On the Oxidation Behaviour of WE43 and MSR-B Magnesium Alloys in CO2 Atmosphere

2012 ◽  
Vol 191 ◽  
pp. 159-168 ◽  
Author(s):  
Roman Przeliorz ◽  
Jaroslaw Piątkowski

The aim of the studies was to determine the oxidation kinetics of two magnesium alloys, i.e. WE43 and MSR-B, in CO2 atmosphere with and without the addition of 2 vol.% H2O. The rate of oxidation was measured by thermogravimetry in the temperature range of 530-580°C, i.e. below and above the eutectic melting point. The melting point of the eutectic mixture was determined by differential scanning calorimetry (DSC). The corrosion products were analysed by scanning electron microscopy (SEM) and X-ray microanalysis combined with EDS. Studies showed that on the WE43 alloy, a two-layer scale was formed, in which the outer part was composed of yttrium and magnesium oxides, while the inner part contained only yttrium oxide. The scale was found to preserve its good protective properties even above the eutectic temperature. Analysis of the results showed that on the MSR-B alloy, under a thin, uneven layer of scale, the process of internal oxidation occurred, and at a temperature of 580°C, the alloy underwent partial melting

1995 ◽  
Vol 60 (11) ◽  
pp. 1855-1868 ◽  
Author(s):  
Ivo Lapeš ◽  
Josef Baldrian ◽  
Ján Biroš ◽  
Julius Pouchlý ◽  
Hanes Mio

Solid-liquid eutectic phase diagrams of mixtures of poly(oxyethylene) (M.w. 2 000) with hydroxy and methoxy endgroups, crystallizing in extended-chain macroconformation only, with glutaric acid, benzoic acid or 1,2-diphenylethane are given. The composition dependence of the melting temperature can be fitted by the Flory-Huggins equation. Interaction parameters X and interaction energy densities B evaluated from the diluent branch of the phase diagram are consistent with those obtained from the polymer branch provided the calorimetric value of enthalpy of polymer fusion is used in the latter computation. Measurements of small- and wide-angle X-ray scatterings showed a stacked lamellar structure of POE. Below the eutectic melting point, the long period of the polymer is almost independent of the diluent concentration. On raising temperature gradually from this melting point to the melting point of pure polymer, the increasing long period indicates the penetration of the diluent between the lamellae. As follows from SAXS measurements, the crystallinity of poly(oxyethylene) in the mixtures remains unchanged compared to that of the pure polymer.


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.


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.


2012 ◽  
Vol 569 ◽  
pp. 297-300 ◽  
Author(s):  
Wei Wang ◽  
Yong Xian Liu ◽  
Xiang Dong Shi ◽  
Jin Hua Li ◽  
J.Y.H. Fuh

This research focused on the synthesis and investigation of the thermal properties and microstructure of the Al2O3/SiO2 /ZrO2 system applied to dental field. The composite ceramic was studied by scanning electron microcopy (SEM), energy dispersive spectroscopy (EDS), X-ray diffraction (XRD) and differential scanning calorimetry (DSC). Detailed investigations of the different proportions of materials on the preparation and microstructural phases of ternary eutectic were presented. Furthermore, the crystallization process was investigated by using DSC and XRD. The results indicate that sintering microstructure of the ternary eutectic composite is greatly influenced by the materials proportions. The synthetically thermal analysis shows that the eutectic temperature of ternary Al2O3/SiO2 /ZrO2 composite is 1040°C, is well matching the phase diagram of Al2O3/SiO2 /ZrO2.


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.


2007 ◽  
Vol 336-338 ◽  
pp. 2340-2343 ◽  
Author(s):  
Song He Meng ◽  
Xing Hong Zhang ◽  
Wei Feng Zhang

The reaction process and kinetics of Al-TiO2-C-Ti-Fe system were investigated by differential scanning calorimetry (DSC) analysis, X-ray diffraction (XRD) analysis and scanning electron microscope (SEM). In order to obtain the information of reaction process for complicated system, the reaction characteristics of Al-TiO2, Al-TiO2-C and Al-TiO2-C-Ti systems are explored firstly. The results show that the reaction process varies with temperature in Al-TiO2-C-Ti-Fe system. At the lower temperature, the dominating reaction in Al-TiO2-C-Ti-Fe system is that between Al and Ti, Al and Fe, and so TiAlx, FeAlx, and Ti2Fe intermetallic compounds form. With the temperature increasing, the intermetallic compounds are decomposed. Then the decomposed Ti and Al react with C and TiO2 respectively and the stable TiC, Al2O3 and Fe three phases form in the final product.


Molecules ◽  
2021 ◽  
Vol 27 (1) ◽  
pp. 197
Author(s):  
Izabela Jendrzejewska ◽  
Robert Musioł ◽  
Tomasz Goryczka ◽  
Ewa Pietrasik ◽  
Joanna Klimontko ◽  
...  

X-ray powder diffraction (XRPD) and thermal analysis (differential scanning calorimetry/derivative of thermogravimetry (DSC/DTG)) are solid-state techniques that can be successfully used to identify and quantify various chemical compounds in polycrystalline mixtures, such as dietary supplements or drugs. In this work, 31 dietary supplements available on the Polish market that contain iron compounds, namely iron gluconate, fumarate, bisglycinate, citrate and pyrophosphate, were evaluated. The aim of the work was to identify iron compounds declared by the manufacturer as food supplements and to try to verify compliance with the manufacturer’s claims. Studies performed by X-ray and thermal analysis confirmed that crystalline iron compounds (iron (II) gluconate, iron (II) fumarate), declared by the manufacturers, were present in the investigated dietary supplements. Iron (II) bisglycinate proved to be semi-crystalline. However, depending on the composition of the formulation, it was possible to identify this compound in the tested supplements. For amorphous iron compounds (iron (III) citrate and iron (III) pyrophosphate), the diffraction pattern does not have characteristic diffraction lines. Food supplements containing crystalline iron compounds have a melting point close to the melting point of pure iron compounds. The presence of excipients was found to affect the shapes and positions of the endothermic peaks significantly. Widening of endothermic peaks and changes in their position were observed, as well as exothermic peaks indicating crystallization of amorphous compounds. Weight loss was determined for all dietary supplements tested. Analysis of the DTG curves showed that the thermal decomposition of most food supplements takes place in several steps. The results obtained by a combination of both simple, relatively fast and reliable XRPD and DSC/DTG methods are helpful in determining phase composition, pharmaceutical abnormalities or by detecting the presence of the correct polymorphic form.


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