers with excellent morphology (250 nm thick and tens of micrometer long nanofibers, which consisted of 20–80 nm particles) and crystallinity (monoclinic WO3) were obtained. The FTIR and Raman measurements confirmed that with these heating parameters the organic matter was effectively removed from the nanofibers and monoclinic WO3 was present in a highly crystalline and ordered form.

90 citations


Journal ArticleDOI
TL;DR: In this article, the effect of aging on various film properties has been investigated, including tensile strength and the percentage of elongation at break (E 2 b ), thermal (TG and DSC) and Attenuated Total Reflectance (ATR)-FTIR spectral properties.
Abstract: Commercial wheat gluten (WG) films, hard wheat gluten films and soft wheat gluten films, plasticized with glycerol have been cast from water–ethanol solutions. The effect of aging on various film properties has been investigated. The films were aged for about 6 months at 50% relative humidity and ~25 °C, and the mechanical (tensile strength and the percentage of elongation at break (E b)), thermal (TG and DSC) and Attenuated Total Reflectance (ATR)-FTIR spectral properties have been studied. Changes in the protein structure were determined by ATR-FTIR spectroscopy. Films from soft WG exhibited the highest E b (508%) and the highest TS (6.33 MPa). The TG analysis results show that the moisture content in all three kinds of WG protein films is about 5%. The absence of the glycerol phase transition in DSC curves implies that there is no separate phase containing glycerol in the WG protein-glycerol films with 40% glycerol.

84 citations


Journal ArticleDOI
TL;DR: In this article, the authors used a thermogravimetric analyzer to investigate the thermal degradation behavior and kinetics of a biomass waste material, namely walnut shell, using three different heating rates (2, 10, and 15°C) under nitrogen flow.
Abstract: Thermal degradation behavior and kinetics of a biomass waste material, namely walnut shell, were investigated by using a thermogravimetric analyzer. The desired final temperature of 800 °C was achieved at three different heating rates (2, 10, and 15 °C min−1) under nitrogen flow (50 mL min−1). The TG and DTG curves exhibited three distinct zones that can mainly be attributed to removal of water, decomposition of hemicellulose + cellulose, and decomposition of lignin, respectively. The kinetic parameters (activation energy, pre-exponential factor, and reaction order) of active pyrolysis zone were determined by applying Arrhenius, Coats–Redfern, and Horowitz–Metzger methods to TG results. The values of activation energies were found to be between 45.6 and 78.4 kJ mol−1. There was a great agreement between the results of Arrhenius and Coats–Redfern methods while Horowitz–Metzger method yielded relatively higher results. The existence of kinetic compensation effect was evident.

82 citations


Journal ArticleDOI
TL;DR: In this paper, a microencapsulated ammonium polyphosphate (MAPP) is prepared using hydroxyl silicone oil by in situ polymerization and characterized by XPS, which gives better water resistance and flame retardance compared with APP in thermoplastic polyurethane (TPU).
Abstract: Microencapsulated ammonium polyphosphate (MAPP) is prepared using hydroxyl silicone oil by in situ polymerization and characterized by XPS. Microencapsulation gives MAPP better water resistance and flame retardance compared with APP in thermoplastic polyurethane (TPU). Thermal stability and fire resistance behavior have been analyzed and compared. The LOI value of the TPU/MAPP composite is higher than that of the TPU/APP composite. The UL 94 rating of the TPU/MAPP composite is V-0 at the 20 wt% additive level, whereas TPU/APP gives V-2 rating at the same loading level. The water resistant properties of the TPU composites are studied. Results of the cone calorimeter and microscale combustion calorimeter experiment show that MAPP is an effective flame retardant in TPU compared with APP.

78 citations


Journal ArticleDOI
TL;DR: In this article, a finite element method associated with ANSYS program is developed for the computation of thermal field and thermal stress field for early age concrete considering the following characters: degree of hydration, thermal properties (such as specific heat, thermal diffusivity), thermal boundary conditions, and mechanical properties such as shrinkage, creep) which occur at early age.
Abstract: The purpose of this study is to simulate the early age concrete behaviors and evaluate the cracking risk with the thermal and thermal stress analysis. A new finite element method program associated with ANSYS program is developed for the computation of thermal field and thermal stress field for early age concrete considering the following characters: degree of hydration, thermal properties (such as specific heat, thermal diffusivity), thermal boundary conditions, and mechanical properties (such as shrinkage, creep) which occur at early age. The results from simulation compared with experimental values found in the literature show a good agreement. Finally, based on this user-developed subroutine, the effects of hydration heat, ambient temperature, wind velocity, shrinkage, and length-height ratio on cracking risk were analyzed for a concrete wall which is one part of the structure of Maridal culvert in Norway. By which, the measures to control the cracking were provided for the engineering application.

Journal ArticleDOI
TL;DR: In this article, the structural and thermal properties of blends were investigated by thermogravometric analysis (TG), differential scanning calorimetry (DSC), wide-angle X-ray diffraction (WAXD), and scanning electron microscopy (SEM).
Abstract: Microwave-assisted chemical modification of lignin was achieved through esterification using maleic anhydride. Modified lignin (ML) was blended in different proportions up to 25 mass% with polypropylene (PP) using Brabender electronic Plasticorder at 190 °C. The structural and thermal properties of blends were investigated by thermogravometric analysis (TG), differential scanning calorimetry (DSC), wide-angle X-ray diffraction (WAXD) and scanning electron microscopy (SEM). TG analysis showed increased thermal stability of blends due to antioxidant property of ML, which opposed oxidative degradation of PP. DSC analysis indicted slight depression in a glass transition temperature and melting temperature of blends due to partial miscible blend behavior between PP and ML. All blends showed higher crystallization temperatures and continuously reducing percentage crystallinity with increasing ML proportion in the blends. WAXD analysis indicated that PP crystallized in β polymeric form in addition to α-form in the presence of ML. However, proportion of β-form did not show linear relation with increase in ML proportion, thus ML acts as β nucleating agent in the PP matrix. SEM analysis showed good dispersion/miscibility in PP matrix indicating modification in lignin is useful.

Journal ArticleDOI
TL;DR: In this article, the authors used thermal analysis to characterize soil organic matter (SOM) quality and found that the results were highly repeatable but strongly sensitive to crucible material, heating rate, and sample amount, and relatively insensitive to the use of a reference material.
Abstract: Thermal analysis is primarily used in the field of materials science, but has a long history in the geosciences. Soil organic matter (SOM) has received a great deal of recent scientific interest because of its role in the global carbon cycle. Conventional methods of characterizing SOM quality are unsatisfactory because they do not adequately capture the complete quality continuum that SOM comprises or the various mechanisms that act to stabilize it in the soil matrix. Thermal analysis techniques have the potential to capture this quality continuum, but are dependent on numerous experimental conditions that limit the comparability of results among different studies. Published methodology on thermal analysis of soils and sediments has largely focused on the characterization of the mineral component, while the organic component has received little attention. We tested several experimental conditions for their effects on the exothermic region of curves generated by thermal analysis of easily dispersed soil clay fractions and non-protected light-density particulate organic matter fractions isolated from the surface horizon of a forest soil. Results were found to be highly repeatable but strongly sensitive to crucible material, heating rate, and sample amount, and relatively insensitive to the use of a reference material. Thermal analysis is an important addition to the set of analytical tools used to characterize SOM quality because it provides direct, quantitative information of the energy potentially available for microbial metabolism. However, users will need to balance the needs of specific scientific objectives with the need for standardized methods and comparability between studies.

Journal ArticleDOI
TL;DR: In this paper, the authors used the vent sizing package 2 (VSP2) to measure the thermal hazard and runaway characteristics of 18650 lithium-ion batteries, which were manufactured by Sanyo Electric Co., Ltd.
Abstract: Vent sizing package 2 (VSP2) was used to measure the thermal hazard and runaway characteristics of 18650 lithium-ion batteries, which were manufactured by Sanyo Electric Co., Ltd. Runaway reaction behaviors of these batteries were obtained: 50% state of charge (SOC), and 100% SOC. The tests evaluated the thermal hazard characteristics, such as initial exothermic temperature (T 0), self-heating rate (dT dt −1), pressure-rise rate (dP dt −1), pressure temperature profiles, maximum temperature, and pressure which were observed by adiabatic calorimetric methodology via VSP2 using customized test cells. The safety assessment of lithium-ion cells proved to be an important subject. The maximum self-heating rate (dT dt −1)max and the largest pressure-rise rate (dP dt −1)max of Sanyo 18650 lithium-ion battery of 100% SOC were measured to be 37,468.8 °C min−1 and 10,845.6 psi min−1, respectively, and the maximum temperature was 733.1 °C. Therefore, a runaway reaction is extremely serious when a lithium-ion battery is exothermic at 100% SOC. This result also demonstrated that the thermal VSP2 is an alternative method of thermal hazard assessment for battery safety research. Finally, self-reactive ratings on thermal hazards of 18650 lithium-ion batteries were studied and elucidated to a deeper extent.

Journal ArticleDOI
TL;DR: In this article, the tensile strength, interfacial adhesion, and heat deflection temperature (HDT) of maleic anhydride-grafted poly(butylene succinate) (PBS-MA) and maleic-anhydride grafted poly (lactic acid) (PLA-MA)-treated biocomposites were examined.
Abstract: This study examined the interfacial adhesion, mechanical, and thermal properties of compatibilizing agent-treated and non-treated biocomposites as a function of the type of compatibilizing agent. The tensile strength, interfacial adhesion, and heat deflection temperature (HDT) of maleic anhydride-grafted poly(butylene succinate) (PBS-MA) and maleic anhydride-grafted poly(lactic acid) (PLA-MA)-treated biocomposites are greater than those of untreated maleic anhydride-grafted poly(styrene-b-ethylene-co-butylene-b-styrene) triblock copolymer (SEBS-MA) and maleic anhydride-grafted polypropylene (MAPP)-treated biocomposites. The storage modulus (E′) values and the tan δmax temperatures (Tg) of PBS-MA and PLA-MA-treated biocomposites were slightly higher than that of the untreated biocomposites.

Journal ArticleDOI
TL;DR: In this paper, the authors developed and characterized insulin nanoparticles systems using chitosan using ionic gelation with tripolyphosphate anions (TPP), and evaluated the interactions between insulin and chitosa using differential scanning calorimetry (DSC), thermogravimetry/derivative thermogram (TG/DTG), and Fourier transform infrared (FTIR) spectroscopy.
Abstract: The purpose of this study was to develop and characterize insulin nanoparticles systems using chitosan. Insulin-loaded nanoparticles were prepared by ionic gelation of chitosan with tripolyphosphate anions (TPP). The interactions between insulin and chitosan were evaluated by differential scanning calorimetry (DSC), thermogravimetry/derivative thermogravimetry (TG/DTG), and Fourier-transform infrared (FTIR) spectroscopy. Besides, particle size distribution, polydispersity index (PDI), zeta potential, and association efficiency (AE%) of the nanoparticles were evaluated. In general, inert nanoparticles and insulin-loaded nanoparticles showed an average size of 260.56 nm (PDI 0.502) and 312.80 nm (PDI 0.481), respectively. Both nanoparticles showed positive charge, but after insulin incorporation the zeta potential was reduced, evidencing its incorporation. Nanoparticles obtained also showed AE% around 70%, measured by high-performance liquid chromatography (HPLC). The results of FTIR, DSC, and TG/DTG corroborated the data presented suggesting that insulin was successfully encapsulated. However, drug incorporation seems to be related not only to electrostatic interactions, but also to physical process and/or adsorption phenomena.

Journal ArticleDOI
TL;DR: In this article, the influence of spent catalyst from catalytic cracking in fluidized bed (FCC) on the hydration of two kinds of calcium aluminate cements (of about 40 and 70% content of alumina) was studied.
Abstract: The influence of spent catalyst from catalytic cracking in fluidized bed (FCC) on the hydration of two kinds of calcium aluminate cements (of about 40 and 70% content of alumina) was studied. Cement pastes were prepared with constant ratio of water/binder = 0.5 and with content of 0, 5 and 25% mass of addition as replacement of cement. The samples were stored at room temperature. Thermal analysis (TG, DTG), infrared absorption (FTIR) and X-ray diffraction methods were applied to investigate changes in various periods of hydration (up to 150 days). The compressive strength of cement mortars was also examined. On the basis of presented results it was affirmed that in studied conditions spent FCC catalyst is a reactive addition in calcium aluminate cement (CAC) pastes, which probably can create a new phase type C–A–S–H. It may be an interesting alternative for limitation of the negative phenomenon of conversion of aluminate hydrates, although the degree of the influence of the mineral additive depends on the composition of CAC and of the quantity of the used waste.

Journal ArticleDOI
TL;DR: An overview of the applications of active thermography to the investigation of art and historic artefacts is presented and discussed in this article, where the authors present an active method where the thermal stimulation of the sample is required.
Abstract: Infrared thermography (IRT) is a non-destructive technique that has recently been extensively applied to the investigation of cultural heritage It provides information on the surface and subsurface structure of the artefacts by the analysis of the heat diffusion process within the sample IRT has been successfully applied to the study of historic large structures and buildings most of the time by means of the so-called passive approach, where only the naturally occurring temperature changes in the sample are analysed On the other hand, IRT has also been applied to the study of other art and historic artefact by applying the so-called active method where the thermal stimulation of the sample is required In this article, an overview of the applications of active thermography to the investigation of art and historic artefacts will be presented and discussed

Journal ArticleDOI
TL;DR: Li-ion batteries with LiFePO4/C composites are difficult to be charged at low temperatures, and a new charging mode under low temperature was proposed in this paper, where the surface temperature of Li-ion battery ascended to 3°C at the end of pulse cycling when the environment temperature was −10°C.
Abstract: Li-ion batteries with LiFePO4/C composites are difficult to be charged at low temperatures. In order to improve the low temperature performance of LiFePO4/C power batteries, the charge–discharge characteristics were studied at different temperatures, and a new charging mode under low temperature was proposed. In the new charging mode, the batteries were excited by current pulses with the charge rates between 0.75 C and 2 C, while the discharge rates between 3 and 4 C before the conventional charging (CC–CV). Results showed that the surface temperature of Li-ion battery ascended to 3 °C at the end of pulse cycling when the environment temperature was −10 °C. Comparing with the conventional charging, the whole charge time was cut by 36 min (23.4%) and the capacity was 7.1% more at the same discharge rate, respectively.

Journal ArticleDOI
TL;DR: In this paper, the analysis of a non-isothermal and isothermal decomposition and oxidation of the CoSb3 powders and polycrystalline samples were performed using simultaneous TG/DTA technique.
Abstract: Thermal durability of CoSb3 in vacuum, helium and air was investigated over the temperature range of 20–850 °C. A scanning electron microscope (SEM) and X-ray powder diffraction technique were used to investigate the microstructure and to carry out the phase analysis of the degradation products. The analysis of a non-isothermal and isothermal decomposition and oxidation of the CoSb3 powders and polycrystalline samples were performed using simultaneous TG/DTA technique. More detailed studies were carried out on the oxidation in the temperature range 400–600 °C. It was established that the decomposition products are CoSb2 and a volatile antimony. In case of oxidation a complex three-layered scale is formed, consisting of CoSb2O4, CoSb2O6 and Sb2O4 layers. Both the decomposition and the oxidation kinetics are determined by a diffusion through the growing layers of products. The electrical resistivity and Seebeck coefficient measurements have been also performed on pure and oxidized samples, which showed a large influence of the oxidation on the electrical properties.

Journal ArticleDOI
TL;DR: In this paper, the authors introduce thermoporometry and review related results of the confinement effects on materials and their solid-liquid phase transition and their potential of becoming a widely utilised characterisation method, although its potential has not yet been widely realised.
Abstract: Thermoporometry is a relatively new method of characterising porous properties of nanostructured materials based on observation of solid–liquid phase transitions of materials confined in pores. It provides several advantages over the conventional characterisation methods, mercury porosimetry and gas sorption. The advantages include possibility of using short measurement times, non-toxic chemicals and wet samples. In addition, complicated sample preparation and specialised instruments are not required. Therefore, it has a great potential of becoming a widely utilised characterisation method, although its potential has not yet been widely realised. In recent years, there has been a significant increase in research activities regarding the method. In the first part of the review, we introduce thermoporometry and review related results of the confinement effects on materials and their solid–liquid phase transition.

Journal ArticleDOI
TL;DR: In this paper, the FGD gypsum degradations were investigated at N2 atmosphere (autogenous and negligible partial pressure of water) in non-isothermal and isothermal condition.
Abstract: The dehydration behaviors of FGD gypsums from three power plants were investigated at N2 atmosphere (autogenous and negligible partial pressure of water, \( P_{{{\text{H}}_{ 2} {\text{O}}}} \)) in non-isothermal and isothermal condition. The dehydration of gypsum proceeded through one step, i.e., CaSO4·2H2O → γ-CaSO4 (γ-anhydrite) or two steps, i.e., CaSO4·2H2O → CaSO4·0.5H2O (hemihydrate) → γ-CaSO4 depending on temperature and \( P_{{{\text{H}}_{ 2} {\text{O}}}} \). The discrepancies of three FGD gypsums on dehydration behavior were very likely due to the different crystalline characteristics (size and habit) and impurities, such as fly ash and limestone. Experimental data of non-isothermal analysis have been fitted with two ‘model-free’ kinetic methods and those of isothermal analysis have been fitted with Avrami and linear equation. The apparent empirical activation energies (Ea) suggest that the transition from gypsum to hemihydrate is mainly controlled by nucleation and growth mechanism, while the transition from gypsum to γ-anhydrite is mostly followed by phase boundary mechanism.

Journal ArticleDOI
TL;DR: In this paper, a self-healing material for coating applications was synthesized using the Diels-Alder (DA) reaction as cross-linking reaction, which allows local mobility and rearrangements in the polymeric network, which is composed of a furan functionalized epoxy-amine and a bismaleimide.
Abstract: A self-healing material for coating applications was synthesized using the Diels–Alder (DA) reaction as cross-linking reaction. The built-in reversibility allows local mobility and rearrangements in the polymeric network, which is composed of a furan functionalized epoxy-amine and a bismaleimide. The self-healing material was characterized by physical–chemical means using Fourier Transform Infrared spectroscopy, thermogravimetric analysis (TG) and rapid heat-cool differential scanning calorimetry. It has been shown that the reversibility, as a result of a change in DA/retro-DA equilibrium, occurs in a temperature window ranging from ca. 80 to 150 °C. The repeatability of the non-autonomous healing was checked by TG, showing no evaporation or degradation of the components involved in the temperature window of interest.

Journal ArticleDOI
TL;DR: In this article, the thermal stability and thermal degradation kinetics of resol resins were studied using thermogravimetric analysis (TG) in air and nitrogen atmospheres in order to understand the steps of degradation and to improve their stabilities in industrial applications.
Abstract: Resol resins are used in many industrial applications as adhesives and coatings, but few studies have examined their thermal degradation. In this work, the thermal stability and thermal degradation kinetics of phenol–formaldehyde (PF) and lignin–phenol–formaldehyde (LPF) resol resins were studied using thermogravimetric analysis (TG) in air and nitrogen atmospheres in order to understand the steps of degradation and to improve their stabilities in industrial applications. The thermal stability of samples was estimated by measuring the degradation temperature (T d), which was calculated according to the maximum reaction rate criterion. In addition, the ash content was determined at 800 °C in order to compare the thermal stability of the resol resin samples. The results indicate that 30 wt% ammonium lignin sulfonate (lignin derivative) as filler in the formulation of LPF resin improves the thermal stability in comparison with PF commercial resin. The activation energies of degradation of two resol resins show a difference in dependence on mass loss, which allows these resins to be distinguished. In addition, the structural changes of both resins during thermal degradation were studied by Fourier transform infrared spectroscopy (FTIR), with the results indicating that PF resin collapses at 300 °C whereas the LPF resin collapses at 500 °C.

Journal ArticleDOI
TL;DR: In this paper, the discrepancies between isoconversional methods when applied to complex transformations are analyzed and the authors conclude that conventional integral methods based on integrated equations are essentially incorrect when dealing with variable activation energy.
Abstract: We will analyze the discrepancies between isoconversional methods when applied to complex transformations. The practical analysis of particular transformations leads us to conclude that (a) conventional integral methods based on integrated equations are essentially incorrect when dealing with variable activation energy; and (b) experimental inaccuracies and noise tend to give an apparent evolution of the energy variation, so that, non-constancy of the activation energy does not necessarily mean deviations from single-step transformations with constant activation energy.

Journal ArticleDOI
TL;DR: In this article, nanoparticles have been synthesized via autocatalytic decomposition of the precursor, cobalt zinc ferrous fumarato hydrazinate (CZfH2O4).
Abstract: Cobalt zinc ferrite, Co0.8Zn0.2Fe2O4, nanoparticles have been synthesized via autocatalytic decomposition of the precursor, cobalt zinc ferrous fumarato hydrazinate. The X-ray powder diffraction of the ‘as prepared’ oxide confirms the formation of single phase nanocrystalline cobalt zinc ferrite nanoparticles. The thermal decomposition of the precursor has been studied by isothermal, thermogravimetric and differential thermal analysis. The precursor has also been characterized by FTIR, and chemical analysis and its chemical composition has been determined as Co0.8Zn0.2Fe2(C4H2O4)3·6N2H4. The Curie temperature of the ‘as-prepared oxide’ was determined by AC susceptibility measurements.

Journal ArticleDOI
TL;DR: In this paper, the thermal stability of the ionic liquids (ILs) 1-n-butyl-3-methylimidazolium bromide, (BMIM)Br, and 1n-n octyl- 3methyloride-morphosynthetic-drugs (OMIM) Br, was evaluated through thermogravimetry (TG).
Abstract: The thermal stability of the ionic liquids (ILs) 1-n-butyl-3-methylimidazolium bromide, (BMIM)Br, and 1-n-octyl-3-methylimidazolium bromide, (OMIM)Br, was evaluated through thermogravimetry (TG). Long-term isothermal TG studies revealed that both of these ILs exhibit appreciable decomposition even at temperatures significantly lower than the onset decomposition tempera- ture, previously determined from fast scan TG experi- ments. The long-term TG studies of both the ILs showed linear mass loss as a function of time at each temperature of 10 C interval in the range 533-573 K over a period of 10 h. The kinetics of isothermal decomposition of ILs was analyzed using pseudo-zero-order rate expression. The activation energies for the isothermal decomposition of (BMIM)Br and (OMIM)Br under nitrogen atmosphere are 219.86 and 212.50 kJ mol -1 , respectively. The moisture absorption kinetics of these ILs at 25 C and 30% relative humidity (RH) and at 85 C and 85% RH were also stud- ied. Water uptake of ILs exposed at 25 C/30%RH follows a simple saturation behavior in agreement with Weibull model while that at 85 C/85%RH fortuitously fit into the Henderson-Pabis model.

Journal ArticleDOI
TL;DR: In this article, gasification of lignocellulosic char derived from sewage sludge was studied under different oxidizing atmospheres containing CO2,O 2 or H2O.
Abstract: Gasification of char derived from sewage sludge was studied under different oxidizing atmospheres containing CO2 ,O 2 or H2O. The gasification tests were carried out in thermobalance at different temperatures and oxidizing reagent concentrations. The most efficient were the gaseous mixtures containing oxygen. The reaction took place at temperature 400-500 C, whilst in the case of CO2 and steam much higher temperatures (700-900 C) were necessary to complete the conversion. Two rate models for gas-solid reaction were applied to describe the effect of char conversion on reaction rate. The shrinking core model for reaction-controlled regime was found to be the best for predicting the rate of char gasification in CO2 and O2 atmosphere. The experimental data for steam gasification of the char were fitted best by the first-order kinetics. The kinetic parameters estimated from the experimental data are in accordance with the literature for lignocellulosic char gasification and are the first published for sewage sludge char gasification.

Journal ArticleDOI
TL;DR: In this paper, it was shown that the Curie temperature is not a fixed point and no authority has decided what the temperature of this point is, and therefore it appeared that it was necessary to further explore measurement of this temperature.
Abstract: Nickel presents a magnetic transition ferromagnetic/paramagnetic with a variation of temperature; this transition is classified as a second order transition using the Ehrenfest criteria. The end of this transition is characterized by a point called Curie point. This temperature is used for the calibration of thermogravimetric apparatus. As the Curie temperature is not a fixed point, no scientific authority has decided what the temperature of this point is. As different values are proposed in the literature, it appeared that it was necessary to further explore measurement of this point.

Journal ArticleDOI
TL;DR: In this paper, the effects of Al-5Ti-1B grain refiner and Al-10Sr modifier were studied on solidification characteristics and microstructural features of aluminum alloy.
Abstract: In this research, the effects of Al–5Ti–1B grain refiner and Al–10Sr modifier were studied on solidification characteristics and microstructural features of 319 aluminum alloy. Important solidification events such as recalescence and nucleation undercooling temperature and aluminum–silicon eutectic depression temperature have been evaluated using cooling curve and its first derivative curve obtained from thermal analysis of a sample. The aim of this article is to show the ability of the thermal analysis technique to predict some key parameters controlling solidification and casting process. It has been found that the thermal analysis is the identified method for a rapid on-line monitoring of metallurgical characteristics of aluminum alloy melts without conventional metallographic examination.