Direct use of the mass output of a thermobalance for controlling the reaction rate of solid-state reactions

2004 ◽  
Vol 75 (8) ◽  
pp. 2620-2624 ◽  
Author(s):  
M. J. Diánez ◽  
L. A. Pérez Maqueda ◽  
J. M. Criado
1991 ◽  
Vol 230 ◽  
Author(s):  
R. B. Schwarz ◽  
J. B. Rubin

AbstractWe have studied the kinetics of the solid-state amorphizing reaction in thin film multilayers of Ni and Zr. Crystalline Ni and Zr films were deposited in ultra-high vacuum onto platinum resistance thermometers embedded in alumina. An electronic feedback circuit controls the temperature of the substrata by adjusting the power dissipated by the platinum resistors. We find that structural relaxation in the asdeposited Ni and Zr films affects the initial stages of the reaction. For long reaction times there is a discontinuous change in the reaction rate. The time to reach this transition increases with film thickness and depends exponentially on 1/T, with an apparent activation energy of 3 eV atom−1.


1995 ◽  
Vol 418 ◽  
Author(s):  
D. P. Smith ◽  
M. M. Chaudhri

AbstractMany reactions of interest occur in the solid state, or with low mobility of the reactants or products, with the result that the physical mechanisms operative during the reaction determine the shape of the reaction rate-time profile; i.e. topochemistry is important. However, often improper account is taken of the physical mechanisms, resulting in erroneous values for the activation energy and kinetic constants.An improved method of analysis is suggested, allowing the mechanisms of reaction to be determined explicitly. This thus allows the activation energy and kinetic constants to be determined with good theoretical justification. The method has been verified by studying the thermal decomposition of barium azide, where the activation energy was determined to better than 1%. The operative mechanisms so determined are in agreement with visual observations and the literature.


1975 ◽  
Vol 30 (3) ◽  
pp. 304-307
Author(s):  
Giorgio Flor ◽  
Vincenzo Massarotti ◽  
Riccardo Riccardi

The kinetics of the solid state reactionsAgI + TiI → AgTlI2 (I)Agl + AgTl2I3 → 2 AgTlI2 (II)AgTlI2 + Til → AgTl2I3 (III)are investigated with reactant pellets by the contact method.With the aid of inert marker experiments and transport number determinations it was possible to state that the governing mechanism is the cation counter-diffusion in all cases and that the rate determining step is the diffusion of Tl+.The experimental reaction rate constants agree reasonably with those calculated on the basis of the Wagner's thermodynamic theory.


Author(s):  
L. A. Bendersky ◽  
W. J. Boettinger

Rapid solidification produces a wide variety of sub-micron scale microstructure. Generally, the microstructure depends on the imposed melt undercooling and heat extraction rate. The microstructure can vary strongly not only due to processing parameters changes but also during the process itself, as a result of recalescence. Hence, careful examination of different locations in rapidly solidified products should be performed. Additionally, post-solidification solid-state reactions can alter the microstructure.The objective of the present work is to demonstrate the strong microstructural changes in different regions of melt-spun ribbon for three different alloys. The locations of the analyzed structures were near the wheel side (W) and near the center (C) of the ribbons. The TEM specimens were prepared by selective electropolishing or ion milling.


Author(s):  
S.R. Summerfelt ◽  
C.B. Carter

The wustite-spinel interface can be viewed as a model interface because the wustite and spinel can share a common f.c.c. oxygen sublattice such that only the cations distribution changes on crossing the interface. In this study, the interface has been formed by a solid state reaction involving either external or internal oxidation. In systems with very small lattice misfit, very large particles (>lμm) with coherent interfaces have been observed. Previously, the wustite-spinel interface had been observed to facet on {111} planes for MgFe2C4 and along {100} planes for MgAl2C4 and MgCr2O4, the spinel then grows preferentially in the <001> direction. Reasons for these experimental observations have been discussed by Henriksen and Kingery by considering the strain energy. The point-defect chemistry of such solid state reactions has been examined by Schmalzried. Although MgO has been the principal matrix material examined, others such as NiO have also been studied.


Author(s):  
W. A. Chiou ◽  
N. L. Jeon ◽  
Genbao Xu ◽  
M. Meshii

For many years amorphous metallic alloys have been prepared by rapid quenching techniques such as vapor condensation or melt quenching. Recently, solid-state reactions have shown to be an alternative for synthesizing amorphous metallic alloys. While solid-state amorphization by ball milling and high energy particle irradiation have been investigated extensively, the growth of amorphous phase by cold-rolling has been limited. This paper presents a morphological and structural study of amorphization of Cu and Ti foils by rolling.Samples of high purity Cu (99.999%) and Ti (99.99%) foils with a thickness of 0.025 mm were used as starting materials. These thin foils were cut to 5 cm (w) × 10 cm (1), and the surface was cleaned with acetone. A total of twenty alternatively stacked Cu and Ti foils were then rolled. Composite layers following each rolling pass were cleaned with acetone, cut into half and stacked together, and then rolled again.


Author(s):  
P. G. Kotula ◽  
D. D. Erickson ◽  
C. B. Carter

High-resolution field-emission-gun scanning electron microscopy (FESEM) has recently emerged as an extremely powerful method for characterizing the micro- or nanostructure of materials. The development of high efficiency backscattered-electron detectors has increased the resolution attainable with backscattered-electrons to almost that attainable with secondary-electrons. This increased resolution allows backscattered-electron imaging to be utilized to study materials once possible only by TEM. In addition to providing quantitative information, such as critical dimensions, SEM is more statistically representative. That is, the amount of material that can be sampled with SEM for a given measurement is many orders of magnitude greater than that with TEM.In the present work, a Hitachi S-900 FESEM (operating at 5kV) equipped with a high-resolution backscattered electron detector, has been used to study the α-Fe2O3 enhanced or seeded solid-state phase transformations of sol-gel alumina and solid-state reactions in the NiO/α-Al2O3 system. In both cases, a thin-film cross-section approach has been developed to facilitate the investigation. Specifically, the FESEM allows transformed- or reaction-layer thicknesses along interfaces that are millimeters in length to be measured with a resolution of better than 10nm.


Author(s):  
F. Ma ◽  
S. Vivekanand ◽  
K. Barmak ◽  
C. Michaelsen

Solid state reactions in sputter-deposited Nb/Al multilayer thin films have been studied by transmission and analytical electron microscopy (TEM/AEM), differential scanning calorimetry (DSC) and X-ray diffraction (XRD). The Nb/Al multilayer thin films for TEM studies were sputter-deposited on (1102)sapphire substrates. The periodicity of the films is in the range 10-500 nm. The overall composition of the films are 1/3, 2/1, and 3/1 Nb/Al, corresponding to the stoichiometric composition of the three intermetallic phases in this system.Figure 1 is a TEM micrograph of an as-deposited film with periodicity A = dA1 + dNb = 72 nm, where d's are layer thicknesses. The polycrystalline nature of the Al and Nb layers with their columnar grain structure is evident in the figure. Both Nb and Al layers exhibit crystallographic texture, with the electron diffraction pattern for this film showing stronger diffraction spots in the direction normal to the multilayer. The X-ray diffraction patterns of all films are dominated by the Al(l 11) and Nb(l 10) peaks and show a merging of these two peaks with decreasing periodicity.


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