On the Mechanism of Milling Induced Disordering in AlFe

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 479 ◽  
pp. 54-61 ◽  
Author(s):  
Fei Wang ◽  
Ya Ping Wang

Microstructure evolution of high energy milled Al-50wt%Si alloy during heat treatment at different temperature was studied. Scanning electron microscope (SEM) and X-ray diffraction (XRD) results show that the size of the alloy powders decreased with increasing milling time. The observable coarsening of Si particles was not seen below 730°C in the high energy milled alloy, whereas, for the alloy prepared by mixed Al and Si powders, the grain growth occurred at 660°C. The activation energy for the grain growth of Si particles in the high energy milled alloy was determined as about 244 kJ/mol by the differential scanning calorimetry (DSC) data analysis. The size of Si particles in the hot pressed Al-50wt%Si alloy prepared by high energy milled powders was 5-30 m at 700°C, which was significantly reduced compared to that of the original Si powders. Thermal diffusivity of the hot pressed Al-50wt%Si alloy was 55 mm2/s at room temperature which was obtained by laser method.


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.


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.


1996 ◽  
Vol 457 ◽  
Author(s):  
J. Zhu ◽  
T. Pradell ◽  
N. Clavaguera ◽  
M. T. Clavaguera-Mora

ABSTRACTDifferential Scanning Calorimetry (DSC), X-ray Diffraction (XRD), Neutron Diffraction (ND) and Mössbauer Spectroscopy (MS) were used to study the nanocrystallization process of Fe73.5Cu1Nb3Si22.5–xBx (x=5, 7, 8, 9 and 12) amorphous alloys. Both the temperature range and the activation energy of Fe(Si) phase precipitation from the amorphous martrix increase with the initial B composition. The initial Si composition influences the mechanism of the nanocrystallization: for the Si rich samples, the beginning of nucleation and growth processes is interface controlled, for the B rich samples it is diffusion controlled. Secondary crystallization from the remaining amorphous is mainly Fe3B and Fe2B, the ratio of Fe3B/Fe2B being dependent on the initial composition too.


2009 ◽  
Vol 23 (16) ◽  
pp. 3391-3402
Author(s):  
WEERAPHAT PON-ON ◽  
PONGTIP WINOTAI ◽  
I-MING TANG

The nanocrystallization process in amorphous Fe 81 B 13.5 Si 3.5 C 2 ribbons caused by isothermal annealing below the crystallization temperature is studied. X-ray diffraction and Mossbauer spectroscopy measurements are used to identify the formation of new Fe containing compounds such as the ribbons annealed at various temperatures. The ferromagnetic resonance measurements for an as-cast ribbon and the 495°, 525°C and 600°C annealed ribbons exhibit a resonance line at 63.64 mT for φ = 0°. The sample annealed at 425°C shows two resonance peaks at 95.45 mT and 295.46 mT. These are due to the nanocrystalline α– Fe(Si) phase. The resonance-line widths are seen to broaden after the ribbons are annealed at 495°C and 525°C, at which time, the amorphous matrix crystallizes into nano-grains of α– Fe(Si) , t– Fe 2 B and t– Fe 3 B phases. The kinetics of the crystallization is discussed in terms of the relative change in the line width of the samples annealed at 495°C for different annealing times. These results yielded an Avrami exponent, n of 0.84 which is consistent with diffusion-controlled growth with a nucleation rate close to zero.


1994 ◽  
Vol 9 (2) ◽  
pp. 275-285 ◽  
Author(s):  
V. Milonopoulou ◽  
K.M. Forster ◽  
J.P. Formica ◽  
J. Kulik ◽  
J.T. Richardson ◽  
...  

The YBa2Cu3O7−x formation kinetics from a spray-roasted precursor powder containing Y2O3, BaCO3, and CuO was followed via in situ, time-resolved x-ray diffraction as a function of gas atmosphere and temperature. In inert atmospheres, BaCO3 and CuO form BaCu2O2 which subsequently reacts with Y2O3 to form YBa2Cu3O6. However, YBa2Cu3O6 decomposes at temperatures exceeding 725 °C with Y2BaCuO5 being one of the decomposition products. In oxidizing atmospheres, YBa2Cu3O7−x formation involves the BaCuO2. At high temperatures (800–840 °C), oxygen increases the yield of YBa2Cu3O6. A nuclei growth model assuming two-dimensional, diffusion-controlled growth with second-order nucleation rate fits the experimental data.


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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