The kinetics of indium/amorphous-selenium multilayer thin film reactions

1999 ◽  
Vol 14 (3) ◽  
pp. 771-779 ◽  
Author(s):  
K. Lu ◽  
M. L. Sui ◽  
J. H. Perepezko ◽  
B. Lanning

The reaction kinetics in vapor-deposited indium/amorphous-selenium (a-Se) multilayer thin films were studied using differential scanning calorimetry (DSC), x-ray diffraction (XRD), and transmission electron microscopy (TEM). A number of reactions were observed upon heating with characteristic temperatures which were found to be independent of the multilayer modulation wavelength. The initial interface reaction between In and a-Se is the formation of an In2Se phase. Kinetic analyses of the In2Se formation process combined with TEM observations indicated that interface reaction is characterized by the two-dimensional growth of pre-existing In2Se regions formed during deposition to impingement in the plane of the original In/a-Se interface. The change of the density of In2Se grains with temperature was analyzed in terms of the derived kinetic parameters, which is consistent with TEM observations and the heat release measurements.

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.


1997 ◽  
Vol 481 ◽  
Author(s):  
K. Landry ◽  
H. Sieber ◽  
M. Sui ◽  
J. H. Perepezko

ABSTRACTThe reaction at the interface between Al and amorphous C in Al/C multilayer thin films with modulation wavelengths of about 25nm and 125nm has been investigated by differential scanning calorimetry, X-ray diffraction, transmission electron microscopy/selected area electron diffraction and high resolution transmission electron microscopy. The reaction was found to take place in two steps. The first step onsets at about 300°C, and was identified as the diffusion of C into Al. The second step starts above 400°C, at a temperature strongly dependent on the modulation wavelength of the film, and is the formation of A14C3. The carbide has been observed to nucleate and grow inside the Al layers. The multilayer structure is preserved in the samples up to at least 550°C, and Al grains start to grow at or below 300°C.


1989 ◽  
Vol 167 ◽  
Author(s):  
J.H. Selverian ◽  
F.S. Ohuchi ◽  
M.R. Notis

AbstractWe studied the reactivity of titanium with the R-plane (112) surface of sapphire by transmission electron microscopy (TEM), x-ray diffraction (XRD), and Rutherford backscattering (RBS) techniques. Cross-section TEM specimens were prepared from 200–400 nm thick titanium films deposited on sapphire at 25, 525, 554, 562, 580, 630, and 663°C to observe the interfacial region. In samples deposited at 25°C, without further annealing, no reaction zone could be seen in the TEM. In all other samples titanium reduced the sapphire to form Ti0 6 7[O0 3 3] and Ti3Al[O], Ti and Ti3Al with oxygen in solid solution. An activation energy of 24.7 ± 6 kcal/deg-mole was determined for the growth of the Ti3Al[O] layer. Layer thickness measurements from the TEM and RBS studies were within 10–20% of one another.


1997 ◽  
Vol 12 (2) ◽  
pp. 385-391 ◽  
Author(s):  
A. S. Edelstein ◽  
R. K. Everett ◽  
J. H. Perepezko ◽  
M. H. da Silva Bassani

The uniformity and reaction kinetics of ion-beam deposited Al/Ni multilayer samples with the same composition, Al81.8Ni18.2, and modulation wavelength, Λ = 20 nm, but with different total film thicknesses were investigated by x-ray diffraction and differential scanning calorimetry measurements. The total film thicknesses varied between approximately 0.5 and 2.0 μm. It was found that the interface widths were approximately 1 nm and the Ni layers are much more disordered than the Al layers. The thicker samples show an increase in disorder on a length scale comparable to Λ. In other experiments, a change was observed with increasing modulation wavelength from semicoherent interfaces with a low density of misfit dislocations to semicoherent interfaces with a high density of misfit dislocations. The reaction kinetics for forming the Al9Ni2 phase is independent of the sample thickness.


Metals ◽  
2021 ◽  
Vol 11 (2) ◽  
pp. 218
Author(s):  
Xianjie Yuan ◽  
Xuanhui Qu ◽  
Haiqing Yin ◽  
Zaiqiang Feng ◽  
Mingqi Tang ◽  
...  

This present work investigates the effects of sintering temperature on densification, mechanical properties and microstructure of Al-based alloy pressed by high-velocity compaction. The green samples were heated under the flow of high pure (99.99 wt%) N2. The heating rate was 4 °C/min before 315 °C. For reducing the residual stress, the samples were isothermally held for one h. Then, the specimens were respectively heated at the rate of 10 °C/min to the temperature between 540 °C and 700 °C, held for one h, and then furnace-cooled to the room temperature. Results indicate that when the sintered temperature was 640 °C, both the sintered density and mechanical properties was optimum. Differential Scanning Calorimetry, X-ray diffraction of sintered samples, Scanning Electron Microscopy, Energy Dispersive Spectroscopy, and Transmission Electron Microscope were used to analyse the microstructure and phases.


1991 ◽  
Vol 246 ◽  
Author(s):  
J.A. Horton ◽  
E.P. George ◽  
C.J. Sparks ◽  
M.Y. Kao ◽  
O.B. Cavin ◽  
...  

AbstractA survey by differential scanning calorimetry (DSC) and recovery during heating of indentations on a series of nickel-aluminum alloys showed that the Ni-36 at.% Al composition has the best potential for a recoverable shape memory effect at temperatures above 100°C. The phase transformations were studied by high temperature transmission electron microscopy (TEM) and by high temperature x-ray diffraction (HTXRD). Quenching from 1200°C resulted in a single phase, fully martensitic structure. The initial quenched-in martensites were found by both TEM and X-ray diffraction to consist of primarily a body centered tetragonal (bct) phase with some body centered orthorhombic (bco) phase present. On the first heating cycle, DSC showed an endothermic peak at 121°C and an exothermic peak at 289°C, and upon cooling a martensite exothermic peak at 115° C. Upon subsequent cycles the 289°C peak disappeared. High temperature X-ray diffraction, with a heating rate of 2°C/min, showed the expected transformation of bct phase to B2 between 100 and 200°C, however the bco phase remained intact. At 400 to 450°C the B2 phase transformed to Ni2Al and Ni5Al3. During TEM heating experiments a dislocation-free martensite transformed reversibly to B2 at temperatures less than 150°C. At higher temperatures (nearly 600°C) 1/3, 1/3, 1/3 reflections from an ω-like phase formed. Upon cooling, the 1/3, 1/3, 1/3 reflections disappeared and a more complicated martensite resulted. Boron additions suppressed intergranular fracture and, as expected, resulted in no ductility improvements. Boron additions and/or hot extrusion encouraged the formation of a superordered bct structure with 1/2, 1/2, 0 reflections.


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.


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