TEM STUDIES OF THE MICROMECHANISMS OF SOLID STATE REACTIONS IN Ni-Zr BULK DIFFUSION COUPLES

1990 ◽  
Vol 51 (C4) ◽  
pp. C4-121-C4-130
Author(s):  
U. KÖSTER ◽  
R. PRIES ◽  
G. BEWERNICK ◽  
B. SCHUHMACHER ◽  
M. BLANK-BEWERSDORFF
Keyword(s):  
Solid State ◽  
Bulk Diffusion ◽  
Solid State Reactions ◽  
Diffusion Couples

A Study of the Kinetics and Energetics of Solid State Reactions in Pd/Sn Diffusion Couples

1995 ◽  
Vol 398 ◽  
Author(s):  
R.R. Chromik ◽  
E. J. Cotts
Keyword(s):  
Differential Scanning Calorimetry ◽  
Solid State ◽  
Heat Of Formation ◽  
Solid State Reactions ◽  
Diffusion Couples ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Limited Temperature ◽  
Reaction Constant ◽  
Limited Temperature Range

ABSTRACTUsing differential scanning calorimetry, supplemented by measurements from scanning electron microscopy images, we have investigated solid state reactions in Pd/Sn multilayer composites to form PdSn4 and PdSn3. Planar diffusion couples of Pd and Sn were prepared by means of mechanical co-deformation in a rolling mill. A phase formation sequence was determined using differential scanning calorimetry and x-ray diffraction. Growth of the PdSru phase was studied from room temperature to the melting point of Sn. For temperatures between 430 and 460K diffusion limited growth of PdSn4 was observed. From heat flow data over this limited temperature range, the form of the reaction constant was found to be k2 −k0 exp(−Ea / kbT), where k0= 0.16 cm2/s and Εn= 0.8 eV/atom. Also determined was a heat of formation, ΔHf = −27±1 kJ/mol for PdSn4 from Pd and Sn.

Non Parabolic Shift of Interfaces and Effect of Diffusion Asymmetry on Nanoscale Solid State Reactions

2009 ◽  
Vol 7 ◽  
pp. 43-49 ◽  
Author(s):  
Dezső L. Beke ◽  
Z. Erdélyi ◽  
Z. Balogh ◽  
Csaba Cserháti ◽  
G.L. Katona
Keyword(s):  
Experimental Data ◽  
Solid State ◽  
Interface Reaction ◽  
Diffuse Interface ◽  
Solid State Reactions ◽  
Diffusion Couples ◽  
Parent Materials ◽  
Parabolic Law ◽  
And Shifts ◽  
Interface Reaction Control

In a set of recent papers we have shown that the diffusion asymmetry in diffusion couples (the diffusion coefficient is orders of magnitude larger in one of the parent materials) leads to interesting phenomena: i) sharp interface remains sharp and shifts with non Fickian (anomalous) kinetics [1-5], ii) originally diffuse interface sharpens even in ideal (completely miscible) systems [6,7], iii) an initially existing thin AB phase in A/AB/B diffusion couple can be dissolved [8], iv) there exists a crossover thickness (typically between few nanometers and 1m) above which the interface shift turns back to the Fickian behaviour [9], v) the growth rate of a product of solid state reaction can be linear even if there is no any extra potential barrier present (which is the classical interpretation of the “interface reaction control” for linear kinetics) [10]. These latter results will be summarized and reformulated according to the usual expression for linear-parabolic law containing the interdiffusion coefficient, D, and interface transfer coefficient, K. Relation between the activation energies of D and K will be analyzed and compared with available experimental data.

Kinetics of Metallic Glass Formation by Solid State Reactions

1985 ◽  
Vol 57 ◽  
Author(s):  
K. Samwer ◽  
H Schröder ◽  
M. Moske
Keyword(s):  
Electron Microscopy ◽  
Solid State ◽  
Metallic Glass ◽  
Glass Formation ◽  
Amorphous Layer ◽  
Solid State Reactions ◽  
Diffusion Couples ◽  
Cross Sectional ◽  
Transmission Electron ◽  
Kinetics Of

AbstractMetallic glass formation by solid state reactions has been observed in multilayer Zr-Co diffusion couples. The kinetics of the reaction are limited by the diffusion of the Co-atoms in the growing amorphous layer, at least for longer times, as shown by cross-sectional transmission electron microscopy and resistance measurements. The latter one provides the interdiffusion constant and the activation energy of about 1.1 eV. Deposition of the crystalline layers at 77 K results in an enhanced amorphization process in the first stage of the reaction and gives preliminary answers about the nucleation of the amorphous phase.

Reaction couples of ceramic thin films prepared by CVD

1988 ◽  
Vol 46 ◽  
pp. 798-799
Author(s):  
D.W. Susnitzky ◽  
S.R. Summerfelt ◽  
C.B. Carter
Keyword(s):  
Thin Film ◽  
Vapor Deposition ◽  
Chemical Vapor ◽  
Deposition Process ◽  
Solid State Reactions ◽  
Spatial Distributions ◽  
Diffusion Couples ◽  
Kinetics Studies ◽  
Ceramic Thin Films ◽  
Initial Stage

Solid-state reactions have traditionally been studied in the form of diffusion couples. This ‘bulk’ approach has been modified, for the specific case of the reaction between NiO and Al2O3, by growing NiAl2O4 (spinel) from electron-transparent Al2O3 TEM foils which had been exposed to NiO vapor at 1415°C. This latter ‘thin-film’ approach has been used to characterize the initial stage of spinel formation and to produce clean phase boundaries since further TEM preparation is not required after the reaction is completed. The present study demonstrates that chemical-vapor deposition (CVD) can be used to deposit NiO particles, with controlled size and spatial distributions, onto Al2O3 TEM specimens. Chemical reactions do not occur during the deposition process, since CVD is a relatively low-temperature technique, and thus the NiO-Al2O3 interface can be characterized. Moreover, a series of annealing treatments can be performed on the same sample which allows both Ni0-NiAl2O4 and NiAl2O4-Al2O3 interfaces to be characterized and which therefore makes this technique amenable to kinetics studies of thin-film reactions.

Microstructural Variations in Melt-Spun Rapidly Solidified Ribbons

1985 ◽  
Vol 43 ◽  
pp. 54-55
Author(s):  
L. A. Bendersky ◽  
W. J. Boettinger
Keyword(s):  
Solid State ◽  
Processing Parameters ◽  
Heat Extraction ◽  
Solid State Reactions ◽  
Careful Examination ◽  
Ion Milling ◽  
Melt Spun ◽  
Wheel Side ◽  
Rapidly Solidified ◽  
Heat Extraction Rate

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.

The wustite-spinel interface

1987 ◽  
Vol 45 ◽  
pp. 268-269
Author(s):  
S.R. Summerfelt ◽  
C.B. Carter
Keyword(s):  
Solid State ◽  
Solid State Reaction ◽  
Strain Energy ◽  
Matrix Material ◽  
Lattice Misfit ◽  
Solid State Reactions ◽  
Oxygen Sublattice ◽  
Large Particles ◽  
Small Lattice ◽  
Coherent Interfaces

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.

TEM study of amorphization of Cu and Ti foils by cold-rolling

1990 ◽  
Vol 48 (4) ◽  
pp. 146-147
Author(s):  
W. A. Chiou ◽  
N. L. Jeon ◽  
Genbao Xu ◽  
M. Meshii
Keyword(s):  
Solid State ◽  
Cold Rolling ◽  
High Energy ◽  
Rapid Quenching ◽  
Vapor Condensation ◽  
Metallic Alloys ◽  
Solid State Reactions ◽  
High Energy Particle ◽  
Amorphous Metallic Alloys ◽  
Thin Foils

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.

The use of high-resolution FESEM to study solid-state phase transformations and reactions

1994 ◽  
Vol 52 ◽  
pp. 1028-1029
Author(s):  
P. G. Kotula ◽  
D. D. Erickson ◽  
C. B. Carter
Keyword(s):  
Solid State ◽  
High Resolution ◽  
Phase Transformations ◽  
High Efficiency ◽  
Sol Gel ◽  
Quantitative Information ◽  
Solid State Reactions ◽  
Critical Dimensions ◽  
Backscattered Electrons ◽  
Backscattered Electron

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.

TEM studies of solid-state reactions in sputter-deposited Nb/Al multilayer thin films

1996 ◽  
Vol 54 ◽  
pp. 1020-1021
Author(s):  
F. Ma ◽  
S. Vivekanand ◽  
K. Barmak ◽  
C. Michaelsen
Keyword(s):  
Thin Films ◽  
Solid State ◽  
Stoichiometric Composition ◽  
Analytical Electron Microscopy ◽  
Grain Structure ◽  
Solid State Reactions ◽  
Multilayer Thin Films ◽  
X Ray Diffraction ◽  
X Ray ◽  
Sputter Deposited

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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