scholarly journals Microstructure and Crystallization Kinetics of Polyurethane Thermoplastics Containing Trisilanol Isobutyl POSS

2012 ◽  
Vol 2012 ◽  
pp. 1-8 ◽  
Author(s):  
Vinicius Pistor ◽  
Daniela de Conto ◽  
Felipe Gustavo Ornaghi ◽  
Ademir José Zattera

The synthesis of thermoplastic polyurethanes (TPU) from the reaction of a NCO group-containing prepolymer and 0, 1.14, 1.71, and 2.28 wt% of trisilanol isobutyl polyhedral oligomeric silsesquioxane (POSS) was carried out in an instrumented batch mixer. The samples were characterized by thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), X-ray diffraction (XRD), and scanning electron microscopy (SEM). SEM analysis shows that the incorporation of POSS promoted strongly aggregation through physical interactions (formation of POSS-rich domains). Modifications in the TPU microstructure and the reduction in the crystal size were observed in the XRD diffractograms. The incorporation of POSS equally altered the TPU crystallization, and samples bearing higher concentrations of POSS formed two distinct types of crystalline structures. The kinetics of crystallization showed that nucleation strongly depends on the balance between TPU crystal formation and POSS-rich domains.

1997 ◽  
Vol 481 ◽  
Author(s):  
R. R. Chromik ◽  
W. K. Neils ◽  
E. J. Cotts

ABSTRACTThe kinetics of the formation of Cu3Si in Cu/a-Si diffusion couples have been investigated by means of differential scanning calorimetry and x-ray diffraction. Multilayered composites of average stoichiometry Cu3Si were prepared by sputter deposition with individual layer thicknesses varying in different samples between 2 and 100 nm. We observed diffusion limited growth of Cu3 Si upon annealing these diffusion couples below 500 K. Reaction constants were measured for a temperature range of 455 to 495 K for thicknesses of growing Cu3Si between 2.6 and 80 nm. The temperature dependence of the reaction constant, k2, was characterized as k2 = k0 exp(− Ea/kbT) with activation energy, Ea = 1.0 eV/atom and pre-factor, k0 = 1.9×10−3 cm2/s.


2020 ◽  
Vol 869 ◽  
pp. 273-279
Author(s):  
Marina A. Gorbunova ◽  
Denis V. Anokhin ◽  
Valentina A. Lesnichaya ◽  
Alexander A. Grishchuk ◽  
Elmira R. Badamshina

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.


2014 ◽  
Vol 2014 ◽  
pp. 1-9
Author(s):  
R. K. Koul ◽  
Shivani Suri ◽  
Vishal Singh ◽  
K. K. Bamzai

Synthesis of mixed gadolinium calcium heptamolybdate (GdCaHM) system in silica gel medium using single gel single tube technique has been successfully achieved. The grown crystal exhibits various morphologies, which includes spherulites, multifaceted, and square platelets. The nature of the grown material was established by X-ray diffraction (XRD) studies. Fourier transform infrared spectroscopy (FTIR) study signifies the presence of heptamolybdate (Mo7O24) and water symmetry structure, whereas energy dispersive X-ray analysis (EDAX) establishes the stoichiometric of the grown crystal as GdCaMo7O24·8H2O. The thermal behaviour was studied using the thermoanalytical techniques, which include thermogravimetry (TG), differential thermal analysis (DTA), and differential scanning calorimetry (DSC). Results obtained on the application of TG based models, namely, Horowitz-Metzger, Coats-Redfern, and Piloyan-Novikova, suggest the contracting cylindrical model as the relevant model for the thermal decomposition of the material. The kinetic parameters, namely, the order of reaction (n), activation energy (Ea), frequency factor (Z), and entropy (ΔS*), were also calculated using these three models.


2014 ◽  
Vol 32 (3) ◽  
pp. 385-390
Author(s):  
Aysel Kantürk Figen ◽  
Bilge Coşkuner ◽  
Sabriye Pişkin

AbstractIn the present study, hydrogen desorption properties of magnesium hydride (MgH2) synthesized from modified waste magnesium chips (WMC) were investigated. MgH2 was synthesized by hydrogenation of modified waste magnesium at 320 °C for 90 min under a pressure of 6 × 106 Pa. The modified waste magnesium was prepared by mixing waste magnesium with tetrahydrofuran (THF) and NaCl additions, applying mechanical milling. Next, it was investigated by X-ray diffraction (XRD), X-ray fluorescence (XRF), scanning electron microscopy (SEM) and Brunauer-Emmett-Teller (BET) techniques in order to characterize its structural properties. Hydrogen desorption properties were determined by differential scanning calorimetry (DSC) under nitrogen atmosphere at different heating rates (5, 10, and 15 °C/min). Doyle and Kissenger non-isothermal kinetic models were applied to calculate energy (Ea) values, which were found equal to 254.68 kJ/mol and 255.88 kJ/mol, respectively.


1996 ◽  
Vol 460 ◽  
Author(s):  
M. T. Clavaguera-Mora ◽  
J. Zhu ◽  
M. Meyer ◽  
L. Mendoza-Zelis ◽  
F. H. Sanchez ◽  
...  

ABSTRACTThe evolution of the B2-AlFe phase during mechanical grinding in Ar has been examined as a function of milling time by X-Ray diffraction, transmission Mössbauer spectroscopy and differential scanning calorimetry. Short and long range disorder was observed to increase with the mechanical treatment up to the attainment of a steady state. The evolution of the long range order parameter and of the local atomic configurations at Fe sites were analyzed in terms of possible mechanisms for milling induced disordering. The kinetics of the thermal reordering was studied under continuous heating and isothermal calorimetrie regimes. Modeling of the reordering processes by diffusion controlled growth of pre-existing ordered grains is presented as well as the estimated values of both the enthalpy and the activation energy of the reordering process. The results are consistent with a non uniform distribution of disorder throughout the sample and will be compared with preceding information on related systems.


CrystEngComm ◽  
2018 ◽  
Vol 20 (22) ◽  
pp. 3105-3116 ◽  
Author(s):  
Roman Svoboda ◽  
Roman Bulánek ◽  
Dušan Galusek ◽  
Roghayeh Hadidimasouleh ◽  
Yadolah Ganjkhanlou

Differential scanning calorimetry and in situ X-ray diffraction analysis were used to study the products and mechanism of crystal formation in VOx–ZrO2 ceramics.


2011 ◽  
Vol 172-174 ◽  
pp. 646-651 ◽  
Author(s):  
Gamra Tellouche ◽  
Khalid Hoummada ◽  
Dominique Mangelinck ◽  
Ivan Blum

The phase formation sequence of Ni silicide for different thicknesses is studied by in situ X ray diffraction and differential scanning calorimetry measurements. The formation of a transient phase is observed during the formation of δ-Ni2Si; transient phases grow and disappear during the growth of another phase. A possible mechanism is proposed for the transient phase formation and consumption. It is applied to the growth and consumption of θ-Ni2Si. A good accordance is found between the proposed model and in situ measurement of the kinetics of phase formation obtained by x-ray diffraction and differential scanning calorimetry for higher thickness.


2014 ◽  
Vol 960-961 ◽  
pp. 161-164 ◽  
Author(s):  
Juan Mu ◽  
Hai Feng Zhang

Glass forming ability and crystallization kinetics of Al-Mg-Ni-La alloys have been investigated by X-ray diffraction (XRD) and differential scanning calorimetry (DSC). The maximum thickness achievable in glasses of Al76Mg11Ni8La5and Al69Mg18Ni8La5ribbons were 200 and 120 μm, respectively. The crystallization temperature and peak temperature indicated by DSC measurements displayed dependence on the heating rate during continuous heating, and were coincident with Lanoka’s relationship. The activation energies for the crystallization reactionExwere obtained from the Kissinger’s equation. The results show the Mg addition is beneficial to the thermal stability of the amorphous phase.


2016 ◽  
Vol 881 ◽  
pp. 83-88 ◽  
Author(s):  
Rafael Bianchini Nuernberg ◽  
Oscar Rubem Klegues Montedo

This work aims to investigate the crystallization kinetics of β-spodumene/cordierite glass-ceramics. Thus, three glasses with compositions based predominantly on cordierite (C), β-spodumene (L) and in a molar ratio 1:1 of both phases (CL) were prepared. The kinetics parameters such as activation energy for crystallization (ranging from 160 to 358 kJ/mol) and Avrami exponent (ranging from 1.4 to 10.7) were determined by means of non-isothermal methods using differential scanning calorimetry (DSC). Additionally, the samples were crystalized according to DSC analyses and characterized by using x-ray diffraction (XRD). The main detected crystalline phases were β-spodumene to the glass L, cordierite to the glass C and β-quartz, mulite and spinel to the glass CL. Considering the thermal and electrical properties of these crystalline phases, these glass-ceramics have potential use for LTCC (Low Thermal Co-fired Ceramics) applications.


1999 ◽  
Vol 14 (4) ◽  
pp. 1570-1575 ◽  
Author(s):  
G. Ennas ◽  
G. Marongiu ◽  
A. Musinu ◽  
A. Falqui ◽  
P. Ballirano ◽  
...  

Homogeneous maghemite (γ–Fe2O3) nanoparticles with an average crystal size around 5 nm were synthesized by successive hydrolysis, oxidation, and dehydration of tetrapyridino-ferrous chloride. Morphological, thermal, and structural properties were investigated by transmission electron microscopy (TEM), differential scanning calorimetry (DSC), and x-ray diffraction (XRD) techniques. Rietveld refinement indicated a cubic cell. The superstructure reflections, related to the ordering of cation lattice vacancies, were not detected in the diffraction pattern. Kinetics of the solid-state phase transition of nanocrystalline maghemite to hematite (α–Fe2O3), investigated by energy dispersive x-ray diffraction (EDXRD), indicates that direct transformation from nanocrystalline maghemite to microcrystalline hematite takes place during isothermal treatment at 385 °C. This temperature is lower than that observed both for microcrystalline maghemite and for nanocrystalline maghemite supported on silica.


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