Papers by Keyword: Differential Scanning Calorimetry

Abstract: A non-Equi atomic W₂₄Ta₂₄Nb₂₄Cr₁₆Al₁₂ high entropy alloy (HEA) was designed based on thermodynamic calculations in order to obtain a single body-centered cubic (BCC) structure. The HEA was further fabricated by using the vacuum arc melting technique. The structural analysis of the HEA revealed the formation of a single BCC phase with the lattice parameter of 3.259Å. The micrograph of the HEA revealed dendritic structure with inter-dendritic segregations. The thermal analysis confirmed that the HEA is quite stable at high temperatures up to 1600°C. The thermal expansion of the HEA was also very low at 1100°C. The mechanical property such as the hardness of the HEA at room temperature, was quite high at 467 ± 20 HV₀.₅. The HEA was further heat treated at a very high temperature (1000°C) and the structural and mechanical properties were evaluated. The heat-treated HEA shows excellent structural stability as no secondary phases were formed in those samples. The mechanical property such as hardness of the HEA was increased continuously on increasing the heat treatment duration, which shows that the current alloy is highly preferable for possible high-temperature applications.

Abstract: In this experimental study, the mechanism and kinetic parameters of the metastable phases precipitation in the Al-Mg-Si alloy were determined thermally by differential scanning calorimetric (DSC) analysis. All samples were treated up to 550 °C at heating rates of 5, 10, 20 and 30 °C/min. The apparent activation energy (56.74 kJ/mol) and the Avrami exponent (0.99), were determined by DSC from the non-isothermal method, using the Ozawa, Boswell and Kissinger methods while those obtained by isothermal method using the Johnson-Mehl-Avrami-Kolmogorov (JMAK) model were 51.04 kJ/mol and 1.18. The activation energies values indicate that the formation of the metastable phases was mainly controlled by the migration of Mg and Si. The values of n, are characteristics of a growth of plate after saturation of nucleation. The frequency factor (k_o) calculated by the isothermal method is found to be 8.36×10⁷ s^-1.

Abstract: An alternative low thermal budget silicon carbide syntheses route is presented. The method is based on self-propagating high-temperature synthesis of binary silicon-carbon-based reactive mul­tilayers. With this technique, it is possible to obtain cubic polycrystalline silicon carbide at relatively low annealing temperatures by a solid state reaction. The reaction starts above 600 °C. The transformation process proceeds in a four-step process. The reaction enthalpy was determined to be (-70 ± 4) kJ/mol.

Abstract: The commercial Al–Zn–Mg–Cu-based alloys (7xxx series) are widely used in metalworking, automotive and aircraft industries as well as in aeronautical applications. The positive effect of the Sc,Zr-addition on mechanical properties of laboratory Al-based alloys is generally known. The microstructure, mechanical and thermal properties of the conventionally cast, heat-treated and cold-rolled Al–Zn–Mg–Cu (–Sc–Zr) alloys during isochronal annealing and natural ageing were studied. Microstructure observation by scanning electron microscopy and transmission electron microscopy proved the Zn,Mg,Cu-containing eutectic phase at grain boundaries. The distinct changes in microhardness curves as well as in a heat flow of the alloys studied are mainly caused by dissolution of the clusters/Guinier-Preston (GP) zones and precipitation of particles from the Al–Zn–Mg–Cu system. An easier diffusion of Zn, Mg and Cu atoms along dislocations in the cold-rolled alloys is responsible for the precipitation of the Zn,Mg,Cu-containing particles at lower temperatures compared to the cast alloys. Microhardness values of the heat-treated alloys increase immediately from the beginning of natural ageing due to the formation of the clusters/GP zones. Addition of Sc and Zr elements results in a higher hardness above ~ 270 °C due to a strengthening by coherent secondary Al₃(Sc,Zr) particles with a good thermal stability. Sc,Zr-addition has probably no influence on the evolution of the solute clusters/GP zones.

Abstract: In this work, we investigated the influence of physical aging on polylactic acid (PLA) films using thermal and optical techniques; Differential Scanning Calorimetry (DSC), Thermally Stimulated Depolarization Current (TSDC), and Attenuated Total Reflection Spectroscopy (ATR). The PLA films were aged for different periods: 60, 90, and 120 minutes at a temperature T_a = 43 °C. The result obtained by DSC showed that the effect of physical aging appeared as an endothermic peak, which increased with increasing aging time and evolved towards higher temperatures. TSDC results showed a thermal current peak located between 30 and 80 ° C, which represented the main relaxation mode (α relaxation) of the dielectric manifestation of the glass transition. The intensity of this peak decreased and was shifted to higher temperatures when aging time increased, this result can be explained by a decrease in the molecular mobility of macromolecular chains due to the decrease in the free volume. The effect of physical aging on the PLA by the ATR technique showed a gradual decrease in all absorption bands during the aging period. In particular, the wide absorption band between 3000 and 3700 cm^-1 attributed to the hydroxyl group (OH), which disappeared after two hours of aging

Abstract: In this article Therban AT 5065 VP, Therban AT 5005 VP - HBNR elastomers of different unsaturation degrees and their combined compositions research results (using optical and atomic force microscopy, DSC, DMA) are described. With these results structure and functional properties operational data of nitrile elastomers was obtained with no need of durable tests under different temperatures. It was found out that filler dispersion rises from 61.8 to 90.5 % and decomposition temperature grows from 261.9 to 275.3 °C while Therban AT 5005 VP share is increased from 20 to 50 weight parts. It is shown that elastomers with rubber ratio of 50:50 within temperature range from minus 30 to plus 150 °C have the lowest elasticity coefficient (from 311 to 1.6 MPa) and mechanical loss tangent (0.20) at the end of the test.

Abstract: High-pressure torsion (HPT) was conducted under 6.0 GPa on commercial purity titanium up to 10 turns. An ultrafine-grained (UFG) pure Ti with an average grain size of ~96 nm was obtained. The thermal properties of these samples were studied by using differential scanning calorimeter (DSC) which allowed the quantitative determination of the evolution of stored energy, the recrystallization temperatures, the activation energy involved in the recrystallization of the material and the evolution of the recrystallized fraction with temperature. The results show that the stored energy increases, beyond which the stored energy seems to level off to a saturated value with increase of HPT up to 5 turns. An average activation energy of about 101 kJ/mol for the recrystallization of 5 turns samples was determined. Also, the thermal stability of the grains of the 5 turns samples with subsequent heat treatments were investigated by microstructural analysis and Vickers microhardness measurements. It is shown that the average grain size remains below 246 nm when the annealing temperature is below 500 °C, and the size of the grains increases significantly for samples at the annealing temperature of 600 °C.

Abstract: Using differential scanning calorimetry, phase transitions in polycarbonate-polytetramethylene oxide block copolymers were studied. It is shown that, depending on the ratio of rigid polycarbonate and flexible polytetramethylene oxide units, block copolymers can be two-phase or four-phase. It is shown that phase transitions in copolymers of a polyester-polyether depend on the ability to crystallize the components.

Abstract: The series of compositions containing thermodynamically incompatible flexible blocks of aliphatic polyesters and rigid blocks of aromatic bis (urethane) imides in the volume of polymers was obtained on the basis of multiblock (segmented) poly (urethane-imides) and related aromatic polyimides. The series includes segmented poly (urethane-imides) with different relative content of flexible and rigid blocks, non-segregating mixtures of poly (urethane-imides) and thermoplastic partially crystalline polyimide, statistical copolymers of poly (urethane-imide) with imide, and non-segregating mixtures of statistical copolymers with thermoplastic polyimide. The derived polymer systems were studied using thermogravimetric analysis, differential scanning calorimetry, and dynamic mechanical analysis. The deformation and strength properties of film samples are determined. It is shown that the properties of the studied polymers change as their content of imides blocks increases, and the transition from thermoplastic poly (urethane-imide) elastomers to thermoplastic polyimides is observed.

Abstract: A synthesis of new di-and triblock polyurethane thermoplastic copolymers containing different mass ratio of two crystallizing blocks - poly (1,4-butylene glycol) adipate and poly-ε-caprolactone diols was developed. Using combination of danamometric analysis, IR-spectroscopy, differential scanning calorimetry and X-ray diffraction, the effect of the soft block composition and crystallization conditions on crystal structure and thermal behavior of the obtained polymers have been studied. For the triblock copolymers we have shown a possibility of control the kinetics of material hardening and final mechanical characteristics due to the mutual influence of polydiols during crystallization. In the result, the second crystallizing component allows to control amount, structure and quality of crystalline domains in polyurethanes by variation of crystallization conditions.