Search NASA⌕ Search

SEARCH · Search NASA

Results for “Microstructural evolution”

Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 901 records · Page 50

Fatigue crack growth mechanisms at the microstructure scale in as-fabricated and heat treated Ti-6Al-4V ELI manufactured by electron beam melting (EBM)

Electron beam melting (EBM) is a metal powder bed fusion additive manufacturing (AM) technology that fabricates parts by selectively scanning consecutive powder layers with an electron beam. Additive manufacturing technologies are increasing in importance for aerospace and medical applications, where the demand for a fundamental understanding and predictability of static and dynamic material properties are high. Ti-6Al-4V is the most widely used and studied alloy for this technology, and is the focus of this work in its Extra Low Interstitial (ELI) variation. The layered manufacturing of metallic components by EBM creates a unique directional microstructure, and consequently, anisotropic properties. Microstructure evolution, and its influence on mechanical properties of the alloy in the as-fabricated condition, has been documented by various researchers. However, fatigue crack propagation and the effects of the directional structure have not been sufficiently studied, imposing a barrier for this technology’s potential extension to high-integrity applications. Here in this study, fatigue crack growth (FCG) both parallel and perpendicular to the build directions was studied for different stress ratios and crack growth stages. The interaction between the directional as-fabricated EBM microstructure and FCG was investigated and compared to that of the equiaxed β annealed microstructure obtained by annealing above the β transus temperature. Finally, the FCG threshold, ΔK th , was analytically modeled for the two relative crack propagation directions at different stress ratios, and FCG microstructural mechanisms were established for all three regions of crack propagation.

36 MATERIALS SCIENCE↗

The importance of properties in modeling

Casting and welding of superalloys, stainless steel and titanium alloys are processes which can be improved through modeling of heat flow, fluid flow, residual stress development, and microstructural evolution. These simulations require inputs of thermophysical data, some of which involves the partially or totally liquid state. In particular, these processes involve melting, flow in the liquid, and solidification. Modeling of such processes can lead to an improved understanding of defects such as shrinkage, inclusions, cracks, incomplete filling (or penetration), macrosegregation, improper grain structure, and deviations from dimensional specifications. Effective modeling can shorten process development time and improve quality. An approach to these problems is to develop efficient models; validate through correlations with thermal, distortion, and microstructural data; run parametric studies; extract knowledge based rules; and apply to adaptive closed loop control systems. With the appropriate pre- and post-processing, such analyses can be made 'user friendly'. This would include graphical user interfaces as well as realistic images and color maps. In such form, these models can be used for sensitivity analyses, which are useful in defining appropriate sensors and in the development of control strategies. Such modeling can be done at several levels, e.g., the MARO level, modeling large scale phenomena such as heat and fluid flow or material deformation; the MICRO level, modeling the development of dendrites, grains or precipitates; or at the NANO level, modeling point defects, dislocations, stacking faults, etc. There are many computational issues associated with these simulations, e.g. computational efficiency and accuracy. In addition, there are many materials issues, not the least of which is the availability of accurate high temperature thermophysical data for complex alloys. This would include latent heat of fusion, temperature dependent heat capacity and thermal conductivity (for liquid and solid), viscosity, surface tension, thermal expansion, mechanical properties, etc. Preliminary data is frequently gathered from the literature; however, this is often not available for modern alloys. If additional data are required, measurements can be used; however, these are costly, time consuming and can be erroneous due to a lack of testing standards or impure materials. Microstructural predictors can be extracted from thermal information, e.g. cooling rate and thermal gradient; the prediction of microstructure is dependent on solidus and liquidus temperature, mushy zone permeability, the solidification curve, volume changes, phase transformations, alloying effects (such as surface tension or viscosity), mold/metal reactions, metal/environment reactions, etc. Defect maps may be needed to predict the onset of shrinkage, hot cracking or 'freckling'. Constants may be needed for stress relaxation, dendrite coarsening, vaporization, etc. Visualization was used as a tool to better comprehend complex data sets associated with the analysis of directional solidification (including crystal growth) and welding. Examples include not only isotherms, but also cooling rate, growth rate and thermal gradient. The latter two are not single valued scalars, but rather time and space dependent vector fields. Efficient models were developed for both casting and welding to predict heat flow and the relationship to dendrite and grain growth. These codes include many of the non-linear effects, e.g. radiation, which dominate these processes. The home-built FDM code(s) were designed to be useful not only to the scientist, but also to the process engineer. Special output can be requested to compare directly to experimental data. Visualization procedures were developed to visualize critical results, e.g. fusion zone width at the surface opposite that where the arc is applied ('penetration'). Both elaborate and simplified distortion analyses were carried out. It is clear that extensive mechanical property data are critical in order to accurately predict residual stress patterns. A scheme is currently being developed to integrate these modeling tools into a set of control algorithms; however, the success of this approach is critically dependent on the availability of accurate high temperature thermophysical data.

Giamei, A. F.↗

Visualizing Uranium Crystallization from Melt: Experiment-Informed Phase Field Modeling and Machine Learning

The focus of this project was to observe and simulate the solidification of uranium metal at the crystallographic level from its molten state. Melting experiments were conducted at two different scales to observe microstructural evolution using either a laboratory-scale induction furnace (hundreds of grams of metal) or a microscope heating stage (hundreds of milligrams of metal), respectively. Experimental parameters and characterization data were then used to inform a phase field model of gamma-U crystal growth as dendrites with or without secondary phase impurities in the form of uranium carbide particles. Finally, training datasets were generated by the phase field model as inputs to a neural network, developed with the aim of providing a faster, cheaper surrogate model for microstructural simulations within a given parameter space. Progress is reported herein for each of these task areas. Ultimately, 1) an optical microscope heating stage capability has been stood-up for uranium metal solidification studies, 2) a phase field model was advanced to simulate multiple uranium grains growing in the presence of carbide impurity particles and 3) a neural network was constructed and optimized to predict the microstructure features of individually growing uranium crystals.

36 MATERIALS SCIENCE↗

Coupling Experiments and Simulations to Understand Metallic Fuel Behavior

The development of metal alloy fuels for minor actinide transmutation in fast reactor systems is of high importance. However, it faces numerous technical challenges such as: i) fuel behavior has to be benign during core off-normal events; ii) fuel has to maintain integrity to high burnup; iii) low minor actinide fabrication loss under remote handling conditions; and iv) fuel has to lend itself to low-loss recycling process. Limited experimental fuel performance data is currently available to support the selection of a fuel type for a transmutation system. Metallic fuels are being considered for application in fast reactor environment due to the high burn-up, high fissile and fertile density capability, inherent safety characteristics, favorable thermal response, and relatively easy recycling process. The uranium-plutonium-zirconium (U-Pu- Zr) based alloys are considered as one of the most promising metallic fuels for such application. In this work, we present results of microstructural characterization of Pu-Zr and U-Pu-Zr alloys and provide much needed linkage between thermal properties and microscopic scale observation. A firm understanding of microstructural evolution in reactor materials is imperative and will lead to deeper understanding of in-reactor degradation behavior, creating a new generation of radiation-resistant materials and fuels with the potential for significant increases in burn-up.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Effect of Multiple Reflow Cycles and Al{sub 2}O{sub 3} Nanoparticles Reinforcement on Performance of SAC305 Lead-Free Solder Alloy

The effect of Al{sub 2}O{sub 3} nanoparticles reinforcement on melting behavior, microstructure evolution at the interface and joint shear strength of 96.5Sn3Ag0.5Cu (SAC305) lead-free solder alloy subjected to multiple reflow cycles was investigated. The reinforced SAC305 solder alloy compositions were prepared by adding Al{sub 2}O{sub 3} nanoparticles in different weight fractions (0.05, 0.1, 0.3 and 0.5 wt.%) through mechanical dispersion. Cu/solder/Cu micro-lap-shear solder joint specimens were used to assess the shear strength of the solder joint. Differential scanning calorimetry was used to investigate the melting behavior of SAC305 solder nanocomposites. The solder joint interfacial microstructure was studied using scanning electron microscopy. The results showed that the increase in melting temperature (T{sub L}) and melting temperature range of the SAC305 solder alloy by addition of Al{sub 2}O{sub 3} nanoparticles were not significant. In comparison with unreinforced SAC305 solder alloy, the reinforcement of 0.05-0.5 wt.% of Al{sub 2}O{sub 3} nanoparticles improved the solder wettability. The addition of nanoparticles in minor quantity effectively suppressed the Cu{sub 6}Sn{sub 5} IMC growth, improved the solder joint shear strength and ductility under multiple reflow cycles. However, the improvement in solder properties was less pronounced on increasing the nanoparticle content above 0.1 wt.% of the solder alloy.

36 MATERIALS SCIENCE↗

Tailoring Thermal and Mechanical Performance Through Multimaterial Laser Powder Directed Energy Deposition of Copper and 17-4PH Stainless Steel

This study investigates the additive manufacturing (AM) processing, microstructural evolution, and resulting mechanical and thermal properties of multimaterial components combining 17-4PH stainless steel and pure copper (Cu) fabricated via laser powder directed energy deposition (LP-DED). Conventional tooling steels exhibit limited thermal conductivity, significantly constraining production throughput in high-volume processes. Incorporating Cu, with its superior thermal conductivity, could significantly enhance tool performance, though Cu and steel present metallurgical incompatibilities when processed via AM. A systematic investigation was conducted across compositions ranging from 0 to 100 wt% Cu, revealing critical thresholds influencing solidification behavior, defect formation, microstructure, hardness, and thermal transport. Optical microscopy, electron backscatter diffraction (EBSD), hardness testing, and thermal conductivity measurements provided comprehensive process–structure–property correlations. Severe hot cracking occurred at low-Cu contents (6–25 wt%), aligning generally well with crack susceptibility modeling, with an unexpected discrepancy at 25 wt%. Porosity remained low (≥99% dense) throughout the compositional spectrum. EBSD analysis revealed a transformation from columnar martensitic structures at low-Cu contents to equiaxed FCC Cu-dominated structures at higher Cu concentrations, highlighting the complex microstructural transitions driven by Cu-induced changes in solidification and phase stability. Hardness decreased from 330 HV (pure 17-4PH) to 62 HV (pure Cu), consistent with microstructural changes. Concurrently, thermal conductivity improved substantially from 13.5 W/m K to 367.9 W/m K, emphasizing Cu’s dominant role in thermal transport. The findings highlight the feasibility of leveraging compositional gradients between 17-4PH and Cu to achieve tailored tooling with optimized thermal and mechanical performance.

17-4PH↗

Controlling reversible phase transitions in rare-earth nickelates for novel memory devices

Resistive switching in correlated complex oxides is lucrative for emerging applications in neuromorphic computing, and densely scaled non-volatile memory. Electrical conductance of such complex oxides can be controllable switched across multiple orders of magnitude by either (a) electroforming a conduction channel (e.g., in tungsten oxide), or (b) inducing Mott-Hubbard transition (e.g., in rare-earth nickelates)– both via controlled migration of defects (such as oxygen vacancies) under applied bias. Nevertheless, the promise of such defect-driven electronic transitions are far from realized due to a lack of fundamental understanding of the atomic-scale processes that underlie migration and spatiotemporal evolution of oxygen vacancies over nano-to-mesoscopic length/timescales under applied electric field. In this project, we employ a synergistic integration of density functional theory (DFT) calculations, ab initio/classical molecular dynamics (AIMD/CMD) simulations, machine learning (ML), precision synthesis, and multi-modal X-ray imaging experiments to address this knowledge gap. Such an integrated approach offers to elucidate the correlations between subtle structural distortion and oxidation states; treat localized charge carriers; describe defect/ion transport in the presence of electric field; and, in turn, greatly advance the current understanding of microstructural evolution in complex oxides under applied bias. The fundamental knowledge gained from this work will enable precise control over hierarchical defect structures and unravel new routes to manipulate resistance states in complex oxides. This, in turn, will accelerate design of novel devices with desired set of neural functionalities, and high-speed densely-scaled resistive random access memory technologies.

36 MATERIALS SCIENCE↗

High-resolution neutron diffraction study of microstructural changes in nanocrystalline ball-milled niobium carbide NbC{sub 0.93}

High resolution neutron diffraction was applied for elucidating of the microstructural evolution of nanocrystalline niobium carbide NbC{sub 0.93} powders subjected to high-energy ball milling. The diffraction patterns were collected with the high resolution Fourier diffractometer HRFD by using the reverse time-of-flight (RTOF) mode of data acquisition. The traditional single diffraction line analysis, the Rietveld method and more advanced Whole Powder Pattern Modeling technique were applied for the data analysis. The comparison of these techniques was performed. It is established that short-time milling produces a non-uniform powder, in which two distinct fractions with differing microstructure can be identified. Part of the material is in fact milled efficiently, with a reduction in grain size, an increase in the quantity of defects, and a corresponding tendency to decarburize reaching a composition NbC{sub 0.80} after 15 h of milling. The rest of the powder is less efficiently processed and preserves its composition and lower defect content. Larger milling times should have homogenized the system by increasing the efficiently milled fraction, but the material is unable to reach a uniform and homogeneous state. It is definitely shown that RTOF neutron diffraction patterns can provide the very accurate data for microstructure analysis of nanocrystalline powders. - Highlights: • The NbC{sub 0.93} powder was processed by high-energy ball milling. • The microstrain and dislocation density increase with milling time increase. • The corresponding decrease in crystallite size with milling time was observed. • The material exhibits the presence of two fractions after ball milling. • The RTOF neutron diffraction data are suitable for accurate microstructure analysis.

36 MATERIALS SCIENCE↗

Quasi-static to Dynamic Response and Microstructure Development of Tantalum-Tungsten Alloys

Lawrence Livermore National Laboratory (LLNL) has a need to understand the quasi-static to dynamic mechanical response and microstructure evolution of tantalum-tungsten (Ta-W) alloys made by conventional wrought processing and additive manufacturing (AM). This two-year work scope will be performed at the Colorado School of Mines (Mines) and will include quasi-static (e.g., 10 -3 s -1 ) mechanical testing in tension and compression, along with high strain rate (Kolsky) pressure bar testing in tension and compression (e.g., 10 3 s -1 ), without and with temperature variations. Gas gun experiments at higher strain rates (e.g., over 10 3 s -1 ) will also be pursued. Complementary microstructure characterization will be performed on undeformed and deformed samples to fundamentally understand the role of processing on the microstructure characteristics and resulting deformation mechanisms that dictate the mechanical response of these alloys with variations in strain rate, temperature, and strain state. Alloys of interest will be Ta-based, containing up to 10 wt.% W. LLNL will supply initial wrought-processed material for sample machining. LLNL will also supply samples built by AM during the project for testing. Arc melting and casting may also be performed at Mines to produce small quantities of different alloys for machining and exploratory testing on an as-needed basis. This project will support multiple postdocs and graduate students at Mines, training them with the knowledge, skills, and abilities needed to study materials under extreme conditions of interest to the National Nuclear Security Agency.

36 MATERIALS SCIENCE↗

On the Effect of Quenching on Postweld Heat Treatment of Friction-Stir-Welded Aluminum 7075 Alloy

This work focuses on the effect of postweld heat treatment (PWHT) on the mechanical properties and microstructural evolution of aluminum 7075 alloy processed via friction stir welding (FSW). FSW is known to be capable of grain refinement in the nugget zone (NZ). Two different quench media (water and air) were employed for PWHT. Regardless of the quench media, the PWHT led to the occurrence of grain growth in the NZ of the FSWed aluminum 7075 alloy. Abnormal grain growth occurred in the water quenched specimen. It is shown that ductility and strength of FSWed aluminum 7075 alloy are strongly dependent on the quenching rate. Changes in the mechanical properties and microstructure reveal that only at lower cooling rate this alloy is prone to the formation of precipitate-free zones (PFZs) in the vicinity of grain boundaries. Eventually, the PFZs deteriorate mechanical properties of this alloy.

36 MATERIALS SCIENCE↗

Creep Behavior of Friction Stir Processed Haynes 282

Haynes 282 is a nickel-based superalloy designed for use in hot sections of turbines for aircraft and power generation. In these applications, elevated temperature creep performance is critical. To that end, creep behavior of friction stir processed material was carried out to investigate the high-temperature performance of this alloy. Friction stir processing of Haynes 282 was successfully completed, and the processed region was found to be defect-free. Various mechanical property characterization approaches were carried out in post-heat treated condition. Transverse tensile samples repeatedly failed in the base metal indicating 100% joint efficiency. Creep property evaluation was completed at 760 °C and at various stress levels. The creep-rupture lifetime of the processed material was similar to the base metal. Detailed electron microscopy analysis of the failed sample was carried out to understand the microstructural evolution in various locations of the sample during creep.

creep↗

Deformation, dislocation evolution and the non-Schmid effect in body-centered-cubic single- and polycrystal tantalum

A physically-informed continuum crystal plasticity model is presented to elucidate deformation mechanisms, dislocation evolution and the non-Schmid effect in body-centered-cubic (bcc) tantalum widely used as a key structural material for mechanical and thermal extremes. We show the unified structural modeling framework informed by mesoscopic dislocation dynamics simulations is capable of capturing salient features of the large inelastic behavior of tantalum at quasi-static (10 -3 s -1 ) to extreme strain rates (5000 s -1 ) and at low (77 K) to high temperatures (873 K) at both single- and polycrystal levels. Here we also present predictive capabilities of the model for microstructural evolution in the material. To this end, we investigate the effects of dislocation interactions on slip activities, instability and the non-Schmid behavior at the single crystal level. Furthermore, ex situ measurements on crystallographic texture evolution and dislocation density growth are carried out for polycrystal tantalum specimens at increasing strains. Numerical simulation results also support that the modeling framework is capable of capturing the main features of the polycrystal behavior over a wide range of strains, strain rates and temperatures. The theoretical, experimental and numerical results at both single- and polycrystal levels provide critical insight into the underlying physical pictures for micro- and macroscopic responses and their relations in this important class of refractory bcc materials undergoing large inelastic deformations.

36 MATERIALS SCIENCE↗

Current-Assisted Diffusion Bonding of Extruded Ti-22Al-25Nb Alloy by Spark Plasma Sintering: Interfacial Microstructure and Mechanical Properties

Spark plasma sintering (SPS) technology was used to current-assisted bond extruded Ti-22Al-25Nb alloy. The effects of bonding temperature (920-980 °C) and bonding time (10-30 min) on the microstructure evolution and shear strength of this alloy were investigated systematically. The temperature distribution in the specimen during the current-assisted bonding process was also analyzed by numerical simulation. It is noted that the highest temperature was obtained at the bonding interface. As the bonding temperature and bonding time increased, the voids in the interface shrank increasingly until they vanished. A complete metallurgical bonding interface could be produced at 960 °C/20 min/10 MPa, exhibiting the highest shear strength of 269.3 MPa. In addition, the shear strength of the bonded specimen depended on its interfacial microstructure. With increased bonding temperature, the fracture mode transformed from the intergranular fracture at the bonding interface to the cleavage fracture in the substrate.

36 MATERIALS SCIENCE↗

Time at Temperature Experiments on Neutron Irradiated Zircaloy-2 using Conventional & Flash DSC

Dryout events in Boiling Water Reactors (BWRs) are currently treated by NRC regulations as automatic disqualification for continued fuel rod operation, even though this criterion does not account for the rate or duration of power increases, associated changes in material behavior, or the possibility of rewetting. Operational history from Anticipated Operational Occurrences (AOOs) shows that short, transient power excursions often demand only modest heat removal, and industry experience suggests that fuel can briefly enter dryout yet return to safe, stable operation. The lack of detailed understanding of the material response during such events motivates the present series of experiments. This study uses unique and innovative methods to investigate microstructural evolution in irradiated Zircaloy-2 exposed to high temperatures in inert environments. Differential Scanning Calorimetry (DSC) and FlashDSC are combined to build a comprehensive experimental framework capable of identifying the a–ß phase transformation in zirconium and examining defect annealing under steep thermal gradients. FlashDSC enables rapid heating and cooling of Focused Ion Beam (FIB)–prepared large-area lift-outs (LALOs) of irradiated Zircaloy-2 at rates of 1,000 K/s to peak temperatures of 600°C, 750°C, and 900°C. The goal is to determine whether these conditions produce measurable microstructural changes that could influence cladding performance in typical BWR environments. Microstructural characterization includes quantifying dislocation density and assessing secondary phase particle (SPP) size and distribution using Transmission Electron Microscopy (TEM). Ongoing analysis, such as diffraction pattern indexing and 4D STEM processing, will further refine these observations.

36 - MATERIALS SCIENCE↗

Clarifying the formation of equiaxed grains and microstructural refinement in the additive manufacturing of Ti-Cu

Controlling microstructural evolution in metallic additive manufacturing (AM) is difficult, especially in producing refined as-built grains instead of coarse, directional grains. Traditional solutions involve adding inoculants to AM feedstocks, but titanium (Ti) alloys cannot employ this approach without producing detrimental secondary phases. Ti-Cu (Ti-copper) alloys offer a solution through constitutional supercooling and/or solid state thermal cycling under AM conditions. This work analyzes a compositionally graded directed energy deposition (DED) Ti-Cu build, single-melt laser tracks, and dilatometric heat treatments to evaluate if, when, and by what mechanism(s) microstructural refinement occurs. Refinement by inoculation of unmelted powder particles was also considered. Constitutional supercooling produced no net microstructural refinement as any equiaxed dendrites which form are remelted with new deposition. This finding agreed with solidification modeling of powder bed fusion-laser beam (PBF-LB) and DED builds. Solid state thermal cycling refined microstructures only during ex-situ dilatometric heat treatments, suggesting build parameter optimization is needed to achieve refinement in-situ. Accidental heterogeneous nucleation on unmelted Ti powder, originating from the different thermophysical properties of Ti and Cu, provided the most significant microstructural refinement. This work systematically assesses the microstructural refinement mechanisms of Ti-Cu in AM builds and offers insights into microstructural control in eutectoid alloys.

36 MATERIALS SCIENCE↗

Hot Deformation Behavior of the 20 vol.% TiC/Cu-Al{sub 2}O{sub 3} Composites

Hot deformation behavior of the 20 vol.% TiC/Cu-Al{sub 2}O{sub 3} composite was studied using the Gleeble-1500D thermo-mechanical simulator with various strain rates at different deformation temperatures. The softening mechanism due to dynamic recrystallization was a feature of the high-temperature true stress–strain curves. The peak stress increased at the lower deformation temperature and the higher strain rate. Microstructure evolution was explored. Thermal deformation activation energy was calculated as 218.9 kJ/mol, and the constitutive equation was established. The processing map was constructed to obtain optimal processing domain of 700-850 °C and 0.001-0.04 s{sup −1} for hot working.

36 MATERIALS SCIENCE↗

Effects of carbon content and size on Ti-C reaction behavior and resultant properties of Cu-Ti-C alloy system

Highlights: • TiC-strengthened Cu alloys were synthesized by an in situ powder metallurgy route. • Effect of C/Ti ratio on electrical and mechanical properties was studied. • Ti-C reaction behavior during powder metallurgy process was discussed. • Microstructure evolution during present process was analyzed. - Abstract: TiC-strengthened Cu alloys with various nominal compositions were prepared by a high-energy ball-milling process, followed by consolidation using spark plasma sintering (SPS), and a subsequent heat treatment. The results indicated that the lower atomic ratio of C/Ti, the more residual Ti in copper matrix, resulting in a lower electrical conductivity but higher microhardness of alloy. The optimal atomic ratio was found to be close to1.0. The reaction behavior of Ti-C in the Cu-Ti-C system during this process was investigated. Microstructural results suggested that TiC formation is through a diffusion-controlled mechanism. A thin TiC layer was formed at the surface of C particles, and the growth of TiC layer was controlled by interdiffusion of C and Ti atoms across the TiC layer. An incomplete chemical reaction between Ti and C, characterized by a core-shell structure, was observed when the initial C particles were large, and the TiC particle size was found to strongly depending on the C particle size.

36 MATERIALS SCIENCE↗

Microstructure of calcite deformed by high-pressure torsion: An X-ray line profile study

Calcite aggregates were deformed to high strain using high-pressure torsion and applying confining pressures of 1–6 GPa and temperatures between room temperature and 450 °C. The run products were characterized by X-ray diffraction, and key microstructural parameters were extracted employing X-ray line profile analysis. The dominant slip system was determined as r {$ 10\bar{1}4 $}⟨$ \bar{2}021 $⟩ with edge dislocation character. The resulting dislocation density and the size of the coherently scattering domains (CSD) exhibit a systematic dependence on the P-T conditions of deformation. While high pressure generally impedes recovery through reducing point defect mobility, the picture is complicated by pressure-induced phase transformations in the CaCO 3 system. Transition from the calcite stability field to those of the high-pressure polymorphs CaCO 3 - II, CaCO 3 - III and CaCO3-IIIb leads to a change of the microstructural evolution with deformation. At 450 °C and pressures within the calcite stability field, dislocation densities and CSD sizes saturate at shear strains exceeding 10 in agreement with earlier studies at lower pressures. In the stability field of CaCO 3 - II, the dislocation density reflects a more complex behavior. Furthermore, at a given strain and strain rate, the dislocation density increases and the CSD size decreases with increasing pressure within the stability fields of either calcite or of the high-pressure polymorphs. There is, in contrast, a jump from high dislocation densities and small CSDs in the upper pressure region of the calcite stability field to lower dislocation densities and larger CSDs in the low-pressure region of the CaCO 3 - II stability field. This jump is more pronounced at higher temperatures and less so at room temperature. The pressure influence on the deformation-induced evolution of dislocation densities implies that pressure variations may change the rheology of carbonate rocks. In particular, a weakening is expected to occur at the transition from the calcite to the CaCO 3 - II stability field, if aragonite does not form.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗