Studies of phase transformation of Fe1-xS by in Situ TEM

Author(s):  
Thao A. Nguyen ◽  
Linn W. Hobbs

The transformation from Fe1-xS (IC) phase to a mixture of FeS (2C) and iron poor Fe1-xS (IC) phases has been investigated by a series of in-situ heating experiments. The purpose of this study is to resolve the controversy over the mechanism of phase transformation (spinodal decomposition versus nucleation and growth) and to explain the different microstructures observed in the two phase mixture of FeS and Fe1-xS (Figure 1).In-situ heating experiments were carried out using a JEOL JEM EM-SHTH double tilt heating holder. Synthetic “single” Fe0.97S crystals were cut into 3 mm disks, mechanically and ion thinned to electron transparency. In all cooling experiments, the sample was first held at 390 K, a temperature above the transition temperature in order to generate an initial single phase material; then, the temperature was quickly reduced to the temperature of interest.Figure 2a shows the development of a lamellar type microstructure after the sample's temperature was reduced from 390 K to 363 K and then held at this temperature for ten minutes. At 363 K, the undercooling is 27 K. The troilite FeS (2C) phase heterogeneously nucleates and grows along the edge of the sample. Diffraction analysis shows that the FeS (2C) phase is embedded in the iron-poor Fe1-x,S matrix with a rod-like structure.

2011 ◽  
Vol 83 (5) ◽  
pp. 1085-1092 ◽  
Author(s):  
Markus Rettenmayr

Supersaturations and depletion or enrichment of solute/solvent are known to be the driving forces for phase transformations. In the present work, a series of different experiments is presented where in a single phase or a two-phase mixture supersaturation or enrichment/depletion of solute occur in at least one of the phases. In all cases the result is a phase transformation, particularly either the precipitation of a secondary phase out of a primary phase, or the migration of the interface in a two-phase mixture. It is demonstrated that solute transport in the phase exhibiting faster kinetics controls the phase transformation process.


2000 ◽  
Vol 646 ◽  
Author(s):  
E. Abe ◽  
K.W. Gao ◽  
M. Nakamura

ABSTRACTWe have investigated an effect of hydrogen gas-charging on the microstructure and the mechanical property of a Ti-49at.%Al alloy. After hydrogen-charging performed under an atmospheric pressure of hydrogen gas at 1023K for 3 hours, the alloy with γ-single phase has become completely brittle, while this hydrogen-induced embrittlement is suppressed for that with (γ+α2) two-phase microstructure composed of lath-precipitates in the γ matrix. A significant microstructural change was found to occur for the two-phase alloy (approximately 340ppm hydrogen in the alloy); a thin amorphous layers with a few nm thickness appear at the preexisting γ/α2 interfaces in the lath-precipitates after hydrogen-charging. In-situ TEM observation confirmed that the amorphous region transforms to a nano-crystalline state after heating to 1000K at which the hydrogen could be removed (degassed), indicating that the amorphous phase is not a binary Ti-Al phase but a ternary Ti-Al-H one. This, in turn, suggests that the γ/α2 interface in the lath packets act as the most preferential sites for hydrogen storage. Therefore, the scavenging is expected to occur effectively for the microstructure composed of γ-α2 fine lamellae in which a large number of γ/α2 interfaces exist. It is worthwhile mentioning that the fine-scale of the lamellae makes it possible to have a large number of interfaces for a given volume of the α2 phase.


2017 ◽  
Vol 3 (4) ◽  
pp. 347-360 ◽  
Author(s):  
J. Burow ◽  
J. Frenzel ◽  
C. Somsen ◽  
E. Prokofiev ◽  
R. Valiev ◽  
...  

2020 ◽  
Vol 26 (S2) ◽  
pp. 1434-1436
Author(s):  
Wenbo Xin ◽  
Igor M. De Rosa ◽  
Jenn-Ming Yang

2019 ◽  
Vol 89 ◽  
pp. 04001 ◽  
Author(s):  
V. H. S. Ferreira ◽  
R. B. Z. L. Moreno

Polymer flooding is an enhanced oil recovery (EOR) method that reduces the mobility ratio between the displaced oil and the displacing injected water. The flow of polymer solutions through porous media is subject to some process-specific phenomena, such as the inaccessible pore volume (IAPV). Due to IAPV, polymer molecules move faster through the porous medium than smaller ones. Thus the IAPV value needs to be accounted for in experiments and field projects. Recent reports found that polymer in-situ rheology correlates with the IAPV. The objective of this paper is to develop a method for estimating IAPV based on the in-situ rheology of polymers. The methodology proposed here can be used in both single- and two-phase experiments. The technique requires measurement of polymer resistance factor (RF) and residual resistance factor (RRF) at steady state conditions. Core permeability, porosity, and residual oil saturation, as well as water and polymer bulk viscosities, also need to be taken into account. Correlations for polymer in-situ viscosity and shear rate are solved simultaneously, to wield an estimative for the IAPV. Aiming at to prove the method, we report 16 core-flooding experiments, eight single- and eight two-phase experiments. We used a flexible polymer and sandstone cores. All the tests were run using similar rock samples. In the single-phase experiments, we compare the alternative method with the classic tracer method to estimate IAPV. The results show an average relative difference of 11.5% between the methods. The two-phase results display, on average, an 18% relative difference to the IAPV measured in the single-phase experiments. The difference between single- and two-phase results can be an effect of the higher shear rates experienced in the two-phase floodings since, in these cases, the aqueous phase shear rate is also dependent on the phase saturation. Additionally, temperature, core length, pore pressure, and iron presence on the core did not show any influence on the IAPV for our two-phase experiments. The method proposed in this paper is limited by the accuracy of the pressure drop measurements across the core. For flexible polymers, the method is valid only for low and mid shear rates, but, accoording to literature, for rigid polymers the method should be accurate for a broad range of shear rates. The method proposed here allows the measurement of polymer IAPV on two- and single- phase core-flooding experiments when a tracer is not used.


2003 ◽  
Vol 792 ◽  
Author(s):  
X. T. Zu ◽  
F.R. Wan ◽  
S. Zhu ◽  
L. M. Wang

ABSTRACTTiNi shape memory alloy (SMA) has potential applications for nuclear reactors and its phase stability under irradiation is becoming an important topic. Some irradiation-induced diffusion-dependent phase transformations, such as amorphization, have been reported before. In the present work, the behavior of diffusion-independent phase transformation in TiNi SMA was studied by electron irradiation at room temperature. The effect of irradiation on the martensitic transformation of TiNi shape memory alloys was studied by Transmission Electron Microscopy (TEM) with in-situ observation and differential scanning calorimeter (DSC). The results of TEM and DSC measurements show that the microstructure of samples is R phase at room temperature. Electron irradiations were carried out using several different TEM with accelerating voltage of 200 kV, 300 kV, 400 kV and 1000 kV. Also the accelerating voltage in the same TEM was changed to investigate the critical voltage for the effect of irradiation on phase transformation. It was found that a phase transformation occurred under electron irradiation above 320 kV, but never appeared at 300 kV or lower accelerating voltage. Such phase transformation took place in a few seconds of irradiation and was independent of atom diffusion. The mechanism of Electron-irradiation-induced the martensitic transformation due to displacements of atoms from their lattice sites produced by the accelerated electrons.


2005 ◽  
Vol 20 (7) ◽  
pp. 1808-1813 ◽  
Author(s):  
X.-G. Ma ◽  
K. Komvopoulos

Transmission electron microscopy (TEM) and nanoindentation, both with in situ heating capability, and electrical resistivity measurements were used to investigate phase transformation phenomena and thermomechanical behavior of shape-memory titanium-nickel (TiNi) films. The mechanisms responsible for phase transformation in the nearly equiatomic TiNi films were revealed by heating and cooling the samples inside the TEM vacuum chamber. Insight into the deformation behavior of the TiNi films was obtained from the nanoindentation response at different temperatures. A transition from elastic-plastic to pseudoelastic deformation of the martensitic TiNi films was encountered during indentation and heating. In contrast to the traditional belief, the martensitic TiNi films exhibited a pseudoelastic behavior during nanoindentation within a specific temperature range. This unexpected behavior is interpreted in terms of the evolution of martensitic variants and changes in the mobility of the twinned structures in the martensitic TiNi films, observed with the TEM during in situ heating.


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