Showing papers on "Differential scanning calorimetry published in 2017"

Effect of preparation methods on the properties of titania nanoparticles: solvothermal versus sol–gel

Abstract: Titania (TiO2) nanoparticles (NP’s) have been prepared by solvothermal and sol–gel techniques using different surfactants such as acetic acid (AA), oleylamine (OM), and AA + OM. The solution was thermally treated at growth temperature 180 °C in solvothermal method. TiO2 powder, prepared using both methods, was subjected to post heat treatment at 550 and 950 °C. The effect of surfactants on the morphology of TiO2 NP’s was studied by transmission electron microscopy (TEM) and field emission scanning electron microscopy (FESEM). The structural and thermal properties of titania NP’s are investigated by means of X-ray diffraction, Raman spectroscopy, thermogravimetric analysis, and differential scanning calorimetry (TGA/DSC). TEM and FESEM images illustrated various shapes of titania NP’s such as irregular spherical, rounded rectangular, truncated rhombic, oval, and rod-like structure in presence of different surfactants. Moreover, TiO2 particles prepared by sol–gel method were almost 40 times greater than those prepared by solvothermal method. In addition to the improvement in the crystallinity, thermal stability has been enhanced due to consolidation of individual particles at higher annealing temperature in solvothermal technique. Furthermore, a reduction in the degradation temperature and phase transformation of TiO2 NP’s were conspicuously corroborated after post-heat treatment.

Quantitative Phase-Change Thermodynamics and Metastability of Perovskite-Phase Cesium Lead Iodide

Abstract: The perovskite phase of cesium lead iodide (α-CsPbI3 or “black” phase) possesses favorable optoelectronic properties for photovoltaic applications. However, the stable phase at room temperature is a nonfunctional “yellow” phase (δ-CsPbI3). Black-phase polycrystalline thin films are synthesized above 330 °C and rapidly quenched to room temperature, retaining their phase in a metastable state. Using differential scanning calorimetry, it is shown herein that the metastable state is maintained in the absence of moisture, up to a temperature of 100 °C, and a reversible phase-change enthalpy of 14.2 (±0.5) kJ/mol is observed. The presence of atmospheric moisture hastens the black-to-yellow conversion kinetics without significantly changing the enthalpy of the transition, indicating a catalytic effect, rather than a change in equilibrium due to water adduct formation. These results delineate the conditions for trapping the desired phase and highlight the significant magnitude of the entropic stabilization of thi...

Impact of the Fused Deposition (FDM) Printing Process on Polylactic Acid (PLA) Chemistry and Structure

Abstract: Polylactic acid (PLA) is an organic polymer commonly used in fused deposition (FDM) printing and biomedical scaffolding that is biocompatible and immunologically inert. However, variations in source material quality and chemistry make it necessary to characterize the filament and determine potential changes in chemistry occurring as a result of the FDM process. We used several spectroscopic techniques, including laser confocal microscopy, Fourier transform infrared (FTIR) spectroscopy and photoacousitc FTIR spectroscopy, Raman spectroscopy, and X-ray photoelectron spectroscopy (XPS) in order to characterize both the bulk and surface chemistry of the source material and printed samples. Scanning electron microscopy (SEM) and differential scanning calorimetry (DSC) were used to characterize morphology, cold crystallinity, and the glass transition and melting temperatures following printing. Analysis revealed calcium carbonate-based additives which were reacted with organic ligands and potentially trace metal impurities, both before and following printing. These additives became concentrated in voids in the printed structure. This finding is important for biomedical applications as carbonate will impact subsequent cell growth on printed tissue scaffolds. Results of chemical analysis also provided evidence of the hygroscopic nature of the source material and oxidation of the printed surface, and SEM imaging revealed micro- and submicron-scale roughness that will also impact potential applications.

High Volumetric Capacity of Hollow Structured SnO2@Si Nanospheres for Lithium-Ion Batteries.

Abstract: A novel design of hollow structured SnO2@Si nanospheres was presented, which not only demonstrates high volumetric capacity as anode of LIBs, but also prevents aggregation of Sn and confines solid electrolyte interphase thickening. An impressive volumetric specific capacity of 1030 mAh cm–3 was maintained after 500 cycles. The electrochemical impedance spectroscopy and differential scanning calorimetry indicated that solid electrolyte interphase can be confined in pores of as-prepared hollow structured SnO2@Si.

Properties of Water Bound in Hydrogels

Abstract: In this review, the importance of water in hydrogel (HG) properties and structure is analyzed. A variety of methods such as ¹H NMR (nuclear magnetic resonance), DSC (differential scanning calorimetry), XRD (X-ray powder diffraction), dielectric relaxation spectroscopy, thermally stimulated depolarization current, quasi-elastic neutron scattering, rheometry, diffusion, adsorption, infrared spectroscopy are used to study water in HG. The state of HG water is rather non-uniform. According to thermodynamic features of water in HG, some of it is non-freezing and strongly bound, another fraction is freezing and weakly bound, and the third fraction is non-bound, free water freezing at 0 °C. According to structural features of water in HG, it can be divided into two fractions with strongly associated and weakly associated waters. The properties of the water in HG depend also on the amounts and types of solutes, pH, salinity, structural features of HG functionalities.

A Smart Latent Catalyst Containing o-Trifluoroacetamide Functional Benzoxazine: Precursor for Low Temperature Formation of Very High Performance Polybenzoxazole with Low Dielectric Constant and High Thermal Stability

Abstract: A novel difunctional benzoxazine with o-trifluoroacetamide functionality has been synthesized via Mannich condensation. The chemical structure of synthesized monomer has also been confirmed by 1H, 13C, and 19F nuclear magnetic resonance (NMR) spectroscopy and Fourier transform infrared (FT-IR) spectroscopy. The ring-opening polymerization of the resin and the subsequent conversion of the freshly generated polybenzoxazine into polybenzoxazole are studied by FT-IR and differential scanning calorimetry (DSC). In addition to the advantage of low polymerization temperature as other reported o-amide benzoxazines, the o-trifluoroacetamide benzoxazine also exhibits an unexpected lower benzoxazole formation temperature. Furthermore, the resulting fluorinated polybenzoxazole derived from the benzoxazine monomer possesses the combined excellent properties of facile synthesis, easy processability, low dielectric constant, high thermal stability, and long shelf life, evidencing its potential applications in microelect...

Self‐Healing Behavior in a Thermo‐Mechanically Responsive Cocrystal during a Reversible Phase Transition

Abstract: The molecular-level motions of a coronene-based supramolecular rotator are amplified into macroscopic changes of crystals by co-assembly of coronene and TCNB (1,2,4,5-tetracyanobenzene) into a charge-transfer complex. The as-prepared cocrystals show remarkable self-healing behavior and thermo-mechanical responses during thermally-induced reversible single-crystal-to-single-crystal (SCSC) phase transitions. Comprehensive analysis of the microscopic observations as well as differential scanning calorimetry (DSC) measurements and crystal habits reveal that a thermally-reduced-rate-dependent dynamic character exists in the phase transition. The crystallographic studies show that the global similarity of the packing patterns of both phases with local differences, such as molecular stacking sequence and orientations, should be the origin of the self-healing behavior of these crystals.

Magnetic activated carbon loaded with tungsten oxide nanoparticles for aluminum removal from waters

Abstract: Magnetic activated carbon/tungsten nanocomposite (AC/Fe/W) was prepared as an environmentally friendly cost-effective adsorbent. Its chemical, morphological, thermal degradation and surface properties were characterized by Fourier transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM), energy dispersive X-ray (EDX), Thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC) and surface area (BET) techniques. The developed adsorbent was used for the remediation of Al(III) ions from aqueous solution. The optimum experimental conditions were found under response surface methodology (RSM) using central composite design (CCD). The adsorption efficiency was achieved up to 90% within 45 min at pH 5 at 24 °C. To investigate the suitability of the process, the equilibrium data were evaluated by Langmuir and Freundlich isotherm models. The adsorption capacity of AC/Fe/W composite was found to be 184.12 mg g−1. The kinetic examinations showed that the pseudo-second order was the best fitting model to explain the adsorption mechanism. The activation energy of adsorption (Ea) was determined as 2.04 kJ mol−1, indicating that the adsorption process was carried out via physical sorption mechanism. Thermodynamic findings indicated the exothermic and spontaneous nature of the adsorption process and increased randomness at the solid-solution interface. By using 1.0 mol L−1 HCl solution, the adsorbed Al(III) ions were desorbed at high effectiveness and also the composite can be reused up to five cycles. Based on all of the results, it can be concluded that the fabricated composite material is effective and promising adsorbent for the cleaning treatment of Al(III) ions from wastewaters by large-scale designed adsorption system.

High-Strength Stereolithographic 3D Printed Nanocomposites: Graphene Oxide Metastability

Abstract: The weak thermomechanical properties of commercial 3D printing plastics have limited the technology’s application mainly to rapid prototyping. In this report, we demonstrate a simple approach that takes advantage of the metastable, temperature-dependent structure of graphene oxide (GO) to enhance the mechanical properties of conventional 3D-printed resins produced by stereolithography (SLA). A commercially available SLA resin was reinforced with minimal amounts of GO nanofillers and thermally annealed at 50 and 100 °C for 12 h. Tensile tests revealed increasing strength and modulus at an annealing temperature of 100 °C, with the highest tensile strength increase recorded at 673.6% (for 1 wt % GO). Thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC) also showed increasing thermal stability with increasing annealing temperature. The drastic enhancement in mechanical properties, which is seen to this degree in 3D-printed samples reported in literature, is attributed to the metastable...

Characterization of Antimicrobial Poly (Lactic Acid)/Nano-Composite Films with Silver and Zinc Oxide Nanoparticles.

Abstract: Antimicrobial active films based on poly (lactic acid) (PLA) were prepared with nano-silver (nano-Ag) and nano-zinc oxide (nano-ZnO) using a solvent volatilizing method. The films were characterized for mechanical, structural, thermal, physical and antimicrobial properties. Scanning electron microscopy (SEM) images characterized the fracture morphology of the films with different contents of nano-Ag and nano-ZnO. The addition of nanoparticles into the pure PLA film decreased the tensile strength and elasticity modulus and increased the elongation of breaks-in other words, the flexibility and extensibility of these composites improved. According to the results of differential scanning calorimetry (DSC), the glass transition temperature of the PLA nano-composite films decreased, and the crystallinity of these films increased; a similar result was apparent from X-ray diffraction (XRD) analysis. The water vapor permeability (WVP) and opacity of the PLA nano-composite films augmented compared with pure PLA film. Incorporation of nanoparticles to the PLA films significantly improved the antimicrobial activity to inhibit the growth of Escherichia coli. The results indicated that PLA films with nanoparticles could be considered a potential environmental-friendly packaging material.

Investigation of structural, thermal properties and shielding parameters for multicomponent borate glasses for gamma and neutron radiation shielding applications

Abstract: Multicomponent borate glasses with the chemical composition (60 − x) B2O3–10 Bi2O3–10 Al2O3–10 ZnO–10 Li2O–(x) Dy2O3 or Tb4O7 (x = 0.5 mol%), and (60 − x − y) B2O3–10 Bi2O3–10 Al2O3–10 ZnO–10 Li2O–(x) Dy2O3–(y) Tb4O7 (x = 0.25, 0.5, 0.75, 1.0, 1.5, and 2.0 mol%, y = 0.5 mol%) have been fabricated by a conventional melt-quenching technique and were characterized by X-ray diffraction (XRD), Attenuated Total reflectance-Fourier transform Infrared (ATR-FTIR) spectroscopy, Raman spectroscopy, thermo-gravimetric analysis (TGA), and differential scanning calorimetry (DSC). Also, the radiation shielding parameters such as mass attenuation coefficient (μ/ρ), half value layer (HVL), mean free path (MFP) and exposure buildup factor (EBF) values were explored within the energy range 0.015 MeV–15 MeV using both XCOM and MCNPX code to determine the penetration of gamma and neutron radiations in the prepared glasses. The main BO3, BO4, BiO6, and ZnO4 structural units and AlOAl bonds were confirmed by ATR-FTIR and Raman spectroscopy. Weight loss, and the glass transition (Tg), onset crystallization (Tx), and crystallization (Tc) temperatures were determined from TGA and DSC measurements, respectively. The stability of the glass against crystallization (ΔT) is varied within the temperature range 114–135 °C for the studied glasses. In addition, the shielding parameters like the (μ/ρ) values investigated using both MCNPX Monte Carlo and XCOM software are in good agreement with each other. The (μ/ρ) values calculated using XCOM software were used to evaluate the HVL and MFP in the photon energy range 0.015 MeV–15 MeV. It is found that all the synthesized glasses possess better shielding properties than ordinary concrete, zinc oxide soda lime silica glass and lead zinc phosphate glass indicating the high potentiality of the prepared glasses to be utilized as radiation shielding materials.