Many kaolinites are known to exhibit limited intercalation capacity which affects their usage. Some reports have linked this lack of reactivity to particular structural features or to slow kinetics; others recommended increasing intercalation temperature as a remedy. The purpose of the current study was to investigate systematically the N-methylformamide (NMF) intercalation capacity of three kaolinites differing in layer stacking order (KGa-1b, KGa-2, and Imerys Hywite Alum) in the 5–150°C temperature range. Near-infrared spectroscopy (NIR) was employed to record the full kinetics of intercalation in closed systems with excess NMF. Increasing intercalation temperature accelerated the reaction, but the NMF uptake decreased and eventually vanished. Complementary thermogravimetric analysis (TGA) confirmed this unexpected trend. All kaolinites exhibited the same behavior, but the amount of inert material was in the order of their stacking-fault concentration at all temperatures: KGa-2 > Hywite > KGa-1b. Subjecting the samples to stepwise temperature changes showed that, once intercalated, the NMF could not deintercalate and was removed from equilibrium with the surrounding fluid. Thus, intercalation capacity was not a unique feature of the material because it depended on thermal history. As stacking order and thermal history had no detectable effect on the NMF-hosting environment, the unusual temperature dependence was attributed tentatively to the adverse effect of temperature on the adsorption of NMF on the edges of the crystallites, which is a prerequisite for intercalation.

Hot deformation and softening response for the titanium aluminide Ti–48Al–2V–0.2B has been investigated. The deformation response to softening mechanisms has been examined. Deformation experiments were carried out in the strain rate range 0.01–10 s−1 keeping the temperature constant at 1200 °C and in the temperature range 1000–1200 °C at the strain rate 1 s−1. With an increase in strain rate, the microstructural changes associated with the softening mechanism include breaking of the lamellae, spheroidization of the broken laths and dynamic recrystallization. For the strain rate 1 s−1, deformation in the (α2 +γ) phase field leads to fine recrystallized grains, remnant lamellae and cavitation along the grain boundaries (for temperatures 1000 and 1100 °C). Deformation in the (α +γ) phase field leads to dynamic recrystallization at the shear bands, within the lamellae, breaking and rotation of the α phase during the continuous increase in the deformation strain.

This study seeks to understand the low temperature reactions of the salt phase that occur during the vitrification of Hanford Low Activity Waste (LAW). Salts (such as nitrates, sulfates, carbonates, halides, etc.) play a key role in these low temperature reactions as they sequentially melt, decompose, and volatilize during batch-to-glass conversion. To further understand these complex processes, simplified LAW melts containing oxyanion salts (sodium salts of carbonate, sulfate, and/or nitrate) and early melting glass formers (boric acid) have been evaluated using thermal analysis, infrared absorption spectroscopy, and X-ray diffraction. Results from this study indicate that the volatilization behavior of particular salts is influenced by the presence or absence of other salts. NaNO3 volatilization is decreased by the presence of Na2SO4. The addition of either Na2SO4 or NaNO3 to the system may enhance the volatilization of Na2CO3. In all cases, Na2SO4 was retained after melting and was often found to be in two different crystalline phases upon quenching.

For a material to be used as energy, understanding its combustion behavior is crucial. Biomass is one such material that is increasingly gaining traction. Biomass may be utilized by direct combustion or transformation into fluid or solid biomass-based fuels. In this work, slow pyrolysis of groundnut shells, bagasse, rice husks and coffee husks was done to produce briquettes with cassava starch binder. Thermogravimetric analysis (TGA) was carried out using an Eltra Thermostep thermogravimetric analyzer. The samples were heated from ambient to 920 deg. Celsius. This analysis provided combustion explanations in terms of the weight loss, burning rates, peak temperatures, char residues and mean reactivity. TGA results showed that binder inclusion reduced the amount of fixed carbon present in the developed briquettes, thus slightly reducing their calorific values. Rice husks briquettes yielded the least weight loss (20.9% and 24.7% for 30g and 50g binder incorporations respectively) compared to others, owing to former’s higher ash contents. Increase in binder contents reduced the amount of char residues, caused by reducing ash contents in the developed briquettes. Peak temperatures and char residues generally increased with increasing binder content. This signifies increasing thermal stabilities of the developed briquettes. Highest char residues were obtained by briquettes developed with rice husks at 30g binder while briquettes developed with bagasse briquettes developed at 50g binder had the least char residues. The highest mean reactivities were obtained in briquettes developed from bagasse and coffee husks while briquettes developed from rice husks had lowest mean reactivities. Briquettes developed in this study showed sufficient combustion properties suitable to provide energy for domestic and industrial applications.

The defect fluorite titanium-doped yttrium niobate samples Y3Nb1−xTixO7−δ have been synthesized and investigated by the means of high-temperature X-ray diffraction, dilatometry, and thermogravimetry. Thermal expansion coefficients (TECs) as well as chemical expansion coefficients for material with 5, 10, and 15 mol% of titanium were determined. All investigated samples exhibit chemical contraction caused by Ti doping. The values of TECs obtained by two different methods show similar results, which suggests the isotropy of the polycrystalline ceramic. Thermogravimetric studies have shown that all of the compositions exhibit a mass increase upon being exposed to a humid air atmosphere. The total proton concentration calculated on the basis of these results was in the range of 0.1 mol%. Moreover, titanium content influences chemical expansion coefficient, water uptake, and protonic defects concentration, whereas it does not significantly affect the values of TECs.

Conducting polymers namely polyaniline (PANI), polypyrrole (PPy) and their copolymer poly(Aniline-co-Pyrrole)(PAPY) were prepared via in-situ polymerization process. The X-ray diffraction (XRD), infra-red (IR)and field emission-scanning electron microscopy (FESEM) studies confirm the formation of polyaniline, polypyrrole and their copolymer with aniline and pyrrole. The XRD pattern of copolymer displayed an amorphous structure as compared to polycrystalline homopolymers. FE-SEM results of Poly (Ani-co-Py) shows the existence of agglomerated spherical structured particles in the copolymer matrix, while the polyaniline and polypyrrole exhibit the porous tubular and spherical structures, respectively. Thermo gravimetric analysis (TGA) shows that the copolymer is more stable as compared to their homopolymers at higher temperature. Four probe resistivity (FPR) studies indicate that copolymer has the lower conductivity and act as a diode. Vector network analyzer (VNA) measurements observe a significant shielding effectiveness (SE) for all the conducting polymers.

Among various methods used for the reduction of graphene oxide (GO) into a purer form of graphene, the thermal reduction method provides a simpler, safer, and economic alternative, compared to other techniques. Thermal reduction of GO causes significant weight loss and volume expansion of the material. Current work investigates the onset temperature where reduction in terms of exfoliation takes place, which is determined to be 325 °C at standard atmospheric pressure. Reduction temperature plays the most crucial role as it controls the quality of reduced graphene oxide in terms of weight percentage of carbon and lattice defect. The study leads to achieving highest content with a minimum defect in the graphene lattice at the optimum temperature, which is found to be 350 °C at standard atmospheric pressure. The thermal reduction process has been analyzed with the help of Fourier transform infrared spectroscopy, thermogravimetric analysis, and thermal degradation kinetics. From thermal degradation kinetics of GO, the rate of reaction has been found to be independent of concentration and is a sole function of temperature.

Zinc borate has long been used as a protector for wood products due to its fungicide, insecticide and flame retardant properties. In this initial study, its capacity as a flame retardant when applied to Eucalyptus grandis wood is evaluated; micronized zinc borate, synthesized from zinc oxide and boric acid in our laboratory was used. The methodology used in the study is the use of the Vandersall tunnel, which allowed analyzing parameters such as the flame spread, the carbonization index, the carbonization area and the wood weight loss. The results show a remarkable improvement in these parameters after the application of micronized zinc borate. For the longest fire exposure time, the percentage decrease of each evaluated parameter is, for tangential and radial plane respectively: 31.27-43.00% for flame spread, 36.66-40.86% for carbonization area, 33.01-52.49% for carbonization index and 19.86-57.80% for mass loss.

A thermoset polymer can be used for specific applications by creating a unique chemical composition that is designed for certain characteristic environments. To know the behavior of a thermoset polymer, it is necessary to thermally analyze its behavior during the curing process, as well as its mechanical behavior under certain loads that are applied in its field of application. In this study, the epoxy resin X was created at high temperatures, which there was no record of its thermal or mechanical behavior; the resin was analyzed to determine if it was possible to make a reduction in its curing cycle that was at temperature of 425° F with a time of 24 hours. As a result, through thermal analysis such as Differential Scanning Calorimetry (DSC), rheometry, Thermogravimetric Analysis (TGA) and Dynamic Mechanical Thermal Analysis (DMTA); as well as mechanical analysis, such as stress, hardness and planar cutting tests; it was possible to reduce the curing cycle of resin X, which is used in aerospace generators, from 24 hours at 425 ° F to 8 hours at 425 ° F. In the same way, this reduction of the cure cycle was verified by means of a qualification of a product that involved the reduction of the curing cycle of the epoxy resin obtaining very similar results to the original ones, verifying that the change of curing in the epoxy resin did not affected the functioning of the component. This methodology can be used and applied for the study of thermoset polymers that are used in several industries such as aerospace, automotive, among others.

The widespread occurrence and availability of coal makes it the world’s prime source of energy for different end use applications. Coal is commonly used for electricity production through coal combustion. However, many researchers have indicated that coal combustion is a prime contributor to emission of greenhouse gases contributing to global warming. During combustion gaseous elements such as sulfur, hydrogen, carbon and nitrogen react with oxygen to produce their respective oxides. These oxides contribute to global warming, air and water pollution as well as acid deposition. Emission of these oxides and their effect on the environment has resulted in increased interest in clean coal technologies. Clean coal technologies, such as coal gasification technology, use multiple technologies to control the emissions so as to minimize environmental effects from coal utilization.

In this paper, the characteristics of Morupule coal from the south and east main sections are determined to establish its suitability for gasification. The characterization was conducted using thermal analysis (Thermogravimetric Analyzer) and an X-Ray Fluorescence (XRF). Numerical simulation was also carried out using Ansys software for species transport. The samples proved the coal to be from a high ash and sulfur content and medium volatiles bituminous parent rock, whilst species transport revealed a sufficient syngas yield per kilogram of coal for downstream processes.

In the safety assessment of a radioactive waste disposal, it is extremely important to assess the migration behavior of long-half-life radionuclides in the disposal environment. The migration behavior in the disposal environment for a radionuclide varies with the chemical form of the nuclide. In particular, C-14 has various chemical forms, and its migration behavior in the disposal environment substantially varies with the chemical forms. It has been reported that hardly soluble C-14 is generated in PWRs. However, the chemical form of this hardly soluble C-14 is little known. In this study, the thermal decomposition behavior of particles containing C-14 and the mass spectra of gases released through thermal decomposition were analyzed in order to examine the chemical form of C-14 generated in PWRs. In this study, the gases released during the thermogravimetric (TG) analysis were partially oxidized to CO2, trapped in an alkaline solution and analysed for C-14. Another part of the gas was analysed directly by mass spectrometry (MS). The residues obtained after TG analysis were also analysed for C-14 by oxidizing the residue to CO2, trapping the CO2 in alkaline solutions and analysing C-14 by LSC. During TG-analysis in inert gas (He) atmosphere, about 90% of C-14 was found in residue, while when air was used during TG-analysis, no C-14 could be detected in residue. From the MS-analysis of species released during TG-analysis in inert gas, fragments regarded as originating from ion-exchange resins were detected in released gases. Based on this result, it was found that while substances originating from ion-exchange resin were present in radioactive particles generated in a PWR, the main part of C-14 was contained in the residue after heating in the form of thermally stable substances, easy to be oxidized by air at high temperature. It was not possible to determine their exact chemical composition in this work but also, In addition, sorption of insoluble C-14 to cementitious materials was preliminarily examined. As a results, the concentration of insoluble C-14 decreased greatly in 7 days. That means insoluble C-14 tended not to stay in water. Elucidation of the sorption mechanism in the disposal environment of these C-14 is also a future task.

An effective way to reduce the impact of cement production on the environment is to use supplementary cementitious materials (SCM) as a partial substitution to cement. In addition to the reduction in cost and energy saving, the use of SCM in cement for the manufacture of mortar and concrete offers technical advantages. In this paper, cement was partially substituted by fines obtained from crushed recycled bricks recovered from a brick plant. The level of substitution was either 0%, 5%, 10% or 15% by weight of cement. The results show that cement substitution by brick fines resulted in a slight loss of workability with the increase of the substitution rate. Substitutions rates of 5% and 10% produced at long-term comparable strength as control mortars. The differential thermal analysis (DTA) and thermo-gravimetric analysis (TGA) results show cement hydration improved significantly with different rates of substitutions at 28 and 180 days of age.

Low volume fraction (0.5, 1, and 2 vol%) SiO2 reinforced magnesium nanocomposites were synthesized using powder metallurgy technique followed by hot extrusion. The nanocomposites were studied for physical, microstructural, ignition, and mechanical properties to study the influence of nanoparticulate addition on monolithic magnesium. The grain size of the developed nanocomposites was observed to marginally decrease with the addition of SiO2 nanoparticulates with 2 vol% SiO2 addition resulting in a grain size of ∼23 μm which is ∼32% lower than that of pure Mg. The ignition temperature of pure Mg was enhanced with the addition of SiO2 nanoparticulates with Mg 2 vol% SiO2 nanocomposite exhibiting an ignition temperature of 611 °C (∼20 °C greater than pure Mg and AZ31 alloy). Under room temperature tensile loading, Hall–Petch strengthening mechanism was the most dominant wherein the addition of SiO2 nanoparticulates to pure magnesium enhances the strength within 0–2 vol% range and ductility in 0–1 vol% range.

Based on the nature of the links and interactions existing at the hybrid interface, hybrid materials can be broadly classified in two main designations: a) Hybrid compounds Class I, that include all systems with electrostatic forces, hydrogen bonding or Van der Waals interactions and b) Hybrid compounds Class II, showing that the inorganic and organic components are linked through strong covalent or ionic-covalent bonds. The physico–chemical properties of nanostructured copolymer acrylates based on butyl acrylate (BA), methyl methacrylate (MMA) and acrylic acid (AA) has been investigated employing un-modified SiO2 (Class I) and modified SiO2 particles (Class II) using 3-(trimethoxysilyl) propyl methacrylate (MPS) as compatibilizing agent. The synthesis was carried out using seeded batch emulsion polymerization system. Metastable nanostructured emulsions containing 1 wt% nanoparticles were obtained. Films casted from the in-situ nanostructured latex exhibited excellent optical transparency suggesting good nanoparticles dispersion. However, the mechanical properties showed by SiO2-MPS nanocomposite, are better than the Class I hybrid compounds. Therefore, SiO2-MPS surface treatment prior to polymerization enhances the physical properties of copolymer BA-MMA-AA film. The mass loss derivative traces for the polyacrylic nanocomposites and the neat polymer obtained by thermogravimetric analysis showed that the onset temperature for thermal decomposition was shifted towards a higher temperature than the neat polyacrylic, indicating the enhancement of thermal stability of the un-modified SiO2 nanocomposite. However, there is a decrease of 40°C in the decomposition temperature for the modified polyacrylic nanocomposite. The results obtained so far have shown that weak Van der Waals and H-bonding interactions may be sufficient to enable improvement of the physical properties of the acrylate nanocomposites.

The increasing demand for energy storage devices has propelled research for developing efficient super-capacitors (SC) with long cycle life and ultrahigh energy density. Carbon-based materials are commonly used as electrode materials for SC. Herein, we report a new approach to improve the SC performance utilizing a Porous Carbon/Cerium Oxide nanoparticle (PC-CON) hybrid as electrode material synthesized via a low temperature hydrothermal method. Through this approach, charges can be stored not only via electrochemical double layer capacitance (EDLC) from PC but also through pseudo-capacitive effect from CeO2 nanoparticles (NPs). The electrode-electrolyte interaction due to the electrochemical properties of the electrolyte provides an enhanced voltage window for the SC. Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM), X-ray Photoelectron Spectroscopy (XPS), and X-Ray Diffraction (XRD) measurements were used for the characterization of this PC/CeO2 hybrid material system. The testing results have shown that a maximum of 500% higher specific capacitance could be obtained using PC/CeO2 instead of using PC only.

Two metal fillers with TiC nanoparticles (TiC NPs) of less than 100 nm for the overlay process is an alternative to hardfacing for treating surfaces subjected to severe wear. In this work, the effect of tribological behavior for TiC NPs addition on two Co-based filler materials, as well as the dilutions, was studied. Mixtures of Co-based filler metals without and with 0.5% and 2% TiC NPs were deposited onto D2 steel plates using PTA (Plasma Transferred Arc). The BET surface area was 0.17 m2 g-1 and 0.31 m2 g-1, respectively, for Stellite 6 and 12. The distribution of ca 23% macroporous for Stellite 6 was sufficient to get inside the TiC NPs, as well as in the case of Stellite 12, with a pore distribution of ca 13%. Stellite 12 has an increase in the dilutions (70%) and enthalpies showed endothermic reactions. Stellite 6 with NPs was determined to be most effective in increasing the wear resistance.

Cr, V, and Fe amino borohydride complexes were synthesized using a solution based approach. Thermogravimetric Analysis with simultaneous Differential Scanning Calorimetry was used to investigate their decomposition behavior. The synthesized Cr and Fe complexes exhibited significant hydrogen release around 100 °C. The synthesized V complex showed a large mass loss at temperatures between 50 °C and 100 °C and release of amine byproducts. FTIR of decomposed intermediates showed the decomposition of Cr amino borohydride occurs through the simultaneous loss of hydrogen from both the borohydride and amino ligands, while the Fe complex displays preferential dehydrogenation of the borohydride over the amino ligand. The decomposed products take on a BN type structure when heated to 400 °C.

Oxidation behavior of alumina forming ferritic stainless steel (FeCrAl type stainless steels) grades APM and APMT, which are candidate alloys for fuel cladding, was studied using thermogravimetric analysis under dry air condition, and compared to that of ZIRLO®. In addition to the dry air condition, we also studied the high temperature oxidation behavior of APM and APMT under 100% steam condition in order to compare the effect of environment on the oxidation behavior of these alloys. APM and APMT showed an excellent oxidation resistance at high temperatures compared to ZIRLO® under dry air condition due to a stable Al2O3 oxide scale formed at the surface. Under steam condition, the oxidation rate of APM and APMT was found to be higher compared to that under the dry air condition.

Nanometer-sized fibers are recently getting increased attention in heterogeneous catalysis due to the superior transport properties and effective dispersion they offer. A key challenge in this application is creation of nanofibers with internal open porosity that can provide larger accessible catalytic surface and easier mass transport into the fibers. The synthesis of potassium doped iron/aluminum oxides ceramic nanofibers with mesoporous structure is presented herein. Uniform fiber mats were prepared by electrospinning (ES) using two different precursors: an aqueous solution of metal nitrates and an organic solution of metal acetylacetonates. The organic precursors gave rise to a promising mesoporous structure with fibers diameter mainly in the 300–400 nm range. Precursor viscosity was used as a stability indicator and its influence on the ES process was studied. Collection efficiency of as high as 90% was achieved. The increased understanding in fiber morphological evolution can open new possibilities in heterogeneous catalysis.

Poly(acrylamide-co-2-hydroxyethyl methacrylate), hydrogel microparticles were prepared by free radical copolymerization of acrylamide (AAm) and 2-hydroxyethyl methacrylate (2-HEMA) using an inverse emulsion polymerization technique, employing ethylene glycol dimethylacrylate (EGDMA) as crosslinker in the presence of w/o emulsifiers span-80 and span-85 (sorbitol mono-oleate) above the lower critical solution temperature. Water absorption capacity and characteristics of the hydrogel microparticles were analyzed by Optical Microscopy (OM), Scanning Electron Microscopy (SEM), Fourier Transform Infrared Spectroscopy (FTIR) and Thermogravimetric Analysis (TGA). Thus, microparticles were submitted to a gravimetric study on their ability to absorb and to retain distilled water at 25°C. One gram of microparticles absorbed at least 15 g of water. By varying the relative ratio between the continuous phase (hexane and emulsifiers) and the dispersed phase (monomers, initiator and crosslinker), non-agglomerated dispersed particles with nearly spherical shape were obtained having a narrow size distribution in the range from 10 to 20 µm. At a constant value of the emulsifier, and as a result of increasing the stirring rate, a particle size reduction was observed from 13 to 7 µm. The PAAm and PHEMA structures of synthesized hydrogel were confirmed using FTIR analysis. Additionally, through thermal analysis the P(AAm-HEMA) hydrogel showed an increase of water retention and thermal stability due to PAAm addition.