simultaneous thermal analysis
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Energies ◽  
2022 ◽  
Vol 15 (1) ◽  
pp. 368
Author(s):  
Karol Sztekler ◽  
Agata Mlonka-Mędrala ◽  
Nezar H. Khdary ◽  
Wojciech Kalawa ◽  
Wojciech Nowak ◽  
...  

Due to a high risk of power outages, a heat-driven adsorption chillers are gaining the attention. To increase the efficiency of the chiller, new adsorbents must be produced and examined. In this study, four newly developed silica–based porous materials were tested and compared with silica gel, an adsorber commonly paired with water. Extended sorption tests using mercury intrusion porosimetry, gas adsorption, and dynamic vapor sorption were performed. The morphology of the samples was determined using a scanning electron microscope. The thermal properties were defined using simultaneous thermal analysis and a laser flash method. Metal organic silica (MOS) nanocomposites analysed in this study had thermal properties similar to those of commonly used silica gel. MOS samples have a thermal diffusivity coefficient in the range of 0.17–0.25 mm2/s, whereas silica gel of about 0.2 mm2/s. The highest water adsorption capacity was measured for AFSMo-Cu and equal to 33–35%. For narrow porous silica gel mass uptake was equal about 25%. In the case of water adsorption, it was observed that the pore size of the sorbent is essential, and adsorbents with pore sizes higher than 5 nm, are most recommended in working pairs with water.


Polymers ◽  
2021 ◽  
Vol 14 (1) ◽  
pp. 57
Author(s):  
Cristina Pérez-Fernández ◽  
Pilar Valles ◽  
Elena González-Toril ◽  
Eva Mateo-Martí ◽  
José Luis de la Fuente ◽  
...  

A systematic study is presented to explore the NH4CN polymerization induced by microwave (MW) radiation, keeping in mind the recent growing interest in these polymers in material science. Thus, a first approach through two series, varying the reaction times and the temperatures between 130 and 205 °C, was conducted. As a relevant outcome, using particular reaction conditions, polymer conversions similar to those obtained by means of conventional thermal methods were achieved, with the advantage of a very significant reduction of the reaction times. The structural properties of the end products were evaluated using compositional data, spectroscopic measurements, simultaneous thermal analysis (STA), X-ray diffraction (XRD), and scanning electron microscopy (SEM). As a result, based on the principal component analysis (PCA) from the main experimental results collected, practically only the crystallographic features and the morphologies in the nanoscale were affected by the MW-driven polymerization conditions with respect to those obtained by classical syntheses. Therefore, MW radiation allows us to tune the morphology, size and shape of the particles from the bidimensional C=N networks which are characteristic of the NH4CN polymers by an easy, fast, low-cost and green-solvent production. These new insights make these macromolecular systems attractive for exploration in current soft-matter science.


Polymers ◽  
2021 ◽  
Vol 13 (24) ◽  
pp. 4374
Author(s):  
Mikhail M. Simunin ◽  
Anton S. Voronin ◽  
Yurii V. Fadeev ◽  
Yurii L. Mikhlin ◽  
Denis A. Lizunov ◽  
...  

Small additions of nanofiber materials make it possible to change the properties of polymers. However, the uniformity of the additive distribution and the strength of its bond with the polymer matrix are determined by the surface of the nanofibers. Silanes, in particular, allow you to customize the surface for better interaction with the matrix. The aim of our work is to study an approach to silanization of nanofibers of aluminum oxide to obtain a perfect interface between the additive and the matrix. The presence of target silanes on the surface of nanofibers was shown by XPS methods. The presence of functional groups on the surface of nanofibers was also shown by the methods of simultaneous thermal analysis, and the stoichiometry of functional groups with respect to the initial hydroxyl groups was studied. The number of functional groups precipitated from silanes is close to the number of the initial hydroxyl groups, which indicates a high uniformity of the coating in the proposed method of silanization. The presented technology for silanizing alumina nanofibers is an important approach to the subsequent use of this additive in various polymer matrices.


Author(s):  
Sebastian Johann Müllner ◽  
Tilo Held ◽  
Achim Schmidt-Rodenkirchen ◽  
Thorsten Gerdes ◽  
Christina Roth

Abstract Lithium-ion batteries with Si anodes are still attracting increasing attention, particularly due to the high specific energy density. The main disadvantage of silicon as anode material is its reduced cell performance in terms of cycling stability. One promising approach to improve this is embedding silicon nanoparticles in a graphene-like matrix via spray drying. All processes described so far need a time- and energy-intensive two-step-synthesis to obtain the graphene-like rGO structure. Here, we present a reactive spray drying process for synthesis of Si/rGO composites. For proper reactor design, the reaction kinetics are investigated by simultaneous thermal analysis in various atmospheres. We can describe thermal decomposition of GO to rGO as a second-order reaction. STA data also show that additional presence of water in the atmosphere due to the one-step synthesis is negligible at temperatures below 600 °C for both the reaction of GO and the additional oxidation of Si. To evaluate the electrochemical performance, the composites are cycled in a half cell setup. Delithiation capacity after cell formation could be raised from 252 mAh g-1 for GO to 327 mAh g-1 for rGO. In addition, we are able to synthesize Si-containing composites suitable for the anode of LiB using our process.


2021 ◽  
Author(s):  
pragnesh N Dave ◽  
Ruksana Sirach ◽  
Riddhi Thakkar ◽  
M P Deshpande

Abstract Less sensitive high energetic materials (HEMs) are explored as a potential replacement of highly sensitive HEMs in propellants, and explosive applications. More research have been devoted to improve the thermal decomposition of such a less sensitive HEMs. Nanosize Cobalt ferrite (CoF) has been successfully synthesized using the co-precipitation method. Synthesis of less sensitive HEM 3-nitro-2,4-dihydro-3H-1,2,4-triazol-5-one(NTO) and its size reduction using solvent-antisolvent method is successfully achieved. Effect of 5 % by weight CoF on the thermolysis of NTO and NTO with reduced size (r-NTO) has been studied using the simultaneous thermal analysis. Three isoconversional methods namely Flynn Ozawa Wall, Kissinger-Akahira-Sunose (KAS), and Starink are employed to evaluate the kinetic parameter of NTO, and r-NTO in the presence of CoF additive. It was found that both the addition of CoF as well as reducing size of NTO can decrease the thermal decomposition temperature of NTO, the later decreasing the thermal decomposition temperature to a good extent compared to former. However, the kinetic study using isoconversional methods suggested that in the presence of CoF additive, the activation energy of both NTO as well as n-NTO is increased.


2021 ◽  
Vol 47 (11) ◽  
pp. 769-779
Author(s):  
E. V. Korneeva ◽  
E. V. Novikova ◽  
O. V. Loseva ◽  
A. I. Smolentsev ◽  
A. V. Ivanov

Abstract The capability of silver(I) cyclo-hexamethylenedithiocarbamate to concentrate gold(III) from solutions characterized by a high level of salinity (5.15 M NaCl) into the solid phase has been established. The double chloroform-solvated Au(III)–Ag(I) complex [Au{S2CN(CH2)6}2]2[AgCl2]Cl·2CHCl3 (I) was preparatively isolated as an individual form of binding of [AuCl4]– anions. The composition of the ionic structural units of compound I indicates that gold(III) binding from a solution to the solid phase is accompanied by the complete redistribution of the HmDtc ligands between the coordination spheres of Ag(I) and Au(III). Complex I characterized by IR spectroscopy, simultaneous thermal analysis, and X-ray structure analysis (CIF file CCDC no. 2051654) exhibits the supramolecular structure containing two oppositely charged pseudo-polymeric subsystems. Complex cations [Au{S2CN(CH2)6}2]+ and anions [AgCl2]– (in a ratio of 2 : 1) form a complicatedly organized cation-anionic pseudo-polymeric ribbon ({[Au(HmDtc)2]⋅⋅⋅[AgCl2]⋅⋅⋅[Au(HmDtc)2]}+)n due to secondary interactions Ag⋅⋅⋅S (3.2613 Å) and Au⋅⋅⋅Cl (3.2765 Å). The pseudo-polymeric ribbon consists of two rows of cations and a row of anions. The outer-sphere chloride ions combine the solvate chloroform molecules by two equivalent hydrogen bonds Cl⋅⋅⋅H–C yielding anion-molecular triads [Cl3CH⋅⋅⋅Cl⋅⋅⋅HCCl3]–, which are involved in the formation of the supramolecular ribbon due to the secondary Cl⋅⋅⋅Cl interactions (3.4058 Å) between the nonequivalent chlorine atoms of the nearest solvate molecules. The study of the thermal behavior of complex I makes it possible to determine the character of thermolysis and conditions for the quantitative regeneration of bound gold.


2021 ◽  
Vol 882 (1) ◽  
pp. 012009
Author(s):  
Imelda Hutabarat

Abstract The development of extracting hydrometallurgical process for copper sulphide mineral becomes one of the promising fields, not only for the copper production but also for the production of metal by-products. The advantage of the thermal analysis is to get the phase form of the minerals on a certain temperature. With this result, the chosen metal can be selectively extracted. The goal of this study is to understand the thermal reaction of the copper sulphide as the basic data to develop a process flowsheet of extracting copper and other important metals from the copper concentrates by using an alternative new hydrometallurgy process to increase the value of the minerals. The thermal behaviour was investigated by simultaneous thermal analysis consisting of differential scanning calorimetry (DSC) in combination with thermo gravimetry (TG) and fourier transform infrared (FTIR) spectroscopy. Samples were pre-treated by roasting at the several temperature transitions and subsequently characterized by XRD and scanning electron microscopy with energy dispersive spectroscopy (SEM-EDS).


Polymers ◽  
2021 ◽  
Vol 13 (21) ◽  
pp. 3702
Author(s):  
David Kalaš ◽  
Karel Šíma ◽  
Petr Kadlec ◽  
Radek Polanský ◽  
Radek Soukup ◽  
...  

The present study is a focused and comprehensive analysis of the dielectric and thermal properties of twenty-four 3D printed polymers suitable for fused filament fabrication (FFF) in electronic applications. The selected polymers include various thermoplastic elastomers, such as thermoplastics based on polycarbonate (PC), polyethylene terephthalate glycol (PETG), and acrylonitrile butadiene styrene (ABS-T). Their overall thermal behavior, including oxidation stability, glass transition, and melting temperature, was explored using simultaneous thermal analysis (STA) and differential scanning calorimetry (DSC). Considering their intended usage in electronic applications, the dielectric strength (Ep) and surface/volume resistivity (ρs/ρv) were comprehensively tested according to IEC 60243-1 and IEC 62631-3, respectively. The values of the dielectric constant (ε’) and loss factor (ε”) were also determined by broadband dielectric spectroscopy (BDS). While, on the one hand, exceptional dielectric properties were observed for some thermoplastic elastomers, the materials based on PCs, on the other hand, stood out from the others due to their high oxidation stability and above average dielectric properties. The low-cost materials based on PETG or ABS-T did not achieve thermal properties similar to those of the other tested polymers; nevertheless, considering the very reasonable price of these polymers, the obtained dielectric properties are promising for undemanding electronic applications.


Catalysts ◽  
2021 ◽  
Vol 11 (10) ◽  
pp. 1256
Author(s):  
Liliya V. Yafarova ◽  
Grigory V. Mamontov ◽  
Irina V. Chislova ◽  
Oleg I. Silyukov ◽  
Irina A. Zvereva

The paper is focused on the Fe for Co substitution effect on the redox and catalytic properties in the perovskite structure of GdFeO3. The solid oxides with the composition GdFe1−xCoxO3 (x = 0; 0.2; 0.5; 0.8; 1) were obtained by the sol-gel method and characterized by various methods: X-Ray diffraction (XRD), temperature-programmed reduction (H2-TPR), N2 sorption, temperature-programmed desorption of oxygen (TPD-O2), simultaneous thermal analysis (STA), and X-ray photoelectron spectroscopy (XPS). The H2-TPR results showed that an increase in the cobalt content in the GdFe1−xCoxO3 (x = 0; 0.2; 0.5; 0.8; 1) leads to a decrease in the reduction temperature. Using the TPD-O2 and STA methods, the lattice oxygen mobility is increasing in the course of the substitution of Fe for Co. Thus, the Fe substitution in the perovskite leads to an improvement in the oxygen reaction ability. Experiments on the soot oxidation reveal that catalytic oxidation ability increases in the series: GdFe0.5Co0.5O3 ˂ GdFe0.2Co0.8O3 ˂ GdCoO3, which is in good correlation with the increasing oxygen mobility according to H2-TPR, TPD-O2, and STA results. The soot oxidation over GdFeO3 and GdFe0.8Co0.2O3 is not in this range due to the impurities of iron oxides and higher specific surface area.


Materials ◽  
2021 ◽  
Vol 14 (20) ◽  
pp. 6108
Author(s):  
David Bombac ◽  
Martin Lamut ◽  
Primož Mrvar ◽  
Brane Širok ◽  
Benjamin Bizjan

A developed methodology for determining the physical properties of mineral fibers prepared from different input mixtures under the same spinning wheel conditions is described and discussed. Energy dispersive X-ray fluorescence spectroscopy was combined with simultaneous thermal analysis and thermogravimetry to study the mineralogical composition and typical melting and crystallization temperatures. The mechanical properties measured with nanoindentation were related to the mineralogical properties and the results obtained are in agreement with the literature. The developed methodology shows reliable performance and demonstrates the ability to study the mechanical properties of mineral fibers, their mineralogical composition, and thermal properties. The presented experimental methodology opens up the possibility of researching the mechanical properties of mineral fibers for the purpose of defining production recipes in the field of mineral thermal insulation materials.


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