Unified Static and Dynamic Recrystallization Model for the Minerals of Earth's Mantle Using Internal State Variable Model

NASA Astrophysics Data System (ADS)

Cho, H. E.; Horstemeyer, M. F.; Baumgardner, J. R.

2017-12-01

In this study, we present an internal state variable (ISV) constitutive model developed to model static and dynamic recrystallization and grain size progression in a unified manner. This method accurately captures temperature, pressure and strain rate effect on the recrystallization and grain size. Because this ISV approach treats dislocation density, volume fraction of recrystallization and grain size as internal variables, this model can simultaneously track their history during the deformation with unprecedented realism. Based on this deformation history, this method can capture realistic mechanical properties such as stress-strain behavior in the relationship of microstructure-mechanical property. Also, both the transient grain size during the deformation and the steady-state grain size of dynamic recrystallization can be predicted from the history variable of recrystallization volume fraction. Furthermore, because this model has a capability to simultaneously handle plasticity and creep behaviors (unified creep-plasticity), the mechanisms (static recovery (or diffusion creep), dynamic recovery (or dislocation creep) and hardening) related to dislocation dynamics can also be captured. To model these comprehensive mechanical behaviors, the mathematical formulation of this model includes elasticity to evaluate yield stress, work hardening in treating plasticity, creep, as well as the unified recrystallization and grain size progression. Because pressure sensitivity is especially important for the mantle minerals, we developed a yield function combining Drucker-Prager shear failure and von Mises yield surfaces to model the pressure dependent yield stress, while using pressure dependent work hardening and creep terms. Using these formulations, we calibrated against experimental data of the minerals acquired from the literature. Additionally, we also calibrated experimental data for metals to show the general applicability of our model. Understanding of realistic mantle dynamics can only be acquired once the various deformation regimes and mechanisms are comprehensively modeled. The results of this study demonstrate that this ISV model is a good modeling candidate to help reveal the realistic dynamics of the Earth's mantle.

Modeling Deformation Flow Curves and Dynamic Recrystallization of BA-160 Steel During Hot Compression

NASA Astrophysics Data System (ADS)

Shahriari, Babak; Vafaei, Reza; Mohammad Sharifi, Ehsan; Farmanesh, Khosro

2018-03-01

The hot deformation behavior of a high strength low carbon steel was investigated using hot compression test at the temperature range of 850-1100 °C and under strain rates varying from 0.001 to 1 s-1. It was found that the flow curves of the steel were typical of dynamic recrystallization at the temperature of 950 °C and above; at tested strain rates lower than 1 s-1. A very good correlation between the flow stress and Zener-Hollomon parameter was obtained using a hyperbolic sine function. The activation energy of deformation was found to be around 390 kJ mol-1. The kinetics of dynamic recrystallization of the steel was studied by comparing it with a hypothetical dynamic recovery curve, and the dynamically fraction recrystallized was modeled by the Kolmogorov-Johnson-Mehl-Avrami relation. The Avrami exponent was approximately constant around 1.8, which suggested that the type of nucleation was one of site saturation on grain boundaries and edges.

The effect of deformation temperature on the microstructure evolution of Inconel 625 superalloy

NASA Astrophysics Data System (ADS)

Guo, Qingmiao; Li, Defu; Guo, Shengli; Peng, Haijian; Hu, Jie

2011-07-01

Hot compression tests of Inconel 625 superalloy were conducted using a Gleeble-1500 simulator between 900 °C and 1200 °C with different true strains and a strain rate of 0.1 s -1. Scanning electron microscope (SEM) and electron backscatter diffraction technique (EBSD) were employed to investigate the effect of deformation temperature on the microstructure evolution and nucleation mechanisms of dynamic recrystallization (DRX). It is found that the relationship between the DRX grain size and the peak stress can be expressed by a power law function. Significant influence of deformation temperatures on the nucleation mechanisms of DRX are observed at different deformation stages. At lower deformation temperatures, continuous dynamic recrystallization (CDRX) characterized by progressive subgrain rotation is considered as the main mechanism of DRX at the early deformation stage. However, discontinuous dynamic recrystallization (DDRX) with bulging of the original grain boundaries becomes the operating mechanism of DRX at the later deformation stage. At higher deformation temperatures, DDRX is the primary mechanism of DRX, while CDRX can only be considered as an assistant mechanism at the early deformation stage. Nucleation of DRX can also be activated by the twinning formation. With increasing the deformation temperature, the effect of DDRX accompanied with twinning formation grows stronger, while the effect of CDRX grows weaker. Meanwhile, the position of subgrain formation shifts gradually from the interior of original grains to the vicinity of the original boundaries.

Forging property, processing map, and mesoscale microstructural evolution modeling of a Ti-17 alloy with a lamellar (α+β) starting microstructure

NASA Astrophysics Data System (ADS)

Matsumoto, Hiroaki; Naito, Daiki; Miyoshi, Kento; Yamanaka, Kenta; Chiba, Akihiko; Yamabe-Mitarai, Yoko

2017-12-01

This work identifies microstructural conversion mechanisms during hot deformation (at temperatures ranging from 750 °C to 1050 °C and strain rates ranging from 10-3 s-1 to 1 s-1) of a Ti-5Al-2Sn-2Zr-4Mo-4Cr (Ti-17) alloy with a lamellar starting microstructure and establishes constitutive formulae for predicting the microstructural evolution using finite-element analysis. In the α phase, lamellae kinking is the dominant mode in the higher strain rate region and dynamic globularization frequently occurs at higher temperatures. In the β phase, continuous dynamic recrystallization is the dominant mode below the transition temperature, Tβ (880 890 °C). Dynamic recovery tends to be more active at conditions of lower strain rates and higher temperatures. At temperatures above Tβ, continuous dynamic recrystallization of the β phase frequently occurs, especially in the lower strain rate region. A set of constitutive equations modeling the microstructural evolution and processing map characteristic are established by optimizing the experimental data and were later implemented in the DEFORM-3D software package. There is a satisfactory agreement between the experimental and simulated results, indicating that the established series of constitutive models can be used to reliably predict the properties of a Ti-17 alloy after forging in the (α+β) region.

Forging property, processing map, and mesoscale microstructural evolution modeling of a Ti-17 alloy with a lamellar (α+β) starting microstructure

PubMed Central

Matsumoto, Hiroaki; Naito, Daiki; Miyoshi, Kento; Yamanaka, Kenta; Chiba, Akihiko; Yamabe-Mitarai, Yoko

2017-01-01

Abstract This work identifies microstructural conversion mechanisms during hot deformation (at temperatures ranging from 750 °C to 1050 °C and strain rates ranging from 10−3 s−1 to 1 s−1) of a Ti-5Al-2Sn-2Zr-4Mo-4Cr (Ti-17) alloy with a lamellar starting microstructure and establishes constitutive formulae for predicting the microstructural evolution using finite-element analysis. In the α phase, lamellae kinking is the dominant mode in the higher strain rate region and dynamic globularization frequently occurs at higher temperatures. In the β phase, continuous dynamic recrystallization is the dominant mode below the transition temperature, T β (880~890 °C). Dynamic recovery tends to be more active at conditions of lower strain rates and higher temperatures. At temperatures above T β, continuous dynamic recrystallization of the β phase frequently occurs, especially in the lower strain rate region. A set of constitutive equations modeling the microstructural evolution and processing map characteristic are established by optimizing the experimental data and were later implemented in the DEFORM-3D software package. There is a satisfactory agreement between the experimental and simulated results, indicating that the established series of constitutive models can be used to reliably predict the properties of a Ti-17 alloy after forging in the (α+β) region. PMID:29152021

Forging property, processing map, and mesoscale microstructural evolution modeling of a Ti-17 alloy with a lamellar (α+β) starting microstructure.

PubMed

Matsumoto, Hiroaki; Naito, Daiki; Miyoshi, Kento; Yamanaka, Kenta; Chiba, Akihiko; Yamabe-Mitarai, Yoko

2017-01-01

This work identifies microstructural conversion mechanisms during hot deformation (at temperatures ranging from 750 °C to 1050 °C and strain rates ranging from 10 -3  s -1 to 1 s -1 ) of a Ti-5Al-2Sn-2Zr-4Mo-4Cr (Ti-17) alloy with a lamellar starting microstructure and establishes constitutive formulae for predicting the microstructural evolution using finite-element analysis. In the α phase, lamellae kinking is the dominant mode in the higher strain rate region and dynamic globularization frequently occurs at higher temperatures. In the β phase, continuous dynamic recrystallization is the dominant mode below the transition temperature, T β (880~890 °C). Dynamic recovery tends to be more active at conditions of lower strain rates and higher temperatures. At temperatures above T β , continuous dynamic recrystallization of the β phase frequently occurs, especially in the lower strain rate region. A set of constitutive equations modeling the microstructural evolution and processing map characteristic are established by optimizing the experimental data and were later implemented in the DEFORM-3D software package. There is a satisfactory agreement between the experimental and simulated results, indicating that the established series of constitutive models can be used to reliably predict the properties of a Ti-17 alloy after forging in the (α+ β ) region.

Study on the dynamic recrystallization model and mechanism of nuclear grade 316LN austenitic stainless steel

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, Shenglong; Zhang, Mingxian; Wu, Huanchun

In this study, the dynamic recrystallization behaviors of a nuclear grade 316LN austenitic stainless steel were researched through hot compression experiment performed on a Gleeble-1500 simulator at temperatures of 900–1250 °C and strain rates of 0.01–1 s{sup −1}. By multiple linear regressions of the flow stress-strain data, the dynamic recrystallization mathematical models of this steel as functions of strain rate, strain and temperature were developed. Then these models were verified in a real experiment. Furthermore, the dynamic recrystallization mechanism of the steel was determined. The results indicated that the subgrains in this steel are formed through dislocations polygonization and thenmore » grow up through subgrain boundaries migration towards high density dislocation areas and subgrain coalescence mechanism. Dynamic recrystallization nucleation performs in grain boundary bulging mechanism and subgrain growth mechanism. The nuclei grow up through high angle grain boundaries migration. - Highlights: •Establish the DRX mathematical models of nuclear grade 316LN stainless steel •Determine the DRX mechanism of this steel •Subgrains are formed through dislocations polygonization. •Subgrains grow up through subgrain boundaries migration and coalescence mechanism. •DRX nucleation performs in grain boundary bulging mechanism and subgrain growth mechanism.« less

Microstructure Evolution and Mechanical Properties of High-Speed Friction Stir Welded Aluminum Alloy Thin Plate Joints

NASA Astrophysics Data System (ADS)

Liu, Fenjun; Fu, Li; Chen, Haiyan

2018-06-01

Sound friction stir welded (FSW) joints of 6061-T6 aluminum alloy sheets with an 0.8 mm thickness were obtained at conventional speed (2000 rpm, 300 mm/min) and high speed (11,000 rpm, 1500 mm/min). The recrystallization mechanism, precipitate evolution, mechanical properties and fracture behavior were investigated in detail. Microstructure analyses revealed that the grain structure evolution in the nugget zone (NZ) was dominated by continuous dynamic recrystallization. In the process of FSW, high speed facilitates the formation of finer equiaxed recrystallized grains, higher density of dislocations and substructures, and a larger number of precipitates in the NZ compared to the conventional speed, which further significantly improves the hardness and tensile strength of the joints. The maximum tensile strength was obtained with 292.6 MPa, 83.2% for the 6061-T6 aluminum alloy and 122.6% for the conventional-speed FSW joints. This work provides an effective method for preparing FSW aluminum alloy thin plate joints with excellent mechanical properties.

The Effect of Dynamic Recrystallization on Monotonic and Cyclic Behaviour of Al-Cu-Mg Alloy.

PubMed

Tomczyk, Adam; Seweryn, Andrzej; Grądzka-Dahlke, Małgorzata

2018-05-23

The paper presents an investigation that was conducted to determine the possibility of the occurrence of the process of dynamic recrystallization in 2024 alloy during monotonic tensile and creep tests at the elevated temperatures of 100 °C, 200 °C, and 300 °C. As-extruded material was subjected to creep process with constant force at elevated temperatures, until two varying degrees of deformation were reached. After cooling at ambient temperature, the pre-deformed material was subjected to monotonic and fatigue tests as well as metallographic analysis. The process of dynamic recrystallization was determined in monotonic tests to occur at low strain rate (0.0015/s) only at the temperature of 300 °C. However, in the creep tests, this process occurred with varying efficiency, both during creep at 200 °C and 300 °C. Dynamic recrystallization was indicated to have a significant influence on the monotonic and cyclic properties of the material.

Dynamic Recrystallization Kinetics of 690 Alloy During Hot Compression of Double-Cone Samples

NASA Astrophysics Data System (ADS)

Wang, Jue; Zhai, Shun-Chao

2017-03-01

Hot compression tests of double-cone samples were conducted for 690 alloy to study the kinetic behavior of the complete dynamic recrystallization (DRX) process under low deformation temperatures from 960 to 1080 °C. The microstructure of 82 points in the vertical section of every deformed sample was quantitatively analyzed to determine the DRX fraction. Corresponding strain of these points was calculated by finite element simulations. Kinetic curves of the specimens with different preheating temperatures were then constructed. The features of various boundaries with different misorientation angles were investigated by electron backscatter diffraction technology and transmission electron microscope. The results showed that the strain is continuously and symmetrically distributed along the centerline of the vertical section. Large strain of 1.84 was obtained when the compression amount is 12 mm for double-cone samples. All the fitted kinetic curves display an "S" type, which possess a low growth rate of DRX at the beginning and the end of compression. The critical strain of recrystallization decreases with the increase in preheating temperature, while the completion strain remains around 1.5 for all the samples. The initial and maximum growth rates of DRX fraction have the opposite trend with the change in temperature, which is considered to be attributed to the behaviors of different misorientation boundaries.

Relationship of Technological Properties with Dynamic Recrystallization of Quartz on the Example of Objects of the Karelian-Kola Region

NASA Astrophysics Data System (ADS)

Skamnitskaya, Lubov; Rakov, Leonid; Bubnova, Tatyana; Shchiptsov, Vladimir

2017-12-01

Despite the significant reserves of quartz raw materials, there is a deficit of high purity quartz. It is due to the strict technical requirements imposed by standards for this type of raw materials and technological properties of quartz, which are determined by the features of the crystal structure. The crystalline structure is of particular importance for the technological properties of quartz, since such important characteristics as the limit of raw material enrichment, dissolution rate in acid, melting point of quartz, etc., are determined. The formation of the crystal structure of quartz under natural conditions is associated with the successive dynamic recrystallization of the mineral. The degree of dynamic recrystallization of quartz reflects the distribution of dispersed impurities. If it is weakly manifested, the dispersed impurities are not displaced from one zone to another, and all quartz microblocks contain approximately the same concentration. In this case, more or less uniform dissolution of various regions of quartz is observed, and the pattern of distribution of submicroscopic inhomogeneities is monotonic. If intensive dynamic recrystallization of quartz takes place, then it causes a significant redistribution of the scattered impurities. Then the treatment in HF leads to the appearance of a contrast pattern of the distribution of submicroscopic inhomogeneities. The details of the crystal structure of quartz in this work were investigated by the electron paramagnetic resonance (EPR) method using the ER-420 “Bruker” spectrometer. In the selected samples of quartz, the concentrations of isomorphic impurities Al and Ti were measured, and the degree of crystallinity D of the mineral was estimated from the EPR spectra of each of them. Thus, the technological properties of quartz are determined by various geological processes. The results of the studies show that when evaluating the prospects of quartz raw materials, it is necessary to take into account the staged dynamic dynamical recrystallization of quartz in natural conditions. This factor can play both a positive and a negative role at various stages of mineral formation. Its influence is reflected in the state of the crystal structure of quartz, which should be taken into account when developing effective technologies for its enrichment. The intermediate stage of dynamic recrystallization corresponding to the end of the second stage-the beginning of the third stage of quartz recrystallization-is optimal for the formation of high-purity quartz. When choosing a site for the first-stage quartz mining at large deposits in the Karelian-Kola region, one should be guided by the stage of dynamic recrystallization.

Diffusion-Controlled Recrystallization of Water Sorbed into Poly(meth)acrylates Revealed by Variable-Temperature Mid-Infrared Spectroscopy and Molecular Dynamics Simulation.

PubMed

Yasoshima, Nobuhiro; Fukuoka, Mizuki; Kitano, Hiromi; Kagaya, Shigehiro; Ishiyama, Tatsuya; Gemmei-Ide, Makoto

2017-05-18

Recrystallization behaviors of water sorbed into four poly(meth)acrylates, poly(2-methoxyethyl acrylate), poly(tetrahydrofurfuryl acrylate), poly(methyl acrylate), and poly(methyl methacrylate), are investigated by variable-temperature mid-infrared (VT-MIR) spectroscopy and molecular dynamics (MD) simulation. VT-MIR spectra demonstrate that recrystallization temperatures of water sorbed into the polymers are positively correlated with their glass-transition temperatures reported previously. The present MD simulation shows that a lower-limit temperature of the diffusion for the sorbed water and the glass-transition temperatures of the polymers also have a positive correlation, indicating that the recrystallization is controlled by diffusion mechanism rather than reorientation mechanism. Detailed molecular processes of not only recrystallization during rewarming but also crystallization during cooling and hydrogen-bonding states of water in the polymers are systematically analyzed and discussed.

Dynamic recrystallization and texture evolution of Mg–Y–Zn alloy during hot extrusion process

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tong, L.B.; Li, X.; Guangzhou Research Institute of Non-ferrous Metals, Guangzhou 510651

2014-06-01

The microstructure and texture evolution of Mg{sub 98.5}Y{sub 1}Zn{sub 0.5} and Mg{sub 92.5}Y{sub 5}Zn{sub 2.5} (atomic percent) alloys during hot extrusion were systematically investigated. The coarse LPSO phases with higher volume fraction (∼ 57%) suppressed the twinning generation in the initial stage of extrusion, and accelerated the dynamic recrystallization through the particle deformation zones. Therefore, the volume fraction of DRXed grains in as-extruded Mg{sub 92.5}Y{sub 5}Zn{sub 2.5} alloy was much higher than that of Mg{sub 98.5}Y{sub 1}Zn{sub 0.5} alloy. The intensive recrystallization process resulted in the conventional basal texture weakening, although the texture evolution was mainly dominated by flow behavior.more » The dynamic recrystallization behavior in Mg{sub 92.5}Y{sub 5}Zn{sub 2.5} alloy restricted the formation of deformation texture, and thus the more random texture was observed during the whole extrusion process. - Highlights: • The densely coarse LPSO phases suppressed the twinning deformation. • Coarse LPSO phases induced the particle stimulated nucleation effect. • Dynamic recrystallization resulted in the basal texture weakening effect.« less

Spatial distribution of quartz recrystallization microstructures across the Aar massif (Swiss Central Alps)

NASA Astrophysics Data System (ADS)

Peters, M.; Herwegh, M.

2012-04-01

In the Aar massif, main foliation and major deformation structures were developed during NW-SE compression associated with the Alpine orogeny (Steck 1968). To be precise, shearing at the brittle to ductile transition may have initiated at different stages between 22-20 Ma and 14-12 Ma, followed by purely brittle deformation at around 10 Ma (Rolland et al. 2009). In light of the onset of dynamic recrystallization in quartz, Bambauer et al. (2009) defined a quartz recrystallization isograd in the northern part of the Aar massif. To the south, the grain size of recrystallized grains increases due to an increase of metamorphic temperatures from N to S. The aim of the current project is to carry out quantitative analysis on changes of the dynamic and static recrystallization behavior of quartz. Across the Aar massif, two general types of microstructures have to be discriminated: (i) weakly to moderately deformed host rocks and (ii) intensely deformed mylonites to ultramylonites out of high strain shear zones. In (i), volume fraction and size of recrystallized quartz grains increase towards the S showing grain size changes from around 5 µm up to ca. 200 µm. Southern microstructures are characterized by complete recrystallization. In terms of recrystallization processes, a transition from bulging recrystallization in the N to subgrain rotation recrystallization in the S occurs. Such a change in dynamic recrystallization processes combined with a grain size increase points towards reduced differential stresses with increasing temperature. This temperature gradient is also corroborated by a switch in the active glide systems in quartz from basal to rhomb dominated glide. In contrast to the granitic host rocks, the mylonites and ultramylonites (ii) show smaller recrystallized grain sizes due to enhanced strain rates. However, they also reveal a general increase of recrystallized grain sizes from N to S. In the S, microstructures from (i) and (ii) show equidimensional grains with 120° triple junctions and straight grain boundaries. Such microstructures are typical for static annealing. For that reason, we propose a post-deformational temperature pulse mainly affecting the southern part of the Aar massif. This annealing stage might correlate with the fluid pulse between 12-10 Ma suggested by Challandes et al. (2008). We will present constraints on the grade of deformation based on grain size data and CPO analyses, supporting the hypothesis that various deformation stages are well preserved in statically recrystallized structures.

Deformation-related recrystallization processes

NASA Astrophysics Data System (ADS)

Drury, Martyn R.; Urai, Janos L.

1990-02-01

Recrystallization is a common microstructural transformation that occurs during deformation, metamorphism and diagenesis of rocks. Studies on minerals and rock analogues have demonstrated that a wide range of recrystallization mechanisms can occur. The range of mechanisms is related to the various ways in which two basic processes, grain boundary migration and new grain boundary formation combine to transform the microstructure. Two recent papers (Drury et al., 1985; Urai et al., 1986) have proposed different schemes for the description of recrystallization mechanisms. The purpose of this paper is to provide a unified framework for the description of mechanisms. Recrystallization mechanisms are divided into three main types; rotation mechanisms which principally involve the formation of new grain boundaries; migration mechanisms which principally involve grain boundary migration; and general mechanisms which involve both basic processes. A further distinction is made on the basis of the continuity of the microstructural transformation with respect to time. Each of the three main types of mechanism can be divided into a number of sub-types depending on whether the processes of grain boundary migration, new grain boundary formation and new grain formation occur in a discontinuous or continuous manner with respect to time. As the terms continuous and discontinuous have been used in the metallurgical literature to signify the spatial continuity of the microstructural transformation, the terms discontinuai and continual are used to refer to the temporal continuity of the transformation. It is recommended that the following aspects should be specified, if possible, in a general description of recrystallization mechanisms: (1) How do the basic processes combine to transform the microstructure. (2) If new grain development occurs, what is the development mechanism, and does new grain formation occur in a continual or discontinuai manner. (3) If grain boundary migration is involved in the transformation, what is the migration mechanism (i.e. fast solute escape migration, slow solute loaded migration, fluid assisted migration, etc.), and is migration a continual or discontinuai process. The application of the unified scheme is illustrated by reviewing studies that have provided detailed information on the recrystallization mechanisms involved. The complicating effects of solid solution impurities, dispersed second phase particles and grain boundary fluid films are also considered and it is demonstrated that variations in content of these types of impurity can significantly effect the types of recrystallization that occur in a given material.

Dynamic recrystallization and grain boundary migration in B2 FeAl

NASA Technical Reports Server (NTRS)

Baker, I.; Gaydosh, D. J.

1987-01-01

Transmission electron microscopy and optical microscopy were used to examine polycrystalline specimens of the B2-structured alloy FeAl strained under tension to fracture at elevated temperature. Strain-induced grain boundary migration was observed above 900 K and dynamic recrystallization was found at 1000 K and 1100 K. Little evidence of dynamic recovery was evident but some networks were formed at 1100 K.

Grain Refinement Kinetics in a Low Alloyed Cu–Cr–Zr Alloy Subjected to Large Strain Deformation

PubMed Central

Morozova, Anna; Borodin, Elijah; Bratov, Vladimir; Zherebtsov, Sergey; Kaibyshev, Rustam

2017-01-01

This paper investigates the microstructural evolution and grain refinement kinetics of a solution-treated Cu–0.1Cr–0.06Zr alloy during equal channel angular pressing (ECAP) at a temperature of 673 K via route BC. The microstructural change during plastic deformation was accompanied by the formation of the microband and an increase in the misorientations of strain-induced subboundaries. We argue that continuous dynamic recrystallization refined the initially coarse grains, and discuss the dynamic recrystallization kinetics in terms of grain/subgrain boundary triple junction evolution. A modified Johnson–Mehl–Avrami–Kolmogorov relationship with a strain exponent of about 1.49 is used to express the strain dependence of the triple junctions of high-angle boundaries. Severe plastic deformation by ECAP led to substantial strengthening of the Cu–0.1Cr–0.06Zr alloy. The yield strength increased from 60 MPa in the initial state to 445 MPa after a total strain level of 12. PMID:29210990

A Continuum Model for the Effect of Dynamic Recrystallization on the Stress⁻Strain Response.

PubMed

Kooiker, H; Perdahcıoğlu, E S; van den Boogaard, A H

2018-05-22

Austenitic Stainless Steels and High-Strength Low-Alloy (HSLA) steels show significant dynamic recovery and dynamic recrystallization (DRX) during hot forming. In order to design optimal and safe hot-formed products, a good understanding and constitutive description of the material behavior is vital. A new continuum model is presented and validated on a wide range of deformation conditions including high strain rate deformation. The model is presented in rate form to allow for the prediction of material behavior in transient process conditions. The proposed model is capable of accurately describing the stress⁻strain behavior of AISI 316LN in hot forming conditions, also the high strain rate DRX-induced softening observed during hot torsion of HSLA is accurately predicted. It is shown that the increase in recrystallization rate at high strain rates observed in experiments can be captured by including the elastic energy due to the dynamic stress in the driving pressure for recrystallization. Furthermore, the predicted resulting grain sizes follow the power-law dependence with steady state stress that is often reported in literature and the evolution during hot deformation shows the expected trend.

Modelling and simulation of dynamic recrystallization (DRX) in OFHC copper at very high strain rates

NASA Astrophysics Data System (ADS)

Testa, G.; Bonora, N.; Ruggiero, A.; Iannitti, G.; Persechino, I.; Hörnqvist, M.; Mortazavi, N.

2017-01-01

At high strain rates, deformation processes are essentially adiabatic and if the plastic work is large enough dynamic recrystallization can occur. In this work, an examination on microstructure evolution of OFHC copper in Dynamic Tensile Extrusion (DTE) test, performed at 400 m/s, was carried out. EBSD investigations, along the center line of the fragment remaining in the extrusion die, showed a progressive elongation of the grains, and an accompanying development of a strong <001> + <111> dual fiber texture. Discontinuous dynamic recrystallization (DRX) occurred at larger strains, and it was showed that nucleation occurred during straining. A criterion for DRX to occur, based on the evolution of Zener-Hollomon parameter during the dynamic deformation process, is proposed. Finally, DTE test was simulated using the modified Rusinek-Klepaczko constitutive model incorporating a model for the prediction of DRX initiation.

Dynamic moisture sorption characteristics of enzyme-resistant recrystallized cassava starch.

PubMed

Mutungi, Christopher; Schuldt, Stefan; Onyango, Calvin; Schneider, Yvonne; Jaros, Doris; Rohm, Harald

2011-03-14

The interaction of moisture with enzyme-resistant recrystallized starch, prepared by heat-moisture treatment of debranched acid-modified or debranched non-acid-modified cassava starch, was investigated in comparison with the native granules. Crystallinities of the powdered products were estimated by X-ray diffraction. Moisture sorption was determined using dynamic vapor sorption analyzer and data fitted to various models. Percent crystallinities of native starch (NS), non-acid-modified recrystallized starch (NAMRS), and acid-modified recrystallized starch (AMRS) were 39.7, 51.9, and 56.1%, respectively. In a(w) below 0.8, sorption decreased in the order NS > NAMRS > AMRS in line with increasing sample crystallinities but did not follow this crystallinity dependence at higher a(w) because of condensation and polymer dissolution effects. Adsorbed moisture became internally absorbed in NS but not in NAMRS and AMRS, which might explain the high resistance of the recrystallized starches to digestion because enzyme and starch cannot approach each other over fairly sufficient surface at the molecular level.

Hot Deformation Behavior and Dynamic Recrystallization of Medium Carbon LZ50 Steel

NASA Astrophysics Data System (ADS)

Du, Shiwen; Chen, Shuangmei; Song, Jianjun; Li, Yongtang

2017-03-01

Hot deformation and dynamic recrystallization behaviors of a medium carbon steel LZ50 were systematically investigated in the temperature range from 1143 K to 1443 K (870 °C to 1170 °C) at strain rates from 0.05 to 3s-1 using a Gleeble-3500 thermo-simulation machine. The flow stress constitutive equation for hot deformation of this steel was developed with the two-stage Laasraoui equation. The activation energy of the tested steel was 304.27 KJ/mol, which was in reasonable agreement with those reported previously. The flow stress of this steel in hot deformation was mainly controlled by dislocation climb during their intragranular motion. The effect of Zener-Hollomon parameter on the characteristic points of the flow curves was studied, and the dependence of critical strain on peak strain obeyed a linear equation. Dynamic recrystallization was the most important softening mechanism for the tested steel during hot deformation. Kinetic equation of this steel was also established based on the flow stress. The austenite grain size of complete dynamic recrystallization was a power law function of Zener-Hollomon parameter with an exponent of -0.2956. Moreover, the microstructures induced under different deformation conditions were analyzed.

A Continuum Model for the Effect of Dynamic Recrystallization on the Stress–Strain Response

PubMed Central

Perdahcıoğlu, E. S.; van den Boogaard, A. H.

2018-01-01

Austenitic Stainless Steels and High-Strength Low-Alloy (HSLA) steels show significant dynamic recovery and dynamic recrystallization (DRX) during hot forming. In order to design optimal and safe hot-formed products, a good understanding and constitutive description of the material behavior is vital. A new continuum model is presented and validated on a wide range of deformation conditions including high strain rate deformation. The model is presented in rate form to allow for the prediction of material behavior in transient process conditions. The proposed model is capable of accurately describing the stress–strain behavior of AISI 316LN in hot forming conditions, also the high strain rate DRX-induced softening observed during hot torsion of HSLA is accurately predicted. It is shown that the increase in recrystallization rate at high strain rates observed in experiments can be captured by including the elastic energy due to the dynamic stress in the driving pressure for recrystallization. Furthermore, the predicted resulting grain sizes follow the power-law dependence with steady state stress that is often reported in literature and the evolution during hot deformation shows the expected trend. PMID:29789492

Plasticity-mediated collapse and recrystallization in hollow copper nanowires: a molecular dynamics simulation.

PubMed

Dutta, Amlan; Raychaudhuri, Arup Kumar; Saha-Dasgupta, Tanusri

2016-01-01

We study the thermal stability of hollow copper nanowires using molecular dynamics simulation. We find that the plasticity-mediated structural evolution leads to transformation of the initial hollow structure to a solid wire. The process involves three distinct stages, namely, collapse, recrystallization and slow recovery. We calculate the time scales associated with different stages of the evolution process. Our findings suggest a plasticity-mediated mechanism of collapse and recrystallization. This contradicts the prevailing notion of diffusion driven transport of vacancies from the interior to outer surface being responsible for collapse, which would involve much longer time scales as compared to the plasticity-based mechanism.

Development of high-temperature Kolsky compression bar techniques for recrystallization investigation

NASA Astrophysics Data System (ADS)

Song, B.; Antoun, B. R.; Boston, M.

2012-05-01

We modified the design originally developed by Kuokkala's group to develop an automated high-temperature Kolsky compression bar for characterizing high-rate properties of 304L stainless steel at elevated temperatures. Additional features have been implemented to this high-temperature Kolsky compression bar for recrystallization investigation. The new features ensure a single loading on the specimen and precise time and temperature control for quenching to the specimen after dynamic loading. Dynamic compressive stress-strain curves of 304L stainless steel were obtained at 21, 204, 427, 649, and 871 °C (or 70, 400, 800, 1200, and 1600 °F) at the same constant strain rate of 332 s-1. The specimen subjected to specific time and temperature control for quenching after a single dynamic loading was preserved for investigating microstructure recrystallization.

On the Coupling between Recrystallization and Precipitation Following Hot Deformation in a γ-γ' Nickel-Based Superalloy

NASA Astrophysics Data System (ADS)

Seret, Anthony; Moussa, Charbel; Bernacki, Marc; Bozzolo, Nathalie

2018-06-01

Postdynamic recrystallization and γ' precipitation during cooling from γ' supersolvus temperature after hot compression were studied in the AD730 (AD730 is a trademark of Aubert et Duval Company in Paris, France) γ-γ' nickel-based superalloy. Emphasis was on not only both phenomena as distinct mechanisms but also on their mutual influence in terms of physical mechanisms. The growth of γ' precipitates is hastened in the unrecrystallized grains compared to the recrystallized ones. This could possibly be attributed to the higher dislocation content acting as high-diffusivity paths. Postdynamic recrystallization is not prevented by Smith-Zener pinning of the recrystallization front by the γ' precipitates. Instead, the recrystallization front dissolves γ' precipitates, which then reprecipitate discontinuously or continuously and coherently with the surrounding γ matrix in the recrystallized grains.

Disclination mediated dynamic recrystallization in metals at low temperature.

PubMed

Aramfard, Mohammad; Deng, Chuang

2015-09-16

Recrystallization is one of the most important physical phenomena in condensed matter that has been utilized for materials processing for thousands of years in human history. It is generally believed that recrystallization is thermally activated and a minimum temperature must be achieved for the necessary atomic mechanisms to occur. Here, using atomistic simulations, we report a new mechanism of dynamic recrystallization that can operate at temperature as low as T = 10 K in metals during deformation. In contrast to previously proposed dislocation-based models, this mechanism relies on the generation of disclination quadrupoles, which are special defects that form during deformation when the grain boundary migration is restricted by structural defects such as triple junctions, cracks or obstacles. This mechanism offers an alternative explanation for the grain refinement in metals during severe plastic deformation at cryogenic temperature and may suggest a new method to tailor the microstructure in general crystalline materials.

Disclination mediated dynamic recrystallization in metals at low temperature

PubMed Central

Aramfard, Mohammad; Deng, Chuang

2015-01-01

Recrystallization is one of the most important physical phenomena in condensed matter that has been utilized for materials processing for thousands of years in human history. It is generally believed that recrystallization is thermally activated and a minimum temperature must be achieved for the necessary atomic mechanisms to occur. Here, using atomistic simulations, we report a new mechanism of dynamic recrystallization that can operate at temperature as low as T = 10 K in metals during deformation. In contrast to previously proposed dislocation-based models, this mechanism relies on the generation of disclination quadrupoles, which are special defects that form during deformation when the grain boundary migration is restricted by structural defects such as triple junctions, cracks or obstacles. This mechanism offers an alternative explanation for the grain refinement in metals during severe plastic deformation at cryogenic temperature and may suggest a new method to tailor the microstructure in general crystalline materials. PMID:26374603

Modeling of the flow behavior of SAE 8620H combing microstructure evolution in hot forming

NASA Astrophysics Data System (ADS)

Fu, Xiaobin; Wang, Baoyu; Tang, Xuefeng

2017-10-01

With the development of net-shape forming technology, hot forming process is widely applied to manufacturing gear parts, during which, materials suffer severe plastic distortion and microstructure changes continually. In this paper, to understand and model the flow behavior and microstructure evolution, SAE 8620H, a widely used gear steel, is selected as the object and the flow behavior and microstructure evolution are observed by an isothermal hot compression tests at 1273-1373 K with a strain rate of 0.1-10 s-1. Depending on the results of the compression test, a set of internal-state-variable based unified constitutive equations is put forward to describe the flow behavior and microstructure evaluation of SAE 8620H. Moreover, the evaluation of the dislocation density and the fraction of dynamic recrystallization based on the theory of thermal activation is modeled and reincorporated into the constitutive law. The material parameters in the constitutive model are calculated based on the measured flow stress and dynamic recrystallization fraction. The predicted flow stress under different deformation conditions has a good agreement with the measured results.

The Microstructural Evolution and Special Flow Behavior of Ti-5Al-2Sn-2Zr-4Mo-4Cr During Isothermal Compression at a Low Strain Rate

NASA Astrophysics Data System (ADS)

Sun, J. Z.; Li, M. Q.; Li, H.

2017-09-01

The microstructural evolution and special flow behavior of Ti-5Al-2Sn-2Zr-4Mo-4Cr during isothermal compression at a strain rate of 0.0001 s-1 were investigated. The dislocation climbs in elongated α grains resulted in the formation of low-angle boundaries that transform into high-angle boundaries with greater deformation, and the elongated α grains subsequently separated into homogenous globular α grains with the penetration of the β phase. The simultaneous occurrence of discontinuous dynamic recrystallization and continuous dynamic recrystallization in the primary β grains resulted in a trimode grain distribution. The β grains surrounded by dislocations presented an equilateral-hexagonal morphology, which suggests that grain boundary sliding through dislocation climbs was the main deformation mechanism. The true stress-strain curves for 1073 and 1113 K abnormally intersect at a strain of 0.35, related to the α → β phase transformation and distinct growth of the β grain size.

Plasticity-mediated collapse and recrystallization in hollow copper nanowires: a molecular dynamics simulation

PubMed Central

Raychaudhuri, Arup Kumar; Saha-Dasgupta, Tanusri

2016-01-01

Summary We study the thermal stability of hollow copper nanowires using molecular dynamics simulation. We find that the plasticity-mediated structural evolution leads to transformation of the initial hollow structure to a solid wire. The process involves three distinct stages, namely, collapse, recrystallization and slow recovery. We calculate the time scales associated with different stages of the evolution process. Our findings suggest a plasticity-mediated mechanism of collapse and recrystallization. This contradicts the prevailing notion of diffusion driven transport of vacancies from the interior to outer surface being responsible for collapse, which would involve much longer time scales as compared to the plasticity-based mechanism. PMID:26977380

Molecular Dynamics at the Interface between Ice and Poly(vinyl alcohol) and Ice Recrystallization Inhibition.

PubMed

Weng, Lindong; Stott, Shannon L; Toner, Mehmet

2018-05-01

Ice formation is a ubiquitous process that poses serious challenges for many areas. Nature has evolved a variety of different mechanisms to regulate ice formation. For example, many cold-adapted species produce antifreeze proteins (AFPs) and/or antifreeze glycoproteins (AFGPs) to inhibit ice recrystallization. Although several synthetic substitutes for AF(G)Ps have been developed, the fundamental principles of designing AF(G)P mimics are still missing. In this study, we explored the molecular dynamics of ice recrystallization inhibition (IRI) by poly(vinyl alcohol) (PVA), a well-recognized ice recrystallization inhibitor, to shed light on the otherwise hidden ice-binding mechanisms of chain polymers. Our molecular dynamics simulations revealed a stereoscopic, geometrical match between the hydroxyl groups of PVA and the water molecules of ice, and provided microscopic evidence of the adsorption of PVA to both the basal and prism faces of ice and the incorporation of short-chain PVA into the ice lattice. The length of PVA, i.e., the number of hydroxyl groups, seems to be a key factor dictating the performance of IRI, as the PVA molecule must be large enough to prevent the joining together of adjacent curvatures in the ice front. The findings in this study will help pave the path for addressing a pressing challenge in designing synthetic ice recrystallization inhibitors rationally, by enriching our mechanistic understanding of IRI process by macromolecules.

Ion-specific ice recrystallization provides a facile approach for the fabrication of porous materials

NASA Astrophysics Data System (ADS)

Wu, Shuwang; Zhu, Chongqin; He, Zhiyuan; Xue, Han; Fan, Qingrui; Song, Yanlin; Francisco, Joseph S.; Zeng, Xiao Cheng; Wang, Jianjun

2017-05-01

Ice recrystallization is of great importance to both fundamental research and practical applications, however understanding and controlling ice recrystallization processes remains challenging. Here, we report the discovery of an ion-specific effect on ice recrystallization. By simply changing the initial type and concentration of ions in an aqueous solution, the size of ice grains after recrystallization can be tuned from 27.4+/-4.1 to 277.5+/-30.9 μm. Molecular dynamics simulations show that the ability of the ion to be incorporated into the ice phase plays a key role in the ultimate size of the ice grains after recrystallization. Moreover, by using recrystallized ice crystals as templates, 2D and 3D porous networks with tuneable pore sizes could be prepared from various materials, for example, NaBr, collagen, quantum dots, silver and polystyrene colloids. These porous materials are suitable for a wide range of applications, for example, in organic electronics, catalysis and bioengineering.

Microstructural evolution and rheology of quartz in a mid-crustal shear zone

NASA Astrophysics Data System (ADS)

Rahl, Jeffrey M.; Skemer, Philip

2016-06-01

We present microstructural and crystallographic preferred orientation (CPO) data on quartz deformed in the middle crust to explore the interaction and feedback between dynamic recrystallization, deformation processes, and CPO evolution. The sample investigated here is a moderately deformed quartz-rich mylonite from the Blue Ridge in Virginia. We have created high-resolution crystallographic orientation maps using electron backscatter diffraction (EBSD) of 51 isolated quartz porphyroclasts with recrystallized grain fractions ranging from 10 to 100%. Recrystallized grains are internally undeformed and display crystallographic orientations dispersed around the orientation of the associated parent porphyroclast. We document a systematic decrease in fabric intensity with recrystallization, suggesting that progressive deformation of the recrystallized domains involves processes that can weaken a pre-existing CPO. Relationships between recrystallization fraction and shear strain suggest that complete microstructural re-equilibration requires strains in excess of γ = 5. Variation in the degree of recrystallization implies that strain was accumulated heterogeneously, and that a steady-state microstructure and rheology were not achieved.

Ion-specific ice recrystallization provides a facile approach for the fabrication of porous materials

PubMed Central

Wu, Shuwang; Zhu, Chongqin; He, Zhiyuan; Xue, Han; Fan, Qingrui; Song, Yanlin; Francisco, Joseph S.; Zeng, Xiao Cheng; Wang, Jianjun

2017-01-01

Ice recrystallization is of great importance to both fundamental research and practical applications, however understanding and controlling ice recrystallization processes remains challenging. Here, we report the discovery of an ion-specific effect on ice recrystallization. By simply changing the initial type and concentration of ions in an aqueous solution, the size of ice grains after recrystallization can be tuned from 27.4±4.1 to 277.5±30.9 μm. Molecular dynamics simulations show that the ability of the ion to be incorporated into the ice phase plays a key role in the ultimate size of the ice grains after recrystallization. Moreover, by using recrystallized ice crystals as templates, 2D and 3D porous networks with tuneable pore sizes could be prepared from various materials, for example, NaBr, collagen, quantum dots, silver and polystyrene colloids. These porous materials are suitable for a wide range of applications, for example, in organic electronics, catalysis and bioengineering. PMID:28462937

Ion-specific ice recrystallization provides a facile approach for the fabrication of porous materials.

PubMed

Wu, Shuwang; Zhu, Chongqin; He, Zhiyuan; Xue, Han; Fan, Qingrui; Song, Yanlin; Francisco, Joseph S; Zeng, Xiao Cheng; Wang, Jianjun

2017-05-02

Ice recrystallization is of great importance to both fundamental research and practical applications, however understanding and controlling ice recrystallization processes remains challenging. Here, we report the discovery of an ion-specific effect on ice recrystallization. By simply changing the initial type and concentration of ions in an aqueous solution, the size of ice grains after recrystallization can be tuned from 27.4±4.1 to 277.5±30.9 μm. Molecular dynamics simulations show that the ability of the ion to be incorporated into the ice phase plays a key role in the ultimate size of the ice grains after recrystallization. Moreover, by using recrystallized ice crystals as templates, 2D and 3D porous networks with tuneable pore sizes could be prepared from various materials, for example, NaBr, collagen, quantum dots, silver and polystyrene colloids. These porous materials are suitable for a wide range of applications, for example, in organic electronics, catalysis and bioengineering.

Orogen-scale along-strike continuity in quartz recrystallization microstructures adjacent to the Main Central Thrust: implications for deformation temperatures, strain rates and flow stresses

NASA Astrophysics Data System (ADS)

Law, Richard

2015-04-01

Traced for ~ 1500 km along the foreland edge of the Himalaya from NW India to Bhutan published reports indicate a remarkable along-strike continuity of quartz recrystallization microstructures in the footwall and hanging wall to the Main Central Thrust (MCT). Recrystallization in Lesser Himalayan Series (LHS) rocks in the footwall to the MCT is dominated by grain boundary bulging (BLG) microstructures, while recrystallization in Greater Himalayan Series (GHS) rocks in the hanging wall is dominated by grain boundary migration microstructures that traced structurally upwards transition in to the anatectic core of the GHS. In foreland-positioned high-strain rocks adjacent to the MCT recrystallization is dominated by subgrain rotation (SGR) with transitional BLG-SGR and SGR-GBM microstructures being recorded at structural distances of up to a few hundred meters below and above the MCT, respectively. Correlation with available information on temperatures of metamorphism indicated by mineral phase equilibria and RSCM data suggests that recrystallization in the structural zones dominated by BLG, SGR and GBM occurred at temperatures of ~ 350-450, 450-550 and 550- > 650 °C, respectively. It should be kept in mind, however, that these temperatures are likely to be 'close-to-peak' temperatures of metamorphism, whereas penetrative shearing and recrystallization may have continued during cooling. The dominance of SGR along the more foreland-positioned exposures of the MCT intuitively suggests that shearing occurred under a relatively restricted range of deformation temperatures and strain rates. Plotting the 'close-to-peak' 450-500 °C temperatures of metamorphism indicated for SGR-dominated rocks located at up to a few hundred meters below/above the MCT on the quartz recrystallization map developed by Stipp et al. (2002) indicates 'ball-park' strain rates of ~ 10-13 to 10-10 sec-1. However, only strain rates slower than 10-12 sec-1 on the MCT are likely to be compatible with know convergence rates between the Indian and Asian plates. If shearing continued during retrograde cooling while remaining in the SGR field, then the recrystallization map suggests that a significant drop in deformation temperature (> ~75-100 °C) would result in a decrease in strain rate. In general, however, the presence of a single recrystallization microstructure traced over a large (regional scale) distance does not necessarily mean that deformation temperature (or strain rate) remains constant but could, for example, indicate that spatial variations in deformation temperature are compensated for by changes in strain rate, with grain-scale deformation remaining within a particular recrystallization regime. Constant stress conditions plot along a straight line in the 1/T versus log strain rate space used in the quartz recrystallization mechanism map. This suggests that the observed along-strike consistency of SGR-dominated recrystallization microstructures may indicate near to constant stress boundary conditions (albeit with varying temperatures and strain rates) prevailing along what are now the more foreland-positioned exposures of the MCT. Extrapolation of the Hirth et al. (2001) flow law suggests a flow stress of ~ 30-50 MPa based on the deformation temperatures and strain rates inferred for foreland-positioned exposures of the MCT, in agreement with flow stresses estimated from recrystallized quartz grain size data.

Texture Development and Material Flow Behavior During Refill Friction Stir Spot Welding of AlMgSc

NASA Astrophysics Data System (ADS)

Shen, Junjun; Lage, Sara B. M.; Suhuddin, Uceu F. H.; Bolfarini, Claudemiro; dos Santos, Jorge F.

2018-01-01

The microstructural evolution during refill friction stir spot welding of an AlMgSc alloy was studied. The primary texture that developed in all regions, with the exception of the weld center, was determined to be 〈110〉 fibers and interpreted as a simple shear texture with the 〈110〉 direction aligned with the shear direction. The material flow is mainly driven by two components: the simple shear acting on the horizontal plane causing an inward-directed spiral flow and the extrusion acting on the vertical plane causing an upward-directed or downward-directed flow. Under such a complex material flow, the weld center, which is subjected to minimal local strain, is the least recrystallized. In addition to the geometric effects of strain and grain subdivision, thermally activated high-angle grain boundary migration, particularly continuous dynamic recrystallization, drives the formation of refined grains in the stirred zone.

Quarzt Fabric Insights Across a Low P-High T Shear Zone

NASA Astrophysics Data System (ADS)

Gomez Barreiro, J.; Martinez-Catalan, J. R.; Benitez Perez, J.; Wenk, H.; Vogel, S. C.; Alcock, J. E.

2013-12-01

The evolution of mylonitic fabric in quartzites across a Low-P / High-T gradient within the Lugo Dome Extensional system (NW Spain) is analyzed. Quantitative texture measurements with TOF neutron diffraction, Shape preferred orientation (SPO) and Crystal Size Distribution (CSD) analyses were correlated with tectonothermal data to constraint the prevalence of ductile deformative fabrics exposed to cycles of dynamic and static recrystallization. Results suggest two stages in the evolution of mylonites in close correlation to thermal gradient, 1) a pervasive ductile deformation affecting most of the shear zone volume, with the development of symmetric cross girdle c-axes fabric suggesting slip on {c,r,m} and dynamically recrystallized microstructures which resulted into the refinement of the grain-size. 2) An heterogeneous deformation stage where strain partition led to the formation of relatively active and passive domains. During this late stage, at deeper levels, High T detachments show [c]{m} slip system and dynamic recrystallization activation, with monoclinic texture patterns, meanwhile, passive domains followed an static recrystallization with abnormal grain growth and minor variation of early orthogonal texture patterns Neutron diffraction data (cross) and Rietveld model obtained with MAUD (solid line) of a mylonitic quartzite. Some important planes are indicated for the major phases.

Hot Deformation Behavior of As-Cast 2101 Grade Lean Duplex Stainless Steel and the Associated Changes in Microstructure and Crystallographic Texture

NASA Astrophysics Data System (ADS)

Patra, Sudipta; Ghosh, Abhijit; Singhal, Lokesh Kumar; Podder, Arijit Saha; Sood, Jagmohan; Kumar, Vinod; Chakrabarti, Debalay

2017-01-01

The hot deformation behavior of 2101 grade lean duplex stainless steel (DSS, containing 5 wt pct Mn, 0.2 wt pct N, and 1.4 wt pct Ni) and associated microstructural changes within δ-ferrite and austenite ( γ) phases were investigated by hot-compression testing in a GLEEBLE 3500 simulator over a range of deformation temperatures, T def [1073 K to 1373 K (800 °C to 1100 °C)], and applied strains, ɛ (0.25 to 0.80), at a constant true strain rate of 1/s. The microstructural softening inside γ was dictated by discontinuous dynamic recrystallization (DDRX) at a higher T def [1273 K to 1373 K (1000 °C to 1100 °C)], while the same was dictated by continuous dynamic recrystallization (CDRX) at a lower T def (1173 K (900 °C)]. Dynamic recovery (DRV) and CDRX dominated the softening inside δ-ferrite at T def ≥ 1173 K (900 °C). The dynamic recrystallization (DRX) inside δ and γ could not take place upon deformation at 1073 K (800 °C). The average flow stress level increased 2 to 3 times as the T def dropped from 1273 to 1173 K (1000 °C to 900 °C) and finally to 1073 K (800 °C). The average microhardness values taken from δ-ferrite and γ regions of the deformed samples showed a different trend. At T def of 1373 K (1100 °C), microhardness decreased with the increase in strain, while at T def of 1173 K (900 °C), microhardness increased with the increase in strain. The microstructural changes and hardness variation within individual phases of hot-deformed samples are explained in view of the chemical composition of the steel and deformation parameters ( T def and ɛ).

Comparison Between Different Processing Schedules for the Development of Ultrafine-Grained Dual-Phase Steel

NASA Astrophysics Data System (ADS)

Karmakar, Anish; Sivaprasad, S.; Nath, S. K.; Misra, R. D. K.; Chakrabarti, Debalay

2014-05-01

A comparative study was carried out on the development of ultrafine-grained dual-phase (DP) (ferrite-martensite) structures in a low-carbon microalloyed steel processed using two thermomechanical processing routes, (i) intercritical deformation and (ii) warm-deformation and intercritical annealing. The samples were deformed using Gleeble3500® simulator, maintaining a constant total strain ( ɛ = 1) and strain rate ( = 1/s). Evolution of microstructure and micro-texture was investigated by SEM, TEM, and EBSD. Ultrafine-grained DP structures could be formed by careful selection of deformation temperature, T def (for intercritical deformation) or annealing temperature, T anneal (for warm-deformation and annealing). Overall, the ferrite grain sizes ranged from 1.5 to 4.0 μm, and the sizes and fractions of the uniformly distributed fine-martensitic islands ranged from 1.5 to 3.0 μm and 15 to 45 pct, respectively. Dynamic strain-induced austenite-to-ferrite transformation followed by continuous (dynamic) recrystallization of the ferrite dictated the grain refinement during intercritical deformation, while, continuous (static) recrystallization by pronounced recovery dictated the grain refinement during the warm-deformation and the annealing. Regarding intercritical deformation, the samples cooled to T def indicated finer grain size compared with the samples heated to T def, which are explained in terms of the effects of strain partitioning on the ferrite and the heating during deformation. Alpha-fiber components dominated the texture in all the samples, and the fraction of high-angle boundaries (with >15 deg misorientation) increased with the increasing T def or T anneal, depending on the processing schedule. Fine carbide particles, microalloyed precipitates and austenitic islands played important roles in defining the mechanism of grain refinement that involved retarding conventional ferrite recrystallization and ferrite grain growth. With regard to the intercritical deformation, warm-deformation followed by annealing is a simpler process to control in the rolling mill; however, the need for high-power rolling mill and controlled annealing facility imposes industrial challenges.

Effect of Initial Microstructure on the Microstructural Evolution and Joint Efficiency of a WE43 Alloy During Friction Stir Welding

DTIC Science & Technology

2013-04-01

to maximize joint efficiency. 15. SUBJECT TERMS friction stir welding, strain rate, dynamic recrystallization , joint efficiency, stir zone (SZ...stir welding, Strain rate, Dynamic recrystallization , Joint efficiency, Stir Zone (SZ) Abstract The initial microstructure plays an important role in... eutectic Mg17Al12 phase. Park et al. [7] demonstrated the importance of texture and related it to the mechanical properties of an AZ61 alloy

Glass-Transition Temperature of the β-Relaxation as the Major Predictive Parameter for Recrystallization of Neat Amorphous Drugs.

PubMed

Kissi, Eric Ofosu; Grohganz, Holger; Löbmann, Korbinian; Ruggiero, Michael T; Zeitler, J Axel; Rades, Thomas

2018-03-15

Recrystallization of amorphous drugs is currently limiting the simple approach to improve solubility and bioavailability of poorly water-soluble drugs by amorphization of a crystalline form of the drug. In view of this, molecular mobility, α-relaxation and β-relaxation processes with the associated transition temperatures T gα and T gβ , was investigated using dynamic mechanical analysis (DMA). The correlation between the transition temperatures and the onset of recrystallization for nine amorphous drugs, stored under dry conditions at a temperature of 296 K, was determined. From the results obtained, T gα does not correlate with the onset of recrystallization under the experimental storage conditions. However, a clear correlation between T gβ and the onset of recrystallization was observed. It is shown that at storage temperature below T gβ , amorphous nifedipine retains its amorphous form. On the basis of the correlation, an empirical correlation is proposed for predicting the onset of recrystallization for drugs stored at 0% RH and 296 K.

Reinforcement of the Cube texture during recrystallization of a 1050 aluminum alloy partially recrystallized and 10% cold-rolled

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang Wei; Helbert, Anne-Laure, E-mail: anne-laure.helbert@u-psud.fr; Baudin, Thierry

In high purity Aluminum, very strong {l_brace}100{r_brace}<001> recrystallization texture is developed after 98% cold rolling and annealing at 500 Degree-Sign C. On the contrary, in Aluminum alloys of commercial purity, the Cube component hardly exceeds 30% after complete recrystallization. Parameters controlling Cube orientation development are mainly the solute dragging due to impurities in solid solution and the stored deformation energy. In the present study, besides the 85% cold rolling, two extra annealings and a slight cold rolling are introduced in the processing route to increase the Cube volume fraction. The Cube development was analyzed by X-ray diffraction and Electron BackScatteredmore » Diffraction (EBSD). The nucleation and growth mechanisms responsible for the large Cube growth were investigated using FEG/EBSD in-situ heating experiments. Continuous recrystallization was observed in Cube oriented grains and competed with SIBM (Strain Induced Boundary Migration) mechanism. This latter was favored by the stored energy gap introduced during the additional cold-rolling between the Cube grains and their neighbors. Finally, a Cube volume fraction of 65% was reached after final recrystallization. - Highlights: Black-Right-Pointing-Pointer EBSD in-situ heating experiments of aluminum alloy of commercial purity. Black-Right-Pointing-Pointer A 10% cold-rolling after a partial recrystallization improved Cube nucleation and growth. Black-Right-Pointing-Pointer Annealing before cold-rolling limited the solute drag effect and permitted a large Cube growth. Black-Right-Pointing-Pointer Cube development is enhanced by continuous recrystallization of Cube sub-grains. Black-Right-Pointing-Pointer The preferential Cube growth occurs by SIBM of small Cube grains.« less

Fracture Behavior of High-Nitrogen Austenitic Stainless Steel Under Continuous Cooling: Physical Simulation of Free-Surface Cracking of Heavy Forgings

NASA Astrophysics Data System (ADS)

Wang, Zhenhua; Xue, Hongpeng; Fu, Wantang

2018-03-01

18Mn18Cr0.6N steel was tension tested at 0.001 s-1 to fracture from 1473 K to 1363 K (1200 °C to 1090 °C, fracture temperature) at a cooling rate of 0.4 Ks-1. For comparison, specimens were tension tested at temperatures of 1473 K and 1363 K (1200 °C and 1090 °C). The microstructure near the fracture surface was examined using electron backscatter diffraction analysis. The lowest hot ductility was observed under continuous cooling and was attributed to the suppression of dynamic recrystallization nucleation.

Strain Evolution in Cold-Warm Forged Steel Components Studied by Means of EBSD Technique

PubMed Central

Bonollo, Franco; Bassan, Fabio; Berto, Filippo

2017-01-01

Electron BackScatter Diffraction (EBSD) in conjunction with Field-Emission Environmental Scanning Electron Microscopy (FEG-ESEM) has been used to evaluate the microstructural and local plastic strain evolution in different alloys (AISI 1005, AISI 304L and Duplex 2205) deformed by a single-stage cold and warm forging process. The present work is aimed to describe the different behavior of the austenite and ferrite during plastic deformation as a function of different forging temperatures. Several topological EBSD maps have been measured on the deformed and undeformed states. Then, image quality factor, distributions of the grain size and misorientation have been analyzed in detail. In the austenitic stainless steel, the γ-phase has been found to harden more easily, then α-phase and γ-phase in AISI 1005 and in duplex stainless steel, sequentially. Compared to the high fraction of continuous dynamic recrystallized austenitic zones observed in stainless steels samples forged at low temperatures, the austenitic microstructure of samples forged at higher temperatures, 600–700 °C, has been found to be mainly characterized by large and elongated grains with some colonies of fine nearly-equiaxed grains attributed to discontinuous dynamic recrystallization. PMID:29258249

Dynamic recrystallization mechanisms and their transition in the Daling Thrust (DT) zone, Darjeeling-Sikkim Himalaya

NASA Astrophysics Data System (ADS)

Ghosh, Subhajit; Bose, Santanu; Mandal, Nibir; Dasgupta, Sujoy

2016-04-01

The Daling Thrust (DT) delineates a zone of intense shear localization in the Lesser Himalayan Sequence (LHS) of the Darjeeling-Sikkim Himalaya. From microstructural studies of deformed quartzite samples, we show a transition in the dynamic recrystallization mechanism with increasing distance from the DT, dominated by grain boundary bulging (BLG) recrystallization closest to the DT, and progressively replaced by sub-grain rotation (SGR) recrystallization away from the thrust. The transition is marked by a characteristic variation in the fractal dimension (D) of grain boundaries, estimated from the area-perimeter method. For the BLG regime, D ≈ 1.046, which decreases significantly to a value as low as 1.025 for the SGR regime. Using the available thermal data for BLG and SGR recrystallization, we infer increasing deformation temperatures away from the DT in the hanging wall. Based on the quartz piezometer our estimates reveal strong variations in the flow stress (59.00 MPa to 16.00 MPa) over a distance of 1.2 km from the DT. Deformation mechanism maps constructed for different temperatures indicate that the strain rates (10- 12 S- 1 to 10- 14 S- 1) comply with the geologically possible range. Finally, we present a mechanical model to provide a possible explanation for the cause of stress intensification along the DT.

A Mechanistic Thermal Fatigue Model for SnAgCu Solder Joints

NASA Astrophysics Data System (ADS)

Borgesen, Peter; Wentlent, Luke; Hamasha, Sa'd.; Khasawneh, Saif; Shirazi, Sam; Schmitz, Debora; Alghoul, Thaer; Greene, Chris; Yin, Liang

2018-02-01

The present work offers both a complete, quantitative model and a conservative acceleration factor expression for the life span of SnAgCu solder joints in thermal cycling. A broad range of thermal cycling experiments, conducted over many years, has revealed a series of systematic trends that are not compatible with common damage functions or constitutive relations. Complementary mechanical testing and systematic studies of the evolution of the microstructure and damage have led to a fundamental understanding of the progression of thermal fatigue and failure. A special experiment was developed to allow the effective deconstruction of conventional thermal cycling experiments and the finalization of our model. According to this model, the evolution of damage and failure in thermal cycling is controlled by a continuous recrystallization process which is dominated by the coalescence and rotation of dislocation cell structures continuously added to during the high-temperature dwell. The dominance of this dynamic recrystallization contribution is not consistent with the common assumption of a correlation between the number of cycles to failure and the total work done on the solder joint in question in each cycle. It is, however, consistent with an apparent dependence on the work done during the high-temperature dwell. Importantly, the onset of this recrystallization is delayed by pinning on the Ag3Sn precipitates until these have coarsened sufficiently, leading to a model with two terms where one tends to dominate in service and the other in accelerated thermal cycling tests. Accumulation of damage under realistic service conditions with varying dwell temperatures and times is also addressed.

A New Cellular Automaton Method Coupled with a Rate-dependent (CARD) Model for Predicting Dynamic Recrystallization Behavior

NASA Astrophysics Data System (ADS)

Azarbarmas, M.; Aghaie-Khafri, M.

2018-03-01

A comprehensive cellular automaton (CA) model should be coupled with a rate-dependent (RD) model for analyzing the RD deformation of alloys at high temperatures. In the present study, a new CA technique coupled with an RD model—namely, CARD—was developed. The proposed CARD model was used to simulate the dynamic recrystallization phenomenon during the hot deformation of the Inconel 718 superalloy. This model is capable of calculating the mean grain size and volume fraction of dynamic recrystallized grains, and estimating the phenomenological flow behavior of the material. In the presented model, an actual orientation definition comprising three Euler angles was used by implementing the electron backscatter diffraction data. For calculating the lattice rotation of grains, it was assumed that all slip systems of grains are active during the high-temperature deformation because of the intrinsic rate dependency of the procedure. Moreover, the morphological changes in grains were obtained using a topological module.

Effect of Mo on dynamic recrystallization and microstructure development of microalloyed steels

NASA Astrophysics Data System (ADS)

Schambron, Thomas; Dehghan-Manshadi, Ali; Chen, Liang; Gooch, Taliah; Killmore, Chris; Pereloma, Elena

2017-07-01

The dynamic recrystallization (DRX) behaviour, mechanical properties and microstructure development of four low carbon, Nb-Ti-containing micro-alloyed steels with Mo contents from 0 to 0.27 wt% were studied. Plane strain compression tests were performed in a Gleeble 3500 thermomechanical simulator. The effects of composition, deformation temperature and strain rate on the DRX parameters and resultant microstructures were examined. The volume fraction of recrystallised grains was estimated from micrographs and a DRX model. The stress-strain curves showed the typical signs of DRX over a wide range of deformation conditions. Dynamic recovery was only observed for higher strain rates (5 s-1) and/or lower deformation temperatures (below 1000 °C). It was shown that Mo increases the hot strength by around 100 MPa per weight percent. In addition, it has an effect on retarding recrystallization in microalloyed steels by increasing the activation energy for DRX by 320 kJ/molK per weight percent. This was attributed to solute drag and the interaction with other microalloying elements.

Activity of slip in amphibolite facies, fine-grained recrystallized quartz aggregates: high differential stress during high-T creep of quartz?

NASA Astrophysics Data System (ADS)

Viegas, G.; Menegon, L. M.; Archanjo, C. J.

2016-12-01

Quartz axis fabrics are a valuable tool to investigate strain partitioning/distribution in both naturally- and experimentally deformed quartz. Previous works have shown that slip dominates at high temperatures (> 600º C) and water-rich, commonly sub-magmatic conditions, typically associated with large grain sizes and grain boundary migration microstructures. In the Pernambuco shear zone, sheared quartz veins from a protomylonitic granitoid formed during the main amphibolite facies event constrained at mid-crustal conditions (550-600ºC, 5 kbar). The veins contain heterogeneously-deformed primary quartz grains, which typically form both flattened and elongated ribbons as well as more equant porphyroclasts surrounded by aggregates of fine-grained (ca. 20 µm) recrystallized aggregates. Recrystallized quartz with the same fine grain size may also occur in intracrystalline bands within the porphyroclasts. Chessboard extinction is widely observed in the porphyroclasts, and subgrain boundaries are either parallel or normal to the (0001) direction, suggesting slip on both basal and prismatic planes during recrystallization. Crystallographic preferred orientations (CPOs) of porphyroclasts (≥ 100 µm) show maxima of (0001) axes subparallel to Z and X, suggesting coeval glide along both basal and prism planes during shearing. In the recrystallized aggregates, fabric strength tends to become weaker, but still records glide along and directions. These preliminary results suggest that naturally deformed quartz veins record coeval activity of and slip during dynamic recrystallization under amphibolite facies conditions. The microstructure suggests that the CPO of the fine-grained aggregates is host-controlled and results from dominant subgrain rotation recrystallization. To our knowledge, activity of slip in fine-grained recrystallized aggregates has never been reported before. Thus, these preliminary results call into question the general view that slip is expected to be active only during dominant high-T grain boundary migration in the lower crust. In our samples, a fine grain size of dynamically recrystallized quartz associated with slip might indicate high differential stress/strain rates during high-T viscous creep along the Pernambuco shear zone.

Constitutive relations for determining the critical conditions for dynamic recrystallization behavior

NASA Astrophysics Data System (ADS)

Choe, J. I.

2016-04-01

A series mathematical model has been developed for the prediction of flow stress and microstructure evolution during the hot deformation of metals such as copper or austenitic steels with low stacking fault energies, involving features of both diffusional flow and dislocation motion. As the strain rate increases, multiple peaks on the stress-strain curve decrease. At a high strain rate, the stress rises to a single peak, while dynamic recrystallization causes an oscillatory behavior. At a low strain rate (when there is sufficient time for the recrystallizing grains to grow before they become saturated with high dislocation density with an increase in strain rate), the difference in stored stress between recrystallizing and old grains diminishes, resulting in reduced driving force for grain growth and rendering smaller grains in the alloy. The final average grain size at the steady stage (large strain) increases with a decrease in the strain rate. During large strain deformation, grain size reduction accompanying dislocation creep might be balanced by the grain growth at the border delimiting the ranges of realization (field boundary) of the dislocation-creep and diffusion-creep mechanisms.

Physical Simulation of a Duplex Stainless Steel Friction Stir Welding by the Numerical and Experimental Analysis of Hot Torsion Tests

NASA Astrophysics Data System (ADS)

da Fonseca, Eduardo Bertoni; Santos, Tiago Felipe Abreu; Button, Sergio Tonini; Ramirez, Antonio Jose

2016-09-01

Physical simulation of friction stir welding (FSW) by means of hot torsion tests was performed on UNS S32205 duplex stainless steel. A thermomechanical simulator Gleeble 3800® with a custom-built liquid nitrogen cooling system was employed to reproduce the thermal cycle measured during FSW and carry out the torsion tests. Microstructures were compared by means of light optical microscopy and electron backscatter diffraction. True strain and strain rate were calculated by numerical simulation of the torsion tests. Thermomechanically affected zone (TMAZ) was reproduced at peak temperature of 1303 K (1030 °C), rotational speeds of 52.4 rad s-1 (500 rpm) and 74.5 rad s-1 (750 rpm), and 0.5 to 0.75 revolutions, which represent strain rate between 10 and 16 s-1 and true strain between 0.5 and 0.8. Strong grain refinement, similar to the one observed in the stir zone (SZ), was attained at peak temperature of 1403 K (1130 °C), rotational speed of 74.5 rad s-1 (750 rpm), and 1.2 revolution, which represent strain rate of 19 s-1 and true strain of 1.3. Continuous dynamic recrystallization in ferrite and dynamic recrystallization in austenite were observed in the TMAZ simulation. At higher temperature, dynamic recovery of austenite was also observed.

Friction stir welding process and material microstructure evolution modeling in 2000 and 5000 series of aluminum alloy

NASA Astrophysics Data System (ADS)

Yalavarthy, Harshavardhan

Interactions between the rotating and advancing pin-shaped tool (terminated at one end with a circular-cylindrical shoulder) with the clamped welding-plates and the associated material and heat transport during a Friction Stir Welding (FSW) process are studied computationally using a fully-coupled thermo-mechanical finite-element analysis. To surmount potential numerical problems associated with extensive mesh distortions/entanglement, an Arbitrary Lagrangian Eulerian (ALE) formulation was used which enabled adaptive re-meshing (to ensure the continuing presence of a high-quality mesh) while allowing full tracking of the material free surfaces. To demonstrate the utility of the present computational approach, the analysis is applied to the cases of same-alloy FSW of two Aluminum-alloy grades: (a) AA5083 (a solid-solution strengthened and strain-hardened/stabilized Al-Mg-Mn alloy); and (b) AA2139 (a precipitation hardened quaternary Al-Cu-Mg-Ag alloy). Both of these alloys are currently being used in military-vehicle hull structural and armor systems. In the case of non-age-hardenable AA5083, the dominant microstructure evolution processes taking place during FSW are extensive plastic deformation and dynamic recrystallization of highly-deformed material subjected to elevated temperatures approaching the melting temperature. To account for the competition between plastic-deformation controlled strengthening and dynamic-recrystallization induced softening phenomena during the FSW process, the original Johnson-Cook strain- and strain-rate hardening and temperature-softening material strength model is modified in the present work using the available recrystallization-kinetics experimental data. In the case of AA2139, in addition to plastic deformation and dynamic recrystallization, precipitates coarsening, over-aging, dissolution and re-precipitation had to be also considered. Limited data available in the open literature pertaining to the kinetics of the aforementioned microstructure-evolution processes are used to predict variation in the material hardness and the residual stresses throughout the various FSW zones of the two alloys. The results showed that with proper modeling of the material behavior under high-temperature/severe-plastic-deformation conditions, significantly improved agreement can be attained between the computed and measured post-FSW residual-stress and material-strength distribution results. Keywords: Friction Stir Welding; AA5083; AA2139; Johnson-Cook Strength Model; Finite Element Analysis; Hardness Prediction.

Deformation-Induced Recrystallization of Magnesium Single Crystals at Ambient Temperature

NASA Astrophysics Data System (ADS)

Molodov, K. D.; Al-Samman, T.; Molodov, D. A.

2015-04-01

Specially oriented magnesium single crystals were subjected to plane strain compression along the <112¯0> direction in c-axis extension at ambient temperature. The samples exhibited outstanding formability deforming up to a logarithmic final strain of -1. Investigations by optical and orientation imaging microscopy revealed that massive {101¯2} extension twinning at low strains consumed the whole sample and resulted in new soft orientations for slip. Observations also indicated that additional twinning took place in the completely twinned matrix by secondary and tertiary twinning events. At advanced stages of deformation newly formed, equiaxed small grains were observed within numerous bands related to former deformation twins. These “recrystallized” grains characterized by a low grain orientation spread of less than 1° generated new orientations, which led to a substantial weakening and randomization of the texture during deformation up to very large strains. The reported results in this paper are discussed with regard to the microstructure evolution arising from multiple twinning and continuous dynamic recrystallization at room temperature.

Investigation of nucleation processes during dynamic recrystallization of ice using cryo-EBSD.

PubMed

Chauve, T; Montagnat, M; Barou, F; Hidas, K; Tommasi, A; Mainprice, D

2017-02-13

Nucleation mechanisms occurring during dynamic recrystallization play a crucial role in the evolution of microstructures and textures during high temperature deformation. In polycrystalline ice, the strong viscoplastic anisotropy induces high strain heterogeneities between grains which control the recrystallization mechanisms. Here, we study the nucleation mechanisms occurring during creep tests performed on polycrystalline columnar ice at high temperature and stress (T=-5°C;σ=0.5 MPa) by post-mortem analyses of deformation microstructures using cryogenic electron backscatter diffraction. The columnar geometry of the samples enables discrimination of the nuclei from the initial grains. Various nucleation mechanisms are deduced from the analysis of the nuclei relations with the dislocation sub-structures within grains and at grain boundaries. Tilt sub-grain boundaries and kink bands are the main structures responsible for development of polygonization and mosaic sub-structures. Nucleation by bulging at serrated grain boundaries is also an efficient nucleation mechanism near the grain boundaries where strain incompatibilities are high. Observation of nuclei with orientations not related to the 'parent' ones suggests the possibility of 'spontaneous' nucleation driven by the relaxation of the dislocation-related internal stress field. The complexity of the nucleation mechanisms observed here emphasizes the impact of stress and strain heterogeneities on dynamic recrystallization mechanisms.This article is part of the themed issue 'Microdynamics of ice'. © 2016 The Author(s).

Investigation of nucleation processes during dynamic recrystallization of ice using cryo-EBSD

PubMed Central

Barou, F.; Hidas, K.; Tommasi, A.; Mainprice, D.

2017-01-01

Nucleation mechanisms occurring during dynamic recrystallization play a crucial role in the evolution of microstructures and textures during high temperature deformation. In polycrystalline ice, the strong viscoplastic anisotropy induces high strain heterogeneities between grains which control the recrystallization mechanisms. Here, we study the nucleation mechanisms occurring during creep tests performed on polycrystalline columnar ice at high temperature and stress (T=−5°C;σ=0.5 MPa) by post-mortem analyses of deformation microstructures using cryogenic electron backscatter diffraction. The columnar geometry of the samples enables discrimination of the nuclei from the initial grains. Various nucleation mechanisms are deduced from the analysis of the nuclei relations with the dislocation sub-structures within grains and at grain boundaries. Tilt sub-grain boundaries and kink bands are the main structures responsible for development of polygonization and mosaic sub-structures. Nucleation by bulging at serrated grain boundaries is also an efficient nucleation mechanism near the grain boundaries where strain incompatibilities are high. Observation of nuclei with orientations not related to the ‘parent’ ones suggests the possibility of ‘spontaneous’ nucleation driven by the relaxation of the dislocation-related internal stress field. The complexity of the nucleation mechanisms observed here emphasizes the impact of stress and strain heterogeneities on dynamic recrystallization mechanisms. This article is part of the themed issue ‘Microdynamics of ice’. PMID:28025294

EBSD characterization of low temperature deformation mechanisms in modern alloys

NASA Astrophysics Data System (ADS)

Kozmel, Thomas S., II

For structural applications, grain refinement has been shown to enhance mechanical properties such as strength, fatigue resistance, and fracture toughness. Through control of the thermos-mechanical processing parameters, dynamic recrystallization mechanisms were used to produce microstructures consisting of sub-micron grains in 9310 steel, 4140 steel, and Ti-6Al-4V. In both 9310 and 4140 steel, the distribution of carbides throughout the microstructure affected the ability of the material to dynamically recrystallize and determined the size of the dynamically recrystallized grains. Processing the materials at lower temperatures and higher strain rates resulted in finer dynamically recrystallized grains. Microstructural process models that can be used to estimate the resulting microstructure based on the processing parameters were developed for both 9310 and 4140 steel. Heat treatment studies performed on 9310 steel showed that the sub-micron grain size obtained during deformation could not be retained due to the low equilibrium volume fraction of carbides. Commercially available aluminum alloys were investigated to explain their high strain rate deformation behavior. Alloys such as 2139, 2519, 5083, and 7039 exhibit strain softening after an ultimate strength is reached, followed by a rapid degradation of mechanical properties after a critical strain level has been reached. Microstructural analysis showed that the formation of shear bands typically preceded this rapid degradation in properties. Shear band boundary misorientations increased as a function of equivalent strain in all cases. Precipitation behavior was found to greatly influence the microstructural response of the alloys. Additionally, precipitation strengthened alloys were found to exhibit similar flow stress behavior, whereas solid solution strengthened alloys exhibited lower flow stresses but higher ductility during dynamic loading. Schmid factor maps demonstrated that shear band formation behavior was influenced by texturing in these alloys.

Microstructural Evolution of Al-1Fe (Weight Percent) Alloy During Accumulative Continuous Extrusion Forming

NASA Astrophysics Data System (ADS)

Wang, Xiang; Guan, Ren-Guo; Tie, Di; Shang, Ying-Qiu; Jin, Hong-Mei; Li, Hong-Chao

2018-04-01

As a new microstructure refining method, accumulative continuous extrusion forming (ACEF) cannot only refine metal matrix but also refine the phases that exist in it. In order to detect the refinements of grain and second phase during the process, Al-1Fe (wt pct) alloy was processed by ACEF, and the microstructural evolution was analyzed by electron backscatter diffraction (EBSD) and transmission electron microscopy (TEM). Results revealed that the average grain size of Al-1Fe (wt pct) alloy decreased from 13 to 1.2 μm, and blocky Al3Fe phase with an average length of 300 nm was granulated to Al3Fe particle with an average diameter of 200 nm, after one pass of ACEF. Refinement of grain was attributed to continuous dynamic recrystallization (CDRX), and the granulation of Al3Fe phase included the spheroidization resulting from deformation heat and the fragmentation caused by the coupling effects of strain and thermal effect. The spheroidization worked in almost the entire deformation process, while the fragmentation required strain accumulation. However, fragmentation contributed more than spheroidization. Al3Fe particle stimulated the formation of substructure and retarded the migration of recrystallized grain boundary, but the effect of Al3Fe phase on refinement of grain could only be determined by the contrastive investigation of Al-1Fe (wt pct) alloy and pure Al.

Titanium concentration in quartz as a record of multiple deformation mechanisms in an extensional shear zone

NASA Astrophysics Data System (ADS)

Nachlas, William O.; Whitney, Donna L.; Teyssier, Christian; Bagley, Brian; Mulch, Andreas

2014-04-01

Results of high precision analysis of Ti concentration ([Ti]) in quartz representing different recrystallization microstructures in a suite of progressively deformed quartzite mylonites show the effect of recrystallization on distribution of Ti in quartz. Petrographic observations and ion microprobe analysis reveals three texturally and geochemically distinct quartz microstructures in mylonites: (1) cores of recrystallized quartz ribbons preserve the highest [Ti] and are interpreted to have recrystallized via grain boundary migration recrystallization, (2) recrystallized rims and grain margins preserve a lower and more variable [Ti] and are interpreted to reflect the combined influence of subgrain rotation and bulging recrystallization, and (3) neocrystallized quartz precipitated in dilatancy sites has low (˜1 ppm) [Ti], reflecting the Ti content of the syndeformational fluid. Muscovite in nonmylonitic quartzite (at the base of the sampling traverse) is compositionally zoned, whereas muscovite in mylonitic quartzite shows a progressive decreasing in zoning in higher strain samples. Three-dimensional phase distribution mapping using X-ray computed tomography analysis of rock hand samples reveals that Ti-bearing accessory phases are less abundant and more dispersed in higher strained mylonites compared to nonmylonitic quartzite. This study demonstrates the influence of dynamic recrystallization on Ti substitution in quartz and evaluates the Ti buffering capacity of aqueous fluids (meteoric versus metamorphic/magmatic) as well as the distribution and reactivity of Ti-bearing accessory phases in a deforming quartzite. Results of this study suggest that Ti-in-quartz thermobarometry of deformed quartz is a sensitive technique for resolving the multistage history of quartz deformation and recrystallization in crustal shear zones.

Strain softening during tension in cold drawn Cu–Ag alloys

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chang, L.L., E-mail: lilichang@sdu.edu.cn; Wen, S.; Li, S.L.

2015-10-15

Experiments were conducted on Cu–0.1wt.%Ag alloys to evaluate the influence of producing procedures and annealing conditions on microstructure evolution and mechanical properties of Cu–Ag alloys. Optical microscopy (OM), electron back-scattered diffraction (EBSD), X-ray diffraction (XRD) and transmission electron microscopy (TEM) were used for microstructural evaluation and mechanical properties were characterized by tensile tests. The results indicated that hot-extruded Cu–Ag alloys had a typical dynamic recrystallized microstructure with equiaxed grains. Cold drawing at room temperature leaded to partial recrystallized microstructure with a mixture of coarse and fine grains. The dominate {001}<100 > cubic texture formed during hot extrusion was changed tomore » be {112}<111 > copper texture by cold drawing. Strain softening occurred during room temperature tension of cold drawn Cu–Ag alloys with an average grain size of 13–19.7 μm. - Highlights: • Strain softening occurred during tension of Cu–Ag alloys with coarse grain size. • Work hardening was observed in hot-extruded and annealed Cu–0.1wt.%Ag alloys. • Strain softening was ascribed to dynamic recovery and dynamic recrystallization.« less

Friction Stir Back Extrusion of Aluminium Alloys for Automotive Applications

NASA Astrophysics Data System (ADS)

Xu, Zeren

Since the invention of Friction Stir Welding in 1991 as a solid state joining technique, extensive scientific investigations have been carried out to understand fundamental aspects of material behaviors when processed by this technique, in order to optimize processing conditions as well as mechanical properties of the welds. Based on the basic principles of Friction Stir Welding, several derivatives have also been developed such as Friction Stir Processing, Friction Extrusion and Friction Stir Back Extrusion. Friction Stir Back Extrusion is a novel technique that is proposed recently and designed for fabricating tubes from lightweight alloys. Some preliminary results have been reported regarding microstructure and mechanical properties of Friction Stir Back Extrusion processed AZ31 magnesium alloy, however, systematic study and in-depth investigations are still needed to understand the materials behaviors and underlying mechanisms when subjected to Friction Stir Back Extrusion, especially for age-hardenable Al alloys. In the present study, Friction Stir Back Extrusion processed AA6063-T5 and AA7075-T6 alloys are analyzed with respect to grain structure evolution, micro-texture change, recrystallization mechanisms, precipitation sequence as well as mechanical properties. Optical Microscopy, Electron Backscatter Diffraction, Transmission Electron Microscopy, Vickers Hardness measurements and uniaxial tensile tests are carried out to characterize the microstructural change as well as micro and macro mechanical properties of the processed tubes. Special attention is paid to the micro-texture evolution across the entire tube and dynamic recrystallization mechanisms that are responsible for grain refinement. Significant grain refinement has been observed near the processing zone while the tube wall is characterized by inhomogeneous grain structure across the thickness for both alloys. Dissolution of existing precipitates is noticed under the thermal hysterias imposed by Friction Stir Back Extrusion process, resulting in decreased strength but improved elongation of the processed tubes; a post-process aging step can effectively restore the mechanical properties of the processed tubes by allowing for the reprecipitation of solute elements in the form of fine, dispersed precipitates. Texture analysis performed for AA6063 alloy suggests the dominance of simple shear type textures with clear transition from initial texture to stable B/ ?B components via intermediate types that are stable under moderate strain levels. In order to identify the texture components properly, rigid body rotations are applied to the existing coordinate system to align it to local shear reference frame. Surprisingly, for AA7075 tubes, and fibers are observed to be the dominant texture components in the transition region as well as thermomechanically affected zone while the processing zone is characterized by random texture. The underlying mechanisms responsible for the formation of random texture are discussed in Chapter 5 based on Electron Backscatter Diffraction analysis. Comparative discussions are also carried out for the recrystallization mechanisms that are responsible for grain structure evolution of both alloys. Continuous grain subdivision and reorientation is cited as the dominant mechanism for the recrystallization of AA6063 alloys, while dynamic recrystallization occurs mainly in the form of Geometric Dynamic Recrystallization and progressive subgrain rotations near grain boundaries in AA7075 alloys.

The deformation record of olivine in mylonitic peridotites from the Finero Complex, Ivrea Zone: Separate deformation cycles during exhumation

NASA Astrophysics Data System (ADS)

Matysiak, Agnes K.; Trepmann, Claudia A.

2015-12-01

Mylonitic peridotites from the Finero complex are investigated to detect characteristic olivine microfabrics that can resolve separate deformation cycles at different metamorphic conditions. The heterogeneous olivine microstructures are characterized by deformed porphyroclasts surrounded by varying amounts of recrystallized grains. A well-developed but only locally preserved foam structure is present in recrystallized grain aggregates. This indicates an early stage of dynamic recrystallization and subsequent recovery and recrystallization at quasi-static stress conditions, where the strain energy was reduced such that a reduction in surface energy controlled grain boundary migration. Ultramylonites record a renewed stage of localized deformation and recrystallization by a second generation of recrystallized grains that do not show a foam structure. This second generation of recrystallized grains as well as sutured grain and kink band boundaries of porphyroclasts indicate that these microstructures developed during a stage of localized deformation after development of the foam structure. The heterogeneity of the microfabrics is interpreted to represent several (at least two) cycles of localized deformation separated by a marked hiatus with quasi-static recrystallization and recovery and eventually grain growth. The second deformation cycle did not only result in reactivation of preexisting shear zones but instead also locally affected the host rock that was not deformed in the first stage. Such stress cycles can result from sudden increases in differential stress imposed by seismic events, i.e., high stress-loading rates, during exhumation of the Finero complex.

Recrystallization as a controlling process in the wear of some f.c.c. metals

NASA Technical Reports Server (NTRS)

Bill, R. C.; Wisander, D.

1977-01-01

Detailed examination of copper specimens after sliding against 440 C steel in liquid methane at speeds up to 25 m/s and loads of up to 2 kg showed the metal comprising the wear surface to possess a fine cell recrystallized structure. Wear proceeded by the plastic shearing of metal in this near surface region without the occurrence of visible metal transfer. A dynamic balance between the intense shear process at the surface and the nucleation of recrystallized grains was proposed to account for the behavior of the metal at the wear surface. Sliding wear experiments were also conducted on Ag, Cu-10% Al, Cu-10% Sn, Ni and Al. It was found that low wear and the absence of heavy metal transfer were associated with those metals observed to undergo recrystallization nucleation without prior recovery.

Microstructure in Worn Surface of Hadfield Steel Crossing

NASA Astrophysics Data System (ADS)

Zhang, F. C.; Lv, B.; Wang, T. S.; Zheng, C. L.; Li, M.; Zhang, M.

In this paper a failed Hadfield (high manganese austenite) steel crossing used in railway system was studied. The microstructure in the worn surfaces of the crossing was investigated using optical microscopy, scanning electron microscopy, transmission electron microscopy and Mössbauer spectroscopy. The results indicated that a nanocrystallization layer formed on the surface of the crossing served. The formation mechanism of the nanocrystalline is the discontinuous dynamic recrystallization. The energy for the recrystallization nucleus formation originates from the interactions between the twins, the dislocations, as well as twin and dislocation. High-density vacancies promoted the recrystallization process including the dislocation climb and the atom diffusion.

Recrystallization of freezable bound water in aqueous solutions of medium concentration

NASA Astrophysics Data System (ADS)

Lishan, Zhao; Liqing, Pan; Ailing, Ji; Zexian, Cao; Qiang, Wang

2016-07-01

For aqueous solutions with freezable bound water, vitrification and recrystallization are mingled, which brings difficulty to application and misleads the interpretation of relevant experiments. Here, we report a quantification scheme for the freezable bound water based on the water-content dependence of glass transition temperature, by which also the concentration range for the solutions that may undergo recrystallization finds a clear definition. Furthermore, we find that depending on the amount of the freezable bound water, different temperature protocols should be devised to achieve a complete recrystallization. Our results may be helpful for understanding the dynamics of supercooled aqueous solutions and for improving their manipulation in various industries. Project supported by the Knowledge Innovation Project of Chinese Academy of Sciences on Water Science Research (Grant No. KJZD-EW-M03) and the National Natural Science Foundation of China (Grant Nos. 11474325 and 11290161).

Surface premelting/recrystallization governing the collapse of open-cell nanoporous Cu via thermal annealing.

PubMed

Wang, L; Zhang, X M; Deng, L; Tang, J F; Xiao, S F; Deng, H Q; Hu, W Y

2018-06-04

We systematically investigate the collapse of a set of open-cell nanoporous Cu (np-Cu) materials with the same porosity and shape but different specific surface areas, during thermal annealing, by performing large-scale molecular dynamics simulations. Two mechanisms govern the collapse of np-Cu. One is direct surface premelting, facilitating the collapse of np-Cu, when the specific surface area is less than a critical value (∼2.38 nm-1). The other is recrystallization followed by surface premelting, accelerating the sloughing of ligaments and the annihilation of voids, when the critical specific surface area is exceeded. Surface premelting results from surface reconstruction by prompting localized "disordering" and "chaos" on the surface, and the melting temperature reduces linearly with the increase of the specific surface area. Recrystallization is followed by surface premelting as the melting temperature is below the supercooling point, where a liquid is unstable and instantaneously recrystallizes.

High-Temperature Flow Stress and Recrystallization Characteristics of Al-Bearing Microalloyed TWIP Steels

NASA Astrophysics Data System (ADS)

Somani, Mahesh Chandra; Porter, David A.; Hamada, Atef S.; Karjalainen, L. Pentti

2015-11-01

In this study, the effects of microalloying (Nb,V) and aluminum on the constitutive flow behavior and static recrystallization (SRX) characteristics of microalloyed TWIP steels (Fe-20Mn-0.6C-Al-(Nb,V)) have been investigated under hot deformation conditions. Compression tests in a Gleeble simulator, including the double-hit technique, enabled the acquisition of flow stress and recrystallization data. These were analyzed to determine the powers of strain and strain rate as well as the activation energies of deformation and recrystallization ( Q def and Q rex). Aluminum increased the flow stress and activation energy of deformation and delayed the onset of dynamic recrystallization of microalloyed TWIP steels. While microalloying with V up to 0.3 pct seems to have little or no effect on the SRX kinetics, microalloying with 0.026 pct Nb significantly slowed down the SRX rate, similarly as in the case of low C-Mn steels. Addition of high aluminum (4.9 pct) marginally retarded the SRX kinetics in comparison with the steels with low aluminum (1.5 pct), with or without microalloying with V.

Deformation Behavior of a Coarse-Grained Mg-8Al-1.5Ca-0.2Sr Magnesium Alloy at Elevated Temperatures

NASA Astrophysics Data System (ADS)

Lou, Yan; Liu, Xiao

2018-02-01

The compression tests were carried out on a coarse-grained Mg-8Al-1.5Ca-0.2Sr magnesium alloy samples at temperatures from 300 to 450 °C and strain rates from 0.001 to 10 s-1. The flow stress curves were analyzed using the double-differentiation method, and double minima were detected on the flow curves. The first set of minima is shown to identify the critical strain for twinning, while the second set indicates the critical strain for the initiation of dynamic recrystallization (DRX). Twin variant selection was numerically identified by comprehensive analysis of the Schmid factors for different deformation modes and the accommodation strains imposed on neighboring grains. It was found that twinning is initiated before DRX. Dynamic recrystallization volume increases with strain rate at a given deformation temperature. At high strain rate, various twin variants are activated to accommodate deformation, leading to the formation of twin intersections and high DRX volume. Fully dynamic recrystallized structure can be obtained at both high and low strain rates due to the high mobility of the grain and twin boundaries at the temperature of 400 °C.

Genesis of Microstructures in Friction Stir Welding of Ti-6Al-4V

NASA Astrophysics Data System (ADS)

Tchein, Gnofam Jacques; Jacquin, Dimitri; Coupard, Dominique; Lacoste, Eric; Girot Mata, Franck

2018-06-01

This paper is focused on the genesis of microstructures in friction stir welding (FSW) of the Ti-6Al-4V alloy. Several titanium joints, initially prepared with four different preheat treatments, were processed by FSW. Detailed microstructural analyses were performed in order to investigate change in the microstructure during the process. In this work, the FSW processing allows a controlled and stable microstructure to be produced in the stirring zone, regardless of the initial heat treatment or the welding conditions. The welded material undergoes a severe thermomechanical treatment which can be divided into two steps. First, the friction in the shoulder and the plastic strain give rise to the necessary conditions to allow a continuous dynamic recrystallization of the β phase. This operation produces a fine and equiaxed β grain structure. Second, once the pin has moved away, the temperature decreases, and the material undergoes a heat treatment equivalent to air quenching. The material thus exhibits a β → β + α transformation with germination of a fine intergranular Widmanstätten phase within the ex-fully-recrystallized- β grains.

Microstructure, texture, and mechanical properties of friction stir welded commercial brass alloy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Heidarzadeh, A., E-mail: ak.hz62@gmail.com

Microstructural evolution during friction stir welding of single-phase brass and corresponding mechanical properties were investigated. For this purpose, 2 mm thick brass plate was friction stir welded at a rotational speed of 450 rpm and traverse speed of 100 mm/min. The microstructure of the joint was studied using optical microscopy, scanning electron microscopy equipped with electron back scattered diffraction system, and scanning transmission electron microscopy. The mechanical properties were measured using hardness and tensile tests. The formation of subgrains and their transformation into new grains in conjunction with existence of A{sub 1}{sup ⁎}, A{sub 2}{sup ⁎} and C texture componentsmore » revealed that the continuous dynamic recrystallization plays a dominant role in the microstructural evolution. However, grain boundary bulging, along with the formation of twin boundaries, and presence of the G texture component showed that the discontinues dynamic recrystallization may participate in the new grain formation. Furthermore, the different strengthening mechanisms, which caused the higher strength of the joint, were discussed. - Highlights: •Microstructural evolution during FSW of a single phase brass was investigated. •CDRX and DDRX were the main mechanisms of the grain structure formation during FSW. •GDRX and SRX were not contributed in grain structure formation. •The lamellas TBs were formed in the SZ of the joints. •Grain boundary, dislocation, and texture effects resulted in higher strength.« less

On a Fast and Accurate In Situ Measuring Strategy for Recrystallization Kinetics and Its Application to an Al-Fe-Si Alloy

NASA Astrophysics Data System (ADS)

Kühbach, Markus; Brüggemann, Thiemo; Molodov, Konstantin D.; Gottstein, Günter

2015-03-01

In the current study, we detail a novel in situ X-ray diffraction-based bulk measurement technique, which allows for the continuous tracking of primary recrystallization kinetics. The approach is based on measuring the diffracted intensity that is correlated with the evolution of the volume fraction of particular texture components during annealing of a sample within a texture goniometer. The method is applied in an experimental study on a cold-rolled industrial Al-Fe-Si alloy. For comparison purposes, the macrotexture and the hardness evolution were monitored ex situ along isothermal and nonisothermal annealing. These measurements were then contrasted to the in situ obtained growth kinetics of recrystallizing grains in beta-fiber deformation and cube orientation. The results showed clearly that this method can be reliably utilized for the characterization of recrystallization kinetics in an industrial context.

A Comparative Study on the Static Recrystallization Behavior of Cold-Rolled Mg-3Al-1Zn Alloy Stimulated by Electropulse Treatment and Conventional Heat Treatment

NASA Astrophysics Data System (ADS)

Li, Xiaopei; Li, Xiaohui; Kure-Chu, Song-Zhu; Tang, Guoyi

2017-12-01

Cold-rolled AZ31 Mg alloy strips, with a reduction of 33 pct, were subjected to electropulse treatment (EPT) and conventional heat treatment (HT) to evaluate the respective influences of electropulses and temperature on the recrystallization behavior of AZ31. The highest measured temperature during the EPT (543 K) was used in HT. The electron backscattered diffraction results demonstrated that the EPT-stimulated recrystallization was completed within 8 seconds, whereas for HT, recrystallization was still far from completion even after 240 seconds. It was found that both the nucleation and grain growth of these two processes were totally different. In the EPT samples, nucleation tended to occur preferentially near extension twin boundaries and grain boundaries by continuous recrystallization, whereas in the HT samples, nucleation occurred mainly by grain boundaries bulging via discontinuous recrystallization. As grain growth proceeded, the texture intensities of the EPT samples decreased gradually and finally evolved into an obvious transverse-direction-split texture. This is likely attributable to the impact of electropulses on the boundary energy and the contribution of nonbasal dislocations; however, the basal-type textures of the HT samples were notably strengthened, which is associated with a 30 deg〈0001〉 orientation with respect to the deformed texture.

A Comparative Study on the Static Recrystallization Behavior of Cold-Rolled Mg-3Al-1Zn Alloy Stimulated by Electropulse Treatment and Conventional Heat Treatment

NASA Astrophysics Data System (ADS)

Li, Xiaopei; Li, Xiaohui; Kure-Chu, Song-Zhu; Tang, Guoyi

2018-02-01

Cold-rolled AZ31 Mg alloy strips, with a reduction of 33 pct, were subjected to electropulse treatment (EPT) and conventional heat treatment (HT) to evaluate the respective influences of electropulses and temperature on the recrystallization behavior of AZ31. The highest measured temperature during the EPT (543 K) was used in HT. The electron backscattered diffraction results demonstrated that the EPT-stimulated recrystallization was completed within 8 seconds, whereas for HT, recrystallization was still far from completion even after 240 seconds. It was found that both the nucleation and grain growth of these two processes were totally different. In the EPT samples, nucleation tended to occur preferentially near extension twin boundaries and grain boundaries by continuous recrystallization, whereas in the HT samples, nucleation occurred mainly by grain boundaries bulging via discontinuous recrystallization. As grain growth proceeded, the texture intensities of the EPT samples decreased gradually and finally evolved into an obvious transverse-direction-split texture. This is likely attributable to the impact of electropulses on the boundary energy and the contribution of nonbasal dislocations; however, the basal-type textures of the HT samples were notably strengthened, which is associated with a 30 deg〈0001〉 orientation with respect to the deformed texture.

Unraveling Recrystallization Mechanisms Governing Texture Development from Rare Earth Element Additions to Magnesium

NASA Astrophysics Data System (ADS)

Imandoust, Aidin

The origin of texture components associated with rare-earth (RE) element additions in wrought magnesium (Mg) alloys is a long-standing problem in magnesium technology. The objective of this research is to identify the mechanisms accountable for rare-earth texture during dynamic recrystallization (DRX). Towards this end, we designed binary Mg-Cerium and Mg-Gadolinium alloys along with complex alloy compositions containing zinc, yttrium and Mischmetal. Binary alloys along with pure Mg were designed to individually investigate their effects on texture evolutions, while complex compositions are designed to develop randomized texture, and be used in automotive and aerospace applications. We selected indirect extrusion to thermo-mechanically process our materials. Different extrusion ratios and speeds were designed to produce partially and fully recrystallized microstructures, allowing us to analyze DRX from its early stages to completion. X-ray diffraction, electron backscattered diffraction (EBSD) and transmission electron microscopy (TEM) were used to conduct microstructure and texture analyses. Our analyses revealed that rare-earth elements in zinc-containing magnesium alloys promote discontinuous dynamic recrystallization at the grain boundaries. During nucleation, the effect of rare earth elements on orientation selection was explained by the concomitant actions of multiple Taylor axes in the same grain. Isotropic grain growth was observed due to rare earth elements segregating to grain boundaries, which lead to texture randomization. The nucleation in binary Mg-RE alloys took place by continuous formation of necklace structures. Stochastic relaxation of basal and non-basal dislocations into low-angle grain boundaries produced chains of embryos with nearly random orientations. Schmid factor analysis showed a lower net activation of dislocations in RE textured grains compared to ones on the other side of the stereographic triangle. Lower dislocation densities within RE grains favored their growth by setting the boundary migration direction toward grains with higher dislocation density, thereby decreasing the system energy. We investigated the influence of RE elements on extension twinning induced hardening. RE addition enhanced tensile twinning induced hardening significantly. EBSD analysis illustrated that tensile twins cross low angle grain boundaries in Mg-RE alloys, which produced large twins and facilitated transmutation of basal to prismatic dislocations. Higher activity of pyramidal II dislocations in Mg-RE alloys resulted in higher twinning induced hardening.

Solid State Research.

DTIC Science & Technology

1982-11-22

48 Fabricated in Zone-Melting-Recrystallized Si Films on Si0 2-Coated Si Substrates V 4. MICROELECTRONICS 55 4.1 Charge-Coupled Devices: Time...OMCVD to the CLEFT (cleavage of lateral epitaxial films for transfer) process, a continuous epitaxial GaAs layer 3 Ym thick has been grown over a...complete-island-etch or local-oxidation-of-Si isolation, that were fabricated in zone-melting-recrystallized Si films on Si02-coated Si substrates. As

Bioinspired Materials for Controlling Ice Nucleation, Growth, and Recrystallization.

PubMed

He, Zhiyuan; Liu, Kai; Wang, Jianjun

2018-05-15

Ice formation, mainly consisting of ice nucleation, ice growth, and ice recrystallization, is ubiquitous and crucial in wide-ranging fields from cryobiology to atmospheric physics. Despite active research for more than a century, the mechanism of ice formation is still far from satisfactory. Meanwhile, nature has unique ways of controlling ice formation and can provide resourceful avenues to unravel the mechanism of ice formation. For instance, antifreeze proteins (AFPs) protect living organisms from freezing damage via controlling ice formation, for example, tuning ice nucleation, shaping ice crystals, and inhibiting ice growth and recrystallization. In addition, AFP mimics can have applications in cryopreservation of cells, tissues, and organs, food storage, and anti-icing materials. Therefore, continuous efforts have been made to understand the mechanism of AFPs and design AFP inspired materials. In this Account, we first review our recent research progress in understanding the mechanism of AFPs in controlling ice formation. A Janus effect of AFPs on ice nucleation was discovered, which was achieved via selectively tethering the ice-binding face (IBF) or the non-ice-binding face (NIBF) of AFPs to solid surfaces and investigating specifically the effect of the other face on ice nucleation. Through molecular dynamics (MD) simulation analysis, we observed ordered hexagonal ice-like water structure atop the IBF and disordered water structure atop the NIBF. Therefore, we conclude that the interfacial water plays a critical role in controlling ice formation. Next, we discuss the design and fabrication of AFP mimics with capabilities in tuning ice nucleation and controlling ice shape and growth, as well as inhibiting ice recrystallization. For example, we tuned ice nucleation via modifying solid surfaces with supercharged unfolded polypeptides (SUPs) and polyelectrolyte brushes (PBs) with different counterions. We found graphene oxide (GO) and oxidized quasi-carbon nitride quantum dots (OQCNs) had profound effects in controlling ice shape and inhibiting ice growth. We also studied the ion-specific effect on ice recrystallization inhibition (IRI) with a large variety of anions and cations. All functionalities are achieved by tuning the properties of interfacial water on these materials, which reinforces the importance of the interfacial water in controlling ice formation. Finally, we review the development of novel application-oriented materials emerging from our enhanced understanding of ice formation, for example, ultralow ice adhesion coatings with aqueous lubricating layer, cryopreservation of cells by inhibiting ice recrystallization, and two-dimensional (2D) and three-dimensional (3D) porous materials with tunable pore sizes through recrystallized ice crystal templates. This Account sheds new light on the molecular mechanism of ice formation and will inspire the design of unprecedented functional materials based on controlled ice formation.

Surface damage and structure evolution of recrystallized tungsten exposed to ELM-like transient loads

NASA Astrophysics Data System (ADS)

Yuan, Y.; Du, J.; Wirtz, M.; Luo, G.-N.; Lu, G.-H.; Liu, W.

2016-03-01

Surface damage and structure evolution of the full tungsten ITER divertor under transient heat loads is a key concern for component lifetime and plasma operations. Recrystallization caused by transients and steady-state heat loads can lead to degradation of the material properties and is therefore one of the most serious issues for tungsten armor. In order to investigate the thermal response of the recrystallized tungsten under edge localized mode-like transient thermal loads, fully recrystallized tungsten samples with different average grain sizes are exposed to cyclic thermal shocks in the electron beam facility JUDITH 1. The results indicate that not only does the microstructure change due to recrystallization, but that the surface residual stress induced by mechanical polishing strongly influences the surface cracking behavior. The stress-free surface prepared by electro-polishing is shown to be more resistant to cracking than the mechanically polished one. The resulting surface roughness depends largely on the loading conditions instead of the recrystallized-grain size. As the base temperature increases from room temperature to 400 °C, surface roughening mainly due to the shear bands in each grain becomes more pronounced, and sub-grains (up to 3 μm) are simultaneously formed in the sub-surface. The directions of the shear bands exhibit strong grain-orientation dependence, and they are generally aligned with the traces of {1 1 2} twin habit planes. The results suggest that twinning deformation and dynamic recrystallization represent the predominant mechanism for surface roughening and related microstructure evolution.

Holographic fabrication of gratings in metal substrates

NASA Technical Reports Server (NTRS)

Fletcher, R. M.; Wagner, D. K.; Ballantyne, J. M.

1982-01-01

A program for investigating the grain enlargement resulting from the laser recrystallization of a thin gallium arsenide film on a patterned substrate, a technique known as graphoepitaxy was evaluated. More specifically, the effects of recrystallizing an uncapped gallium arsenide film using a continuous wave neodymium YAG laser operating at 1.06 microns were studied. In an effort to minimize arsenic loss from the film, the specimens were held in an arsine atmosphere during recrystallization. Two methods for fabricating patterned substrates were developed, one using reactive ion etching of a molybdenum film on both sapphire and silicon substates and another by preferential wet etching of a silicon substrate onto which a film of molybdenum was subsequently deposited.

Effect of Severe Plastic Deformation on Structure and Properties of Al-Sc-Ta and Al-Sc-Ti Alloys

NASA Astrophysics Data System (ADS)

Berezina, Alla; Monastyrska, Tetiana; Davydenko, Olexandr; Molebny, Oleh; Polishchuk, Sergey

2017-03-01

The comparative analysis of the effect of monotonous and non-monotonous severe plastic deformations (SPD) on the structure and properties of aluminum alloys has been carried out. Conventional hydrostatic extrusion (HE) with a constant deformation direction and equal-channel angular hydroextrusion (ECAH) with an abrupt change in the deformation direction were chosen for the cases of monotonous and non-monotonous SPD, respectively. Model cast hypoeutectic Al-0.3%Sc alloys and hypereutectic Al-0.6%Sc alloys with Ta and Ti additives were chosen for studying. It was demonstrated that SPD of the alloys resulted in the segregation of the material into active and inactive zones which formed a banded structure. The active zones were shown to be bands of localized plastic deformation. The distance between zones was found to be independent of the accumulated strain degree and was in the range of 0.6-1 μm. Dynamic recrystallization in the active zones was observed using TEM. The dynamic recrystallization was accompanied by the formation of disclinations, deformation bands, low-angle, and high-angle boundaries, i.e., rotational deformation modes developed. The dynamic recrystallization was more intense during the non-monotonous deformation as compared with the monotonous one, which was confirmed by the reduction of texture degree in the materials after ECAH.

The Prediction of Microstructure Evolution of 6005A Aluminum Alloy in a P-ECAP Extrusion Study

NASA Astrophysics Data System (ADS)

Lei, Shi; Jiu-Ba, Wen; Chang, Ren

2018-05-01

Finite element modeling (FEM) was applied for predicting the recrystallized structure in extruded 6005 aluminum alloy, and simulated results were experimentally validated. First, microstructure evolution of 6005 aluminum alloy during deformation was studied by means of isothermal compression test, where the processing parameters were chosen to reproduce the typical industrial conditions. Second, microstructure evolution was analyzed, and the obtained information was used to fit a dynamic recrystallization model implementing inside the DEFORM-3D FEM code environment. FEM of deformation of 6005 aluminum has been established and validated by microstructure comparison. Finally, the obtained dynamic recrystallization model was applied to tube extrusion by using a portholes-equal channel angular pressing die. The finite element analysis results showed that coarse DRX grains occur in the extruded tube at higher temperature and in the extruded tube at the faster speed of the stem. The test results showed material from the front end of the extruded tube has coarse grains (60 μm) and other extruded tube has finer grains (20 μm).

The Prediction of Microstructure Evolution of 6005A Aluminum Alloy in a P-ECAP Extrusion Study

NASA Astrophysics Data System (ADS)

Lei, Shi; Jiu-Ba, Wen; Chang, Ren

2018-04-01

Finite element modeling (FEM) was applied for predicting the recrystallized structure in extruded 6005 aluminum alloy, and simulated results were experimentally validated. First, microstructure evolution of 6005 aluminum alloy during deformation was studied by means of isothermal compression test, where the processing parameters were chosen to reproduce the typical industrial conditions. Second, microstructure evolution was analyzed, and the obtained information was used to fit a dynamic recrystallization model implementing inside the DEFORM-3D FEM code environment. FEM of deformation of 6005 aluminum has been established and validated by microstructure comparison. Finally, the obtained dynamic recrystallization model was applied to tube extrusion by using a portholes-equal channel angular pressing die. The finite element analysis results showed that coarse DRX grains occur in the extruded tube at higher temperature and in the extruded tube at the faster speed of the stem. The test results showed material from the front end of the extruded tube has coarse grains (60 μm) and other extruded tube has finer grains (20 μm).

Understanding the Effect of Grain Boundary Character on Dynamic Recrystallization in Stainless Steel 316L

NASA Astrophysics Data System (ADS)

Beck, Megan; Morse, Michael; Corolewski, Caleb; Fritchman, Koyuki; Stifter, Chris; Poole, Callum; Hurley, Michael; Frary, Megan

2017-08-01

Dynamic recrystallization (DRX) occurs during high-temperature deformation in metals and alloys with low to medium stacking fault energies. Previous simulations and experimental research have shown the effect of temperature and grain size on DRX behavior, but not the effect of the grain boundary character distribution. To investigate the effects of the distribution of grain boundary types, experimental testing was performed on stainless steel 316L specimens with different initial special boundary fractions (SBF). This work was completed in conjunction with computer simulations that used a modified Monte Carlo method which allowed for the addition of anisotropic grain boundary energies using orientation data from electron backscatter diffraction (EBSD). The correlation of the experimental and simulation work allows for a better understanding of how the input parameters in the simulations correspond to what occurs experimentally. Results from both simulations and experiments showed that a higher fraction of so-called "special" boundaries ( e.g., Σ3 twin boundaries) delayed the onset of recrystallization to larger strains and that it is energetically favorable for nuclei to form on triple junctions without these so-called "special" boundaries.

Continuous recrystallization during thermomechanical processing of a superplastic Al-10Mg-0.1Zr alloy

NASA Technical Reports Server (NTRS)

Hales, S. J.; Mcnelley, T. R.; Crooks, R.

1990-01-01

Microstructural evolution via static continuous recrystallization during thermomechanical processing of an Al-Mg-Zr alloy is addressed. Mechanical property data demonstrated that as-rolled material was capable of superplastic response without further treatment. Further, superplastic ductility at 300 C was enhanced by a factor of five by increasing the reheating time between rolling passes during processing also at 300 C. This enhanced ductility was associated with a Cu-texture and a microstructure consisting of predominantly high-angle boundaries. Processing to minimize recovery resulted in a strong Brass-texture component, a predominantly low-angle boundary microstructure and poorer ductility.

Microstructure evolution and texture development in a friction stir-processed AISI D2 tool steel

NASA Astrophysics Data System (ADS)

Yasavol, N.; Abdollah-zadeh, A.; Vieira, M. T.; Jafarian, H. R.

2014-02-01

Crystallographic texture developments during friction stir processing (FSP) of AISI D2 tool were studied with respect to grain sizes in different tool rotation rates. Comparison of the grain sizes in various rotation rates confirmed that grain refinement occurred progressively in higher rotation rates by severe plastic deformation. It was found that the predominant mechanism during FSP should be dynamic recovery (DRV) happened concurrently with continuous dynamic recrystallization (CDRX) caused by particle-stimulated nucleation (PSN). The developed shear texture relates to the ideal shear textures of D1 and D2 in bcc metals. The prevalence of highly dense arrangement of close-packed planes of bcc and the lowest Taylor factor showed the lowest compressive residual stress which is responsible for better mechanical properties compared with the grain-precipitate refinement.

Characterization of friction stir welded joint of low nickel austenitic stainless steel and modified ferritic stainless steel

NASA Astrophysics Data System (ADS)

Mondal, Mounarik; Das, Hrishikesh; Ahn, Eun Yeong; Hong, Sung Tae; Kim, Moon-Jo; Han, Heung Nam; Pal, Tapan Kumar

2017-09-01

Friction stir welding (FSW) of dissimilar stainless steels, low nickel austenitic stainless steel and 409M ferritic stainless steel, is experimentally investigated. Process responses during FSW and the microstructures of the resultant dissimilar joints are evaluated. Material flow in the stir zone is investigated in detail by elemental mapping. Elemental mapping of the dissimilar joints clearly indicates that the material flow pattern during FSW depends on the process parameter combination. Dynamic recrystallization and recovery are also observed in the dissimilar joints. Among the two different stainless steels selected in the present study, the ferritic stainless steels shows more severe dynamic recrystallization, resulting in a very fine microstructure, probably due to the higher stacking fault energy.

Research on flow stress model and dynamic recrystallization model of X12CrMoWVNbN10-1-1 steel

NASA Astrophysics Data System (ADS)

Sui, Da-shan; Wang, Wei; Fu, Bo; Cui, Zhen-shan

2013-05-01

Plastic deformation behavior of X12CrMoWVNbN10-1-1 ferrite heat-resistant steel was studied systematically at high temperature. The stress-strain curves were measured at the temperature of 950°C-1250°C and strain rate of 0.0005s-1-0.1s-1 by Gleeble thermo-mechanical simulator. The flow stress model and dynamic recrystallization model were established based on Laasraoui two-stage model. The activation energy was calculated and the parameters were determined accordingly based on the experimental results and Sellars creep equation. The verification was performed to prove the models and it indicated the calculated results were identical to the experimental data.

Effect of Extrusion Parameters on Texture and Microstructure Evolution of Extruded Mg-1 pctMn and Mg-1 pctMn-Sr Alloys

NASA Astrophysics Data System (ADS)

Borkar, Hemant; Pekguleryuz, Mihriban

2015-01-01

Three Mg alloys Mg-1 pctMn (M1), Mg-1 pctMn-1.3 pctSr, and Mg-1 pctMn-2.1 pctSr were subjected to two different extrusion temperatures and two different extrusion speeds in lab-scale extrusion. The extrusion temperatures of 573 K and 673 K (300 °C and 400 °C) and two ram speeds of 4 and 8 mm/s were used at constant extrusion ratio of 7. M1 exhibited strong basal texture after extrusion at 673 K (400 °C) at higher speed. At 573 K (300 °C), recrystallization in all alloys takes place completely or partially by continuous dynamic recrystallization mechanism, while particle stimulated nucleation (PSN) occurs in all M1-Sr alloys at both extrusion temperatures and speeds. At 673 K (400 °C), grain boundary bulging is the only recrystallization mechanism in alloy M1, while it occurs in combination with PSN in M1-Sr alloys. The effect of texture weakening by PSN is more significant in M1-Sr alloys extruded at 573 K (400 °C). The plant extrusion trials were carried out on Mg-1 pctMn, Mg-1 pctMn-0.3 pctSr, and Mg-1 pctMn-2.1 pctSr at 623 K (350 °C) with different speeds than in lab-scale extrusion. M1 alloy exhibited strong basal texture at both speeds, while Sr additions of 0.3 and 2.1 pct promoted similar amount of texture weakening.

Automatic twin vessel recrystallizer. Effective purification of acetaminophen by successive automatic recrystallization and absolute determination of purity by DSC.

PubMed

Nara, Osamu

2011-01-24

I describe an interchangeable twin vessel (J, N) automatic glass recrystallizer that eliminates the time-consuming recovery and recycling of crystals for repeated recrystallization. The sample goes in the dissolution vessel J containing a magnetic stir-bar K; J is clamped to the upper joint H of recrystallizer body D. Empty crystallization vessel N is clamped to the lower joint M. Pure solvent is delivered to the dissolution vessel and the crystallization vessel via the head of the condenser A. Crystallization vessel is heated (P). The dissolution reservoir is stirred and heated by the solvent vapor (F). Continuous outflow of filtrate E out of J keeps N at a stable boiling temperature. This results in efficient dissolution, evaporation and separation of pure crystals Q. Pure solvent in the dissolution reservoir is recovered by suction. Empty dissolution and crystallization vessels are detached. Stirrer magnet is transferred to the crystallization vessel and the role of the vessels are then reversed. Evacuating mother liquor out of the upper twin vessel, the apparatus unit is ready for the next automatic recrystallization by refilling twin vessels with pure solvent. We show successive automatic recrystallization of acetaminophen from diethyl ether obtaining acetaminophen of higher melting temperatures than USP and JP reference standards by 8× automatic recrystallization, 96% yield at each stage. Also, I demonstrate a novel approach to the determination of absolute purity by combining the successive automatic recrystallization with differential scanning calorimetry (DSC) measurement requiring no reference standards. This involves the measurement of the criterial melting temperature T(0) corresponding to the 100% pure material and quantitative ΔT in DSC based on the van't Hoff law of melting point depression. The purity of six commercial acetaminophen samples and reference standards and an eight times recrystallized product evaluated were 98.8 mol%, 97.9 mol%, 99.1 mol%, 98.3 mol%, 98.4 mol%, 98.5 mol% and 99.3 mol% respectively. Copyright © 2010 Elsevier B.V. All rights reserved.

Influence of warm rolling temperature on ferrite recrystallization in low C and IF steels

NASA Astrophysics Data System (ADS)

Barnett, Matthew Robert

Experiments involving single pass laboratory rolling and isothermal salt bath annealing were carried out; three steels were studied: a titanium stabilized interstitial free grade and two low carbon grades, one of which contained a particularly low level of manganese (˜0.009wt.%). The two low carbon grades were produced such that any complication from AlN precipitation was avoided. X-ray, neutron diffraction, optical metallography and mechanical testing measurements were carried out on the samples before and after annealing. The main aim of this work was to further the understanding of the metallurgy of recrystallization after ferrite rolling at temperatures between room temperature and 700sp°C. Deformation textures, recrystallization kinetics, final grain sizes and recrystallization textures were quantified for all the samples and experimental conditions. A major conclusion based on these data is that the influence of rolling temperature is far greater in the low carbon samples than in the IF grade. Indeed, the IF results alter only marginally with increasing temperature. In the low carbon grades, however, the rolling texture sharpens, recrystallization slows, the final grain size coarsens, and the recrystallization texture changes when the rolling temperature is increased. This distinct difference between the two steel types is explained in terms of their contrasting deformation behaviors. Solute carbon and nitrogen in the low carbon grades interact with dislocations causing high stored energy levels after low temperature rolling (due to dynamic strain aging) and high strain rate sensitivities during high temperature rolling (due to the solute drag of dislocations in the transition region between DSA and DRC). Nucleation during subsequent recrystallization is strongly influenced by both the stored energy and the strain rate sensitivity. The latter affects the occurrence of the flow localisations that enhance nucleation.

Combination of dynamic transformation and dynamic recrystallization for realizing ultrafine-grained steels with superior mechanical properties

PubMed Central

Zhao, Lijia; Park, Nokeun; Tian, Yanzhong; Shibata, Akinobu; Tsuji, Nobuhiro

2016-01-01

Dynamic recrystallization (DRX) is an important grain refinement mechanism to fabricate steels with high strength and high ductility (toughness). The conventional DRX mechanism has reached the limitation of refining grains to several microns even though employing high-strain deformation. Here we show a DRX phenomenon occurring in the dynamically transformed (DT) ferrite, by which the required strain for the operation of DRX and the formation of ultrafine grains is significantly reduced. The DRX of DT ferrite shows an unconventional temperature dependence, which suggests an optimal condition for grain refinement. We further show that new strategies for ultra grain refinement can be evoked by combining DT and DRX mechanisms, based on which fully ultrafine microstructures having a mean grain size down to 0.35 microns can be obtained without high-strain deformation and exhibit superior mechanical properties. This study will open the door to achieving optimal grain refinement to nanoscale in a variety of steels requiring no high-strain deformation in practical industrial application. PMID:27966603

Pioneering In Situ Recrystallization during Bead Milling: A Top-down Approach to Prepare Zeolite A Nanocrystals.

PubMed

Anand, Chokkalingam; Yamaguchi, Yudai; Liu, Zhendong; Ibe, Sayoko; Elangovan, Shanmugam P; Ishii, Toshihiro; Ishikawa, Tsuyoshi; Endo, Akira; Okubo, Tatsuya; Wakihara, Toru

2016-07-05

Top-down approach has been viewed as an efficient and straightforward method to prepare nanosized zeolites. Yet, the mechanical breaking of zeolite causes amorphization, which usually requires a post-milling recrystallization to obtain fully crystalline nanoparticles. Herein we present a facile methodology to prepare zeolite nanocrystals, where milling and recrystallization can be performed in situ. A milling apparatus specially designed to work under conditions of high alkalinity and temperature enables the in situ recrystallization during milling. Taking zeolite A as an example, we demonstrate its size reduction from ~3 μm to 66 nm in 30 min, which is quite faster than previous methods reported. Three functions, viz., miniaturization, amorphization and recrystallization were found to take effect concurrently during this one-pot process. The dynamic balance between these three functions was achieved by adjusting the milling period and temperature, which lead to the tuning of zeolite A particle size. Particle size and crystallinity of the zeolite A nanocrystals were confirmed by X-ray diffraction, scanning electron microscopy, transmission electron microscopy and water adsorption-desorption. This work presents a pioneering advancement in this field of nanosized zeolites, and will facilitate the mass production as well as boost the wide applications of nanosized zeolites.

Pioneering In Situ Recrystallization during Bead Milling: A Top-down Approach to Prepare Zeolite A Nanocrystals

PubMed Central

Anand, Chokkalingam; Yamaguchi, Yudai; Liu, Zhendong; Ibe, Sayoko; Elangovan, Shanmugam P.; Ishii, Toshihiro; Ishikawa, Tsuyoshi; Endo, Akira; Okubo, Tatsuya; Wakihara, Toru

2016-01-01

Top-down approach has been viewed as an efficient and straightforward method to prepare nanosized zeolites. Yet, the mechanical breaking of zeolite causes amorphization, which usually requires a post-milling recrystallization to obtain fully crystalline nanoparticles. Herein we present a facile methodology to prepare zeolite nanocrystals, where milling and recrystallization can be performed in situ. A milling apparatus specially designed to work under conditions of high alkalinity and temperature enables the in situ recrystallization during milling. Taking zeolite A as an example, we demonstrate its size reduction from ~3 μm to 66 nm in 30 min, which is quite faster than previous methods reported. Three functions, viz., miniaturization, amorphization and recrystallization were found to take effect concurrently during this one-pot process. The dynamic balance between these three functions was achieved by adjusting the milling period and temperature, which lead to the tuning of zeolite A particle size. Particle size and crystallinity of the zeolite A nanocrystals were confirmed by X-ray diffraction, scanning electron microscopy, transmission electron microscopy and water adsorption-desorption. This work presents a pioneering advancement in this field of nanosized zeolites, and will facilitate the mass production as well as boost the wide applications of nanosized zeolites. PMID:27378145

The Deformation Behavior and Microstructure Evolution of a Mn- and Cr-Containing Al-Mg-Si-Cu Alloy During Hot Compression and Subsequent Heat Treatment

NASA Astrophysics Data System (ADS)

Xu, Yi; Nagaumi, Hiromi; Han, Yi; Zhang, Gongwang; Zhai, Tongguang

2017-03-01

Hot compression tests on a newly developed Mn- and Cr-containing Al-Mg-Si-Cu alloy were carried out at temperatures ranging from 623 K (350 °C) to 823 K (550 °C) and strain rates between 0.001 and 1 s-1 after casting and subsequent homogenization heat treatment. The true stress-true strain curves of the alloy exhibited a peak stress at a small plastic strain followed by dynamic flow softening. Using the constitutive equation containing the strain rate, peak stress, and temperature, the activation energy for hot deformation in the alloy was determined to be 249.67 kJ/mol, much higher than that (143.4 kJ/mol) for self-diffusion in pure Al. Scanning transmission electron microscopy experiments revealed that Mn- and Cr-containing α-dispersoids formed during homogenization showed a strong pinning effect on dislocations and grain boundaries, which was responsible for the increase in activation energy for hot deformation in the alloy. A threshold stress was consequently introduced and determined in the constitutive equation to count for the dispersoid hardening effect on hot deformation in the alloy. Electron back-scatter diffraction measurements revealed that the softening occurred in the alloy was mainly due to dynamic recovery taking place at relatively large Z values, and that it was dominated by continuous dynamic recrystallization at relatively low Z. In subsequent annealing after hot deformation at large Z, abnormal grain growth could occur, as a result of the critical strain-annealing effect. After upsetting at higher temperatures, the alloy showed superior tensile properties due to a high non-recrystallized area fraction.

Dynamic recrystallization during deformation of polycrystalline ice: insights from numerical simulations

PubMed Central

Griera, Albert; Steinbach, Florian; Bons, Paul D.; Jansen, Daniela; Roessiger, Jens; Lebensohn, Ricardo A.

2017-01-01

The flow of glaciers and polar ice sheets is controlled by the highly anisotropic rheology of ice crystals that have hexagonal symmetry (ice lh). To improve our knowledge of ice sheet dynamics, it is necessary to understand how dynamic recrystallization (DRX) controls ice microstructures and rheology at different boundary conditions that range from pure shear flattening at the top to simple shear near the base of the sheets. We present a series of two-dimensional numerical simulations that couple ice deformation with DRX of various intensities, paying special attention to the effect of boundary conditions. The simulations show how similar orientations of c-axis maxima with respect to the finite deformation direction develop regardless of the amount of DRX and applied boundary conditions. In pure shear this direction is parallel to the maximum compressional stress, while it rotates towards the shear direction in simple shear. This leads to strain hardening and increased activity of non-basal slip systems in pure shear and to strain softening in simple shear. Therefore, it is expected that ice is effectively weaker in the lower parts of the ice sheets than in the upper parts. Strain-rate localization occurs in all simulations, especially in simple shear cases. Recrystallization suppresses localization, which necessitates the activation of hard, non-basal slip systems. This article is part of the themed issue ‘Microdynamics of ice’. PMID:28025295

Dynamic recrystallization during deformation of polycrystalline ice: insights from numerical simulations.

PubMed

Llorens, Maria-Gema; Griera, Albert; Steinbach, Florian; Bons, Paul D; Gomez-Rivas, Enrique; Jansen, Daniela; Roessiger, Jens; Lebensohn, Ricardo A; Weikusat, Ilka

2017-02-13

The flow of glaciers and polar ice sheets is controlled by the highly anisotropic rheology of ice crystals that have hexagonal symmetry (ice lh). To improve our knowledge of ice sheet dynamics, it is necessary to understand how dynamic recrystallization (DRX) controls ice microstructures and rheology at different boundary conditions that range from pure shear flattening at the top to simple shear near the base of the sheets. We present a series of two-dimensional numerical simulations that couple ice deformation with DRX of various intensities, paying special attention to the effect of boundary conditions. The simulations show how similar orientations of c-axis maxima with respect to the finite deformation direction develop regardless of the amount of DRX and applied boundary conditions. In pure shear this direction is parallel to the maximum compressional stress, while it rotates towards the shear direction in simple shear. This leads to strain hardening and increased activity of non-basal slip systems in pure shear and to strain softening in simple shear. Therefore, it is expected that ice is effectively weaker in the lower parts of the ice sheets than in the upper parts. Strain-rate localization occurs in all simulations, especially in simple shear cases. Recrystallization suppresses localization, which necessitates the activation of hard, non-basal slip systems.This article is part of the themed issue 'Microdynamics of ice'. © 2016 The Author(s).

Effect of Severe Plastic Deformation on Structure and Properties of Al-Sc-Ta and Al-Sc-Ti Alloys.

PubMed

Berezina, Alla; Monastyrska, Tetiana; Davydenko, Olexandr; Molebny, Oleh; Polishchuk, Sergey

2017-12-01

The comparative analysis of the effect of monotonous and non-monotonous severe plastic deformations (SPD) on the structure and properties of aluminum alloys has been carried out. Conventional hydrostatic extrusion (HE) with a constant deformation direction and equal-channel angular hydroextrusion (ECAH) with an abrupt change in the deformation direction were chosen for the cases of monotonous and non-monotonous SPD, respectively. Model cast hypoeutectic Al-0.3%Sc alloys and hypereutectic Al-0.6%Sc alloys with Ta and Ti additives were chosen for studying. It was demonstrated that SPD of the alloys resulted in the segregation of the material into active and inactive zones which formed a banded structure. The active zones were shown to be bands of localized plastic deformation. The distance between zones was found to be independent of the accumulated strain degree and was in the range of 0.6-1 μm. Dynamic recrystallization in the active zones was observed using TEM. The dynamic recrystallization was accompanied by the formation of disclinations, deformation bands, low-angle, and high-angle boundaries, i.e., rotational deformation modes developed. The dynamic recrystallization was more intense during the non-monotonous deformation as compared with the monotonous one, which was confirmed by the reduction of texture degree in the materials after ECAH.

Determination of Dynamic Recrystallization Process by Equivalent Strain

NASA Astrophysics Data System (ADS)

Qin, Xiaomei; Deng, Wei

Based on Tpнoвckiй's displacement field, equivalent strain expression was derived. And according to the dynamic recrystallization (DRX) critical strain, DRX process was determined by equivalent strain. It was found that equivalent strain distribution in deformed specimen is inhomogeneous, and it increases with increasing true strain. Under a certain true strain, equivalent strains at the center, demisemi radius or on tangential plane just below the surface of the specimen are higher than the true strain. Thus, micrographs at those positions can not exactly reflect the true microstructures under the certain true strain. With increasing strain rate, the initial and finish time of DRX decrease. The frozen microstructures of 20Mn23AlV steel with the experimental condition validate the feasibility of predicting DRX process by equivalent strain.

The Cora Lake Shear Zone: Strain Localization in an Ultramylonitic, Deep Crustal Shear Zone, Athabasca Granulite Terrain, Western Churchill Province, Canada

NASA Astrophysics Data System (ADS)

Regan, S.; Williams, M. L.; Mahan, K. H.; Orlandini, O. F.; Jercinovic, M. J.; Leslie, S. R.; Holland, M.

2012-12-01

Ultramylonitic shear zones typically involve intense strain localization, and when developed over large regions can introduce considerable heterogeneity into the crust. The Cora Lake shear zone (CLsz) displays several 10's to 100's of meters-wide zones of ultramylonite distributed throughout its full 3-5 km mylonitized width. Detailed mapping, petrography, thermobarometry, and in-situ monazite geochronology suggest that it formed during the waning phases of granulite grade metamorphism and deformation, within one of North America's largest exposures of polydeformed lower continental crust. Anastomosing zones of ultramylonite contain recrystallized grain-sizes approaching the micron scale and might appear to suggest lower temperature mylonitization. However, feldspar and even clinopyroxene are dynamically recrystallized, and quantitative thermobarometry of syn-deformational assemblages indicate high P and T conditions ranging from 0.9 -10.6 GPa and 775-850 °C. Even at these high T's, dynamic recovery and recrystallization were extremely limited. Rocks with low modal quartz have extremely small equilibrium volumes. This is likely the result of inefficient diffusion, which is further supported by the unannealed nature of the crystals. Local carbonate veins suggests that H2O poor, CO2 rich conditions may have aided in the preservation of fine grain sizes, and may have inhibited dynamic recovery and recrystallization. The Cora Lake shear zone is interpreted to have been relatively strong and to have hardened during progressive deformation. Garnet is commonly fractured perpendicular to host rock fabric, and statically replaced by both biotite and muscovite. Pseudotachylite, with the same sense of shear, occurs in several ultramylonitized mafic granulites. Thus, cataclasis and frictional melt are interpreted to have been produced in the lower continental crust, not during later reactivation. We suggest that strengthening of rheologically stiffer lithologies led to extreme localization, and potentially earthquakes in quartz-absent hardened lithologies. Cora Lake shearing represents the culmination of a deformation trend of increasing strength, strain partitioning, and localization within a polydeformed, strengthened lower continental crust.

Large-scale recrystallization of the S-layer of Bacillus coagulans E38-66 at the air/water interface and on lipid films.

PubMed Central

Pum, D; Weinhandl, M; Hödl, C; Sleytr, U B

1993-01-01

S-layer protein isolated from Bacillus coagulans E38-66 could be recrystallized into large-scale coherent monolayers at an air/water interface and on phospholipid films spread on a Langmuir-Blodgett trough. Because of the asymmetry in the physiochemical surface properties of the S-layer protein, the subunits were associated with their more hydrophobic outer face with the air/water interface and oriented with their negatively charged inner face to the zwitterionic head groups of the dipalmitoylphosphatidylcholine and dipalmitoylphosphatidylethanolamine (DPPE) monolayer films. The dynamic crystal growth at both types of interfaces was first initiated at several distant nucleation points. The individual monocrystalline areas grew isotropically in all directions until the front edge of neighboring crystals was met. The recrystallized S-layer protein and the S-layer-DPPE layer could be chemically cross-linked from the subphase with glutaraldehyde. Images PMID:8478338

Structure and mechanical properties of aging Al-Li-Cu-Zr-Sc-Ag alloy after severe plastic deformation by high-pressure torsion

NASA Astrophysics Data System (ADS)

Kaigorodova, L. I.; Rasposienko, D. Yu.; Pushin, V. G.; Pilyugin, V. P.; Smirnov, S. V.

2015-04-01

The structural and phase transformations have been studied in aging commercial aluminum-lithium alloy Al-1.2 Li-3.2 Cu-0.09 Zr-0.11 Sc-0.4 Ag-0.3 Mg in the as-delivered state and after severe plastic deformation by torsion for 1, 5 and 10 revolutions under a high pressure of 4 GPa. Deformation-induced nanofragmentation and dynamic recrystallization have been found to occur in the alloy. The degree of recrystallization increases with deformation. Nanofragmentation and recrystallization processes are accompanied by the deformation-induced decomposition of solid solution and changes in both the nucleation mechanism of precipitation and the phase composition of the alloy. The influence of a nanostructured nanophase state of the alloy on its mechanical properties (microhardness, plasticity, elastic modulus, and stiffness) is discussed.

Effect of strain and deformation route on grain boundary characteristics and recrystallization behavior of aluminum

NASA Astrophysics Data System (ADS)

Sakai, Tetsuo; Utsunomiya, Hiroshi; Takahashi, Yasuo

2014-08-01

The effect of strain and deformation route on the recrystallization behavior of aluminum sheets has been investigated using well lubricated cold rolling and continuous equal channel angular extrusion. Three different deformation routes in plane strain corresponding to (1) simple shear, (2) compression, and (3) the combination of simple shear and compression were performed on 1100 aluminum sheet. Fixed amounts of the equivalent strain of 1.28 and 1.06 were accumulated in each route. In case of the combined deformation route, the ratio of shear strain to the total equivalent strain was varied. The recrystallized grain size was finer if the combined deformation route was employed instead of the monotonic route under the same amount of equivalent strain at either strain level. The density of high angle grain boundaries that act as nucleation sites for recrystallization was higher in materials deformed by the combined route. The orientation imaging micrographs revealed that the change in deformation route is effective for introducing a larger number of new high angle grain boundaries with relatively low misorientation angle.

Microstructural and fabric characterization of brittle-ductile transitional deformation of middle crustal rocks along the Jinzhou detachment fault zone, Northeast China

NASA Astrophysics Data System (ADS)

Zhang, Juyi; Jiang, Hao; Liu, Junlai

2017-04-01

Detachment fault zones (DFZs) of metamorphic core complexes generally root into the middle crust. Exhumed DFZs therefore generally demonstrate structural, microstructural and fabric features characteristic of middle to upper crustal deformation. The Jinzhou detachment fault zone from the Liaonan metamorphic core complex is characterized by the occurrence of a sequence of fault rocks due to progressive shearing along the fault zone during exhumation of the lower plate. From the exhumed fabric zonation, cataclastic rocks formed in the upper crust occur near the Jinzhou master detachment fault, and toward the lower plate gradually changed to mylonites, mylonitic gneisses and migmatitic gneisses. Correspondingly, these fault rocks have various structural, microstructural and fabric characteristics that were formed by different deformation and recrystallization mechanisms from middle to upper crustal levels. At the meanwhile, various structural styles for strain localization were formed in the DFZ. As strain localization occurs, rapid changes in deformation mechanisms are attributed to increases in strain rates or involvement of fluid phases during the brittle-ductile shearing. Optical microscopic studies reveal that deformed quartz aggregates in the lower part of the detachment fault zone are characterized by generation of dynamically recrystallized grains via SGR and BLG recrystallization. Quartz rocks from the upper part of the DFZ have quartz porphyroclasts in a matrix of very fine recrystallized grains. The porphyroclasts have mantles of sub-grains and margins grain boundary bulges. Electron backscattered diffraction technique (EBSD) quartz c-axis fabric analysis suggests that quartz grain aggregates from different parts of the DFZ possess distinct fabric complexities. The c-axis fabrics of deformed quartz aggregates from mylonitic rocks in the lower part of the detachment fault zone preserve Y-maxima which are ascribed to intermediate temperature deformation (500-630˚ C), whereas complicated fabric patterns (e.g. asymmetric single girdles) are formed in fault rocks from the upper part of the DFZ. The increasing fabric complexity is here interpreted as the result of progressive superposition of fault rocks by shearing either at relatively shallow levels or high rate of strain, during exhumation of the lower plate and shear zone rocks. The above observations and interpretations imply that dislocation creep processes contribute to the dynamic recrystallization of quartz in the middle crustal brittle-ductile transition. Progressive shearing as a consequence of exhumation of the lower plate of the MCC contributed to the obvious structural, microstructural and fabric superpositions. Strain localization occurs as the progressive shearing proceeded. Transition of mechanisms of deformation and dynamic recrystallization during strain localization may be resulted from changes in temperature conditions, in strain rates or addition of minor amount water.

The Rheological Evolution of Brittle-Ductile Transition Rocks During the Earthquake Cycle: Evidence for a Ductile Precursor to Pseudotachylyte in an Extensional Fault System, South Mountains, Arizona

NASA Astrophysics Data System (ADS)

Stewart, Craig A.; Miranda, Elena A.

2017-12-01

We investigate how the rheological evolution of shear zone rocks from beneath the brittle-ductile transition (BDT) is affected by coeval ductile shear and pseudotachylyte development associated with seismicity during the earthquake cycle. We focus our study on footwall rocks of the South Mountains core complex, and we use electron backscatter diffraction (EBSD) analyses to examine how strain is localized in granodiorite mylonites both prior to and during pseudotachylyte development beneath the BDT. In mylonites that are host to pseudotachylytes, deformation is partitioned into quartz, where quartz exhibits crystallographic-preferred orientation patterns and microstructures indicative of dynamic recrystallization during dislocation creep. Grain size reduction during dynamic recrystallization led to the onset of grain boundary sliding (GBS) accommodated by fluid-assisted grain size-sensitive (GSS) creep, localizing strain in quartz-rich layers prior to pseudotachylyte development. The foliation-parallel zones of GBS in the host mylonites, and the presence of GBS traits in polycrystalline quartz survivor clasts indicate that GBS zones were the ductile precursors to in situ pseudotachylyte generation. During pseudotachylyte development, strain was partitioned into the melt phase, and GSS deformation in the survivor clasts continued until crystallization of melt impeded flow, inducing pseudotachylyte development in other GBS zones. We interpret the coeval pseudotachylytes with ductile precursors as evidence of seismic events near the BDT. Grain size piezometry yields high differential stresses in both host mylonites ( 160 MPa) and pseudotachylyte survivor clasts (> 200 MPa), consistent with high stresses during interseismic and coseismic phases of the earthquake cycle, respectively.

Influence of the Starting Microstructure on the Hot Deformation Behavior of a Low Stacking Fault Energy Ni-based Superalloy

NASA Astrophysics Data System (ADS)

McCarley, Joshua; Alabbad, B.; Tin, S.

2018-03-01

The influence of varying fractions of primary gamma prime precipitates on the hot deformation and annealing behavior of an experimental Nickel-based superalloy containing 24 wt pct. Co was investigated. Billets heat treated at 1110 °C or 1135 °C were subjected to hot compression tests at temperatures ranging from 1020 °C to 1060 °C and strain rates ranging from 0.001 to 0.1/s. The microstructures were characterized using electron back scatter diffraction in the as-deformed condition as well as following a super-solvus anneal heat treatment at 1140 °C for 1 hour. This investigation sought to quantify and understand what effect the volume fraction of primary gamma prime precipitates has on the dynamic recrystallization behavior and resulting length fraction ∑3 twin boundaries in the low stacking fault superalloy following annealing. Although deformation at the lower temperatures and higher strain rates led to dynamic recrystallization for both starting microstructures, comparatively lower recrystallized fractions were observed in the 1135 °C billet microstructures deformed at strain rates of 0.1/s and 0.05/s. Subsequent annealing of the 1135 °C billet microstructures led to a higher proportion of annealing twins when compared to the annealed 1110 °C billet microstructures.

In situ electron backscatter diffraction investigation of recrystallization in a copper wire.

PubMed

Brisset, François; Helbert, Anne-Laure; Baudin, Thierry

2013-08-01

The microstructural evolution of a cold drawn copper wire (reduction area of 38%) during primary recrystallization and grain growth was observed in situ by electron backscatter diffraction. Two thermal treatments were performed, and successive scans were acquired on samples undergoing heating from ambient temperature to a steady state of 200°C or 215°C. During a third in situ annealing, the temperature was continuously increased up to 600°C. Nuclei were observed to grow at the expense of the deformed microstructure. This growth was enhanced by the high stored energy difference between the nuclei and their neighbors (driving energy in recrystallization) and by the presence of high-angle grain boundaries of high mobility. In the early stages of growth, the nuclei twin and the newly created orientations continue to grow to the detriment of the strained copper. At high temperatures, the disappearance of some twins was evidenced by the migration of the incoherent twin boundaries. Thermal grooving of grain boundaries is observed at these high temperatures and affects the high mobile boundaries but tends to preserve the twin boundaries of lower energy. Thus, grooving may contribute to the twin vanishing.

Friction stir welded AM50 and AZ31 Mg alloys: Microstructural evolution and improved corrosion resistance

DOE Office of Scientific and Technical Information (OSTI.GOV)

Templeman, Yael

One of the major drawbacks of Mg alloys is poor weldability, caused by porosity formation during conventional fusion welding processes. Friction Stir Welding (FSW) is promising technique in this context since it is a solid state technique. Contradicting results were published in the literature regarding the FSWed Mg alloys joint's properties. Current research was performed in order to investigate the microstructure and corrosion properties of FSWed Mg alloys, studying representatives of two commercial families: wrought AZ31-H24 and die cast AM50. It was found that in both alloys recrystallization occurred during the FSW. In AM50 the mechanism of the recrystallization wasmore » continuous, manifested by dislocation rearrangement into sub grain boundaries. In AZ31 discontinuous recrystallization had occurred through grain boundaries migration - twins rotated with respect to the matrix, turning into low angle grain boundaries. Corrosion resistance has improved during the FSW in both alloys to different extents. In the AM50 alloy, the nugget exhibited significantly higher surface potential than the base metal mainly due to the higher Al concentration in the matrix of the nugget, resulting from the dissolution of Al-enrichment and β-Mg{sub 17}Al{sub 12} phase. In the AZ31 alloy, no change in Al concentration had occurred, and the surface potential measured in the nugget was only slightly higher than in the base metal. These results underline the appropriateness of the FSW for Mg alloys since during the conventional welding deterioration of the corrosion resistance occurs. - Highlights: • Following FSW, AZ31-H24 experienced discontinuous recrystallization. • In AZ31 grain boundaries migration occurred, thus twins rotated. • In die cast AM50 continuous recrystallization occurred during the FSW. • In AM50 - dislocations rearranged into sub grain boundaries. • Corrosion resistance has improved during the FSW in both alloys to different extent.« less

Rapid solidification and dynamic compaction of Ni-base superalloy powders

NASA Technical Reports Server (NTRS)

Field, R. D.; Hales, S. J.; Powers, W. O.; Fraser, H. L.

1984-01-01

A Ni-base superalloy containing 13Al-9Mo-2Ta (in at. percent) has been characterized in both the rapidly solidified condition and after dynamic compaction. Dynamically compacted specimens were examined in the as-compacted condition and observations related to current theories of interparticle bonding. In addition, the recrystallization behavior of the compacted material at relatively low temperature (about 0.5-0.75 Tm) was investigated.

The clumped-isotope geochemistry of exhumed marbles from Naxos, Greece

NASA Astrophysics Data System (ADS)

Ryb, U.; Lloyd, M. K.; Stolper, D. A.; Eiler, J. M.

2017-07-01

Exhumation and accompanying retrograde metamorphism alter the compositions and textures of metamorphic rocks through deformation, mineral-mineral reactions, water-rock reactions, and diffusion-controlled intra- and inter-mineral atomic mobility. Here, we demonstrate that these processes are recorded in the clumped- and single-isotope (δ13 C and δ18 O) compositions of marbles, which can be used to constrain retrograde metamorphic histories. We collected 27 calcite and dolomite marbles along a transect from the rim to the center of the metamorphic core-complex of Naxos (Greece), and analyzed their carbonate single- and clumped-isotope compositions. The majority of Δ47 values of whole-rock samples are consistent with exhumation- controlled cooling of the metamorphic complex. However, the data also reveal that water-rock interaction, deformation driven recrystallization and thermal shock associated with hydrothermal alteration may considerably impact the overall distribution of Δ47 values. We analyzed specific carbonate fabrics influenced by deformation and fluid-rock reaction to study how these processes register in the carbonate clumped-isotope system. Δ47 values of domains drilled from a calcite marble show a bimodal distribution. Low Δ47 values correspond to an apparent temperature of 260 °C and are common in static fabrics; high Δ47 values correspond to an apparent temperature of 200 °C and are common in dynamically recrystallized fabrics. We suggest that the low Δ47 values reflect diffusion-controlled isotopic reordering during cooling, whereas high Δ47 values reflect isotopic reordering driven by dynamic recrystallization. We further studied the mechanism by which dynamic recrystallization may alter Δ47 values by controlled heating experiments. Results show no significant difference between laboratory reactions rates in the static and dynamic fabrics, consistent with a mineral-extrinsic mechanism, in which slip along crystal planes was associated with atomic-scale isotopic reordering in the calcite lattice. An intrinsic mechanism (enhanced isotopic reordering rate in deformed minerals) is contraindicated by these experiments. We suggest that Δ47 values of dynamically recrystallized fabrics that form below the diffusion-controlled blocking-temperature for calcite constrain the temperature of deformation. We find that Δ47-based temperatures of static fabrics from Naxos marbles are ∼60-80 °C higher than commonly observed in slowly cooled metamorphic rocks, and would suggest cooling rates of ∼105 °CMyr-1. A similar thermal history is inferred for dolomite marbles from the core vicinity, which preserve apparent temperatures up to 200 °C higher than a typical blocking temperature (∼300 °C). This finding could be explained by a hydrothermal event driving a brief thermal pulse and locally resetting Δ47 values. Rapid cooling of the core-complex region is consistent with a compilation of published cooling ages and a new apatite U-Th/He age, associating the thermal event with the emplacement of a granodiorite pluton at ∼12 Ma.

Recrystallization inhibition in ice due to ice binding protein activity detected by nuclear magnetic resonance.

PubMed

Brown, Jennifer R; Seymour, Joseph D; Brox, Timothy I; Skidmore, Mark L; Wang, Chen; Christner, Brent C; Luo, Bing-Hao; Codd, Sarah L

2014-09-01

Liquid water present in polycrystalline ice at the interstices between ice crystals results in a network of liquid-filled veins and nodes within a solid ice matrix, making ice a low porosity porous media. Here we used nuclear magnetic resonance (NMR) relaxation and time dependent self-diffusion measurements developed for porous media applications to monitor three dimensional changes to the vein network in ices with and without a bacterial ice binding protein (IBP). Shorter effective diffusion distances were detected as a function of increased irreversible ice binding activity, indicating inhibition of ice recrystallization and persistent small crystal structure. The modification of ice structure by the IBP demonstrates a potential mechanism for the microorganism to enhance survivability in ice. These results highlight the potential of NMR techniques in evaluation of the impact of IBPs on vein network structure and recrystallization processes; information useful for continued development of ice-interacting proteins for biotechnology applications.

Evolution of twinning in extruded AZ31 alloy with bimodal grain structure

DOE Office of Scientific and Technical Information (OSTI.GOV)

Garcés, G., E-mail: ggarces@cenim.csic.es

2017-04-15

Twinning in extruded AZ31 alloy with a bimodal grain structure is studied under compression along the extrusion direction. This study has combined in-situ measurements during the compression tests by Synchrotron Radiation Diffraction and Acoustic Emission techniques and the evaluation of the microstructure and texture in post-mortem compression samples deformed at different strains. The microstructure of the alloy is characterized by the coexistence of large areas of fine dynamic recrystallized grains and coarse non-recrystallized grains elongated along extrusion direction. Twinning occurs initially in large elongated grains before the macroscopic yield stress which is controlled by the twinning in equiaxed dynamically recrystallizedmore » grains. - Highlights: • The AZ31 extruded at low temperature exhibits a bimodal grains structure. • Twinning takes place before macroscopic yielding in coarse non-DRXed grains. • DRXed grains controls the beginning of plasticity in magnesium alloys with bimodal grain structure.« less

Microstructural and rheological evolution of calcite mylonites during shear zone thinning: Constraints from the Mount Irene shear zone, Fiordland, New Zealand

NASA Astrophysics Data System (ADS)

Negrini, Marianne; Smith, Steven A. F.; Scott, James M.; Tarling, Matthew S.

2018-01-01

Layers of calc-mylonite in the Mount Irene shear zone, Fiordland, New Zealand, show substantial variations in thickness due to deflection of the shear zone boundaries around wall rock asperities. In relatively thick parts (c. 2.6 m) of the shear zone, calcite porphyroclasts are internally strained, contain abundant subgrain boundaries and have a strong shape preferred orientation (SPO) and crystallographic preferred orientation (CPO), suggesting that deformation occurred mainly by dislocation creep involving subgrain-rotation recrystallization. In relatively thin parts (c. 1.5 m) of the shear zone, aggregates of fine-grained recrystallized calcite surrounding flattened porphyroclasts have a weak SPO and CPO, and contain polygonal calcite grains with low degrees of internal misorientation. The recrystallized aggregates also contain microstructures (e.g. grain quadruple junctions, randomized misorientation axes) similar to those reported for neighbor-switching processes during grain-boundary sliding. Comparison of subgrain sizes in the porphyroclasts to published grain-size differential-stress relationships indicates that stresses and strain rates were substantially higher in relatively thin parts of the shear zone. The primary microstructural response to higher stresses and strain rates was an increase in the amount of recrystallization to produce aggregates that deformed by grain-boundary sliding. However, even after the development of interconnected networks of recrystallized grains, dislocation creep by subgrain-rotation recrystallization continued to occur within porphyroclasts. This behavior suggests that the bulk rheology of shear zones undergoing thinning and thickening can be controlled by concomitant grain-size insensitive and grain-size sensitive mechanisms. Overall, our observations show that shear zone thickness variations at constant P-T can result in highly variable stresses and strain rates, which in turn modifies microstructure, deformation mechanism and shear zone rheology.

The deformation behavior and microstructure evolution of duplex Mg-9Li-1Al alloy during superplasticity tensile testing

NASA Astrophysics Data System (ADS)

Liu, Meiduo; Zheng, Haipeng; Zhang, Tianlong; Wu, Ruizhi

2017-12-01

The superplastic mechanical properties and microstructure evolution of the duplex Mg-9Li-1Al alloy were investigated. The tensile testing results show that, the elongation of the as-extruded Mg-9Li-1Al alloy reaches 510% at 573 K with a strain rate of 2×10-4 s-1. During the deformation process, the strips of α phase break into equiaxed structure. This phenomenon can be attributed to a particular dynamic recrystallization, which suggests that the β phase can recrystallize in the α phase due to the small misfit degree between α phase and β phase.

Laser recrystallization and inscription of compositional microstructures in crystalline SiGe-core fibres

PubMed Central

Coucheron, David A.; Fokine, Michael; Patil, Nilesh; Breiby, Dag Werner; Buset, Ole Tore; Healy, Noel; Peacock, Anna C.; Hawkins, Thomas; Jones, Max; Ballato, John; Gibson, Ursula J.

2016-01-01

Glass fibres with silicon cores have emerged as a versatile platform for all-optical processing, sensing and microscale optoelectronic devices. Using SiGe in the core extends the accessible wavelength range and potential optical functionality because the bandgap and optical properties can be tuned by changing the composition. However, silicon and germanium segregate unevenly during non-equilibrium solidification, presenting new fabrication challenges, and requiring detailed studies of the alloy crystallization dynamics in the fibre geometry. We report the fabrication of SiGe-core optical fibres, and the use of CO2 laser irradiation to heat the glass cladding and recrystallize the core, improving optical transmission. We observe the ramifications of the classic models of solidification at the microscale, and demonstrate suppression of constitutional undercooling at high solidification velocities. Tailoring the recrystallization conditions allows formation of long single crystals with uniform composition, as well as fabrication of compositional microstructures, such as gratings, within the fibre core. PMID:27775066

Microstructures and mechanical properties of Cu-Sn alloy subjected to elevated-temperature heat deformation

NASA Astrophysics Data System (ADS)

Hui, Jun; Feng, Zaixin; Fan, Wenxin; Wang, Pengfei

2018-04-01

Cu-Sn alloy was subjected to elevated-temperature isothermal compression with 0.01 s‑1 strain rate and 500 ∼ 700 °C temperature range. The thermal compression curve reflected a competing process of work hardening versus dynamic recovery (DRV) and recrystallization, which exhibited an obvious softening trend. Meanwhile, high-temperature deformation and microstructural features in different regions of the alloy was analyzed through EBSD. The results show that grains grow as the temperature rises, competition among recrystallization, substructural, and deformation regions tends to increase with the increase of temperature, and distribution frequency of recrystallization regions gradually increases and then drops suddenly at 650 °C. At 500 ∼ 550 °C, preferentially oriented texturing phenomenon occurs, low angle boundaries(LABs) are gradually transformed into high angle boundaries (HABs) and the Σ (CSL) boundaries turn gradually into Σ3 boundaries. In tensile test of tin bronze, elongation at break increases slowly, whereas yield strength (YS) and ultimate tensile strength (TS) decrease gradually.

Laser recrystallization and inscription of compositional microstructures in crystalline SiGe-core fibres

NASA Astrophysics Data System (ADS)

Coucheron, David A.; Fokine, Michael; Patil, Nilesh; Breiby, Dag Werner; Buset, Ole Tore; Healy, Noel; Peacock, Anna C.; Hawkins, Thomas; Jones, Max; Ballato, John; Gibson, Ursula J.

2016-10-01

Glass fibres with silicon cores have emerged as a versatile platform for all-optical processing, sensing and microscale optoelectronic devices. Using SiGe in the core extends the accessible wavelength range and potential optical functionality because the bandgap and optical properties can be tuned by changing the composition. However, silicon and germanium segregate unevenly during non-equilibrium solidification, presenting new fabrication challenges, and requiring detailed studies of the alloy crystallization dynamics in the fibre geometry. We report the fabrication of SiGe-core optical fibres, and the use of CO2 laser irradiation to heat the glass cladding and recrystallize the core, improving optical transmission. We observe the ramifications of the classic models of solidification at the microscale, and demonstrate suppression of constitutional undercooling at high solidification velocities. Tailoring the recrystallization conditions allows formation of long single crystals with uniform composition, as well as fabrication of compositional microstructures, such as gratings, within the fibre core.

Shock induced crystallization of amorphous Nickel powders

NASA Astrophysics Data System (ADS)

Cherukara, Mathew; Strachan, Alejandro

2015-06-01

Recent experimental work has shown the efficacy of amorphous Ni/crystalline Al composites as energetic materials, with flame velocities twice that of a comparable crystalline Ni/crystalline Al system. Of further interest is the recrystallization mechanisms in the pure amorphous Ni powders, both thermally induced and mechanically induced. We present large-scale molecular dynamics simulations of shock-induced recrystallization in loosely packed amorphous Nickel powders. We study the time dependent nucleation and growth processes by holding the shocked samples at the induced pressures and temperatures for extended periods following the passage of the shock (up to 6 ns). We find that the nanostructure of the recrystallized Ni and time scales of recrystallization are dependent on the piston velocity. At low piston velocities, nucleation events are rare, leading to long incubation times and a relatively coarse nanostructure. At higher piston velocities, local variations in temperature due to jetting phenomena and void collapse, give rise to multiple nucleation events on time scales comparable to the passage of the shock wave, leading to the formation of a fine-grained nanostructure. Interestingly, we observe that the nucleation and growth process occurs in two steps, with the first nuclei crystallizing into the BCC structure, before evolving over time into the expected FCC structure. U.S. Defense Threat Reduction Agency, HDTRA1-10-1-0119 (Program Manager Suhithi Peiris).

An extension of the Saltykov method to quantify 3D grain size distributions in mylonites

NASA Astrophysics Data System (ADS)

Lopez-Sanchez, Marco A.; Llana-Fúnez, Sergio

2016-12-01

The estimation of 3D grain size distributions (GSDs) in mylonites is key to understanding the rheological properties of crystalline aggregates and to constraining dynamic recrystallization models. This paper investigates whether a common stereological method, the Saltykov method, is appropriate for the study of GSDs in mylonites. In addition, we present a new stereological method, named the two-step method, which estimates a lognormal probability density function describing the 3D GSD. Both methods are tested for reproducibility and accuracy using natural and synthetic data sets. The main conclusion is that both methods are accurate and simple enough to be systematically used in recrystallized aggregates with near-equant grains. The Saltykov method is particularly suitable for estimating the volume percentage of particular grain-size fractions with an absolute uncertainty of ±5 in the estimates. The two-step method is suitable for quantifying the shape of the actual 3D GSD in recrystallized rocks using a single value, the multiplicative standard deviation (MSD) parameter, and providing a precision in the estimate typically better than 5%. The novel method provides a MSD value in recrystallized quartz that differs from previous estimates based on apparent 2D GSDs, highlighting the inconvenience of using apparent GSDs for such tasks.

Microstructural evolution of a superaustenitic stainless steel during a two-step deformation process

NASA Astrophysics Data System (ADS)

Bayat, N.; Ebrahimi, G. R.; Momeni, A.; Ezatpour, H. R.

2018-02-01

Single- and two-step hot compression experiments were carried out on 16Cr25Ni6Mo superaustenitic stainless steel in the temperature range from 950 to 1150°C and at a strain rate of 0.1 s-1. In the two-step tests, the first pass was interrupted at a strain of 0.2; after an interpass time of 5, 20, 40, 60, or 80 s, the test was resumed. The progress of dynamic recrystallization at the interruption strain was less than 10%. The static softening in the interpass period increased with increasing deformation temperature and increasing interpass time. The static recrystallization was found to be responsible for fast static softening in the temperature range from 950 to 1050°C. However, the gentle static softening at 1100 and 1150°C was attributed to the combination of static and metadynamic recrystallizations. The correlation between calculated fractional softening and microstructural observations showed that approximately 30% of interpass softening could be attributed to the static recovery. The microstructural observations illustrated the formation of fine recrystallized grains at the grain boundaries at longer interpass time. The Avrami kinetics equation was used to establish a relationship between the fractional softening and the interpass period. The activation energy for static softening was determined as 276 kJ/mol.

Physical stability of the amorphous anticholesterol agent (ezetimibe): the role of molecular mobility.

PubMed

Knapik, J; Wojnarowska, Z; Grzybowska, K; Hawelek, L; Sawicki, W; Wlodarski, K; Markowski, J; Paluch, M

2014-11-03

The purpose of this paper is to examine the role of molecular mobility in the recrystallization process from the amorphous state of the anticholesterol drug ezetimibe. Both the molecular dynamics and crystallization kinetics have been studied using various experimental techniques, such as broadband dielectric spectroscopy (BDS), differential scanning calorimetry (DSC), and X-ray diffraction (XRD). Our investigations have shown that ezetimibe easily recrystallizes from the disordered state, both below and above its glass transition temperature (Tg = 336 K). Moreover, we found that an only slightly elevated pressure (5 MPa) significantly accelerates the recrystallization process at T > Tg. We predict that the structural relaxation time of amorphous ezetimibe at 293 K (storage temperature) and ambient pressure is only 22 days. This result corresponds to the characteristic time, determined from XRD measurements, for amorphous ezetimibe to recrystallize during storage at Troom = 298 K. It leads to the conclusion that the molecular mobility reflected in structural relaxation of ezetimibe is mainly responsible for devitrification of this drug. Finally, we determined a relatively easy way to improve the physical stability of the drug by preparing a binary amorphous ezetimibe-Soluplus mixture. Ezetimibe in an amorphous mixture with 20 wt % Soluplus has a much better (over six times) solubility than the pure crystalline material.

Morphology Controls on Calcite Recrystallization.

PubMed

Heberling, Frank; Paulig, Leonie; Nie, Zhe; Schild, Dieter; Finck, Nicolas

2016-11-01

Environmental scientists and geoscientists working in different fields regard the reactivity of calcite and corresponding changes in its trace elemental- or isotopic composition from diametrically opposed points of view. As one extreme, calcite based environmental remediation strategies rely on the fast recrystallization of calcite and the concurrent uptake and immobilization of pollutants. Paleo-ecological investigations denote the other extreme, and rely on the invariability of calcite composition over geological periods of time. We use long-term radiotracer experiments to quantify recrystallization rates of seven types of calcite powder with diverse morphology and particle size distribution. On the one hand our results demonstrate the long-term metastability of calcite with equilibrated crystal surfaces even at isotopic dis-equilibrium. On the other hand, we document the extremely high reactivity and interfacial free energy of freshly ground, rough calcite. Our results indicate that bulk calcite recrystallization is an interfacial free energy driven Ostwald-ripening process, in which particle roughness effects dominate over the effect of crystal habitus and particle size. We confirm that the dynamic equilibrium exchange of crystal constituents between kink sites involves an activation barrier of about 25 kJ/mol. At room temperature the equilibrium exchange is limited to a near surface region and proceeds at a rate of (3.6 ± 1.4)·10 -13 mol/(m 2 ·s).

Characterizing 3D grain size distributions from 2D sections in mylonites using a modified version of the Saltykov method

NASA Astrophysics Data System (ADS)

Lopez-Sanchez, Marco; Llana-Fúnez, Sergio

2016-04-01

The understanding of creep behaviour in rocks requires knowledge of 3D grain size distributions (GSD) that result from dynamic recrystallization processes during deformation. The methods to estimate directly the 3D grain size distribution -serial sectioning, synchrotron or X-ray-based tomography- are expensive, time-consuming and, in most cases and at best, challenging. This means that in practice grain size distributions are mostly derived from 2D sections. Although there are a number of methods in the literature to derive the actual 3D grain size distributions from 2D sections, the most popular in highly deformed rocks is the so-called Saltykov method. It has though two major drawbacks: the method assumes no interaction between grains, which is not true in the case of recrystallised mylonites; and uses histograms to describe distributions, which limits the quantification of the GSD. The first aim of this contribution is to test whether the interaction between grains in mylonites, i.e. random grain packing, affects significantly the GSDs estimated by the Saltykov method. We test this using the random resampling technique in a large data set (n = 12298). The full data set is built from several parallel thin sections that cut a completely dynamically recrystallized quartz aggregate in a rock sample from a Variscan shear zone in NW Spain. The results proved that the Saltykov method is reliable as long as the number of grains is large (n > 1000). Assuming that a lognormal distribution is an optimal approximation for the GSD in a completely dynamically recrystallized rock, we introduce an additional step to the Saltykov method, which allows estimating a continuous probability distribution function of the 3D grain size population. The additional step takes the midpoints of the classes obtained by the Saltykov method and fits a lognormal distribution with a trust region using a non-linear least squares algorithm. The new protocol is named the two-step method. The conclusion of this work is that both the Saltykov and the two-step methods are accurate and simple enough to be useful in practice in rocks, alloys or ceramics with near-equant grains and expected lognormal distributions. The Saltykov method is particularly suitable to estimate the volumes of particular grain fractions, while the two-step method to quantify the full GSD (mean and standard deviation in log grain size). The two-step method is implemented in a free, open-source and easy-to-handle script (see http://marcoalopez.github.io/GrainSizeTools/).

The microstructure of polar ice. Part II: State of the art

NASA Astrophysics Data System (ADS)

Faria, Sérgio H.; Weikusat, Ilka; Azuma, Nobuhiko

2014-04-01

An important feature of natural ice, in addition to the obvious relevance of glaciers and ice sheets for climate-related issues, is its ability to creep on geological time scales and low deviatoric stresses at temperatures very close to its melting point, without losing its polycrystalline character. This fact, together with its strong mechanical anisotropy and other notable properties, makes natural ice an interesting model material for studying the high-temperature creep and recrystallization of rocks in Earth's interior. After having reviewed the major contributions of deep ice coring to the research on natural ice microstructures in Part I of this work (Faria et al., 2014), here in Part II we present an up-to-date view of the modern understanding of natural ice microstructures and the deformation processes that may produce them. In particular, we analyze a large body of evidence that reveals fundamental flaws in the widely accepted tripartite paradigm of polar ice microstructure (also known as the "three-stage model," cf. Part I). These results prove that grain growth in ice sheets is dynamic, in the sense that it occurs during deformation and is markedly affected by the stored strain energy, as well as by air inclusions and other impurities. The strong plastic anisotropy of the ice lattice gives rise to high internal stresses and concentrated strain heterogeneities in the polycrystal, which demand large amounts of strain accommodation. From the microstructural analyses of ice cores, we conclude that the formation of many and diverse subgrain boundaries and the splitting of grains by rotation recrystallization are the most fundamental mechanisms of dynamic recovery and strain accommodation in polar ice. Additionally, in fine-grained, high-impurity ice layers (e.g. cloudy bands), strain may sometimes be accommodated by diffusional flow (at low temperatures and stresses) or microscopic grain boundary sliding via microshear (in anisotropic ice sheared at high temperatures). Grain boundaries bulged by migration recrystallization and subgrain boundaries are endemic and very frequent at almost all depths in ice sheets. Evidence of nucleation of new grains is also observed at various depths, provided that the local concentration of strain energy is high enough (which is not seldom the case). As a substitute for the tripartite paradigm, we propose a novel dynamic recrystallization diagram in the three-dimensional state space of strain rate, temperature, and mean grain size, which summarizes the various competing recrystallization processes that contribute to the evolution of the polar ice microstructure.

Subgrain Rotation Behavior in Sn3.0Ag0.5Cu-Sn37Pb Solder Joints During Thermal Shock

NASA Astrophysics Data System (ADS)

Han, Jing; Tan, Shihai; Guo, Fu

2018-01-01

Ball grid array (BGA) samples were soldered on a printed circuit board with Sn37Pb solder paste to investigate the recrystallization induced by subgrain rotation during thermal shock. The composition of the solder balls was Sn3.0Ag0.5Cu-Sn37Pb, which comprised mixed solder joints. The BGA component was cross-sectioned before thermal shock. The microstructure and grain orientations were obtained by a scanning electron microscope equipped with an electron back-scattered diffraction system. Two mixed solder joints at corners of the BGA component were selected as the subjects. The results showed that recrystallization occurred at the corner of the solder joints after 200 thermal shock cycles. The recrystallized subgrains had various new grain orientations. The newly generated grain orientations were closely related to the initial grain orientations, which indicated that different subgrain rotation behaviors could occur in one mixed solder joint with the same initial grain orientation. When the misorientation angles were very small, the rotation axes were about Sn [100], [010] and [001], as shown by analyzing the misorientation angles and subgrain rotation axes, while the subgrain rotation behavior with large misorientation angles in the solder joints was much more complicated. As Pb was contained in the solder joints and the stress was concentrated on the corner of the mixed solder joints, concaves and cracks were formed. When the adjacent recrystallized subgrains were separated, and the process of the continuous recrystallization was limited.

Grain size evolution and convection regimes of the terrestrial planets

NASA Astrophysics Data System (ADS)

Rozel, A.; Golabek, G. J.; Boutonnet, E.

2011-12-01

A new model of grain size evolution has recently been proposed in Rozel et al. 2010. This new approach stipulates that the grain size dynamics is governed by two additive and simultaneous processes: grain growth and dynamic recrystallization. We use the usual normal grain growth laws for the growth part. For dynamic recrystallization, reducing the mean grain size increases the total area of grain boundaries. Grain boundaries carry some surface tension, so some energy is required to decrease the mean grain size. We consider that this energy is available during mechanical work. It is usually considered to produce some heat via viscous dissipation. A partitioning parameter f is then required to know what amount of energy is dissipated and what part is converted in surface tension. This study gives a new calibration of the partitioning parameter on major Earth materials involved in the dynamic of the terrestrial planets. Our calibration is in adequation with the published piezometric relations available in the literature (equilibrium grain size versus shear stress). We test this new model of grain size evolution in a set of numerical computations of the dynamics of the Earth using stagYY. We show that the grain size evolution has a major effect on the convection regimes of terrestrial planets.

Deformation induced dynamic recrystallization and precipitation strengthening in an Mg−Zn−Mn alloy processed by high strain rate rolling

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jiang, Jimiao; Song, Min

2016-11-15

The microstructure of a high strain-rate rolled Mg−Zn−Mn alloy was investigated by transmission electron microscopy to understand the relationship between the microstructure and mechanical properties. The results indicate that: (1) a bimodal microstructure consisting of the fine dynamic recrystallized grains and the largely deformed grains was formed; (2) a large number of dynamic precipitates including plate-like MgZn{sub 2} phase, spherical MgZn{sub 2} phase and spherical Mn particles distribute uniformly in the grains; (3) the major facets of many plate-like MgZn{sub 2} precipitates deviated several to tens of degrees (3°–30°) from the matrix basal plane. It has been shown that themore » high strength of the alloy is attributed to the formation of the bimodal microstructure, dynamic precipitation, and the interaction between the dislocations and the dynamic precipitates. - Highlights: •A bimodal microstructure was formed in a high strain-rate rolled Mg−Zn−Mn alloy. •Plate-like MgZn{sub 2}, spherical MgZn{sub 2} and spherical Mn phases were observed. •The major facet of the plate-like MgZn{sub 2} deviated from the matrix basal plane.« less

Hot Deformation Behavior and Intrinsic Workability of Carbon Nanotube-Aluminum Reinforced ZA27 Composites

NASA Astrophysics Data System (ADS)

Liu, Yang; Geng, Cong; Zhu, Yunke; Peng, Jinfeng; Xu, Junrui

2017-04-01

Using a controlled thermal simulator system, hybrid carbon nanotube-aluminum reinforced ZA27 composites were subjected to hot compression testing in the temperature range of 473-523 K with strain rates of 0.01-10 s-1. Based on experimental results, a developed-flow stress model was established using a constitutive equation coupled with strain to describe strain softening arising from dynamic recrystallization. The intrinsic workability was further investigated by constructing three-dimensional (3D) processing maps aided by optical observations of microstructures. The 3D processing maps were constructed based on a dynamic model of materials to delineate variations in the efficiency of power dissipation and flow instability domains. The instability domains exhibited adiabatic shear band and flow localization, which need to be prevented during hot processing. The recommended domain is predicated to be within the temperature range 550-590 K and strain rate range 0.01-0.35 s-1. In this state, the main softening mechanism is dynamic recrystallization. The results from processing maps agree well with the microstructure observations.

Continuous nanoparticle production by microfluidic-based emulsion, mixing and crystallization

DOE Office of Scientific and Technical Information (OSTI.GOV)

Su, Y.-F.; Kim, H.; Kovenklioglu, S.

2007-09-15

BaSO{sub 4} and 2,2'-dipyridylamine (DPA) nanoparticles were synthesized as reactive crystallization and anti-solvent recrystallization examples, respectively, of using the microfluidic-based emulsion and mixing approach as a new avenue of continuously producing inorganic and organic nanoparticles. BaSO{sub 4} nanoparticles in the size range of 15-100 nm were reactively precipitated within the confinement of an aqueous droplet which was coalesced from two separate aqueous droplets containing BaCl{sub 2} and (NH{sub 4}){sub 2}SO{sub 4} using a three T-junction micromixer configuration constructed with commercially available simple tubing and fitting supplies. Also, DPA nanoparticles of about 200 nm were crystallized by combining DPA+ethanol and watermore » droplets using the same micromixer configuration. - Graphical abstract: BaSO{sub 4} and 2,2'-dipyridylamine (DPA) nanoparticles were synthesized as reactive crystallization and anti-solvent recrystallization examples, respectively, of using the microfluidic-based emulsion and mixing approach as a new avenue of continuously producing inorganic and organic nanoparticles.« less

Cyclic Ductile-Brittle Deformation during Temperature Decrease in Quartz-Rich Mylonites: Insights from the Calamita Schists (Elba Island, Italy)

NASA Astrophysics Data System (ADS)

Papeschi, S.; Menegon, L. M.; Musumeci, G.

2017-12-01

The Calamita Schists are a metamorphic complex that experienced transient (< 1 Ma) upper Miocene HT/LP metamorphism related to the emplacement of the Porto Azzurro pluton at P<0.2 GPa. HT/LP metamorphism was coeval with regional scale contractional tectonics leading to the development of meter to decameter ductile east-verging high-strain domains marked by mylonitic fabric overprinted by non-Andersonian brittle faults. In order to investigate the switch in deformation mechanism during temperature decrease at constant pressure (P<0.2 GPa), a sample of mylonitic quartzite with S-C' fabric was examined by Electron Backscatter Diffraction (EBSD), optical microscopy and Scanning Electron Microscope (SEM). Mylonitic fabric is marked by synkinematic biotite + cordierite + andalusite + K-feldspar assemblage, which is progressively replaced by retrograde white mica + chlorite. Quartz microfabric is defined by coarse-grained (100-900 µm) quartz porphyroclasts wrapped by ribbons of dynamically recrystallized finer grains ( 50 µm) showing a strong CPO. This fabric is cross cut by conjugate and synthetic C'-shear bands localized in porphyroclasts and marked by recrystallized fine grains (5-50 µm). EBSD data indicate that prism was the dominant slip system during crystal plastic deformation and dynamic recrystallization in the polycrystalline ribbons. Subsequently, brittle deformation localized along intracrystalline bands (both in conjugate sets and parallel to C' shear bands) within quartz porphyroclasts. The bands evolved in localized cataclastic micro-shear zones and in shear fractures, which localized fluid infiltration and healing by solution precipitation. The quartz new grains filling the bands are preferentially oriented with their c-axis parallel to the shear band boundary. This work highlights that deformation in the Calamita Schists switched over time from high-temperature dynamic recrystallization, accommodated by prism slip to low grade brittle-ductile processes. At the brittle-ductile transition strain partitioning was controlled by grain size and fluid penetration and was characterized by cyclical ductile-brittle mechanisms. In particular brittle failure localized in coarse-grains acted as the precursor for ductile C' shear bands.

Effect of Hot Rolling on the Microstructure and Mechanical Properties of Nitrogen Alloyed Austenitic Stainless Steel

NASA Astrophysics Data System (ADS)

Chenna Krishna, S.; Karthick, N. K.; Jha, Abhay K.; Pant, Bhanu; Cherian, Roy M.

2018-05-01

In the present investigation, the effect of multi-pass hot rolling in the temperature range of 700-1000 °C on the microstructure and mechanical properties of nitrogen alloyed austenitic stainless steel was studied with the aid of optical microscopy, tensile testing and x-ray diffraction measurements. The microstructural changes that occurred in the hot rolled specimens were elongation of grains in rolling direction, nucleation of new grains at the grain boundaries of elongated grains and growth of nucleated grains to form fully recrystallized grains. Elongated grains formed at lower rolling temperature (700-800 °C) due to inadequate strain/temperature for the initiation of dynamic recrystallization. At higher rolling temperature (900-1000 °C), fine grains formed due to dynamic recrystallization. Tensile properties showed strong dependency on the rolling temperature. Tensile strength increased with the decrease in the rolling temperature at the cost of ductility. Maximum strength was observed in samples hot rolled at 700 °C with yield strength of 917 MPa and ductility of 25%. This variation in the tensile properties with the rolling temperature is attributed to changes in the dislocation density and grain structure. The estimated yield strength from the dislocation density, solid solution and grain boundary strengthening closely matched with experimentally determined yield strength confirming the role of dislocation density and grain size in the strengthening.

Effect of Hot Rolling on the Microstructure and Mechanical Properties of Nitrogen Alloyed Austenitic Stainless Steel

NASA Astrophysics Data System (ADS)

Chenna Krishna, S.; Karthick, N. K.; Jha, Abhay K.; Pant, Bhanu; Cherian, Roy M.

2018-04-01

In the present investigation, the effect of multi-pass hot rolling in the temperature range of 700-1000 °C on the microstructure and mechanical properties of nitrogen alloyed austenitic stainless steel was studied with the aid of optical microscopy, tensile testing and x-ray diffraction measurements. The microstructural changes that occurred in the hot rolled specimens were elongation of grains in rolling direction, nucleation of new grains at the grain boundaries of elongated grains and growth of nucleated grains to form fully recrystallized grains. Elongated grains formed at lower rolling temperature (700-800 °C) due to inadequate strain/temperature for the initiation of dynamic recrystallization. At higher rolling temperature (900-1000 °C), fine grains formed due to dynamic recrystallization. Tensile properties showed strong dependency on the rolling temperature. Tensile strength increased with the decrease in the rolling temperature at the cost of ductility. Maximum strength was observed in samples hot rolled at 700 °C with yield strength of 917 MPa and ductility of 25%. This variation in the tensile properties with the rolling temperature is attributed to changes in the dislocation density and grain structure. The estimated yield strength from the dislocation density, solid solution and grain boundary strengthening closely matched with experimentally determined yield strength confirming the role of dislocation density and grain size in the strengthening.

Validation of the Dynamic Recrystallization (DRX) Mechanism for Whisker and Hillock Growth on Sn Thin Films

NASA Astrophysics Data System (ADS)

Vianco, P. T.; Neilsen, M. K.; Rejent, J. A.; Grant, R. P.

2015-10-01

A study was performed to validate a first-principles model for whisker and hillock formation based on the cyclic dynamic recrystallization (DRX) mechanism in conjunction with long-range diffusion. The test specimens were evaporated Sn films on Si having thicknesses of 0.25 μm, 0.50 μm, 1.0 μm, 2.0 μm, and 4.9 μm. Air annealing was performed at 35°C, 60°C, 100°C, 120°C, or 150°C over a time duration of 9 days. The stresses, anelastic strains, and strain rates in the Sn films were predicted by a computational model based upon the constitutive properties of 95.5Sn-3.9Ag-0.6Cu (wt.%) as a surrogate for pure Sn. The cyclic DRX mechanism and, in particular, whether long whiskers or hillocks were formed, was validated by comparing the empirical data against the three hierarchal requirements: (1) DRX to occur at all: ɛc = A D o m Z n , (2) DRX to be cyclic: D o < 2 D r, and (3) Grain boundary pinning (thin films): h versus d. Continuous DRX took place in the 2.0- μm and 4.9- μm films that resulted in short stubby whiskers. Depleted zones, which resulted solely from a tensile stress-driven diffusion mechanism, confirmed the pervasiveness of long-range diffusion so that it did not control whisker or hillock formation other than a small loss of activity by reduced thermal activation at lower temperatures. A first-principles DRX model paves the way to develop like mitigation strategies against long whisker growth.

Detailed Microstructural Characterization and Restoration Mechanisms of Duplex and Superduplex Stainless Steel Friction-Stir-Welded Joints

NASA Astrophysics Data System (ADS)

Santos, T. F. A.; Torres, E. A.; Lippold, J. C.; Ramirez, A. J.

2016-12-01

Duplex stainless steels are successfully used in a wide variety of applications in areas such as the food industry, petrochemical installations, and sea water desalination plants, where high corrosion resistance and high mechanical strength are required. However, during fusion welding operations, there can be changes to the favorable microstructure of these materials that compromise their performance. Friction stir welding with a non-consumable pin enables welded joints to be obtained in the solid state, which avoids typical problems associated with solidification of the molten pool, such as segregation of alloying elements and the formation of solidification and liquefaction cracks. In the case of superduplex stainless steels, use of the technique can avoid unbalanced proportions of ferrite and austenite, formation of deleterious second phases, or growth of ferritic grains in the heat-affected zone. Consolidated joints with full penetration were obtained for 6-mm-thick plates of UNS S32101 and S32205 duplex stainless steels, and S32750 and S32760 superduplex steels. The welding heat cycles employed avoided the conditions required for formation of deleterious phases, except in the case of the welded joint of the S32760 steel, where SEM images indicated the formation of secondary phases, as corroborated by decreased mechanical performance. Analysis using EBSD and transmission electron microscopy revealed continuous dynamic recrystallization by the formation of cellular arrays of dislocations in the ferrite and discontinuous dynamic recrystallization in the austenite. Microtexture evaluation indicated the presence of fibers typical of shear in the thermomechanically affected zone. These fibers were not obviously present in the stir zone, probably due to the intensity of microstructural reformulation to which this region was subjected.

Validation of the dynamic recrystallization (DRX) mechanism for whisker and hillock growth on thin films

DOE PAGES

Vianco, Paul T.; Neilsen, Michael K.; Rejent, Jerome A.; ...

2015-05-01

Our study was performed to validate a first-principles model for whisker and hillock formation based on the cyclic dynamic recrystallization (DRX) mechanism in conjunction with long-range diffusion. The test specimens were evaporated Sn films on Si having thicknesses of 0.25 μm, 0.50 μm, 1.0 μm, 2.0 μm, and 4.9 μm. Air annealing was performed at 35°C, 60°C, 100°C, 120°C, or 150°C over a time duration of 9 days. The stresses, anelastic strains, and strain rates in the Sn films were predicted by a computational model based upon the constitutive properties of 95.5Sn-3.9Ag-0.6Cu (wt.%) as a surrogate for pure Sn. Themore » cyclic DRX mechanism and, in particular, whether long whiskers or hillocks were formed, was validated by comparing the empirical data against the three hierarchal requirements: (1) DRX to occur at all: εc = A D o m Z n , (2) DRX to be cyclic: D o < 2D r, and (3) Grain boundary pinning (thin films): h versus d. Continuous DRX took place in the 2.0-μm and 4.9-μm films that resulted in short stubby whiskers. Depleted zones, which resulted solely from a tensile stress-driven diffusion mechanism, confirmed the pervasiveness of long-range diffusion so that it did not control whisker or hillock formation other than a small loss of activity by reduced thermal activation at lower temperatures. Furthermore, a first-principles DRX model paves the way to develop like mitigation strategies against long whisker growth.« less

Contrasting accessory mineral behavior in minimum-temperature melts: Empirical constraints from the Himalayan metamorphic core

NASA Astrophysics Data System (ADS)

Cottle, John M.; Larson, Kyle P.; Yakymchuk, Chris

2018-07-01

Medium-grained leucogranite in the Tama Kosi region of the Nepalese Himalayan Metamorphic Core yields a relatively narrow range of monazite 208Pb/232Th dates with a dominant population at 21.0 Ma inferred to represent crystallization of an early plutonic phase. In contrast, the pegmatitic portion of the same intrusive complex, that cross-cuts the medium-grained leucogranite, contains zircon, monazite and xenotime that each display near-identical age spectra, recording semi-continuous (re-)crystallization from 27.5 Ma to 21.0 Ma, followed by a 2 m.y. hiatus then further (re-)crystallization between 19.4 and 18.6 Ma. The "gap" in pegmatite dates corresponds well to the crystallization age of the older leucogranite, whereas the end of accessory phase growth in the pegmatite coincides with the onset of regional-scale cooling. Detailed textural, trace element and thermochronologic data indicate that the range of zircon, monazite and xenotime dates recorded in the pegmatite reflect inherited components that underwent semi-continuous (re-)crystallization during metamorphism and/or anatexis in the source region(s), whereas dates younger than the hiatus indicate accessory phase recrystallization, related to both fluid influx and a concomitant increase in temperature. In contrast, the lack of an inherited component(s) in the medium-grained leucogranite phase is inferred to be a result of complete dissolution during partial melting. A model is proposed in which influx of heat and H2O-rich fluids associated with early leucogranite emplacement temporarily delayed zircon and monazite and xenotime crystallization, respectively. These data highlight the importance of measuring spatially resolved dates, trace elements and textural patterns from multiple accessory minerals combined with model constraints to better understand the often-complex crystallization history of anatectic melts in collisional orogens.

Rotation-induced grain growth and stagnation in phase-field crystal models.

PubMed

Bjerre, Mathias; Tarp, Jens M; Angheluta, Luiza; Mathiesen, Joachim

2013-08-01

We consider grain growth and stagnation in polycrystalline microstructures. From the phase-field crystal modeling of the coarsening dynamics, we identify a transition from a grain-growth stagnation upon deep quenching below the melting temperature T(m) to a continuous coarsening at shallower quenching near T(m). The grain evolution is mediated by local grain rotations. In the deep quenching regime, the grain assembly typically reaches a metastable state where the kinetic barrier for recrystallization across boundaries is too large and grain rotation with subsequent coalescence or boundary motion is infeasible. For quenching near T(m), we find that the grain growth depends on the average rate of grain rotation, and follows a power-law behavior with time, with a scaling exponent that depends on the quenching depth.

Barite recrystallization in the presence of 226Ra and 133Ba

NASA Astrophysics Data System (ADS)

Heberling, Frank; Metz, Volker; Böttle, Melanie; Curti, Enzo; Geckeis, Horst

2018-07-01

Despite the long history of studies on (Ba,Ra)SO4, various recent investigations aimed at improving our understanding of its formation processes and thermodynamics. Accumulation of natural Ra isotopes (mainly 226Ra and 228Ra) in (Ba,Ra)SO4 plays an important role in many geotechnical applications and water desalination facilities. In the near field of a nuclear waste repository, barite formation may be expected e.g. as a consequence of contact of spent nuclear fuel or vitrified high level waste with sulfate containing ground water, and may control the potential release of Ra from waste forms upon leakage. Here, we present results of long term batch-type barite recrystallization experiments conducted in the simultaneous presence of 226Ra and 133Ba as a function of initial Ra2+ concentration and pH with the same type and charge of barite powder as used in previous studies (Curti et al., 2010; Klinkenberg et al., 2014; Brandt et al., 2015). Due to the simultaneous measurement of 133Ba and 226Ra our data allow for a direct relation of 226Ra uptake with barite recrystallization, which leads to more accurate partition coefficients compared to previous studies. During a reaction period of five years, barite is continuously recrystallizing. Within the investigated radium concentration range (Ba(1-X)RaXSO4 with X < 0.0006), we measure a partition coefficient of D = 2.1 ± 0.5. The partition coefficient is constant within uncertainty during almost five years (1793 days) of experimental duration. This value is in line with a description of (Ba,Ra)SO4 as an ideal solid solution based on the solubility products (KSP) of the endmembers barite (log10(KSP(barite)) = -9.97) and radium sulfate (log10(KSP(RaSO4)) = -10.26; dimensionless Guggenheim parameter, a0 = 0.0 ± 0.3). Apparent discrepancies to previous theoretical results (a0 = 1.0 ± 0.4) may be resolved when the uncertainties related to the solubility of RaSO4 are considered. Compared to results of previous publications, recrystallization is extremely slow in the experiments presented here. While previous authors suggested complete equilibration of bulk microcrystalline barite within less than three years, a recrystallization of less than 7% of the barite mass is observed within five years. We describe the progress of recrystallization with a new modified homogeneous recrystallization model. Observed recrystallization rates are in the range 0.11-1.5 nmol/(m2 s) and increase with decreasing pH. According to this modified homogeneous recrystallization model, complete bulk barite equilibration is expected in about 1400-16,900 years. The strongly decreased recrystallization kinetics in our experiments is likely related to a strongly prolonged pre-equilibration time (0.8 years), which according to XRD investigations, leads to a higher crystallinity (higher crystal domain size and lower Debye-Waller parameters) of the barite powder.

Hydration index--a better parameter for explaining small molecule hydration in inhibition of ice recrystallization.

PubMed

Tam, Roger Y; Ferreira, Sandra S; Czechura, Pawel; Chaytor, Jennifer L; Ben, Robert N

2008-12-24

Several simple mono- and disaccharides have been assessed for their ability to inhibit ice recrystallization. Two carbohydrates were found to be effective recrystallization inhibitors. D-galactose (1) was the best monosaccharide and D-melibiose (5) was the most active disaccharide. The ability of each carbohydrate to inhibit ice growth was correlated to its respective hydration number reported in the literature. A hydration number reflects the number of tightly bound water molecules to the carbohydrate and is a function of carbohydrate stereochemistry. It was discovered that using the absolute hydration number of a carbohydrate does not allow one to accurately predict its ability to inhibit ice recrystallization. Consequently, we have defined a hydration index in which the hydration number is divided by the molar volume of the carbohydrate. This new parameter not only takes into account the number of water molecules tightly bound to a carbohydrate but also the size or volume of a particular solute and ultimately the concentration of hydrated water molecules. The hydration index of both mono- and disaccharides correlates well with experimentally measured RI activity. C-Linked derivatives of the monosaccharides appear to have RI activity comparable to that of their O-linked saccharides but a more thorough investigation is required. The relationship between carbohydrate concentration and RI activity was shown to be noncolligative and a 0.022 M solution of D-galactose (1) and C-linked galactose derivative (10) inhibited recrystallization as well as a 3% DMSO solution. The carbohydrates examined in this study did not possess any thermal hysteresis activity (selective depression of freezing point relative to melting point) or dynamic ice shaping. As such, we propose that they are inhibiting recrystallization at the interface between bulk water and the quasi liquid layer (a semiordered interface between ice and bulk water) by disrupting the preordering of water.

Properties of Rolled AZ31 Magnesium Alloy Sheet Fabricated by Continuous Variable Cross-Section Direct Extrusion

NASA Astrophysics Data System (ADS)

Liu, Yang; Li, Feng; Li, Xue Wen; Shi, Wen Yong

2018-03-01

Rolling is currently a widely used method for manufacturing and processing high-performance magnesium alloy sheets and has received widespread attention in recent years. Here, we combined continuous variable cross-section direct extrusion (CVCDE) and rolling processes. The microstructure and mechanical properties of the resulting sheets rolled at different temperatures from CVCDE extrudate were investigated by optical microscopy, scanning electron microscope, transmission electron microscopy and electron backscatter diffraction. The results showed that a fine-grained microstructure was present with an average grain size of 3.62 μm in sheets rolled from CVCDE extrudate at 623 K. Dynamic recrystallization and a large strain were induced by the multi-pass rolling, which resulted in grain refinement. In the 573-673 K range, the yield strength, tensile strength and elongation initially increased and then declined as the CVCDE temperature increased. The above results provide an important scientific basis of processing, manufacturing and the active control on microstructure and property for high-performance magnesium alloy sheet.

Analytical modeling of the thermomechanical behavior of ASTM F-1586 high nitrogen austenitic stainless steel used as a biomaterial under multipass deformation.

PubMed

Bernardes, Fabiano R; Rodrigues, Samuel F; Silva, Eden S; Reis, Gedeon S; Silva, Mariana B R; Junior, Alberto M J; Balancin, Oscar

2015-06-01

Precipitation-recrystallization interactions in ASTM F-1586 austenitic stainless steel were studied by means of hot torsion tests with multipass deformation under continuous cooling, simulating an industrial laminating process. Samples were deformed at 0.2 and 0.3 at a strain rate of 1.0s(-1), in a temperature range of 900 to 1200°C and interpass times varying from 5 to 80s. The tests indicate that the stress level depends on deformation temperature and the slope of the equivalent mean stress (EMS) vs. 1/T presents two distinct behaviors, with a transition at around 1100°C, the non-recrystallization temperature (Tnr). Below the Tnr, strain-induced precipitation of Z-phase (NbCrN) occurs in short interpass times (tpass<30s), inhibiting recrystallization and promoting stepwise stress build-up with strong recovery, which is responsible for increasing the Tnr. At interpass times longer than 30s, the coalescence and dissolution of precipitates promote a decrease in the Tnr and favor the formation of recrystallized grains. Based on this evidence, the physical simulation of controlled processing allows for a domain refined grain with better mechanical properties. Copyright © 2015 Elsevier B.V. All rights reserved.

Influence of initial heating during final high temperature annealing on the offset of primary and secondary recrystallization in Cu-bearing grain oriented electrical steels

NASA Astrophysics Data System (ADS)

Rodriguez-Calvillo, P.; Leunis, E.; Van De Putte, T.; Jacobs, S.; Zacek, O.; Saikaly, W.

2018-04-01

The industrial production route of Grain Oriented Electrical Steels (GOES) is complex and fine-tuned for each grade. Its metallurgical process requires in all cases the abnormal grain growth (AGG) of the Goss orientation during the final high temperature annealing (HTA). The exact mechanism of AGG is not yet fully understood, but is controlled by the different inhibition systems, namely MnS, AlN and CuxS, their size and distribution, and the initial primary recrystallized grain size. Therefore, among other parameters, the initial heating stage during the HTA is crucial for the proper development of primary and secondary recrystallized microstructures. Cold rolled 0.3 mm Cu-bearing Grain Oriented Electrical Steel has been submitted to interrupted annealing experiments in a lab tubular furnace. Two different annealing cycles were applied:• Constant heating at 30°C/h up to 1000°C. Two step cycle with initial heating at 100°C/h up to 600°C, followed by 18 h soaking at 600°C and then heating at 30°C/h up to 1050°C. The materials are analyzed in terms of their magnetic properties, grain size, texture and precipitates. The characteristic magnetic properties are analyzed for the different extraction temperatures and Cycles. As the annealing was progressing, the coercivity values (Hc 1.7T [A/m]) decreased, showing two abrupt drops, which can be associated to the on-set of primary and secondary recrystallization. The primary recrystallized grain sizes and recrystallized fractions are fitted to a model using a non-isothermal approach. This analysis shows that, although the resulting grain sizes were similar, the kinetics for the two step annealing were faster due to the lower recovery. The on-set of secondary recrystallization was also shifted to higher temperatures in the case of the continuous heating cycle, which might end in different final grain sizes and final magnetic properties. In both samples, nearly all the observed precipitates are Al-Si-Mn nitrides, ranging from pure AlN to Si4Mn-nitride.

Compositional changes of minerals associated with dynamic recrystallizatin

NASA Astrophysics Data System (ADS)

Yund, Richard A.; Tullis, Jan

1991-09-01

The rate of compositional and isotopic exchange between minerals may be enhanced significantly if the rock is deformed simultaneously. The enhanced exchange rate may result from a reduction in grain size (shorter distance for volume diffusion), dissolution and growth of grains by diffusion creep (pressure solution), or the movement of high-angle grain boundaries through strained grains during recrystallization in the dislocation creep regime. The migration of high-angle grain boundaries provides high diffusivity paths for the rapid exchange of components during recrystallization. The operation of the latter process has been demonstrated by deforming aggregates consisting of two plagioclases (An1 and An79) at 900°C, 1 GPa confining pressure, and a strain rate of ˜2x10-6s-1. The polygonal, recrystallized grains were analyzed using an analytical transmission electron microscope and have a variable but often intermediate composition. At the conditions of these experiments, the volume interdiffusion rate of NaSi/CaAl is too slow to produce any observable chemical change, and microstructural-chemical relations indicate that the contribution from diffusion creep was insignificant except for initially fine-grained (2 10 μm) aggregates. These results indicate that strain-induced recrystallization can be an effective mechanism for enhancing the kinetics of metamorphic reactions and for resetting the isotope systematics of minerals such as feldspars, pyroxenes, and amphiboles.

Molecular Factors Governing the Liquid and Glassy States Recrystallization of Celecoxib in Binary Mixtures with Excipients of Different Molecular Weights.

PubMed

Grzybowska, K; Chmiel, K; Knapik-Kowalczuk, J; Grzybowski, A; Jurkiewicz, K; Paluch, M

2017-04-03

Transformation of poorly water-soluble crystalline pharmaceuticals to the amorphous form is one of the most promising strategies to improve their oral bioavailability. Unfortunately, the amorphous drugs are usually thermodynamically unstable and may quickly return to their crystalline form. A very promising way to enhance the physical stability of amorphous drugs is to prepare amorphous compositions of APIs with certain excipients which can be characterized by significantly different molecular weights, such as polymers, acetate saccharides, and other APIs. By using different experimental techniques (broadband dielectric spectroscopy, differential scanning calorimetry, X-ray diffraction) we compare the effect of adding the large molecular weight polymer-polyvinylpyrrolidone (PVP K30)-and the small molecular weight excipient-octaacetylmaltose (acMAL)-on molecular dynamics as well as the tendency to recrystallization of the amorphous celecoxib (CEL) in the amorphous solid dispersions: CEL-PVP and CEL-acMAL. The physical stability investigations of the binary systems were performed in both the supercooled liquid and glassy states. We found that acMAL is a better inhibitor of recrystallization of amorphous CEL than PVP K30 deep in the glassy state (T < T g ). In contrast, PVP K30 is a better crystallization inhibitor of CEL than acMAL in the supercooled liquid state (at T > T g ). We discuss molecular factors governing the recrystallization of amorphous CEL in examined solid dispersions.

Influence of Copper on the Hot Ductility of 20CrMnTi Steel

NASA Astrophysics Data System (ADS)

Peng, Hong-bing; Chen, Wei-qing; Chen, Lie; Guo, Dong

2015-02-01

The hot ductility of 20CrMnTi steel with x% copper (x = 0, 0.34) was investigated. Results show that copper can reduce its hot ductility, but there is no significant copper-segregation at the boundary tested by EPMA. The average copper content at grain boundaries and substrate is 0.352% and 0.318% respectively in steel containing 0.34% copper tensile-tested at 950 °C. The fracture morphology was examined with SEM and many small and shallow dimples were found on the fracture of steel with copper, and fine copper sulfide was found from carbon extraction replicas using TEM. Additionally, adding 0.34% copper caused an increase in the dynamic recrystallization temperature from 950 °C to 1000 °C, which indicates that copper can retard the dynamic recrystallization (DRX) of austenite. The detrimental influence of copper on hot ductility of 20CrMnTi steel is due mainly to the fine copper sulfide in the steel and its retarding the DRX.

Dynamic Recrystallization Behavior of AISI 422 Stainless Steel During Hot Deformation Processes

NASA Astrophysics Data System (ADS)

Ahmadabadi, R. Mohammadi; Naderi, M.; Mohandesi, J. Aghazadeh; Cabrera, Jose Maria

2018-02-01

In this work, hot compression tests were performed to investigate the dynamic recrystallization (DRX) process of a martensitic stainless steel (AISI 422) at temperatures of 950, 1000, 1050, 1100 and 1150 °C and strain rates of 0.01, 0.1 and 1 s-1. The dependency of strain-hardening rate on flow stress was used to estimate the critical stress for the onset of DRX. Accordingly, the critical stress to peak stress ratio was calculated as 0.84. Moreover, the effect of true strain was examined by fitting stress values to an Arrhenius type constitutive equation, and then considering material constants as a function of strain by using a third-order polynomial equation. Finally, two constitutive models were used to investigate the competency of the strain-dependent constitutive equations to predict the flow stress curves of the studied steel. It was concluded that one model offers better precision on the flow stress values after the peak stress, while the other model gives more accurate results before the peak stress.

Effect of Strain Rate on Hot Ductility Behavior of a High Nitrogen Cr-Mn Austenitic Steel

NASA Astrophysics Data System (ADS)

Wang, Zhenhua; Meng, Qing; Qu, Minggui; Zhou, Zean; Wang, Bo; Fu, Wantang

2016-03-01

18Mn18Cr0.6N steel specimens were tensile tested between 1173 K and 1473 K (900 °C and 1200 °C) at 9 strain rates ranging from 0.001 to 10 s-1. The tensile strained microstructures were analyzed through electron backscatter diffraction analysis. The strain rate was found to affect hot ductility by influencing the strain distribution, the extent of dynamic recrystallization and the resulting grain size, and dynamic recovery. The crack nucleation sites were primarily located at grain boundaries and were not influenced by the strain rate. At 1473 K (1200 °C), a higher strain rate was beneficial for grain refinement and preventing hot cracking; however, dynamic recovery appreciably occurred at 0.001 s-1 and induced transgranular crack propagation. At 1373 K (1100 °C), a high extent of dynamic recrystallization and fine new grains at medium strain rates led to good hot ductility. The strain gradient from the interior of the grain to the grain boundary increased with decreasing strain rate at 1173 K and 1273 K (900 °C and 1000 °C), which promoted hot cracking. Grain boundary sliding accompanied grain rotation and did not contribute to hot cracking.

Microstructure and Mechanical Properties of Laser Solid Formed Ti-6Al-4V Alloy Under Dynamic Shear Loading

NASA Astrophysics Data System (ADS)

Zhou, Ping; Guo, Wei-Guo; Su, Yu; Wang, Jianjun; Lin, Xin; Huang, Weidong

2017-07-01

To investigate the mechanical properties of the Ti-6Al-4V alloy fabricated by laser solid forming technology, both static and dynamic shear tests were conducted on hat-shaped specimens by a servohydraulic testing machine and an enhanced split Hopkinson pressure bar system, over a temperature range of 173-573 K. The microstructure of both the original and deformed specimens was characterized by optical microscopy and scanning electron microscopy. The results show that: (1) the anisotropy of shear properties is not significant regardless of the visible stratification and the prior- β grains that grow epitaxially along the depositing direction; (2) the ultimate shear strength of this material is lower than that of those Ti-6Al-4V alloys fabricated by forging and extrusion; (3) the adiabatic shear bands of approximately 25.6-36.4 μm in width can develop at all selected temperatures during the dynamic shear deformation; and (4) the observed microstructure and measured microhardness indicate that the grains become refined in adiabatic shear band. Estimation of the temperature rise shows that the temperature in shear band exceeds the recrystallization temperature. The process of rotational dynamic recrystallization is considered to be the cause of the grain refinement in shear band.

Evaluating flow laws for dynamically recrystallized quartz based on field data

NASA Astrophysics Data System (ADS)

Peters, Max; Herwegh, Marco

2013-04-01

The extrapolation of experimentally controlled deformation conditions, and the resulting relations between physical parameters acting during ductile deformation, to nature is considered controversial (see Herwegh et al., 2005 and references therein). Whereas the relationship between flow stress and recrystallized grain size can be empirically derived from lab experiments using paleopiezometers (e.g. Stipp & Tullis, 2003), the relation between recrystallized grain size, strain rate, differential stress, temperature and activation energy for dislocation creep requires further constraints. For these relations, various power law flow laws for dynamically recrystallized quartz were proposed over the past years (Paterson & Luan, 1990; Luan & Paterson, 1992; Gleason & Tullis, 1995; Hirth et al., 2001, Rutter & Brodie, 2004). The variations in the flow laws are mainly characterized by different starting materials, experimental conditions, the activation energy for dislocation creep and the stress exponent n. In this study we compare and evaluate experimentally derived flow laws regarding their reliability for the prediction of rheology of background deformation of naturally deformed crystalline samples from mylonites of the Aar massif (Swiss Central Alps). The majority of samples comprises highly deformed rocks (e.g. Central Aare granite), which exhibit severe grain size reduction. This reduction dominantly occurred by subgrain rotation (SGR), in the case of low temperature overprint by bulging recrystallization (BLG). Towards elevated temperatures, grain boundary migration (GBM) and SGR recrystallization were active. Along the metamorphic gradient (300 - 475°C) quartz microstructures and associated recrystallized grain size distributions indicate steady state mean grain sizes. The quantification of the metamorphic gradient (temperature, pressure, water fugacity) over the sampling area allowed the application of flow laws, yielding variations of 6 orders of magnitude in deformation rates between different calibrations for one corresponding grain size. The calibrations of Paterson & Luan (1990) and Hirth et al. (2001) yield most reliable results for peak metamorphic conditions, which are in line with the geological framework. Strain rates range between 10E-13 and 10E-10 s-1 (Paterson & Luan, 1990) with corresponding flow stresses between ca. 200 MPa (BLG) to ca. 20 MPa (SGR and transition SGR-GBM). Nevertheless, the applicability of single flow laws shall be discussed in greater detail. REFERENCES Herwegh, M., de Bresser, J.H.P. and ter Heege, J.H. 2005: Combining natural microstructures with composite flow laws: an improved approach for the extrapolation of lab data to nature. Journal of Structural Geology, 27. Hirth, G., Teyssier, C. and Dunlap, W.J. 2011: An evaluation of quartzite flow laws based on comparisons between experimentally and naturally deformed rocks. International Journal of Earth Sciences, 90. Luan, F.C. and Paterson, S.R. 1992: Perparation and deformation of synthetic aggregates of quartz. Journal of Geophysical Research, 97. Paterson, S.R. and Luan, F.C. 1990: Quartzite rheology under geological conditions. In: de Meer, S., Drury, M.R., de Bresser, J.H.P., Pennock, G.M Deformation mechanisms, rheology and tectonics: from minerals to the lithosphere. Geological Society of Lonodn Special Publications, 54. Rutter, E.H. and Brodie, K.H. 2004: Experimental grain size-sensitive flow of hot-pressed Brazilian quartz aggregates. Journal of Structural Geology, 26. Stipp, M. and Tullis, J. 2003: The recrystallized grain size piezometer for quartz. Geophysical Research Letters, 30.

Microstructure effects on the recrystallization of low-symmetry alpha-uranium

DOE Office of Scientific and Technical Information (OSTI.GOV)

McCabe, Rodney James; Richards, Andrew Walter; Coughlin, Daniel Robert

2015-10-01

We employ electron backscatter diffraction (EBSD) to investigate microstructural evolution of uranium during recrystallization. To understand the relationship between microstructure and recrystallization, we use measures of intra-granular misorientation within grains and near grain boundaries in both deformed (non-recrystallized) uranium and recrystallizing uranium. The data show that the level of intra-granular misorientation depends on crystallographic orientation. However, contrary to expectation, this relationship does not significantly affect the recrystallization texture. Rather, the analysis suggests that recrystallization nucleation occurs along high angle grain boundaries in the deformed microstructure. Specifically, we show that the nucleation of recrystallized grains correlates well with the spatially heterogeneousmore » distribution of high angle boundaries. Due to the inhomogeneous distribution of high angle boundaries, the recrystallized microstructure after long times exhibits clustered distributions of small and large grains. Twin boundaries do not appear to act as recrystallization nucleation sites.« less

A Rate-Theory-Phase-Field Model of Irradiation-Induced Recrystallization in UMo Nuclear Fuels

NASA Astrophysics Data System (ADS)

Hu, Shenyang; Joshi, Vineet; Lavender, Curt A.

2017-12-01

In this work, we developed a recrystallization model to study the effect of microstructures and radiation conditions on recrystallization kinetics in UMo fuels. The model integrates the rate theory of intragranular gas bubble and interstitial loop evolutions and a phase-field model of recrystallization zone evolution. A first passage method is employed to describe one-dimensional diffusion of interstitials with a diffusivity value several orders of magnitude larger than that of fission gas xenons. With the model, the effect of grain sizes on recrystallization kinetics is simulated. The results show that (1) recrystallization in large grains starts earlier than that in small grains, (2) the recrystallization kinetics (recrystallization volume fraction) decrease as the grain size increases, (3) the predicted recrystallization kinetics are consistent with the experimental results, and (4) the recrystallization kinetics can be described by the modified Avrami equation, but the parameters of the Avrami equation strongly depend on the grain size.

Development of a Model for Dynamic Recrystallization Consistent with the Second Derivative Criterion.

PubMed

Imran, Muhammad; Kühbach, Markus; Roters, Franz; Bambach, Markus

2017-11-02

Dynamic recrystallization (DRX) processes are widely used in industrial hot working operations, not only to keep the forming forces low but also to control the microstructure and final properties of the workpiece. According to the second derivative criterion (SDC) by Poliak and Jonas, the onset of DRX can be detected from an inflection point in the strain-hardening rate as a function of flow stress. Various models are available that can predict the evolution of flow stress from incipient plastic flow up to steady-state deformation in the presence of DRX. Some of these models have been implemented into finite element codes and are widely used for the design of metal forming processes, but their consistency with the SDC has not been investigated. This work identifies three sources of inconsistencies that models for DRX may exhibit. For a consistent modeling of the DRX kinetics, a new strain-hardening model for the hardening stages III to IV is proposed and combined with consistent recrystallization kinetics. The model is devised in the Kocks-Mecking space based on characteristic transition in the strain-hardening rate. A linear variation of the transition and inflection points is observed for alloy 800H at all tested temperatures and strain rates. The comparison of experimental and model results shows that the model is able to follow the course of the strain-hardening rate very precisely, such that highly accurate flow stress predictions are obtained.

Development of a Model for Dynamic Recrystallization Consistent with the Second Derivative Criterion

PubMed Central

Imran, Muhammad; Kühbach, Markus; Roters, Franz; Bambach, Markus

2017-01-01

Dynamic recrystallization (DRX) processes are widely used in industrial hot working operations, not only to keep the forming forces low but also to control the microstructure and final properties of the workpiece. According to the second derivative criterion (SDC) by Poliak and Jonas, the onset of DRX can be detected from an inflection point in the strain-hardening rate as a function of flow stress. Various models are available that can predict the evolution of flow stress from incipient plastic flow up to steady-state deformation in the presence of DRX. Some of these models have been implemented into finite element codes and are widely used for the design of metal forming processes, but their consistency with the SDC has not been investigated. This work identifies three sources of inconsistencies that models for DRX may exhibit. For a consistent modeling of the DRX kinetics, a new strain-hardening model for the hardening stages III to IV is proposed and combined with consistent recrystallization kinetics. The model is devised in the Kocks-Mecking space based on characteristic transition in the strain-hardening rate. A linear variation of the transition and inflection points is observed for alloy 800H at all tested temperatures and strain rates. The comparison of experimental and model results shows that the model is able to follow the course of the strain-hardening rate very precisely, such that highly accurate flow stress predictions are obtained. PMID:29099068

Hot deformation characteristics of as-cast high-Cr ultra-super-critical rotor steel with columnar grains

NASA Astrophysics Data System (ADS)

Ding, Zong-ye; Hu, Qiao-dan; Zeng, Long; Li, Jian-guo

2016-11-01

Isothermal hot compression tests of as-cast high-Cr ultra-super-critical (USC) rotor steel with columnar grains perpendicular to the compression direction were carried out in the temperature range from 950 to 1250°C at strain rates ranging from 0.001 to 1 s-1. The softening mechanism was dynamic recovery (DRV) at 950°C and the strain rate of 1 s-1, whereas it was dynamic recrystallization (DRX) under the other conditions. A modified constitutive equation based on the Arrhenius model with strain compensation reasonably predicted the flow stress under various deformation conditions, and the activation energy was calculated to be 643.92 kJ•mol-1. The critical stresses of dynamic recrystallization under different conditions were determined from the work-hardening rate ( θ)-flow stress ( σ) and -∂ θ/∂ σ-σ curves. The optimum processing parameters via analysis of the processing map and the softening mechanism were determined to be a deformation temperature range from 1100 to 1200°C and a strain-rate range from 0.001 to 0.08 s-1, with a power dissipation efficiency η greater than 31%.

The Work Softening Behavior of Pure Mg Wire during Cold Drawing.

PubMed

Sun, Liuxia; Bai, Jing; Xue, Feng; Chu, Chenglin; Meng, Jiao

2018-04-13

We performed multiple-pass cold drawing for pure Mg wire which showed excellent formability (~138% accumulative true strain) at room temperature. Different from the continuous work hardening occurring during cold drawing of Mg alloy wires, for pure Mg, an initially rapid increase in hardness and strength was followed by significant work softening and finally reached a steady-state level, approximately 40~45 HV. The work softening can be attributed to the dynamic recovery and recrystallization of pure Mg at room temperature. Meanwhile, an abrupt change in texture component also was detected with the transition from work hardening to softening in the strain range of 28~34%. During the whole drawing, the strongest texture component gradually transformed from as-extruded basal to <10 1 ¯ 0> fiber (~28% accumulative true strain), and then rapidly returned to the weak basal texture.

The effect of hydrocarbons on the microstructural evolution in rock salt: a case study on hydrocarbon bearing Ara salt from the South Oman Salt Basin

NASA Astrophysics Data System (ADS)

Schmatz, Joyce; Urai, Janos L.; Wübbeler, Franziska M. M.; Sadler, Marc

2014-05-01

It has been shown that dilatant deformation promotes the incorporation of hydrocarbons into typically low permeable rock salt (Schoenherr et al., 2007). However, there is not much knowledge on subsequent mechanisms related to recrystallization processes, which cause morphological and chemical changes of the carbonic inclusions. This work aims to contribute to an increased understanding of fluid inclusion dynamics related to grain boundary migration recrystallization and hence to facilitate the interpretation of complex microstructures in recrystallized, multiphase salt rocks. In this case study we investigate hydrocarbon-impregnated salt from the Cambrian Ara Group in the South Oman Salt Basin. The samples were cored from cm-m thick anhydrite-salt sequences overlying hydrocarbon bearing carbonate stringers in 3300 m depth. The anhydrite layers consist mainly of fine-grained anhydrite, which contains calcite, dolomite, and olivine inclusions. Solid bitumen and lighter hydrocarbon phases are observed in between the anhydrite grains and along cracks. Anhydrite layers host salt veins, which contain fragments of anhydrite. These fragments do not differ in composition or structure from the host material and the related vein microstructures indicate crack-seal mechanisms. Halite in the salt layers is almost entirely recrystallized with solid inclusions consisting of anhydrite, calcite, dolomite and olivine with hydrocarbon-coatings present inside grains and along grain boundaries. Solid inclusions cause pinning indicated by a decreased recrystallized grain size and by the presence of grains with preserved substructures representing earlier deformation phases. We observe two types of carbonic inclusions: I) solid bitumen coatings along grain boundaries and microcracks, interpreted to be incorporated into the salt in an overpressure state that allowed dilatancy of the salt, and II) less degraded, liquid hydrocarbons along grain boundaries in the vicinity of the anhydrite, interpreted to be incorporated into the salt in a subsequent deformation phase. Type II inclusions usually form arrays of isolated inclusions (liquid hydrocarbons, vapor, and aqueous phases in minor proportions) along grain boundaries of the recrystallized grains, presumably formed in a surface-energy controlled shrinking process from thin fluid films. Here, the contact with mobile grain boundaries promoted necking down and decomposition of multiphase inclusions. We present a model, which describes the dynamic behavior of liquid hydrocarbons in mobile grain boundaries after their enclosure into the salt layers. The model is based on numerous microanalytical methods, such as optical microscopy, fluorescence microscopy, cryo-SEM, and EDX. Schoenherr, J., et al. (2007), Limits to the sealing capacity of rock salt: A case study of the infra-Cambrian Ara Salt from the South Oman salt basin, AAPG Bulletin, 91(11), 1541-1557

High-Temperature Deformation Behavior of HCP Alloys -- An Internal Variable Approach

DTIC Science & Technology

2006-05-31

successfully to characterize the high temperature deformation behavior of various metallic materials such as Al alloys, Pb-Sn hyper- eutectic alloy, and...implying dynamic recrystallization (DRX) and GBS as the major deformation mechanisms at 523 K and 10-4 /s. Large cavities are observed at the

Fundamental Investigation of the Microstructural Parameters to Improve Dynamic Response in Al-Cu Model System

DTIC Science & Technology

2014-05-01

grain size. Recrystallization was then induced via annealing just above the solvus temperature. After quenching , the bars were immediately placed into...that the values were statistically significant. Precipitate sizes ranged from approximately 100 nanometers in diameter up to 2-5 microns in diameter

Susceptibility of Goethite to Fe2+-Catalyzed Recrystallization over Time.

PubMed

Joshi, Prachi; Fantle, Matthew S; Larese-Casanova, Philip; Gorski, Christopher A

2017-10-17

Recent work has shown that iron oxides, such as goethite and hematite, may recrystallize in the presence of aqueous Fe 2+ under anoxic conditions. This process, referred to as Fe 2+ -catalyzed recrystallization, can influence water quality by causing the incorporation/release of environmental contaminants and biological nutrients. Accounting for the effects of Fe 2+ -catalyzed recrystallization on water quality requires knowing the time scale over which recrystallization occurs. Here, we tested the hypothesis that nanoparticulate goethite becomes less susceptible to Fe 2+ -catalyzed recrystallization over time. We set up two batches of reactors in which 55 Fe 2+ tracer was added at two different time points and tracked the 55 Fe partitioning in the aqueous and goethite phases over 60 days. Less 55 Fe uptake occurred between 30 and 60 days than between 0 and 30 days, suggesting goethite recrystallization slowed with time. Fitting the data with a box model indicated that 17% of the goethite recrystallized after 30 days of reaction, and an additional 2% recrystallized between 30 and 60 days. The decreasing susceptibility of goethite to recrystallize as it reacted with aqueous Fe 2+ suggested that recrystallization is likely only an important process over short time scales.

Resonant absorption induced fast melting studied with mid-IR QCLs.

PubMed

Lu, Jie; Lv, Yankun; Ji, Youxin; Tang, Xiaoliang; Qi, Zeming; Li, Liangbin

2017-02-01

We demonstrate the use of a pump-probe setup based on two mid-infrared quantum cascade lasers (QCLs) to investigate the melting and crystallization of materials through resonant absorption. A combination of pump and probe beams fulfills the two-color synchronous detection. Furthermore, narrow linewidth advances the accuracy of measurements and the character of broad tuning range of QCLs enables wide applications in various sample and multiple structures. 1-Eicosene was selected as a simple model system to verify the feasibility of this method. A pulsed QCL was tuned to the absorption peak of CH 2 bending vibration at 1467 cm -1 to resonantly heat the sample. The other QCL in continuous mode was tuned to 1643 cm -1 corresponding the C=C stretching vibration to follow the fast melting dynamics. By monitoring the transmission intensity variation of pump and probe beams during pump-probe experiments, the resonant absorption induced fast melting and re-crystallization of 1-Eicosene can be studied. Results show that the thermal effect and melting behaviors strongly depend on the pump wavelength (resonant or non-resonant) and energy, as well as the pump time. The realization and detection of melting and recrystallization can be performed in tens of milliseconds, which improves the time resolution of melting process study based on general mid-infrared spectrum by orders of magnitude. The availability of resonant heating and detections based on mid-infrared QCLs is expected to enable new applications in melting study.

The Recrystallization Behavior of Unalloyed Mg and a Mg-Al Alloy

NASA Astrophysics Data System (ADS)

Murphy, Aeriel D.; Allison, John E.

2018-02-01

The static recrystallization behavior of pure Mg and Mg-4Al was characterized over a range of annealing temperatures. The electron backscatter diffraction grain orientation spread technique was used to quantify the level of recrystallization at various annealing times. Recrystallization kinetics were characterized using the Johnson-Mehl-Avrami-Kolmogorov (JMAK) relationship and it was found that two sequential annealing stages exist. Stage 1 involves heterogeneous nucleation of recrystallization in regions with a high stored energy, including twins and grain boundaries, and can be represented by an Avrami exponent of n 1 ranging from 0.35 to 0.6. During Stage 2, recrystallization occurred predominately in the interior of deformed grains with incomplete recrystallization generally observed even at annealing times in excess of two weeks. The second recrystallization stage exhibited a much lower Avrami exponent, n 2, ranging from 0.02 to 0.2. Increasing the starting grain size in the pure Mg condition led to a significant delay in recrystallization. The addition of Al had a minimal effect on the recrystallization kinetics of Mg.

Oman Drilling Project GT3 site survey: dynamics at the roof of an oceanic magma chamber

NASA Astrophysics Data System (ADS)

France, L.; Nicollet, C.; Debret, B.; Lombard, M.; Berthod, C.; Ildefonse, B.; Koepke, J.

2017-12-01

Oman Drilling Project (OmanDP) aims at bringing new constraints on oceanic crust accretion and evolution by drilling Holes in the whole ophiolite section (mantle and crust). Among those, operations at GT3 in the Sumail massif drilled 400 m to sample the dike - gabbro transition that corresponds to the top (gabbros) and roof (dikes) of the axial magma chamber, an interface where hydrothermal and magmatic system interacts. Previous studies based on oceanic crust formed at present day fast-spreading ridges and preserved in ophiolites have highlighted that this interface is a dynamic horizon where the axial melt lens that top the main magma chamber can intrude, reheat, and partially assimilate previously hydrothermally altered roof rocks. Here we present the preliminary results obtained in GT3 area that have allowed the community to choose the drilling site. We provide a geological and structural map of the area, together with new petrographic and chemical constraints on the dynamics of the dike - gabbro transition. Our new results allow us to quantify the dynamic processes, and to propose that 1/ the intrusive contact of the varitextured gabbro within the dikes highlights the intrusion of the melt lens top in the dike rooting zone, 2/ both dikes and previously crystallized gabbros are reheated, and recrystallized by underlying melt lens dynamics (up to 1050°C, largely above the hydrous solidus temperature of altered dikes and gabbros), 3/ the reheating range can be > 200°C, 4/ the melt lens depth variations for a given ridge position is > 200m, 5/ the reheating stage and associated recrystallization within the dikes occurred under hydrous conditions, 6/ the reheating stage is recorded at the root zone of the sheeted dike complex by one of the highest stable conductive thermal gradient ever recorded on Earth ( 3°C/m), 7/ local chemical variations in recrystallized dikes and gabbros are highlighted and used to quantify crystallization and anatectic processes, and the presence of trapped melt, 8/ melt lens cannibalism is attested by numerous assimilation figures close its roof. Besides providing a general context for future studies at OmanDP GT3 site, those new results allow us to quantify the dynamic processes that govern the layer 2 - layer 3 transition in ocean lithosphere.

Influence of Al on the Microstructural Evolution and Mechanical Behavior of Low-Carbon, Manganese Transformation-Induced-Plasticity Steel

NASA Astrophysics Data System (ADS)

Suh, Dong-Woo; Park, Seong-Jun; Lee, Tae-Ho; Oh, Chang-Seok; Kim, Sung-Joon

2010-02-01

Microstructural design with an Al addition is suggested for low-carbon, manganese transformation-induced-plasticity (Mn TRIP) steel for application in the continuous-annealing process. With an Al content of 1 mass pct, the competition between the recrystallization of the cold-rolled microstructure and the austenite formation cannot be avoided during intercritical annealing, and the recrystallization of the deformed matrix does not proceed effectively. The addition of 3 mass pct Al, however, allows nearly complete recrystallization of the deformed microstructure by providing a dual-phase cold-rolled structure consisting of ferrite and martensite and by suppressing excessive austenite formation at a higher annealing temperature. An optimized annealing condition results in the room-temperature stability of the intercritical austenite in Mn TRIP steel containing 3 mass pct Al, permitting persistent transformation to martensite during tensile deformation. The alloy presents an excellent strength-ductility balance combining a tensile strength of approximately 1 GPa with a total elongation over 25 pct, which is comparable to that of Mn TRIP steel subjected to batch-type annealing.

Recrystallization of polycrystalline silicon

NASA Technical Reports Server (NTRS)

Lall, C.; Kulkarni, S. B.; Graham, C. D., Jr.; Pope, D. P.

1981-01-01

Optical metallography is used to investigate the recrystallization properties of polycrystalline semiconductor-grade silicon. It is found that polycrystalline silicon recrystallizes at 1380 C in relatively short times, provided that the prior deformation is greater than 30%. For a prior deformation of about 40%, the recrystallization process is essentially complete in about 30 minutes. Silicon recrystallizes at a substantially slower rate than metals at equivalent homologous temperatures. The recrystallized grain size is insensitive to the amount of prestrain for strains in the range of 10-50%.

Molecular Dynamics, Recrystallization Behavior, and Water Solubility of the Amorphous Anticancer Agent Bicalutamide and Its Polyvinylpyrrolidone Mixtures.

PubMed

Szczurek, Justyna; Rams-Baron, Marzena; Knapik-Kowalczuk, Justyna; Antosik, Agata; Szafraniec, Joanna; Jamróz, Witold; Dulski, Mateusz; Jachowicz, Renata; Paluch, Marian

2017-04-03

In this paper, we investigated the molecular mobility and physical stability of amorphous bicalutamide, a poorly water-soluble drug widely used in prostate cancer treatment. Our broadband dielectric spectroscopy measurements and differential scanning calorimetry studies revealed that amorphous BIC is a moderately fragile material with a strong tendency to recrystallize from the amorphous state. However, mixing the drug with polymer polyvinylpyrrolidone results in a substantial improvement of physical stability attributed to the antiplasticizing effect governed by the polymer additive. Furthermore, IR study demonstrated the existence of specific interactions between the drug and excipient. We found out that preparation of bicalutamide-polyvinylpyrrolidone mixture in a 2-1 weight ratio completely hinder material recrystallization. Moreover, we determined the time-scale of structural relaxation in the glassy state for investigated materials. Because molecular mobility is considered an important factor governing crystallization behavior, such information was used to approximate the long-term physical stability of an amorphous drug and drug-polymer systems upon their storage at room temperature. Moreover, we found that such systems have distinctly higher water solubility and dissolution rate in comparison to the pure amorphous form, indicating the genuine formulation potential of the proposed approach.

Microgravity crystallization of macromolecules: An interim report and proposal for continued research

NASA Technical Reports Server (NTRS)

Goldberg, Benjamin E.

1986-01-01

An initial investigation exploring the effects of gravity on the crystallization of macromolecular systems has been completed. Monodisperse poly(ethylene), molecular weight 48,000 was melted and recrystallized under gravitational conditions: 0, 1, and 2 g. No correlations to gravitational environment were noted for the 20 C/min melt, as monitored with a photodensitometer system. However, post-crystallization testing of the recrystallized samples revealed thicker samples with more regions of large, well defined spherulites for the zero gravity crystallization environment. The results of the post-crystallization analysis have been reviewed and the results related to nucleation concerns. Finally, birefringence data, consistent with, but not explained by, the nucleation scenarios is detailed, and further investigations are proposed.

Evolution of microstructure of Haynes 230 and Inconel 617 under mechanical testing at high temperatures

NASA Astrophysics Data System (ADS)

Hrutkay, Kyle

Haynes 230 and Inconel 617 are austenitic nickel based superalloys, which are candidate structural materials for next generation high temperature nuclear reactors. High temperature deformation behavior of Haynes 230 and Inconel 617 have been investigated at the microstructural level in order to gain a better understanding of mechanical properties. Tensile tests were performed at strain rates ranging from 10-3-10-5 s -1 at room temperature, 600 °C, 800 °C and 950 °C. Subsequent microstructural analysis, including Scanning Electron Microscopy, Transmission Electron Microscopy, Energy-Dispersive X-ray Spectroscopy, and X-Ray Diffraction were used to relate the microstructural evolution at high temperatures to that of room temperature samples. Grain sizes and precipitate morphologies were used to determine high temperature behavior and fracture mechanics. Serrated flow was observed at intermediate and high temperatures as a result of discontinuous slip and dynamic recrystallization. The amplitude of serration increased with a decrease in the strain rate and increase in the temperature. Dynamic strain ageing was responsible for serrations at intermediate temperatures by means of a locking and unlocking phenomenon between dislocations and solute atoms. Dynamic recrystallization nucleated by grain and twin bulging resulting in a refinement of grain size. Existing models found in the literature were discussed to explain both of these phenomena.

Low-Temperature Friction-Stir Welding of 2024 Aluminum

NASA Technical Reports Server (NTRS)

Benavides, S.; Li, Y.; Murr, L. E.; Brown, D.; McClure, J. C.

1998-01-01

Solid state friction-stir welding (FSW) has been demonstrated to involve dynamic recrystallization producing ultra-fine, equiaxed grain structures to facilitate superplastic deformation as the welding or joining mechanism. However, the average residual, equiaxed, grain size in the weld zone has ranged from roughly 0.5 micron to slightly more than 10 micron, and the larger weld zone grain sizes have been characterized as residual or static grain growth as a consequence of the temperatures in the weld zone (where center-line temperatures in the FSW of 6061 Al have been shown to be as high as 480C or -0.8 T(sub M) where T(sub M) is the absolute melting temperature)). In addition, the average residual weld zone grain size has been observed to increase near the top of the weld, and to decrease with distance on either side of the weld-zone centerline, an d this corresponds roughly to temperature variations within the weld zone. The residual grain size also generally decreases with decreasing FSW tool rotation speed. These observations are consistent with the general rules for recrystallization where the recrystallized grain size decreases with increasing strain (or deformation) at constant strain rate, or with increasing strain-rate, or with increasing strain rate at constant strain; especially at lower ambient temperatures, (or annealing temperatures). Since the recrystallization temperature also decreases with increasing strain rate, the FSW process is somewhat complicated because the ambient temperature, the frictional heating fraction, and the adiabatic heating fraction )proportional to the product of strain and strain-rate) will all influence both the recrystallization and growth within the FSW zone. Significantly reducing the ambient temperature of the base metal or work pieces to be welded would be expected to reduce the residual weld-zone grain size. The practical consequences of this temperature reduction would be the achievement of low temperature welding. This study compares the residual grain sizes and microstructures in 2024 Al friction-stir welded at room temperature (about 30C and low temperature (-30C).

Microstructural characterization in dissimilar friction stir welding between 304 stainless steel and st37 steel

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jafarzadegan, M.; State Key Laboratory of Advanced Welding Production Technology, School of Materials Science and Eng., Harbin Institute of Technology, P.O. Box: 150001, Harbin; Feng, A.H.

2012-12-15

In the present study, 3 mm-thick plates of 304 stainless steel and st37 steel were welded together by friction stir welding at a welding speed of 50 mm/min and tool rotational speed of 400 and 800 rpm. X-ray diffraction test was carried out to study the phases which might be formed in the welds. Metallographic examinations, and tensile and microhardness tests were used to analyze the microstructure and mechanical properties of the joint. Four different zones were found in the weld area except the base metals. In the stir zone of the 304 stainless steel, a refined grain structure withmore » some features of dynamic recrystallization was evidenced. A thermomechanically-affected zone was characterized on the 304 steel side with features of dynamic recovery. In the other side of the stir zone, the hot deformation of the st37 steel in the austenite region produced small austenite grains and these grains transformed to fine ferrite and pearlite and some products of displacive transformations such as Widmanstatten ferrite and martensite by cooling the material after friction stir welding. The heat-affected zone in the st37 steel side showed partially and fully refined microstructures like fusion welding processes. The recrystallization in the 304 steel and the transformations in the st37 steel enhanced the hardness of the weld area and therefore, improved the tensile properties of the joint. - Highlights: Black-Right-Pointing-Pointer FSW produced sound welds between st37 low carbon steel and 304 stainless steel. Black-Right-Pointing-Pointer The SZ of the st37 steel contained some products of allotropic transformation. Black-Right-Pointing-Pointer The material in the SZ of the 304 steel showed features of dynamic recrystallization. Black-Right-Pointing-Pointer The finer microstructure in the SZ increased the hardness and tensile strength.« less

Paleozoic-Mesozoic boundary in the Berry Creek Quadrangle, northwestern Sierra Nevada, California

USGS Publications Warehouse

Hietanen, Anna Martta

1977-01-01

Structural and petrologic studies in the Berry Creek quadrangle at the north end of the western metamorphic belt of the Sierra Nevada have yielded new information that helps in distinguishing between the chemically similar Paleozoic and Mesozoic rocks. The distinguishing features are structural and textural and result from different degrees of deformation. Most Paleozoic rocks are strongly deformed and thoroughly recrystallized. Phenocrysts in meta volcanic rocks are granulated and drawn out into lenses that have sutured outlines. In contrast, the phenocrysts in the Mesozoic metavolcanic rocks show well-preserved straight crystal faces, are only slightly or not at all granulated, and contain fewer mineral inclusions than do those in the Paleozoic rocks. The groundmass in the Paleozoic rocks is recrystallized to a fairly coarse grained albite-epidote-amphibole-chlorite rock, whereas in the Mesozoic rocks the groundmass is a very fine grained feltlike mesh with only spotty occurrence of well-recrystallized finegrained albite-epidote-chlorite-actinolite rock. Primary minerals, such as augite, are locally preserved in the Mesozoic rocks but are altered to a mixture of amphibole, chlorite, and epidote in the Paleozoic rocks. In the contact aureoles of the plutons, and within the Big Bend fault zone, which crosses the area parallel to the structural trends, all rocks are thoroughly recrystallized and strongly deformed. Identification of the Paleozoic and Mesozoic rocks in these parts of the area was based on the continuity of the rock units in the field and on gradual changes in microscopic textures toward the plutons.

Continuous Inkjet Printing of Enalapril Maleate onto Orodispersible Film Formulations.

PubMed

Thabet, Yasmin; Lunter, Dominique; Breitkreutz, Joerg

2018-05-10

Piezoelectric inkjet printing onto orodispersible films (ODFs) was proven to be a successful technique applying flexible doses of active pharmaceutical ingredients (APIs) onto edible substrates. The reported API printing and ODF production was conducted in a non-continuous production approach. Within this study, drug-free and hydrochlorothiazide (HCT) containing ODFs should be imprinted in-line with enalapril maleate (EM) ink during continuous ODF production. Macrogol inks based on various solvents and solvent-water mixtures were developed providing dynamic viscosities from 7 to 17 mPa∗s. Water based inks contained 1.25%, methanol based inks up to 10% EM. Both inks could be printed (500-1000 Hz) during continuous ODF production. No EM recrystallization was observed for water-based inks. Mechanical properties were not affected by drug printing using various firing frequencies. ODF imprinted with water-based EM inks contained 0.04 mg EM / 6cm 2 . EM amount can be increased to a paediatric therapeutic dose of 0.5 mg EM utilizing methanol-based inks. These inks were successfully printed onto HCT ODFs resulting in a therapeutically relevant fixed-dose combination. No EM migration into the HCT layer could be observed. In conclusion, it was feasible to print EM doses onto drug-free and HCT ODFs during an in-line continuous manufacturing process. Copyright © 2018 Elsevier B.V. All rights reserved.

Modeling and simulation framework for dynamic strain localization in elasto-viscoplastic metallic materials subject to large deformations

DOE PAGES

Mourad, Hashem Mourad; Bronkhorst, Curt Allan; Livescu, Veronica; ...

2016-09-23

This study describes a theoretical and computational framework for the treatment of adiabatic shear band formation in rate-sensitive polycrystalline metallic materials. From a computational perspective, accurate representation of strain localization behavior has been a long-standing challenge. In addition, the underlying physical mechanisms leading to the localization of plastic deformation are still not fully understood. The proposed framework is built around an enhanced-strain finite element formulation, designed to alleviate numerical pathologies known to arise in localization problems, by allowing a localization band of given finite width (weak discontinuity) to be embedded within individual elements. The mechanical threshold strength (MTS) model ismore » used to represent the temperature and strain rate-dependent viscoplastic response of the material. This classical flow stress model employs an internal state variable to quantify the effect of dislocation structure evolution (work hardening and recovery). In light of growing evidence suggesting that the softening effect of dynamic recrystallization may play a significant role, alongside thermal softening, in the process of shear band formation and growth, a simple dynamic recrystallization model is proposed and cast within the context of the MTS model with the aid of the aforementioned internal state variable. An initiation criterion for shear localization in rate and temperature-sensitive materials is introduced and used in the present context of high-rate loading, where material rate-dependence is pronounced and substantial temperature increases are achieved due to the dissipative nature of viscoplastic processes. In addition, explicit time integration is adopted to facilitate treatment of the dynamic problems under consideration, where strain rates in excess of 10 4 s –1 are typically attained. Two series of experiments are conducted on AISI 316L stainless steel, employing the commonly used top-hat sample geometry and the Split-Hopkinson Pressure Bar dynamic test system. Axi-symmetric finite element simulation results are compared to cross-sectional micrographs of recovered samples and experimental load–displacement results, in order to examine the performance of the proposed framework and demonstrate its effectiveness in treating the initiation and growth of adiabatic shear banding in dynamically loaded metallic materials. These comparisons demonstrate that thermal softening alone is insufficient to induce shear localization behaviors observed in some materials, such as stainless steel, and support the hypothesis that dynamic recrystallization and/or other softening mechanisms play an essential role in this process.« less

Hot Deformation Behavior of Hot-Extruded AA7175 Through Hot Torsion Tests.

PubMed

Lee, Se-Yeon; Jung, Taek-Kyun; Son, Hyeon-Woo; Kim, Sang-Wook; Son, Kwang-Tae; Choi, Ho-Joon; Oh, Sang-Ho; Lee, Ji-Woon; Hyun, Soong-Keun

2018-03-01

The hot deformation behavior of hot-extruded AA7175 was investigated with flow curves and processing maps through hot torsion tests. The flow curves and the deformed microstructures revealed that dynamic recrystallization (DRX) occurred in the hot-extruded AA7175 during hot working. The failure strain was highest at medium temperature. This was mainly influenced by the dynamic precipitation of fine rod-shaped MgZn2. The processing map determined the optimal deformation condition for the alloy during hot working.

A STATE-VARIABLE APPROACH FOR PREDICTING THE TIME REQUIRED FOR 50% RECRYSTALLIZATION

DOE Office of Scientific and Technical Information (OSTI.GOV)

M. STOUT; ET AL

2000-08-01

It is important to be able to model the recrystallization kinetics in aluminum alloys during hot deformation. The industrial relevant process of hot rolling is an example of where the knowledge of whether or not a material recrystallizes is critical to making a product with the correct properties. Classically, the equations that describe the kinetics of recrystallization predict the time to 50% recrystallization. These equations are largely empirical; they are based on the free energy for recrystallization, a Zener-Holloman parameter, and have several adjustable exponents to fit the equation to engineering data. We have modified this form of classical theorymore » replacing the Zener-Hollomon parameter with a deformation energy increment, a free energy available to drive recrystallization. The advantage of this formulation is that the deformation energy increment is calculated based on the previously determined temperature and strain-rate sensitivity of the constitutive response. We modeled the constitutive response of the AA5182 aluminum using a state variable approach, the value of the state variable is a function of the temperature and strain-rate history of deformation. Thus, the recrystallization kinetics is a function of only the state variable and free energy for recrystallization. There are no adjustable exponents as in classical theory. Using this approach combined with engineering recrystallization data we have been able to predict the kinetics of recrystallization in AA5182 as a function of deformation strain rate and temperature.« less

Mesoscale model for fission-induced recrystallization in U-7Mo alloy

DOE PAGES

Liang, Linyun; Mei, Zhi -Gang; Kim, Yeon Soo; ...

2016-08-09

A mesoscale model is developed by integrating the rate theory and phase-field models and is used to study the fission-induced recrystallization in U-7Mo alloy. The rate theory model is used to predict the dislocation density and the recrystallization nuclei density due to irradiation. The predicted fission rate and temperature dependences of the dislocation density are in good agreement with experimental measurements. This information is used as input for the multiphase phase-field model to investigate the fission-induced recrystallization kinetics. The simulated recrystallization volume fraction and bubble induced swelling agree well with experimental data. The effects of the fission rate, initial grainmore » size, and grain morphology on the recrystallization kinetics are discussed based on an analysis of recrystallization growth rate using the modified Avrami equation. Here, we conclude that the initial microstructure of the U-Mo fuels, especially the grain size, can be used to effectively control the rate of fission-induced recrystallization and therefore swelling.« less

Dynamic oxidation behavior of TD-NiCr alloy with different surface pretreatments

NASA Technical Reports Server (NTRS)

Young, C. T.; Tenney, D. R.; Herring, H. W.

1975-01-01

Oxidation tests of TD-NiCr alloy with different surface pretreatments were conducted in a Mach-5 arc-jet at 1200 C and 0.002 lb/sec flowing air environment. The mechanisms responsible for the observed oxidation behavior are examined. The presence of atomic oxygen in the air stream plays a significant role in determining the oxidation characteristic of the alloy. The rate of Cr2O3 vaporization by formation of volatile CrO3 is greatly enhanced by the flowing conditions. The typical microstructure of oxides formed in the dynamic tests consists of an external layer of NiO with a porous mushroom-type morphology, an intermediate layer of NiO and Cr2O3 oxide mixture, and a continuous inner layer of Cr2O3 in contact with the Cr-depleted alloy substrate. Three basic processes underlying the formation of mushroom-type NiO are identified and discussed. The oxidation rate is determined by the rate of vaporization of NiO. Surface pretreatment has a significant effect on the oxidation behavior of the alloy in the early stage of oxidation, but becomes less important as exposure time increases. Mechanical polishing induces surface recrystallization, but promotes the concurrence of external growth of NiO and internal oxidation of the alloy in the dynamic atmosphere.

Effect of Carbon Nanotube on High-Temperature Formability of AZ31 Magnesium Alloy

NASA Astrophysics Data System (ADS)

Hassan, S. Fida; Paramsothy, M.; Gasem, Z. M.; Patel, F.; Gupta, M.

2014-08-01

Room-temperature tensile properties of AZ31 alloy have significantly been improved when reinforced with carbon nanotube via ingot metallurgy process. However, high-temperature (up to 250 °C) elongation-to-failure tensile test of the developed nanocomposite revealed a considerable softening in the AZ31 alloy matrix accompanied by an incredible ductility increment (up to 132%). Microstructural characterization of the fractured samples revealed that the dynamic recrystallization process has induced a complete recrystallization in the AZ31 alloy at a lower temperature (150 °C) followed by substantial grain growth at a higher temperature used in this study. Fractography on the fractured surfaces revealed that the room-temperature mixed brittle-ductile modes of fracture behavior of AZ31 alloy have transformed into a complete ductile mode of fracture at high temperature.

Effects of homogenization treatment on recrystallization behavior of 7150 aluminum sheet during post-rolling annealing

DOE Office of Scientific and Technical Information (OSTI.GOV)

Guo, Zhanying; Department of Applied Science, University of Québec at Chicoutimi, Saguenay, QC G7H 2B1; Zhao, Gang

2016-04-15

The effects of two homogenization treatments applied to the direct chill (DC) cast billet on the recrystallization behavior in 7150 aluminum alloy during post-rolling annealing have been investigated using the electron backscatter diffraction (EBSD) technique. Following hot and cold rolling to the sheet, measured orientation maps, the recrystallization fraction and grain size, the misorientation angle and the subgrain size were used to characterize the recovery and recrystallization processes at different annealing temperatures. The results were compared between the conventional one-step homogenization and the new two-step homogenization, with the first step being pretreated at 250 °C. Al{sub 3}Zr dispersoids with highermore » densities and smaller sizes were obtained after the two-step homogenization, which strongly retarded subgrain/grain boundary mobility and inhibited recrystallization. Compared with the conventional one-step homogenized samples, a significantly lower recrystallized fraction and a smaller recrystallized grain size were obtained under all annealing conditions after cold rolling in the two-step homogenized samples. - Highlights: • Effects of two homogenization treatments on recrystallization in 7150 Al sheets • Quantitative study on the recrystallization evolution during post-rolling annealing • Al{sub 3}Zr dispersoids with higher densities and smaller sizes after two-step treatment • Higher recrystallization resistance of 7150 sheets with two-step homogenization.« less

The Effect of Heat Treatment on the Sensitized Corrosion of the 5383-H116 Al-Mg Alloy

PubMed Central

Lin, Ying-Kai; Wang, Shing-Hai; Chen, Ren-Yu; Hsieh, Tso-Sheng; Tsai, Liren; Chiang, Chia-Chin

2017-01-01

In this study, the effects of heat treatment and sensitized corrosion on the 5383-H116 Al-Mg alloy were investigated for temperatures ranging from 100 to 450 °C. The results show that the heat treatment temperature is the main factor that causes changes to the microstructure and mechanical strength of the 5383-H116 Al-Mg alloy, inducing β-phase (Al3Mg2) precipitation in the form of a continuous layer along the grain boundaries. Intergranular corrosion was caused by the β-phase of the grain boundary precipitation, and the corrosion susceptibility of the recrystallized structure was significantly higher than the corrosion susceptibility of the recovered structure. According to the conductivity values detected, β-phase precipitation can enhance the 5383-H116 Al-Mg alloy conductivity, with the response due to structural dislocation density being higher than that due to the recrystallized structure. As such, the β-phase precipitation after sensitization is more significant than the β-phase precipitation prior to the sensitization, such that after sensitization, the conductivity rises to a significantly higher level than that exhibited by the recrystallization structure. PMID:28772635

Recrystallization and superplasticity at 300 C in an aluminum-magnesium alloy

NASA Technical Reports Server (NTRS)

Hales, S. J.; Mcnelley, T. R.; Mcqueen, H. J.

1991-01-01

Variations in thermomechanical processing (TMP) which regulate the microstructural characteristics and superplastic response of an Al-10Mg-0.1Zr alloy at 300 C were evaluated. Mechanical property data revealed that the superplastic ductility can be enhanced by simultaneously increasing the total rolling strain, the reduction per pass, and the duration of reheating intervals between passes during isothermal rolling. Texture and microscopy data were consistent with the development of a refined microstructure by recovery-dominated processes, i.e., continuous recrystallization, during the processing. The mechanisms by which a refined substructure can be progressively converted into a fine-grained structure during repeated cycles of deformation and annealing are addressed. A qualitative description of the complex sequence of developments leading to a microstructure better suited to support superplastic response is presented.

The importance of grain size to mantle dynamics and seismological observations

NASA Astrophysics Data System (ADS)

Gassmoeller, R.; Dannberg, J.; Eilon, Z.; Faul, U.; Moulik, P.; Myhill, R.

2017-12-01

Grain size plays a key role in controlling the mechanical properties of the Earth's mantle, affecting both long-timescale flow patterns and anelasticity on the timescales of seismic wave propagation. However, dynamic models of Earth's convecting mantle usually implement flow laws with constant grain size, stress-independent viscosity, and a limited treatment of changes in mineral assemblage. We study grain size evolution, its interplay with stress and strain rate in the convecting mantle, and its influence on seismic velocities and attenuation. Our geodynamic models include the simultaneous and competing effects of dynamic recrystallization resulting from dislocation creep, grain growth in multiphase assemblages, and recrystallization at phase transitions. They show that grain size evolution drastically affects the dynamics of mantle convection and the rheology of the mantle, leading to lateral viscosity variations of six orders of magnitude due to grain size alone, and controlling the shape of upwellings and downwellings. Using laboratory-derived scaling relationships, we convert model output to seismologically-observable parameters (velocity, attenuation) facilitating comparison to Earth structure. Reproducing the fundamental features of the Earth's attenuation profile requires reduced activation volume and relaxed shear moduli in the lower mantle compared to the upper mantle, in agreement with geodynamic constraints. Faster lower mantle grain growth yields best fit to seismic observations, consistent with our re-examination of high pressure grain growth parameters. We also show that ignoring grain size in interpretations of seismic anomalies may underestimate the Earth's true temperature variations.

Hot Ductility Characterization of Sanicro-28 Super-Austenitic Stainless Steel

NASA Astrophysics Data System (ADS)

Mirzaei, A.; Zarei-Hanzaki, A.; Abedi, H. R.

2016-05-01

The hot ductility behavior of a super-austenitic stainless steel has been studied using tensile testing method in the temperature range from 1073 K to 1373 K (800 °C to 1100 °C) under the strain rates of 0.1, 0.01, and 0.001 s-1. The hot compression tests were also performed at the same deformation condition to identify the activated restoration mechanisms. At lower temperatures [ i.e., 1073 K and 1173 K (800 °C and 900 °C)], the serration of initial grain boundaries confirms the occurrence of dynamic recovery as the predominant restoration process. However, in the course of applied deformation, the initial microstructure is recrystallized at higher temperatures [ i.e., 1273 K and 1373 K (1000 °C and 1100 °C)]. In this respect, annealing the twin boundaries could well stimulate the recrystallization kinetic through initiation new annealing twins on prior annealing twin boundaries. The hot tensile results show that there is a general trend of increasing ductility by temperature. However, two regions of ductility drop are recognized at 1273 K and 1373 K (1000°C)/0.1s-1 and (1100°C)/0.01s-1. The ductility variations at different conditions of temperature and strain rate are discussed in terms of simultaneous activation of grain boundary sliding and restoration processes. The observed ductility troughs are attributed to the occurrence of grain boundary sliding and the resulting R-type and W-type cracks. The occurrence of dynamic recrystallization is also considered as the main factor increasing the ductility at higher temperatures. The enhanced ductility is primarily originated from the post-uniform elongation behavior, which is directly associated with the strain rate sensitivity of the experimental material.

Deformation ages within the Klong Marui continental wrench fault, southern Thailand

NASA Astrophysics Data System (ADS)

Kanjanapayont, P.; Grasemann, B.; Edwards, M. A.

2009-04-01

The Klong Marui Fault is a ductile to brittle dextral strike-slip shear zone characterized by strong NNE-SSW geomorphic ridges trending up to 150 km. from Thai Gulf to Andaman Sea. At it southern part in the Phung Nga region, the ductile core forms a 40km long ridge. The geology within this wrench zone consisted of steep strongly deformed layers of migmatitic gneisses, mylonitic granites/pegmatites and phyllonitic metapelites. Brittle cataclasitc zones were localized in the eastern and western margin of this ductile core zone. The first deformation stage was dextral ductile strike-slip movement at mid to upper crustal levels and formed the main mylonitic foliation (c), secondary synthetic foliations (c'), and lineation in the migmatitic gneisses, mylonitic granites and metapelites. Locally sillimanite-clasts in high-temperature recrystallization quartz fabric fabric suggest deformation at amphibolite facies condition. More typically, quartz dynamically recrystallize by subgrain rotation and grain boundary migration under greenschist facies conditions. Microstructure of myrmekite and "V"-pull-apart clearly indicates dextral sense of shear. Pegmatites cross-cut the main mylonitic foliation but were sheared at the rims indicating syn-kinematic emplacement. Dynamically recrystallizing quartz mainly by basal gliding, bulging and low-temperature subgrain rotation record the latest stage of ductile dextral strike-slip deformation during decreasing temperature conditions. The NNE-SSW trending dextral strike-slip deformation accommodated the E-W transpression as a result of the differential movement of the northward drifting Indian craton and Asia. The brittle/ductile deformation produced cataclasites and minor faults which overprint the higher temperature fabric causing exhumation and juxtaposition of fault rocks developed under different metamorphic conditions in a positive flower structure.

Influence of Fe(2+)-catalysed iron oxide recrystallization on metal cycling.

PubMed

Latta, Drew E; Gorski, Christopher A; Scherer, Michelle M

2012-12-01

Recent work has indicated that iron (oxyhydr-)oxides are capable of structurally incorporating and releasing metals and nutrients as a result of Fe2+-induced iron oxide recrystallization. In the present paper, we briefly review the current literature examining the mechanisms by which iron oxides recrystallize and summarize how recrystallization affects metal incorporation and release. We also provide new experimental evidence for the Fe2+-induced release of structural manganese from manganese-doped goethite. Currently, the exact mechanism(s) for Fe2+-induced recrystallization remain elusive, although they are likely to be both oxide-and metal-dependent. We conclude by discussing some future research directions for Fe2+-catalysed iron oxide recrystallization.

Negative Temperature Dependence of Recrystallized Grain Size: Formulation and Experimental Confirmation on Copper

PubMed Central

Elmasry, Mohamed; Liu, Fan; Jiang, Yao; Mao, Ze Ning; Liu, Ying; Wang, Jing Tao

2017-01-01

The catalyzing effect on nucleation of recrystallization from existing grains resulting from previous lower temperature deformation is analyzed, analogous to the size effect of foreign nucleus in heterogeneous nucleation. Analytical formulation of the effective nucleation site for recrystallization leads to a negative temperature dependence of recrystallized grain size of metals. Non-isochronal annealing—where annealing time is set just enough for the completion of recrystallization at different temperatures—is conducted on pure copper after severe plastic deformation. More homogeneous and smaller grains are obtained at higher annealing temperature. The good fit between analytical and experimental results unveils the intrinsic feature of this negative temperature dependence of recrystallized grain size. PMID:28772676

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liang, Linyun; Mei, Zhi -Gang; Kim, Yeon Soo

A mesoscale model is developed by integrating the rate theory and phase-field models and is used to study the fission-induced recrystallization in U-7Mo alloy. The rate theory model is used to predict the dislocation density and the recrystallization nuclei density due to irradiation. The predicted fission rate and temperature dependences of the dislocation density are in good agreement with experimental measurements. This information is used as input for the multiphase phase-field model to investigate the fission-induced recrystallization kinetics. The simulated recrystallization volume fraction and bubble induced swelling agree well with experimental data. The effects of the fission rate, initial grainmore » size, and grain morphology on the recrystallization kinetics are discussed based on an analysis of recrystallization growth rate using the modified Avrami equation. Here, we conclude that the initial microstructure of the U-Mo fuels, especially the grain size, can be used to effectively control the rate of fission-induced recrystallization and therefore swelling.« less

Adaptive characterization of recrystallization kinetics in IF steel by electron backscatter diffraction.

PubMed

Kim, Dong-Kyu; Park, Won-Woong; Lee, Ho Won; Kang, Seong-Hoon; Im, Yong-Taek

2013-12-01

In this study, a rigorous methodology for quantifying recrystallization kinetics by electron backscatter diffraction is proposed in order to reduce errors associated with the operator's skill. An adaptive criterion to determine adjustable grain orientation spread depending on the recrystallization stage is proposed to better identify the recrystallized grains in the partially recrystallized microstructure. The proposed method was applied in characterizing the microstructure evolution during annealing of interstitial-free steel cold rolled to low and high true strain levels of 0.7 and 1.6, respectively. The recrystallization kinetics determined by the proposed method was found to be consistent with the standard method of Vickers microhardness. The application of the proposed method to the overall recrystallization stages showed that it can be used for the rigorous characterization of progressive microstructure evolution, especially for the severely deformed material. © 2013 The Authors Journal of Microscopy © 2013 Royal Microscopical Society.

Modeling the Controlled Recrystallization of Particle-Containing Aluminum Alloys

NASA Astrophysics Data System (ADS)

Adam, Khaled; Root, Jameson M.; Long, Zhengdong; Field, David P.

2017-01-01

The recrystallized fraction for AA7050 during the solution heat treatment is highly dependent upon the history of deformation during thermomechanical processing. In this work, a state variable model was developed to predict the recrystallization volume fraction as a function of processing parameters. Particle stimulated nucleation (PSN) was observed as a dominant mechanism of recrystallization in AA7050. The mesoscale Monte Carlo Potts model was used to simulate the evolved microstructure during static recrystallization with the given recrystallization fraction determined already by the state variable model for AA7050 alloy. The spatial inhomogeneity of nucleation is obtained from the measurement of the actual second-phase particle distribution in the matrix identified using backscattered electron (BSE) imaging. The state variable model showed good fit with the experimental results, and the simulated microstructures were quantitatively comparable to the experimental results for the PSN recrystallized microstructure of 7050 aluminum alloy. It was also found that the volume fraction of recrystallization did not proceed as dictated by the Avrami equation in this alloy because of the presence of the growth inhibitors.

Through-thickness recrystallization characteristics of a laminated AA3xxx–AA6xxx aluminum alloy system

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liao, L.H., E-mail: l2liao@uwaterloo.ca; Jin, H.; Gallerneault, M.

2015-03-15

The through-thickness annealing behavior of a laminated AA3xxx–AA6xxx alloy system at 300 °C has been studied by scanning electron microscopy, electron backscatter diffraction analysis, electron probe micro-analysis, differential scanning calorimetry, and hardness measurement. Results show that the recrystallization process starts at the interface region between the AA3xxx (clad) and AA6xxx (core) layers. Subsequently, the recrystallization process front progresses into the core layer, while the clad layer is the last region to recrystallize. It is also found that precipitation precedes recrystallization in the entire laminate at the investigated temperature. The preferential onset of recrystallization at the interface region is attributed tomore » the net driving pressure being the highest in this region. The factors that lead to such enhanced net driving pressure are (a) deformation incompatibility between the two alloy layers, (b) lower solute content of the interface, which also leads to lower volume fraction of precipitates, and (c) an accelerated rate of precipitate coarsening due to the presence of a higher density of dislocations. The gradual progress of recrystallization from the interface towards the core layer is dictated by precipitate coarsening and the dependence of its rate on the density of deformation-induced dislocations. The lower driving pressure due to lower work hardening capacity, high solute drag pressure due to Mn, and additional Zener drag from precipitates that form due to solute redistribution during annealing explain the late initiation of recrystallization in the clad layer. - Highlights: • The through-thickness recrystallization of a laminated system is investigated. • The early onset of recrystallization at the interface is discussed. • The effects of precipitation and coarsening on recrystallization are analyzed.« less

Effect of milling on particle shape and surface energy heterogeneity of needle-shaped crystals.

PubMed

Ho, Raimundo; Naderi, Majid; Heng, Jerry Y Y; Williams, Daryl R; Thielmann, Frank; Bouza, Peter; Keith, Adam R; Thiele, Greg; Burnett, Daniel J

2012-10-01

Milling and micronization of particles are routinely employed in the pharmaceutical industry to obtain small particles with desired particle size characteristics. The aim of this study is to demonstrate that particle shape is an important factor affecting the fracture mechanism in milling. Needle-shaped crystals of the β polymorph of D-mannitol were prepared from recrystallization in water. A portion of the recrystallized materials was ball-milled. Unmilled and milled sieved fractions of recrystallized D-mannitol were analyzed by dynamic image analysis (DIA) and inverse gas chromatography (IGC) at finite concentration to explain the breakage/fracture behavior. In the process of ball-milling, D-mannitol preferentially fractured along their shortest axis, exposing (011) plane with increased hydrophilicity and increased bounding rectangular aspect ratio. This is in contrary to attachment energy modeling which predicts a fracture mechanism across the (010) plane with increased hydrophobicity, and small change in particle shape. Crystal size, and more importantly, crystal shape and facet-specific mechanical properties, can dictate the fracture/cleavage behavior of organic crystalline materials. Thorough understanding of the crystal slip systems, combining attachment energy prediction with particle shape and surface characterization using DIA and IGC, are important in understanding fracture behavior of organic crystalline solids in milling and micronization.

Infiltration of meteoric fluids in an extensional detachment shear zone (Kettle dome, WA, USA): How quartz dynamic recrystallization relates to fluid-rock interaction

NASA Astrophysics Data System (ADS)

Quilichini, Antoine; Siebenaller, Luc; Nachlas, William O.; Teyssier, Christian; Vennemann, Torsten W.; Heizler, Matthew T.; Mulch, Andreas

2015-02-01

We document the interplay between meteoric fluid flow and deformation processes in quartzite-dominated lithologies within a ductile shear zone in the footwall of a Cordilleran extensional fault (Kettle detachment system, Washington, USA). Across 150 m of shear zone section, hydrogen isotope ratios (δD) from synkinematic muscovite fish are constant (δD ˜ -130‰) and consistent with a meteoric fluid source. Quartz-muscovite oxygen isotope thermometry indicates equilibrium fractionation temperatures of ˜365 ± 30 °C in the lower part of the section, where grain-scale quartz deformation was dominated by grain boundary migration recrystallization. In the upper part of the section, muscovite shows increasing intragrain compositional zoning, and quartz microstructures reflect bulging recrystallization, solution-precipitation, and microcracking that developed during progressive cooling and exhumation. The preserved microstructural characteristics and hydrogen isotope fingerprints of meteoric fluids developed over a short time interval as indicated by consistent mica 40Ar/39Ar ages ranging between 51 and 50 Ma over the entire section. Pervasive fluid flow became increasingly channelized during detachment activity, leading to microstructural heterogeneity and large shifts in quartz δ18O values on a meter scale. Ductile deformation ended when brittle motion on the detachment fault rapidly exhumed the mylonitic footwall.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hu, Shenyang; Joshi, Vineet; Lavender, Curt A.

Experiments showed that recrystallization dramatically speeds up the gas bubble swelling kinetics in metallic UMo fuels. In this work a recrystallization model is developed to study the effect of microstructures and radiation conditions on recrystallization kinetics. The model integrates the rate theory of intra-granular gas bubble and interstitial loop evolution and a phase field model of recrystallization zone evolution. A fast passage method is employed to describe one dimensional diffusion of interstitials which have diffusivity several order magnitude larger than that of the fission gas Xe. With the model, the effect of grain sizes on recrystallization kinetics is simulated.

Hot deformation characteristics of INCONEL alloy MA 754 and development of a processing map

DOE Office of Scientific and Technical Information (OSTI.GOV)

Somani, M.C.; Muraleedharan, K.; Birla, N.C.

1994-08-01

The characteristics of hot deformation of INCONEL alloy MA 754 have been studies using processing maps obtained on the basis of flow stress data generated in compression in the temperature range 700 C to 1,150 C and strain rate range 0.001 to 100 s[sup [minus]1]. The map exhibited three domains. (1) A domain of dynamic recovery occurs in the temperature range 800 C to 1,075 C and strain rate range 0.02 to 2 s[sup [minus]1], with a peak efficiency of 18 pct occurring at 950 C and 0.1 s [sup [minus]1]. Transmission electron microscope (TEM) micrographs revealed stable subgrain structuremore » in this domain with the subgrain size increasing exponentially with an increase in temperature. (2) A domain exhibiting grain boundary cracking occurs at temperatures lower than 800 C and strain rates lower than 0.01 s[sup [minus]1]. (3) A domain exhibiting intense grain boundary cavitation occurs at temperatures higher than 1075 C. The material did not exhibit a dynamic recrystallization (DRX) domain, unlike other superalloys. At strain rates higher than about 1 s[sup [minus]1], the material exhibits flow instabilities manifesting as kinking of the elongated grains and adiabatic shear bands. The materials may be safely worked in the domain of dynamic recovery but can only be statically recrystallized.« less

Imaging Water in Deformed Quartzites: Examples from Caledonian and Himalayan Shear Zones

NASA Astrophysics Data System (ADS)

Kronenberg, Andreas; Ashley, Kyle; Hasnan, Hasnor; Holyoke, Caleb; Jezek, Lynna; Law, Richard; Thomas, Jay

2016-04-01

Infrared IR measurements of OH absorption bands due to water in deformed quartz grains have been collected from major shear zones of the Caledonian and Himalayan orogens. Mean intragranular water contents were determined from the magnitude of the broad OH absorption at 3400 cm-1 as a function of structural position, averaging over multiple grains, using an IR microscope coupled to a conventional FTIR spectrometer with apertures of 50-100 μm. Images of water content were generated by scanning areas of up to 4 mm2 of individual specimens with a 10 μm synchrotron-generated IR beam and contouring OH absorptions. Water contents vary with structural level relative to the central cores of shear zones and they vary at the grain scale corresponding to deformation and recrystallization microstructures. Gradients in quartz water content expressed over structural distances of 10 to 400 m from the centers of the Moine Thrust (Stack of Glencoul, NW Scotland), the Main Central Thrust (Sutlej valley of NW India), and the South Tibetan Detachment System (Rongbuk valley north of Mount Everest) indicate that these shear zones functioned as fluid conduits. However, the gradients differ substantially: in some cases, enhanced fluid fluxes appear to have increased quartz water contents, while in others, they served to decrease water contents. Water contents of Moine thrust quartzites appear to have been reduced during shear at greenschist facies by processes of regime II BLG/SGR dislocation creep. Intragranular water contents of the protolith 70 m below the central fault core are large (4078 ± 247 ppm, H/106 Si) while mylonites within 5 mm of the Moine hanging wall rocks have water contents of only 1570 (± 229) ppm. Water contents between these extremes vary systematically with structural level and correlate inversely with the extent of dynamic recrystallization (20 to 100%). Quartz intragranular water contents of Himalayan thrust and low-angle detachment zones sheared at upper amphibolite conditions by regime III GBM creep show varying trends with structural level. Water contents increase toward the Lhotse detachment of the Rongbuk valley, reaching 11,350 (± 1095) ppm, whereas they decrease toward the Main Central Thrust exposed in the western part of the Sutlej valley to values as low as 170 (± 25) ppm. Maps of intragranular water content correspond to populations of fluid inclusions, which depend on the history of deformation and dynamic recrystallization. Increases in water content require the introduction of secondary fluid inclusions, generally by brittle microcracking followed by crack healing and processes of inclusion redistribution documented in milky quartz experiments. Decreases in water content result from dynamic recrystallization, as mobile grain boundaries sweep through wet porphyroclasts, leaving behind dry recrystallized grains. Intragranular water contents throughout greenschist mylonites of the Moine thrust are comparable to those of quartz weakened by water in laboratory experiments. However, water contents of upper amphibolite mylonites of the Main Central Thrust are far below those required for water weakening at experimental strain rates and offer challenges to our understanding of quartz rheology.

Stable mineral recrystallization in low temperature aqueous systems: A critical review

NASA Astrophysics Data System (ADS)

Gorski, Christopher A.; Fantle, Matthew S.

2017-02-01

Minerals may undergo recrystallization reactions in low temperature (<100 °C) aqueous systems, during which they exchange isotopes and trace elements with the dissolved reservoir without undergoing overt structural, bulk compositional, or morphological changes. These interfacial reactions, which are often referred to in the literature as "atom exchange" and herein as "stable mineral recrystallization", have important implications for the use of isotopic and elemental proxies to interpret past temperatures, oxidation states, and aqueous chemistries on Earth. The reactions are also significant for modern environments, including engineered systems, as they imply that mineral lattices may be substantially more open to exchanging toxic elements and radionuclides with coexisting solutions than previously thought. To date, observations of stable mineral recrystallization are distributed among several disciplines, and no work has attempted to review their findings comprehensively. Accordingly, this review article presents laboratory evidence for stable mineral recrystallization, describes data collection and interpretation strategies, summarizes similar recrystallization systematics observed in multiple studies, explores the potential occurrence of stable mineral recrystallization in natural systems, and discusses possible mechanisms by which stable mineral recrystallization occurs. The review focuses primarily on carbonates, sulfates, and iron oxides because these minerals have been studied most extensively to date. The review concludes by presenting key questions that should be addressed in this field to further understand and account for stable mineral recrystallization in natural and engineered aqueous systems at low temperatures.

Mechanisms for pressure-induced crystal-crystal transition, amorphization, and devitrification of SnI{sub 4}

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liu, H.; Tse, J. S., E-mail: john.tse@usask.ca; Hu, M. Y.

2015-10-28

The pressure-induced amorphization and subsequent recrystallization of SnI{sub 4} have been investigated using first principles molecular dynamics calculations together with high-pressure {sup 119}Sn nuclear resonant inelastic x-ray scattering measurements. Above ∼8 GPa, we observe a transformation from an ambient crystalline phase to an intermediate crystal structure and a subsequent recrystallization into a cubic phase at ∼64 GPa. The crystalline-to-amorphous transition was identified on the basis of elastic compatibility criteria. The measured tin vibrational density of states shows large amplitude librations of SnI{sub 4} under ambient conditions. Although high pressure structures of SnI{sub 4} were thought to be determined by randommore » packing of equal-sized spheres, we detected electron charge transfer in each phase. This charge transfer results in a crystal structure packing determined by larger than expected iodine atoms.« less

Mechanisms for pressure-induced crystal-crystal transition, amorphization, and devitrification of Snl 4

DOE PAGES

Liu, Hanyu; Tse, John S.; Hu, Michael Y.; ...

2015-10-27

The pressure-induced amorphization and subsequent recrystallization of SnI 4 have been investigated using first principles molecular dynamics calculations together with high-pressure 119Sn nuclear resonant inelastic x-ray scattering measurements. Above ~8 GPa, we observe a transformation from an ambient crystalline phase to an intermediate crystal structure and a subsequent recrystallization into a cubic phase at ~64 GPa. The crystalline-to-amorphous transition was identified on the basis of elastic compatibility criteria. The measured tin vibrational density of states shows large amplitude librations of SnI 4 under ambient conditions. Although high pressure structures of SnI 4 were thought to be determined by random packingmore » of equal-sized spheres, we detected electron charge transfer in each phase. As a result, this charge transfer results in a crystal structure packing determined by larger than expected iodine atoms. (C) 2015 AIP Publishing LLC.« less

Microstructure and Mechanical Characterization of Friction-Stir-Welded Dual-Phase Brass

NASA Astrophysics Data System (ADS)

Ramesh, R.; Dinaharan, I.; Akinlabi, E. T.; Murugan, N.

2018-03-01

Friction stir welding (FSW) is an ideal process to join brass to avoid the evaporation of zinc. In the present investigation, 6-mm-thick dual-phase brass plates were joined efficiently using FSW at various tool rotational speeds. The microstructures were studied using optical microscopy, electron backscattered diffraction and transmission electron microscopy. The optical micrographs revealed the evolution of various zones across the joint line. The microstructure of the heat-affected zone was similar to that of base metal. The weld zone exhibited finer grains due to dynamic recrystallization. The recrystallization was inhomogeneous and the inhomogeneity reduced with increased tool rotational speed. The dual phase was preserved in the weld zone due to the retention of zinc. The severe plastic deformation created a lot of dislocations in the weld zone. The weld zone was strengthened after welding. The role of tool rotational speed on the joint strength is further reported.

Investigation on the effect of friction stir processing on tribological and mechanical properties of Al 7075-T651 alloy

NASA Astrophysics Data System (ADS)

Murthy, Veeresh; Rajaprakash, B. M.

2018-04-01

Friction Stir Processing (FSP) is generally used as a novel method for surface properties enhancement. The surface developed through FSP alters the tribological and mechanical properties of the material in a single step. This commendable enhancement in the properties by recrystallized equiaxed microstructure attained by dynamic recrystallization can be achieved in just one step there by increasing the performance. In this study, the effect of the FSP passes on the tribological & mechanical properties such as hardness, wear resistance and tensile strength for commercially available AA7075-T651 of 6mm thick sheet was studied. Properties in terms of hardness, wear rate and tensile strength were compared with the base alloy and Friction Stir Processed (FSPed) alloy. It was observed that the hardness, wear rate of the FSPed FSP3 was enhanced by 44% and 60% as compared to that of the unprocessed sample.

Mechanisms for pressure-induced crystal-crystal transition, amorphization, and devitrification of SnI4.

PubMed

Liu, H; Tse, J S; Hu, M Y; Bi, W; Zhao, J; Alp, E E; Pasternak, M; Taylor, R D; Lashley, J C

2015-10-28

The pressure-induced amorphization and subsequent recrystallization of SnI4 have been investigated using first principles molecular dynamics calculations together with high-pressure (119)Sn nuclear resonant inelastic x-ray scattering measurements. Above ∼8 GPa, we observe a transformation from an ambient crystalline phase to an intermediate crystal structure and a subsequent recrystallization into a cubic phase at ∼64 GPa. The crystalline-to-amorphous transition was identified on the basis of elastic compatibility criteria. The measured tin vibrational density of states shows large amplitude librations of SnI4 under ambient conditions. Although high pressure structures of SnI4 were thought to be determined by random packing of equal-sized spheres, we detected electron charge transfer in each phase. This charge transfer results in a crystal structure packing determined by larger than expected iodine atoms.

Effect of aging and ice structuring proteins on the morphology of frozen hydrated gluten networks.

PubMed

Kontogiorgos, Vassilis; Goff, H Douglas; Kasapis, Stefan

2007-04-01

The present investigation constitutes an attempt to rationalize the effect of aging and ice structuring proteins (ISPs) on the network morphology of frozen hydrated gluten. In doing so, it employs differential scanning calorimetry, time-domain NMR, dynamic oscillation on shear, creep testing, and electron microscopy. Experimentation and first principles modeling allows identification and description of the processes of ice formation and recrystallization in molecular terms. It is demonstrated that in the absence of a readily discernible glass transition temperature in gluten-ice composites, the approach of considering the melting point and aging at constant or fluctuating temperature conditions in the vicinity of this point can provide a valid index of functional quality. A theoretical framework supporting the concept of capillary confined frozen water in the gluten matrix was advanced, and it was found that ISPs were effective in controlling recrystallization both within these confines and within ice in the bulk.

Using a Simulated Industrial Setting for the Development of an Improved Solvent System for the Recrystallization of Benzoic Acid: A Student-Centered Project

ERIC Educational Resources Information Center

Hightower, Timothy R.; Heeren, Jay D.

2006-01-01

Recrystallization of benzoic acid is an excellent way to remove insoluble impurities. In a traditional organic laboratory experiment, insoluble impurities are removed through the recrystallization of benzoic acid utilizing water as the recrystallization solvent. It was our goal to develop a peer-led, problem-solving organic laboratory exercise…

Static Recrystallization Behavior of Z12CN13 Martensite Stainless Steel

NASA Astrophysics Data System (ADS)

Luo, Min; Zhou, Bing; Li, Rong-bin; Xu, Chun; Guo, Yan-hui

2017-09-01

In order to increase the hot workability and provide proper hot forming parameters of forging Z12CN13 martensite stainless steel for the simulation and production, the static recrystallization behavior has been studied by double-pass hot compression tests. The effects of deformation temperature, strain rate and inter-pass time on the static recrystallization fraction by the 2% offset method are extensively studied. The results indicate that increasing the inter-pass time and the deformation temperature as well as strain rate appropriately can increase the fraction of static recrystallization. At the temperature of 1050-1150 °C, inter-pass time of 30-100 s and strain rate of 0.1-5 s-1, the static recrystallization behavior is obvious. In addition, the kinetics of static recrystallization behavior of Z12CN13 steel has been established and the activation energy of static recrystallization is 173.030 kJ/mol. The substructure and precipitates have been studied by TEM. The results reveal that the nucleation mode is bulging at grain boundary. Undissolved precipitates such as MoNi3 and Fe3C have a retarding effect on the recrystallization kinetics. The effect is weaker than the accelerating effect of deformation temperature.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liang, Linyun; Mei, Zhi-Gang; Yacout, Abdellatif M.

We have developed a mesoscale phase-field model for studying the effect of recrystallization on the gas-bubble-driven swelling in irradiated U-Mo alloy fuel. The model can simulate the microstructural evolution of the intergranular gas bubbles on the grain boundaries as well as the recrystallization process. Our simulation results show that the intergranular gas-bubble-induced fuel swelling exhibits two stages: slow swelling kinetics before recrystallization and rapid swelling kinetics with recrystallization. We observe that the recrystallization can significantly expedite the formation and growth of gas bubbles at high fission densities. The reason is that the recrystallization process increases the nucleation probability of gasmore » bubbles and reduces the diffusion time of fission gases from grain interior to grain boundaries by increasing the grain boundary area and decreasing the diffusion distance. The simulated gas bubble shape, size distribution, and density on the grain boundaries are consistent with experimental measurements. We investigate the effect of the recrystallization on the gas-bubble-driven fuel swelling in UMo through varying the initial grain size and grain aspect ratio. We conclude that the initial microstructure of fuel, such as grain size and grain aspect ratio, can be used to effectively control the recrystallization and therefore reduce the swelling in U-Mo fuel.« less

A continuum theory of grain size evolution and damage

NASA Astrophysics Data System (ADS)

Ricard, Y.; Bercovici, D.

2009-01-01

Lithospheric shear localization, as occurs in the formation of tectonic plate boundaries, is often associated with diminished grain size (e.g., mylonites). Grain size reduction is typically attributed to dynamic recrystallization; however, theoretical models of shear localization arising from this hypothesis are problematic because (1) they require the simultaneous action of two creep mechanisms (diffusion and dislocation creep) that occur in different deformation regimes (i.e., in grain size stress space) and (2) the grain growth ("healing") laws employed by these models are derived from normal grain growth or coarsening theory, which are valid in the absence of deformation, although the shear localization setting itself requires deformation. Here we present a new first principles grained-continuum theory, which accounts for both coarsening and damage-induced grain size reduction in a monomineralic assemblage undergoing irrecoverable deformation. Damage per se is the generic process for generation of microcracks, defects, dislocations (including recrystallization), subgrains, nuclei, and cataclastic breakdown of grains. The theory contains coupled macroscopic continuum mechanical and grain-scale statistical components. The continuum level of the theory considers standard mass, momentum, and energy conservation, as well as entropy production, on a statistically averaged grained continuum. The grain-scale element of the theory describes both the evolution of the grain size distribution and mechanisms for both continuous grain growth and discontinuous grain fracture and coalescence. The continuous and discontinuous processes of grain size variation are prescribed by nonequilibrium thermodynamics (in particular, the treatment of entropy production provides the phenomenological laws for grain growth and reduction); grain size evolution thus incorporates the free energy differences between grains, including both grain boundary surface energy (which controls coarsening) and the contribution of deformational work to these free energies (which controls damage). In the absence of deformation, only two mechanisms that increase the average grain size are allowed by the second law of thermodynamics. One mechanism, involving continuous diffusive mass transport from small to large grains, captures the essential components of normal grain growth theories of Lifshitz-Slyosov and Hillert. The second mechanism involves the aggregation of grains and is described using a Smoluchovski formalism. With the inclusion of deformational work and damage, the theory predicts two mechanisms for which the thermodynamic requirement of entropy positivity always forces large grains to shrink and small ones to grow. The first such damage-driven mechanism involving continuous mass transfer from large to small grains tends to homogenize the distribution of grain size toward its initial mean grain size. The second damage mechanism favors the creation of small grains by discontinuous division of larger grains and reduces the mean grain size with time. When considered separately, most of these mechanisms allow for self-similar grain size distributions whose scales (i.e., statistical moments such as the mean, variance, and skewness) can all be described by a single grain scale, such as the mean or maximum. However, the combination of mechanisms, e.g., one that captures the competition between continuous coarsening and mean grain size reduction by breakage, does not generally permit a self-similar solution for the grain size distribution, which contradicts the classic assumption that grain growth laws allowing for both coarsening and recrystallization can be treated with a single grain scale such as the mean size.

Rheology linked with phase changes as recorded by development of shear bands in the South Armorican Shear Zone

NASA Astrophysics Data System (ADS)

Jeřábek, Petr; Bukovská, Zita

2015-04-01

The South Armorican Shear Zone in France represents a major right-lateral strike slip shear zone formed in the late stages of Variscan orogeny. The active deformation in this shear zone is associated with the development of S-C fabrics in granitoids where thin shear bands (C) overprint an earlier higher grade metamorphic foliation (S). In the studied samples covering low to high intensity of shear band overprint, we identified three stages of shear band evolution associated with distinct microstructures and deformation mechanisms. The initiation of shear bands stage I is associated with the formation of microcracks crosscutting the S fabric and detected namely in the recrystallized quartz aggregates. The microcracks of suitable orientation are filled by microcline, albite, muscovite and chlorite which is a typical assemblage also for the well developed shear bands. Phase equilibrium modeling in PERPLEX indicates that this assemblage formed at pressure-temperature range of 0.1-0.4 GPa and 300-340 °C. Stage II of shear band evolution is characterized by dynamic recrystallization and grain size reduction of quartz aggregates along the microcracks and replacement of quartz by microcline along grain boundaries. This process leads to disintegration of quartz aggregate fabric and phase mixing in the shear bands. The inferred deformation mechanism for this stage is solution-precipitation creep although recrystallization of quartz is still active at the contact between quartz aggregates and shear bands. The coarse grained microstructure of quartz aggregates with ca ~250 microns average grain size reduces to ~10 microns grain size when recrystallized along extremely thin shear bands/microcracks and to ~20 microns grain size when recrystallized along the thicker shear bands. By using the flow law of Patterson and Luan (1990) for dislocation creep in quartz and the quartz piezometer of Stipp and Tullis (2003) corrected after Holyoke and Kronenberg (2010), the quartz recrystallization along thin shear bands records strain rates of ~10^-14 whereas the recrystallization along thick shear bands records strain rates of ~10^-15. The contemporaneous operation of solution-precipitation creep in shear bands and dislocation creep in quartz along the shear band boundary suggests low viscosity contrast between the mixed phase shear band matrix and pure quartz aggregate implying that the solution-precipitation creep reflect similar stress and strain rate conditions as the dislocation creep in quartz. Stage III of shear band evolution is characterized by interconnection of dispersed muscovite grains and the deformation becomes accommodated by dislocation creep in thin muscovite bands separating the inactive domains of stage II microstructure. References: Holyoke III, C. W., & Kronenberg, A. K. (2010). Accurate differential stress measurement using the molten salt cell and solid salt assemblies in the Griggs apparatus with applications to strength, piezometers and rheology. Tectonophysics, 494(1-2), 17-31. Paterson, M. S., & Luan, F. C. (1990). Quartzite rheology under geological conditions. In R. J. Knipe & E. H. Rutter (Eds.), Deformation Mechanisms, Rheology and Tectonics (pp. 299-307). London: Geological Society Special Publications. Stipp, M., & Tullis, J. (2003). The recrystallized grain size piezometer for quartz. Geophysical Research Letters, 30(21), 1-5.

Solvent Selection for Recrystallization: An Undergraduate Organic Experiment.

ERIC Educational Resources Information Center

Baumann, Jacob B.

1979-01-01

This experiment develops the students' ability to carry out a simple recrystallization effectively, and demonstrates how a solvent may be selected or rejected for the recrystallization of a specific organic compound. (Author/BB)

Nano-Sized Grain Refinement Using Friction Stir Processing

DTIC Science & Technology

2013-03-01

friction stir weld is a very fine grain microstructure produced as a result of dynamic recrystallization. The friction stir ... Friction Stir Processing, Magnesium, Nano-size grains Abstract A key characteristic of a friction stir weld is a very fine grain microstructure...state process developed on the basis of the friction stir welding (FSW) technique invented by The Welding Institute (TWI) in 1991 [2]. During

Thermomechanical processing of aluminum micro-alloyed with Sc, Zr, Ti, B, and C

NASA Astrophysics Data System (ADS)

McNamara, Cameron T.

Critical exploration of the minimalistic high strength low alloy aluminum (HSLA-Al) paradigm is necessary for the continued development of advanced aluminum alloys. In this study, scandium (Sc) and zirconium (Zr) are examined as the main precipitation strengthening additions, while magnesium (Mg) is added to probe the synergistic effects of solution and precipitation hardening, as well as the grain refinement during solidification afforded by a moderate growth restriction factor. Further, pathways of recrystallization are explored in several potential HSLA-Al syste =ms sans Sc. Aluminum-titanium-boron (Al-Ti-B) and aluminum-titanium-carbon (Al-Ti-C) grain refining master alloys are added to a series of Al-Zr alloys to examine both the reported Zr poisoning effect on grain size reduction and the impact on recrystallization resistance through the use of electron backscattered diffraction (EBSD) imaging. Results include an analysis of active strengthening mechanisms and advisement for both constitution and thermomechanical processing of HSLA-Al alloys for wrought or near-net shape cast components. The mechanisms of recrystallization are discussed for alloys which contain a bimodal distribution of particles, some of which act as nucleation sites for grain formation during annealing and others which restrict the growth of the newly formed grains.

Inhibition of Ice Growth and Recrystallization by Zirconium Acetate and Zirconium Acetate Hydroxide

PubMed Central

Mizrahy, Ortal; Bar-Dolev, Maya; Guy, Shlomit; Braslavsky, Ido

2013-01-01

The control over ice crystal growth, melting, and shaping is important in a variety of fields, including cell and food preservation and ice templating for the production of composite materials. Control over ice growth remains a challenge in industry, and the demand for new cryoprotectants is high. Naturally occurring cryoprotectants, such as antifreeze proteins (AFPs), present one solution for modulating ice crystal growth; however, the production of AFPs is expensive and inefficient. These obstacles can be overcome by identifying synthetic substitutes with similar AFP properties. Zirconium acetate (ZRA) was recently found to induce the formation of hexagonal cavities in materials prepared by ice templating. Here, we continue this line of study and examine the effects of ZRA and a related compound, zirconium acetate hydroxide (ZRAH), on ice growth, shaping, and recrystallization. We found that the growth rate of ice crystals was significantly reduced in the presence of ZRA and ZRAH, and that solutions containing these compounds display a small degree of thermal hysteresis, depending on the solution pH. The compounds were found to inhibit recrystallization in a manner similar to that observed in the presence of AFPs. The favorable properties of ZRA and ZRAH suggest tremendous potential utility in industrial applications. PMID:23555701

Electrical Conductivity, Thermal Stability, and Lattice Defect Evolution During Cyclic Channel Die Compression of OFHC Copper

NASA Astrophysics Data System (ADS)

Satheesh Kumar, S. S.; Raghu, T.

2015-02-01

Oxygen-free high-conductivity (OFHC) copper samples are severe plastically deformed by cyclic channel die compression (CCDC) technique at room temperature up to an effective plastic strain of 7.2. Effect of straining on variation in electrical conductivity, evolution of deformation stored energy, and recrystallization onset temperatures are studied. Deformation-induced lattice defects are quantified using three different methodologies including x-ray diffraction profile analysis employing Williamson-Hall technique, stored energy based method, and electrical resistivity-based techniques. Compared to other severe plastic deformation techniques, electrical conductivity degrades marginally from 100.6% to 96.6% IACS after three cycles of CCDC. Decrease in recrystallization onset and peak temperatures is noticed, whereas stored energy increases and saturates at around 0.95-1.1J/g after three cycles of CCDC. Although drop in recrystallization activation energy is observed with the increasing strain, superior thermal stability is revealed, which is attributed to CCDC process mechanics. Low activation energy observed in CCDC-processed OFHC copper is corroborated to synergistic influence of grain boundary characteristics and lattice defects distribution. Estimated defects concentration indicated continuous increase in dislocation density and vacancy with strain. Deformation-induced vacancy concentration is found to be significantly higher than equilibrium vacancy concentration ascribed to hydrostatic stress states experienced during CCDC.

On the use of copper-based substrates for YBCO coated conductors

NASA Astrophysics Data System (ADS)

Vannozzi, A.; Fabbri, F.; Augieri, A.; Angrisani Armenio, A.; Galluzzi, V.; Mancini, A.; Rizzo, F.; Rufoloni, A.; Padilla, J. A.; Xuriguera, E.; De Felicis, D.; Bemporad, E.; Celentano, G.

2014-05-01

It is well known that the recrystallization texture of heavily cold-rolled pure copper is almost completely cubic. However, one of the main drawbacks concerning the use of pure copper cube-textured substrates for YBCO coated conductor is the reduced secondary recrystallization temperature. The onset of secondary recrystallization (i.e., the occurrence of abnormal grains with unpredictable orientation) in pure copper substrate was observed within the typical temperature range required for buffer layer and YBCO processing (600-850 °C). To avoid the formation of abnormal grains the effect of both grain size adjustment (GSA) and recrystallization annealing was analyzed. The combined use of a small initial grain size and a recrystallization two-step annealing (TSA) drastically reduced the presence of abnormal grains in pure copper tapes. Another way to overcome the limitation imposed by the formation of abnormal grains is to deposit a buffer layer at temperatures where secondary recrystallization does not occur. For example, La2Zr2O7 (LZO) film with a high degree of epitaxy was grown by metal-organic decomposition (MOD) at 1000 °C on pure copper substrate. In several samples the substrate underwent secondary recrystallization. Our experiments indicate that the motion of grain boundaries occurring during secondary recrystallization process does not affect the quality of LZO film.

Effect of Sn Micro-alloying on Recrystallization Nucleation and Growth Processes of Ferritic Stainless Steels

NASA Astrophysics Data System (ADS)

He, Tong; Bai, Yang; Liu, Xiuting; Guo, Dan; Liu, Yandong

2018-04-01

We investigated the effect of Sn micro-alloying on recrystallization nucleation and growth processes of ferritic stainless steels. The as-received hot rolled sheets were cold rolled up to 80% reduction and then annealed at 740-880 °C for 5 min. The cold rolling and recrystallization microstructures and micro-textures of Sn-containing and Sn-free ferritic stainless steels were all determined by electron backscatter diffraction. Our Results show that Sn micro-alloying has important effects on recrystallization nucleation and growth processes of ferritic stainless steels. Sn micro-alloying conduces to grain fragmentation in the deformation band, more fragmented grains are existed in Sn-containing cold rolled sheets, which provides more sites for recrystallization nucleation. Sn micro-alloying also promotes recrystallization process and inhibits the growth of recrystallized grains. The recrystallization nucleation and growth mechanism of Sn-containing and Sn-free ferritic stainless steels are both characterized by orientation nucleation and selective growth, but Sn micro-alloying promotes the formation of γ-oriented grains. Furthermore, Sn micro-alloying contributes to the formation of Σ13b CSL boundaries and homogeneous γ-fiber texture. Combining the results of microstructure and micro-texture, the formability of Sn-containing ferritic stainless steels will be improved to some extent.

Mechanism of secondary recrystallization of Goss grains in grain-oriented electrical steel

NASA Astrophysics Data System (ADS)

Hayakawa, Yasuyuki

2017-12-01

Since its invention by Goss in 1934, grain-oriented (GO) electrical steel has been widely used as a core material in transformers. GO exhibits a grain size of over several millimeters attained by secondary recrystallization during high-temperature final batch annealing. In addition to the unusually large grain size, the crystal direction in the rolling direction is aligned with <001>, which is the easy magnetization axis of α-iron. Secondary recrystallization is the phenomenon in which a certain very small number of {110}<001> (Goss) grains grow selectively (about one in 106 primary grains) at the expense of many other primary recrystallized grains. The question of why the Goss orientation is exclusively selected during secondary recrystallization has long been a main research subject in this field. The general criterion for secondary recrystallization is a small and uniform primary grain size, which is achieved through the inhibition of normal grain growth by fine precipitates called inhibitors. This paper describes several conceivable mechanisms of secondary recrystallization of Goss grains mainly based on the selective growth model.

Mechanism of secondary recrystallization of Goss grains in grain-oriented electrical steel

PubMed Central

Hayakawa, Yasuyuki

2017-01-01

Abstract Since its invention by Goss in 1934, grain-oriented (GO) electrical steel has been widely used as a core material in transformers. GO exhibits a grain size of over several millimeters attained by secondary recrystallization during high-temperature final batch annealing. In addition to the unusually large grain size, the crystal direction in the rolling direction is aligned with <001>, which is the easy magnetization axis of α-iron. Secondary recrystallization is the phenomenon in which a certain very small number of {110}<001> (Goss) grains grow selectively (about one in 106 primary grains) at the expense of many other primary recrystallized grains. The question of why the Goss orientation is exclusively selected during secondary recrystallization has long been a main research subject in this field. The general criterion for secondary recrystallization is a small and uniform primary grain size, which is achieved through the inhibition of normal grain growth by fine precipitates called inhibitors. This paper describes several conceivable mechanisms of secondary recrystallization of Goss grains mainly based on the selective growth model. PMID:28804524

Evaluation of the recrystallization kinetics of hot-melt extruded polymeric solid dispersions using an improved Avrami equation

PubMed Central

Feng, Xin; Ye, Xingyou; Park, Jun-Bom; Lu, Wenli; Morott, Joe; Beissner, Brad; Lian, Zhuoyang John; Pinto, Elanor; Bi, Vivian; Porter, Stu; Durig, Tom; Majumdar, Soumyajit; Repka, Michael A.

2017-01-01

The recrystallization of an amorphous drug in a solid dispersion system could lead to a loss in the drug solubility and bioavailability. The primary objective of the current research was to use an improved kinetic model to evaluate the recrystallization kinetics of amorphous structures and to further understand the factors influencing the physical stability of amorphous solid dispersions. Amorphous solid dispersions of fenofibrate with different molecular weights of hydroxypropylcellulose, HPC (Klucel™ LF, EF, ELF) were prepared utilizing hot-melt extrusion technology. Differential scanning calorimetry was utilized to quantitatively analyze the extent of recrystallization in the samples stored at different temperatures and relative humidity (RH) conditions. The experimental data were fitted into the improved kinetics model of a modified Avrami equation to calculate the recrystallization rate constants. Klucel LF, the largest molecular weight among the HPCs used, demonstrated the greatest inhibition of fenofibrate recrystallization. Additionally, the recrystallization rate (k) decreased with increasing polymer content, however exponentially increased with higher temperature. Also k increased linearly rather than exponentially over the range of RH studied. PMID:25224341

Investigating the principles of recrystallization from glyceride melts.

PubMed

Windbergs, Maike; Strachan, Clare J; Kleinebudde, Peter

2009-01-01

Different lipids were melted and resolidified as model systems to gain deeper insight into the principles of recrystallization processes in lipid-based dosage forms. Solid-state characterization was performed on the samples with differential scanning calorimetry and X-ray powder diffraction. Several recrystallization processes could be identified during storage of the lipid layers. Pure triglycerides that generally crystallize to the metastable alpha-form from the melt followed by a recrystallization process to the stable beta-form with time showed a chain-length-dependent behavior during storage. With increasing chain length, the recrystallization to the stable beta-form was decelerated. Partial glycerides exhibited a more complex recrystallization behavior due to the fact that these substances are less homogenous. Mixtures of a long-chain triglyceride and a partial glyceride showed evidence of some interaction between the two components as the partial glyceride hindered the recrystallization of the triglyceride to the stable beta-form. In addition, the extent of this phenomenon depended on the amount of partial glyceride in the mixture. Based on these results, changes in solid dosage forms based on glycerides during processing and storage can be better understood.

Evaluation of the recrystallization kinetics of hot-melt extruded polymeric solid dispersions using an improved Avrami equation.

PubMed

Feng, Xin; Ye, Xingyou; Park, Jun-Bom; Lu, Wenli; Morott, Joe; Beissner, Brad; Lian, Zhuoyang John; Pinto, Elanor; Bi, Vivian; Porter, Stu; Durig, Tom; Majumdar, Soumyajit; Repka, Michael A

2015-01-01

The recrystallization of an amorphous drug in a solid dispersion system could lead to a loss in the drug solubility and bioavailability. The primary objective of the current research was to use an improved kinetic model to evaluate the recrystallization kinetics of amorphous structures and to further understand the factors influencing the physical stability of amorphous solid dispersions. Amorphous solid dispersions of fenofibrate with different molecular weights of hydroxypropylcellulose, HPC (Klucel™ LF, EF, ELF) were prepared utilizing hot-melt extrusion technology. Differential scanning calorimetry was utilized to quantitatively analyze the extent of recrystallization in the samples stored at different temperatures and relative humidity (RH) conditions. The experimental data were fitted into the improved kinetics model of a modified Avrami equation to calculate the recrystallization rate constants. Klucel LF, the largest molecular weight among the HPCs used, demonstrated the greatest inhibition of fenofibrate recrystallization. Additionally, the recrystallization rate (k) decreased with increasing polymer content, however exponentially increased with higher temperature. Also k increased linearly rather than exponentially over the range of RH studied.

Mechanism of secondary recrystallization of Goss grains in grain-oriented electrical steel.

PubMed

Hayakawa, Yasuyuki

2017-01-01

Since its invention by Goss in 1934, grain-oriented (GO) electrical steel has been widely used as a core material in transformers. GO exhibits a grain size of over several millimeters attained by secondary recrystallization during high-temperature final batch annealing. In addition to the unusually large grain size, the crystal direction in the rolling direction is aligned with <001>, which is the easy magnetization axis of α-iron. Secondary recrystallization is the phenomenon in which a certain very small number of {110}<001> (Goss) grains grow selectively (about one in 10 6 primary grains) at the expense of many other primary recrystallized grains. The question of why the Goss orientation is exclusively selected during secondary recrystallization has long been a main research subject in this field. The general criterion for secondary recrystallization is a small and uniform primary grain size, which is achieved through the inhibition of normal grain growth by fine precipitates called inhibitors. This paper describes several conceivable mechanisms of secondary recrystallization of Goss grains mainly based on the selective growth model.

Texture transition in experimentally deformed quartzite

NASA Astrophysics Data System (ADS)

Kilian, Rüdiger; Heilbronner, Renée

2017-04-01

Quartz crystallographic preferred orientations (textures), most commonly presented in the form of pole figures, are often used to infer deformation processes or conditions - despite the fact that we still do not understand fully how the different types of texture are generated. Here, we re-analyse experimentally deformed Black Hills Quartzite using EBSD maps. Samples were deformed in general shear in the dislocation creep regimes 1 to 3 at temperatures ranging from 875 to 915°C, constant shear strain rates of 1e-5/s (Heilbronner & Tullis, 2006), and resulting flow stresses of (600 MPa ≥ Tau ≥ 100 MPa). Already at low strain, a strong alignment of <11-20> in the shear plane and of {10-11} with the maximum principal stress direction is observed. [0001] pole figures of recrystallized grains in regime 1 exhibit a peripheral maximum, roughly perpendicular to the shear plane while in regime 3 two elongated maxima are formed very close to the kinematic y-direction. Regime 2 shows a mixture of these two texture types. In regime 1, dynamic recrystallization is dominated by bulging recrystallization (nucleation of new grains), and in regime 3 by subgrain rotation recrystallization. In regime 2, again a mixture of regime 1 and 3 can be observed. Texture strength increases with the amount of crystal plastic deformation and is generally the lowest for the texture type with peripheral [0001]. During crystal plastic deformation [0001] rotate towards the kinematic y-direction. The coexistence and transition from one to the other texture type is suggested to result from two different texture-forming processes. The first process is thought to be crystal plasticity by glide on various <11-20> slip systems and associated rotation of the crystal lattice, with the attractor of [0001] close to - but not exactly parallel to - the kinematic y-direction. The second process is suggested to be the growth of oriented grains during bulging recrystallization and associated (fracturing and) grain boundary sliding. The contribution of both processes results in the final texture type. The most distinctive difference of the three suites of experiments is the flow stress, decreasing from regime 1 to regime 3. Since the temperature and strain rate differences in these experiments are very small indeed, it is argued that the two end-member texture types do not indicate a temperature dependence of a slip system. Rather, they seem to depend on the flow stress and hence on the recrystallization mechanism. It remains to be tested whether this relation also holds in natural quartz mylonites where those texture types are frequently observed.

Structure and mechanical properties of a high-carbon steel subjected to severe deformation

NASA Astrophysics Data System (ADS)

Gorkunov, E. S.; Zadvorkin, S. M.; Goruleva, L. S.; Makarov, A. V.; Pecherkina, N. L.

2017-10-01

The structure and mechanical properties of a high-carbon eutectic steel subjected to the cold plastic deformation by hydrostatic extrusion in a wide range of true strain have been studied. Using scanning and transmission electron microscopy, it has been shown that the formation of cellular, fragmented, and submicrocrystalline structures occurs in the ferritic constituent of the pearlite structure of the steel upon extrusion. This is a consequence of the occurrence of dynamic recovery and continuous dynamic and post-dynamic recrystallization, which cause a decrease in the density of free dislocations at the true strain of more than 1.62. The partial dissolution of the carbide phase is also observed. It has been found that, at a true strain of up to 0.81, the strength properties of the investigated steel are determined mainly by subgrain, dislocation, and precipitation mechanisms of the strengthening; in the deformation range of 0.81-1.62, the role of the grainboundary strengthening increases. At strains above 1.62, grain-boundary strengthening is a prevailing mechanism in the formation of the level of strength properties of the extruded U8A steel. The ultimate tensile strength and yield stress over the entire strain range only uniquely correlate with the density of highangle boundaries; the dependences of the strength characteristics on other structural parameters are not monotonic.

Effect of controlling recrystallization from the melt on the residual stress and structural properties of the Silica-clad Ge core fiber

NASA Astrophysics Data System (ADS)

Zhao, Ziwen; Cheng, Xueli; He, Ting; Xue, Fei; Zhang, Wei; Chen, Na; Wen, Jianxiang; Zeng, Xianglong; Wang, Tingyun

2017-09-01

Effect of controlling recrystallization from the melt (1000 °C) on the residual stress and structural properties of a Ge core fiber via molten core drawing (MCD) method is investigated. Ge core fibers is investigated using Raman spectroscopy, scanning electron microscope (SEM), and X-ray diffraction (XRD). Compared with the as-drawn Ge fiber, the Raman peak of the recrystallized Ge fiber shift from 300 cm-1 to 300.6 cm-1 and full width at half maximum (FWHM) decreased from 5.36 cm-1 to 4.48 cm-1. The Ge crystal grains which sizes are of 200-600 nm were formed during the process of recrystallization; the XRD peak of (1 1 1) plane is observed after recrystallization. These results show that controlling recrystallization allows the release of the thermal stress, and improvement of the crystal quality of Ge core.

Microstructure heterogeneity after the ECAP process and its influence on recrystallization in aluminium

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wronski, S., E-mail: wronski@fis.agh.edu.pl; Tarasiuk, J., E-mail: tarasiuk@ftj.agh.edu.pl; Bacroix, B., E-mail: brigitte.bacroix@univ-paris13.fr

The main purpose of the present work is to describe the qualitative and quantitative behaviours of aluminium during high strain plastic deformation and the effect of deformation on the subsequent recrystallization process. An Electron Backscatter Diffraction analysis of aluminium after the Equal channel angular pressing (ECAP) and recrystallization process is presented. In order to do this, several topological maps are measured for samples processed by 4 and 8 passes and recrystallized. The processing was conducted with route C. For all samples, distributions of grain size, misorientation, image quality factor (IQ) and texture were preceded and then analysed in some detail.more » - Highlights: ► Describe the microstructure fragmentation in aluminum. ► High strain plastic deformation and effect of deformation on recrystallization. ► The microstructure fragmentation and its influence on recrystallization. ► Image quality factor and misorientation characteristics are examined using EBSD.« less

Finite element simulation of texture evolution and Swift effect in NiAl under torsion

NASA Astrophysics Data System (ADS)

Böhlke, Thomas; Glüge, Rainer; Klöden, Burghardt; Skrotzki, Werner; Bertram, Albrecht

2007-09-01

The texture evolution and the Swift effect in NiAl under torsion at 727 °C are studied by finite element simulations for two different initial textures. The material behaviour is modelled by an elastic-viscoplastic Taylor model. In order to overcome the well-known shortcomings of Taylor's approach, the texture evolution is also investigated by a representative volume element (RVE) with periodic boundary conditions and a compatible microstructure at the opposite faces of the RVE. Such a representative volume element takes into account the grain morphology and the grain interaction. The numerical results are compared with experimental data. It is shown that the modelling of a finite element based RVE leads to a better prediction of the final textures. However, the texture evolution path is not accounted for correctly. The simulated Swift effect depends much more on the initial orientation distribution than observed in experiment. Deviations between simulation and experiment may be due to continuous dynamic recrystallization.

Quantification of Microtexture at Weld Nugget of Friction Stir-Welded Carbon Steel

NASA Astrophysics Data System (ADS)

Husain, Md M.; Sarkar, R.; Pal, T. K.; Ghosh, M.; Prabhu, N.

2017-05-01

Friction stir welding of C-Mn steel was carried out under 800-1400 rpm tool rotation. Tool traversing speed of 50 mm/min remained same for all joints. Effect of thermal state and deformation on texture and microstructure at weld nugget was investigated. Weld nugget consisted of ferrite + bainite/Widmanstatten ferrite with different matrix grain sizes depending on peak temperature. A texture around ( ϕ 2 = 0°, φ = 30°, ϕ 2 = 45°) was developed at weld nugget. Grain boundary misorientation at weld nugget indicated that continuous dynamic recrystallization influenced the development of fine equiaxed grain structure. Pole figures and orientation distribution function were used to determine crystallographic texture at weld nugget and base metal. Shear texture components D1, D2 and F were present at weld nugget. D1 shear texture was more prominent among all. Large number of high-angle grain boundaries ( 60-70%) was observed at weld nugget and was the resultant of accumulation of high amount of dislocation, followed by subgrain formation.

Modifications in the AA5083 Johnson-Cook Material Model for Use in Friction Stir Welding Computational Analyses

NASA Astrophysics Data System (ADS)

Grujicic, M.; Pandurangan, B.; Yen, C.-F.; Cheeseman, B. A.

2012-11-01

Johnson-Cook strength material model is frequently used in finite-element analyses of various manufacturing processes involving plastic deformation of metallic materials. The main attraction to this model arises from its mathematical simplicity and its ability to capture the first-order metal-working effects (e.g., those associated with the influence of plastic deformation, rate of deformation, and the attendant temperature). However, this model displays serious shortcomings when used in the engineering analyses of various hot-working processes (i.e., those utilizing temperatures higher than the material recrystallization temperature). These shortcomings are related to the fact that microstructural changes involving: (i) irreversible decrease in the dislocation density due to the operation of annealing/recrystallization processes; (ii) increase in grain-size due to high-temperature exposure; and (iii) dynamic-recrystallization-induced grain refinement are not accounted for by the model. In this study, an attempt is made to combine the basic physical-metallurgy principles with the associated kinetics relations to properly modify the Johnson-Cook material model, so that the model can be used in the analyses of metal hot-working and joining processes. The model is next used to help establish relationships between process parameters, material microstructure and properties in friction stir welding welds of AA5083 (a non-age-hardenable, solid-solution strengthened, strain-hardened/stabilized Al-Mg-Mn alloy).

Unraveling Recrystallization Mechanisms Governing Texture Development from Rare-Earth Element Additions to Magnesium

NASA Astrophysics Data System (ADS)

Imandoust, Aidin; Barrett, Christopher D.; Al-Samman, Talal; Tschopp, Mark A.; Essadiqi, Elhachmi; Hort, Norbert; El Kadiri, Haitham

2018-03-01

The origin of texture components often associated with rare-earth element (REE) additions in wrought magnesium alloys is a long-standing problem in magnesium technology. While their influence on the texture is unquestionable, it is not yet clear why certain texture components, such as < 11\\bar{2}1 > ||{extrusion}{direction}, are favored over other components typically observed in traditional magnesium alloys. The objective of this research is to identify the mechanisms accountable for these RE textures during early stages of recrystallization. Electron backscattered diffraction and transmission electron microscopy analyses reveal that REEs in zinc-containing magnesium alloys corroborate discontinuous dynamic recrystallization. REEs promote isotropic growth for all nuclei generated through the bulging mechanism. During nucleation, the effect of REEs on orientation selection was explained by the diversified activity of both < 10\\bar{1}0 > and [0001] Taylor axes in the same grain with a marked preference for [0001] rotations to occur first. During nuclei growth, no growth preference was observed when sufficient REEs are added in the zinc-containing magnesium alloys, instead isotropic nuclei growth across all grain orientations occurs. This phenomenon is attributed to REEs segregating to grain boundaries (GBs), in agreement with prior computational and theoretical results (Barrett et al., Scripta Mater 146:46-50, 2018) that show a more isotropic GB energy and mobility after segregation.

Stress Dependence of Microstructures in Experimentally Deformed Calcite

NASA Astrophysics Data System (ADS)

Platt, J. P.; De Bresser, J. H. P.

2017-12-01

Measurements of dynamically recrystallized grain size (Dr), subgrain size (Sg), minimum bulge size (Blg), and the maximum scale length for surface-energy driven grain-boundary migration (γGBM) in experimentally deformed Cararra marble help define the dependence of these microstructural features on stress and temperature. Measurements were made optically on ultra-thin sections in order to allow these features to be defined during measurement on the basis of microstructural setting and geometry. Taken together with previously published data Dr defines a paleopiezometer with a stress exponent of -1.09. There is no discernible temperature dependence over the 500°C temperature range of the experiments. Recrystallization occured mainly by bulging and subgrain rotation, and the two processes operated together, so that it is not possible to separate grains nucleated by the two mechanisms. Sg and Dr measured in the same samples are closely similar in size, suggesting that new grains do not grow significantly after nucleation, and that subgrain size is likely to be the primary control on recrystallized grain size. Blg and γGBM measured on each sample define a relationship to stress with an exponent of approximately -1.6, which helps define the boundary in stress - grain-size space between a region of dominant strain-energy-driven grain-boundary migration at high stress, from a region of dominant surface-energy-driven grain-boundary migration at low stress.

Diverse dissolution-recrystallization structural transformations and sequential Förster resonance energy transfer behavior of a luminescent porous Cd-MOF.

PubMed

Cao, Li-Hui; Li, Hai-Yang; Xu, Hong; Wei, Yong-Li; Zang, Shuang-Quan

2017-09-12

Metal-organic frameworks (MOFs) with light-harvesting building blocks provide an excellent platform to study energy transfer in networks with well-defined structures. Here, we report the synthesis, dissolution-recrystallization structural transformation (DRST) and the Förster resonance energy transfer (FRET) properties of a 2D microporous MOF {[Cd 2 (L 1 ) 3 (Hdabco) 2 ]·5DMAc·6H 2 O} n (Cd-MOF, 1). Complex 1 can be dissolved in water and three other products with different dimensions recrystallized from the aqueous solution under diverse reaction conditions were obtained. Due to the porosity and excellent blue luminescence properties of complex 1, we also studied the FRET process between 1 and guest dyes. Two distinct organic dye molecules viz., acridine orange (AO) and rhodamine B (RhB), are encapsulated in 1 which has honeycomb-type nanochannels, and their influence on fluorescence emission has also been studied. The microporous complex 1 in (AO + RhB)@1 serves as an energy funnel that harvests high energy excitation and channels it onto AO and then onto RhB. The steady-state fluorescence and fluorescence dynamics of emission reveal successfully the process of stepwise vectorial energy transfer. Therefore, MOFs could be a class of promising host materials to be further explored in the field of energy transfer between MOF-host and organic guests.

Strain induced grain boundary migration effects on grain growth of an austenitic stainless steel during static and metadynamic recrystallization

DOE Office of Scientific and Technical Information (OSTI.GOV)

Paggi, A., E-mail: alpaggi@tenaris.com; Angella, G.; Donnini, R.

Static and metadynamic recrystallization of an AISI 304L austenitic stainless steel was investigated at 1100 °C and 10{sup −} {sup 2} s{sup −} {sup 1} strain rate. The kinetics of recrystallization was determined through double hit compression tests. Two strain levels were selected for the first compression hit: ε{sub f} = 0.15 for static recrystallization (SRX) and 0.25 for metadynamic recrystallization (MDRX). Both the as-deformed and the recrystallized microstructures were investigated through optical microscopy and electron back-scattered diffraction (EBSD) technique. During deformation, strain induced grain boundary migration appeared to be significant, producing a square-like grain boundary structure aligned along themore » directions of the maximum shear stresses in compression. EBSD analysis revealed to be as a fundamental technique that the dislocation density was distributed heterogeneously in the deformed grains. Grain growth driven by surface energy reduction was also investigated, finding that it was too slow to explain the experimental data. Based on microstructural results, it was concluded that saturation of the nucleation sites occurred in the first stages of recrystallization, while grain growth driven by strain induced grain boundary migration (SIGBM) dominated the subsequent stages. - Highlights: • Recrystallization behavior of a stainless steel was investigated at 1100 °C. • EBSD revealed that the dislocation density distribution was heterogeneous during deformation. • Saturation of nucleation sites occurred in the first stages of recrystallization. • Strain induced grain boundary migration (SIGBM) effects were significant. • Grain growth driven by SIGBM dominated the subsequent stages.« less

Gelatinization and freeze-concentration effects on recrystallization in corn and potato starch gels.

PubMed

Ronda, Felicidad; Roos, Yrjö H

2008-04-07

Freeze-concentration of starch gels was controlled by temperature and gelatinization with glucose and lactose. The aim of the study was to evaluate the effects of freezing temperature and gel composition on starch recrystallization behaviour of corn and potato starch gels (water content 70%, w/w) in water or glucose or lactose (10%, w/w) solutions. Starch gels were obtained by heating in differential scanning calorimetry (DSC). Samples of starch gels were frozen at -10 degrees C, -20 degrees C and -30 degrees C for 24h and, after thawing, stored at +2 degrees C for 0, 1, 2, 4 and 8 days. The extent of starch recrystallization was taken from the enthalpy of melting of the recrystallized starch by DSC. Freezing temperatures, glucose, lactose and the origin of the starch affected the recrystallization behaviour greatly. The recrystallization of amorphous starch during storage was enhanced by freeze-concentration of gels at temperatures above T'(m). Molecular mobility was enhanced by unfrozen water and consequently molecular rearrangements for nucleation could take place. Further storage at a higher temperature enhanced the growth and the maturation of crystals. In particular, glucose decreased the T'(m) of the gels and consequently lower freezing temperatures were needed to reduce enhanced recrystallization during storage. Freeze-concentration temperatures also showed a significant effect on the size and the perfection of crystals formed in starch recrystallization.

Ultrasonic Determination Of Recrystallization

NASA Technical Reports Server (NTRS)

Generazio, Edward R.

1988-01-01

State of recrystallization identified. Measurement of ultrasonic attenuation shows promise as means of detecting recrystallization in metal. Technique applicable to real-time acoustic monitoring of thermomechanical treatments. Starting with work-hardened material, one ultrasonically determines effect of annealing, using correlation between ultrasonic attenuation and temperature.

Synthesis and deformation of a Ti doped quartz aggregate

NASA Astrophysics Data System (ADS)

Nachlas, William O.; Hirth, Greg; Teyssier, Christian; Whitney, Donna L.; Zimmerman, Mark

2013-04-01

A primary advantage of studying mylonites for thermobarometric reconstructions of tectonic events is that it enables direct comparison of P-T estimates with the mechanics of quartz deformation. Quartz is a common phase in crustal mylonites and is a particularly sensitive recorder of metamorphic and rheologic conditions in shear zones, owing to its responsiveness to dynamic recrystallization, involvement in metamorphic reaction, and propensity for dissolution and precipitation. The signature of its trace element chemistry, particularly Ti, can reflect involvement from each of these processes. The concentration of Ti in mylonites is typically heterogeneous at the thin section scale, providing a rich record of the different factors that influence the incorporation of Ti in quartz. Observations of quartz in deformed mylonite and undeformed protolith from an extensional shear zone in the North American Cordillera (Shuswap Complex, Canada) show that an originally uniform Ti distribution was modified during deformation to form zoned crystals in which the core preserves a higher Ti concentration than the rim. The zoned Ti concentration likely records a continuum of deformation conditions during extension-related exhumation, and this presents a challenge in resolving the effect of deformation on the equilibrium solubility of Ti in quartz in natural settings. By conducting deformation experiments on synthetic quartz aggregates with known Ti concentration at a constant, elevated temperature and pressure under high strain conditions, we investigate the influence of progressive dynamic recrystallization on Ti solubility in quartz. This study applies a novel doping technique that enables the synthesis of a large population of quartz crystals with a precisely controlled Ti concentration and distribution. This produces a sample that most closely replicates the protolith of extensional shear zones that typically develop under retrograde conditions. This strategy can be used to generate the equilibrium concentration predicted by previous solubility calibrations for selected P-T conditions. Experiments were performed using a shear assembly to deform quartz samples to high shear strain in dislocation creep at constant temperature, pressure, and strain rate for 24, 48, and 72 h with and without the addition of 0.1 wt% H2O. Experiments were also run under hydrostatic conditions for equivalent lengths of time for comparison with deformed samples. Experimental specimens were prepared as a two layer sample with a doped half and an undoped half to study Ti mobility during deformation. Experimental samples are analyzed with EMPA and SIMS to determine the Ti concentration of quartz in the sample, SEM-CL to observe the distribution of Ti in quartz grains, and SEM-EBSD to evaluate crystallographic fabrics and grain size. Results suggest that the duration of dynamic recrystallization influences the final Ti concentration, implying the importance of kinetics and diffusion even at the elevated temperatures of the experiments. Water content affects Ti concentration, potentially owing to the importance of point defect concentration on the solubility of Ti in quartz. Furthermore, recrystallized grain size shows a dependence on Ti concentration, as samples doped at supersaturated levels recrystallize with finer grain sizes relative to undoped samples. This suggests that exceeding the equilibrium solubility of Ti in quartz may pin grain boundary migration. The ultimate expression of Ti supersaturation in quartz is strain-induced rutilation and the progressive rotation and boudinage of exsolved rutile needles.

A texture-component Avrami model for predicting recrystallization textures, kinetics and grain size

NASA Astrophysics Data System (ADS)

Raabe, Dierk

2007-03-01

The study presents an analytical model for predicting crystallographic textures and the final grain size during primary static recrystallization of metals using texture components. The kinetics is formulated as a matrix variant of the Johnson-Mehl-Avrami-Kolmogorov equation. The matrix form is required since the kinetic and crystallographic evolution of the microstructure is described in terms of a limited set of growing (recrystallizing) and swept (deformed) texture components. The number of components required (5-10) defines the order of the matrix since the kinetic coupling occurs between all recrystallizing and all deformed components. Each such couple is characterized by corresponding values for the nucleation energy and grain boundary mobility. The values of these parameters can be obtained by analytical or numerical coarse graining according to a renormalization scheme which replaces many individual grains which grow via recrystallization in a deformed texture component by a single equivalent recrystallization texture component or by fitting to experimental data. Each deformed component is further characterized by an average stored deformation energy. Each element of the kinetic matrix, reflecting one of the possible couplings between a deformed and a recrystallizing texture component, is then derived in each time step by a set of two differential equations. The first equation describes the thermally activated nucleation and growth processes for the expanded (free) volume for a particular couple of a deformed and a recrystallizing texture component and the second equation is used for calculating the constrained (real) volume for that couple which corrects the free volume for those portions of the deformation component which were already swept. The new method is particularly developed for the fast and physically based process simulation of recrystallization textures with respect to processing. The present paper introduces the method and applies it to the primary recrystallization of low carbon steels.

Mesoscale Modeling of Dynamic Compression of Boron Carbide Polycrystals

DTIC Science & Technology

2013-05-01

reported later. Recrystallization has not been reported in the literature and is precluded by the model, meaning : 0 →1 is irreversible. Following...average HEL, above which a measurable strength loss is evident (Vogler et al., 2004), though amorphization has not been definitively proven to cause... definition (A.7) is exact when ı2 E→ 0 (Clayton, 2012). This criterion agrees exactly with that for classical stability under hydrostatic loading

Comparisons of Different Models on Dynamic Recrystallization of Plate during Asymmetrical Shear Rolling

PubMed Central

Zhang, Tao; Li, Lei; Lu, Shi-Hong; Gong, Hai; Wu, Yun-Xin

2018-01-01

Asymmetrical shear rolling with velocity asymmetry and geometry asymmetry is beneficial to enlarge deformation and refine grain size at the center of the thick plate compared to conventional symmetrical rolling. Dynamic recrystallization (DRX) plays a vital role in grain refinement during hot deformation. Finite element models (FEM) coupled with microstructure evolution models and cellular automata models (CA) are established to study the microstructure evolution of plate during asymmetrical shear rolling. The results show that a larger DRX fraction and a smaller average grain size can be obtained at the lower layer of the plate. The DRX fraction at the lower part increases with the ascending speed ratio, while that at upper part decreases. With the increase of the offset distance, the DRX fraction slightly decreases for the whole thickness of the plate. The differences in the DRX fraction and average grain size between the upper and lower surfaces increase with the ascending speed ratio; however, it varies little with the change of the speed ratio. Experiments are conducted and the CA models have a higher accuracy than FEM models as the grain morphology, DRX nuclei, and grain growth are taken into consideration in CA models, which are more similar to the actual DRX process during hot deformation. PMID:29342080

Structure/property (constitutive and dynamic strength/damage) characterization of additively manufactured 316L SS

NASA Astrophysics Data System (ADS)

Gray, G. T., III; Livescu, V.; Rigg, P. A.; Trujillo, C. P.; Cady, C. M.; Chen, S. R.; Carpenter, J. S.; Lienert, T. J.; Fensin, S.

2015-09-01

For additive manufacturing (AM), the certification and qualification paradigm needs to evolve as there exists no "ASTM-type" additive manufacturing certified process or AM-material produced specifications. Accordingly, utilization of AM materials to meet engineering applications requires quantification of the constitutive properties of these evolving materials in comparison to conventionally-manufactured metals and alloys. Cylinders of 316L SS were produced using a LENS MR-7 laser additive manufacturing system from Optomec (Albuquerque, NM) equipped with a 1kW Yb-fiber laser. The microstructure of the AM-316L SS is detailed in both the as-built condition and following heat-treatments designed to obtain full recrystallization. The constitutive behavior as a function of strain rate and temperature is presented and compared to that of nominal annealed wrought 316L SS plate. The dynamic damage evolution and failure response of all three materials was probed using flyer-plate impact driven spallation experiments at a peak stress of 4.5 GPa to examine incipient spallation response. The spall strength of AM-produced 316L SS was found to be very similar for the peak shock stress studied to that of annealed wrought or AM-316L SS following recrystallization. The damage evolution as a function of microstructure was characterized using optical metallography.

Comparisons of Different Models on Dynamic Recrystallization of Plate during Asymmetrical Shear Rolling.

PubMed

Zhang, Tao; Li, Lei; Lu, Shi-Hong; Gong, Hai; Wu, Yun-Xin

2018-01-17

Asymmetrical shear rolling with velocity asymmetry and geometry asymmetry is beneficial to enlarge deformation and refine grain size at the center of the thick plate compared to conventional symmetrical rolling. Dynamic recrystallization (DRX) plays a vital role in grain refinement during hot deformation. Finite element models (FEM) coupled with microstructure evolution models and cellular automata models (CA) are established to study the microstructure evolution of plate during asymmetrical shear rolling. The results show that a larger DRX fraction and a smaller average grain size can be obtained at the lower layer of the plate. The DRX fraction at the lower part increases with the ascending speed ratio, while that at upper part decreases. With the increase of the offset distance, the DRX fraction slightly decreases for the whole thickness of the plate. The differences in the DRX fraction and average grain size between the upper and lower surfaces increase with the ascending speed ratio; however, it varies little with the change of the speed ratio. Experiments are conducted and the CA models have a higher accuracy than FEM models as the grain morphology, DRX nuclei, and grain growth are taken into consideration in CA models, which are more similar to the actual DRX process during hot deformation.

An improved kinetics approach to describe the physical stability of amorphous solid dispersions.

PubMed

Yang, Jiao; Grey, Kristin; Doney, John

2010-01-15

The recrystallization of amorphous solid dispersions may lead to a loss in the dissolution rate, and consequently reduce bioavailability. The purpose of this work is to understand factors governing the recrystallization of amorphous drug-polymer solid dispersions, and develop a kinetics model capable of accurately predicting their physical stability. Recrystallization kinetics was measured using differential scanning calorimetry for initially amorphous efavirenz-polyvinylpyrrolidone solid dispersions stored at controlled temperature and relative humidity. The experimental measurements were fitted by a new kinetic model to estimate the recrystallization rate constant and microscopic geometry of crystal growth. The new kinetics model was used to illustrate the governing factors of amorphous solid dispersions stability. Temperature was found to affect efavirenz recrystallization in an Arrhenius manner, while recrystallization rate constant was shown to increase linearly with relative humidity. Polymer content tremendously inhibited the recrystallization process by increasing the crystallization activation energy and decreasing the equilibrium crystallinity. The new kinetic model was validated by the good agreement between model fits and experiment measurements. A small increase in polyvinylpyrrolidone resulted in substantial stability enhancements of efavirenz amorphous solid dispersion. The new established kinetics model provided more accurate predictions than the Avrami equation.

Pairing Heterocyclic Cations with closo-Icosahedral Borane and Carborane Anions, II: Benchtop Alternative Synthetic Methodologies for Binary Triazolium and Tetrazolium Salts with Significant Water Solubility (POSTPRINT)

DTIC Science & Technology

2012-01-01

interesting property, eutectic melting-point depression. Recrystallization of ternary salts 12–14 was not attempted because of a concern that a cation... recrystallization solvent mixture for these powders, and while some individual successes resulted, a general efficient solvent system for all salt...product recrystallizations could not be found. So, rather than recrystallizing each individual adduct, spectroscopic examination of the amorphous solids was

Ultrasonic determination of recrystallization

NASA Technical Reports Server (NTRS)

Generazio, E. R.

1986-01-01

Ultrasonic attenuation was measured for cold worked Nickel 200 samples annealed at increasing temperatures. Localized dislocation density variations, crystalline order and colume percent of recrystallized phase were determined over the anneal temperature range using transmission electron microscopy, X-ray diffraction, and metallurgy. The exponent of the frequency dependence of the attenuation was found to be a key variable relating ultrasonic attenuation to the thermal kinetics of the recrystallization process. Identification of this key variable allows for the ultrasonic determination of onset, degree, and completion of recrystallization.

Feedbacks Between Deformation and Fluid Flow in Mantle Shear Zones from Zabargad, Red Sea

NASA Astrophysics Data System (ADS)

Tommasi, A.; Boudier, F. I.; Vauchez, A. R.; Zaderatzky, M.

2016-12-01

Peridotites in the Zabargad island, Red Sea, record different stages of lithospheric thinning and asthenospheric upwelling during rifting. Field mapping highlights a pervasive high-temperature NW-SE, subvertical foliation with lineations pluning 50°NW. This foliation is overprinted by a series of lower-temperature mylonitic zones with slightly oblique foliations and subhorizontal lineations, which record progressive strain localization under retrogressive conditions during the final exhumation of the peridotites (Nicolas and Boudier, JGR 1987). We performed a petrostructural study of ca. 50 samples collected by A. Nicolas and F. Boudier in the 80s from the different deformation facies. This study highlights: (1) a rather pervasive, but highly heterogeneous distribution of the LT deformation and (2) a feedback between deformation and fluid flow. The HT deformation is recorded in medium grained plagioclase- and spinel-peridotites by a homogeneous foliation and lineation marked by a shape-preferred orientation of plagioclase and olivine and a consistent CPO of all major-rock forming phases. The LT temperature deformation results in dynamic recrystallization of olivine leading to a marked grain size reduction by dynamic recrystallization of olivine, remobilization of orthopyroxene by dissolution-precipitation, and crystallization of amphibole. Increasing finite strain is recorded by the increase in the volume of the fine-grained material and of the amphibole proportion. The latter may attain in totally recrystallized cm-wide ultramylonite bands up to 30%. This together with the strong amphibole SPO and CPO corroborate fluid focusing and enhanced reaction rates into active shear zones. In the LT shear zones we also document: (1) changes in the olivine CPO, indicating changes in the dominant slip system and (2) unusual orthopyroxene CPO, which we interpret as due to oriented crystallization. Static replacement of pyroxenes by amphibole with no associated LT deformation is also observed indicating that the presence of fluids does not suffice to trigger strain localization.

Microstructural Evolution of HSLA ISO 3183 X80M (API 5L X80) Friction Stir Welded Joints

NASA Astrophysics Data System (ADS)

Hermenegildo, Tahiana F. C.; Santos, Tiago F. A.; Torres, Edwar A.; Afonso, Conrado R. M.; Ramirez, Antonio J.

2018-03-01

Evaluation was made of friction stir welded joints, identifying conditions that resulted in satisfactory welded joints free from defects and with microstructural characteristics that provided good mechanical properties. Microstructural characterization and cooling curve analysis of the joints with lower and higher heat inputs evidenced deformation below and above the non-recrystallization temperature (Tnr) and dynamic recrystallization during microstructural evolution. Microscopy analyses showed acicular ferrite, bainitic ferrite, and coalesced bainite microstructures in the stir zone of the cold weld (lower heat input), while the stir zone of the hot weld (higher heat input) contained bainitic ferrite, acicular ferrite, coalesced bainite, martensite, and dispersed carbides. Granular bainite and dispersed carbides were observed in all the heat affected zones. Analysis of the microstructural transformations, together with the thermal history of the joints, showed that the variable that had the greatest influence on the morphology of the bainite (granular bainite/bainitic ferrite) was the deformation temperature.

Microstructure Characterization of Weakly Textured and Fine Grained AZ61 Sheet

NASA Astrophysics Data System (ADS)

Berman, T. D.; Donlon, W.; Hung, C. K.; Milligan, P.; Decker, R.; Pollock, T. M.; Jones, J. W.

Formability in magnesium alloy sheet is strongly limited by a strong basal texture in the as-rolled material, which is difficulty to remove by thermal processing. We introduce a new process to the control of texture by combining Thixomolding and Thermomechanical Processing (TTMP). Plates of AZ61L with a divorced β-Mg17Al12 eutectic are produced by Thixomolding, resulting in a non-textured, fine grained (2.8 µm) precursor. Sheet produced from the plate by single pass warm-rolling exhibits a weaker texture, and more isotropic tensile deformation than generally observed in AZ-series alloy sheet. Recrystallization annealing produces a further reduction in texture and average grain size (2.3 µm) and results in nearly isotropic room temperature deformation, a yield strength of 220 MPa, and an elongation of 23%. Particle stimulated nucleation of new grains by the β-phase during both dynamic and static recrystallization, is critical for achieving the low levels of texture. The influence of β-phase distribution in microstructure development is discussed.

Matrix recrystallization for MALDI-MS imaging of maize lipids at high-spatial resolution

DOE Office of Scientific and Technical Information (OSTI.GOV)

Duenas, Maria Emilia; Carlucci, Laura; Lee, Young Jin

Matrix recrystallization is optimized and applied to improve lipid ion signals in maize embryos and leaves. A systematic study was performed varying solvent and incubation time. During this study, unexpected side reactions were found when methanol was used as a recrystallization solvent, resulting in the formation of a methyl ester of phosphatidic acid. Furthermore, using an optimum recrystallization condition with isopropanol, there is no apparent delocalization demonstrated with a transmission electron microscopy (TEM) pattern and maize leaf images obtained at 10 μm spatial resolution.

Matrix recrystallization for MALDI-MS imaging of maize lipids at high-spatial resolution

DOE PAGES

Duenas, Maria Emilia; Carlucci, Laura; Lee, Young Jin

2016-06-27

Matrix recrystallization is optimized and applied to improve lipid ion signals in maize embryos and leaves. A systematic study was performed varying solvent and incubation time. During this study, unexpected side reactions were found when methanol was used as a recrystallization solvent, resulting in the formation of a methyl ester of phosphatidic acid. Furthermore, using an optimum recrystallization condition with isopropanol, there is no apparent delocalization demonstrated with a transmission electron microscopy (TEM) pattern and maize leaf images obtained at 10 μm spatial resolution.

Matrix Recrystallization for MALDI-MS Imaging of Maize Lipids at High-Spatial Resolution

NASA Astrophysics Data System (ADS)

Dueñas, Maria Emilia; Carlucci, Laura; Lee, Young Jin

2016-09-01

Matrix recrystallization is optimized and applied to improve lipid ion signals in maize embryos and leaves. A systematic study was performed varying solvent and incubation time. During this study, unexpected side reactions were found when methanol was used as a recrystallization solvent, resulting in the formation of a methyl ester of phosphatidic acid. Using an optimum recrystallization condition with isopropanol, there is no apparent delocalization demonstrated with a transmission electron microscopy (TEM) pattern and maize leaf images obtained at 10 μm spatial resolution.

Correlation buildup during recrystallization in three-dimensional dusty plasma clusters

DOE Office of Scientific and Technical Information (OSTI.GOV)

Schella, André; Mulsow, Matthias; Melzer, André

2014-05-15

The recrystallization process of finite three-dimensional dust clouds after laser heating is studied experimentally. The time-dependent Coulomb coupling parameter is presented, showing that the recrystallization starts with an exponential cooling phase where cooling is slower than damping by the neutral gas friction. At later times, the coupling parameter oscillates into equilibrium. It is found that a large fraction of cluster states after recrystallization experiments is in metastable states. The temporal evolution of the correlation buildup shows that correlation occurs on even slower time scale than cooling.

Matrix Recrystallization for MALDI-MS Imaging of Maize Lipids at High-Spatial Resolution.

PubMed

Dueñas, Maria Emilia; Carlucci, Laura; Lee, Young Jin

2016-09-01

Matrix recrystallization is optimized and applied to improve lipid ion signals in maize embryos and leaves. A systematic study was performed varying solvent and incubation time. During this study, unexpected side reactions were found when methanol was used as a recrystallization solvent, resulting in the formation of a methyl ester of phosphatidic acid. Using an optimum recrystallization condition with isopropanol, there is no apparent delocalization demonstrated with a transmission electron microscopy (TEM) pattern and maize leaf images obtained at 10 μm spatial resolution. Graphical Abstract ᅟ.

Ultrasonic attenuation measurements determine onset, degree, and completion of recrystallization

NASA Technical Reports Server (NTRS)

Generazio, E. R.

1988-01-01

Ultrasonic attenuation was measured for cold worked Nickel 200 samples annealed at increasing temperatures. Localized dislocation density variations, crystalline order and volume percent of recrystallized phase were determined over the anneal temperature range using transmission electron microscopy, X-ray diffraction, and metallurgy. The exponent of the frequency dependence of the attenuation was found to be a key variable relating ultrasonic attenuation to the thermal kinetics of the recrystallization process. Identification of this key variable allows for the ultrasonic determination of onset, degree, and completion of recrystallization.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhang, Y. B.; Budai, J. D.; Tischler, J. Z.

How boundaries surrounding recrystallization grains migrate through the 3D network of dislocation boundaries in deformed crystalline materials is unknown and critical for the resulting recrystallized crystalline materials. Furthermore, by using X-ray Laue diffraction microscopy, we show for the first time the migration pattern of a typical recrystallization boundary through a well-characterized deformation matrix. The data provide a unique possibility to investigate effects of both boundary misorientation and plane normal on the migration, information which cannot be accessed with any other techniques. Our results show that neither of these two parameters can explain the observed migration behavior. Instead we suggest thatmore » the subdivision of the deformed microstructure ahead of the boundary plays the dominant role. Our experimental observations challenge the assumptions of existing recrystallization theories, and set the stage for determination of mobilities of recrystallization boundaries.« less

Grain Boundary Evolution of Cold-Rolled FePd Alloy during Recrystallization at Disordering Temperature

PubMed Central

Lin, Hung-Pin; Chen, Delphic; Kuo, Jui-Chao

2015-01-01

In this study, the grain boundary character and texture of 50% and 90% cold-rolled FePd alloy was investigated during recrystallization at 700 °C. Electron backscatter diffraction (EBSD) measurements were performed on the rolling direction to normal direction section. Kernel average misorientation (KAM) calculated from EBSD measurements was employed to determine the recrystallization fraction. The Avrami exponent n of recrystallization is 1.9 and 4.9 for 50% and 90% cold rolling, respectively. The new formation of texture reveals random texture during the recrystallization process. As annealing time increased, the number of high angle boundary (HAGB) and coincidence site lattice (CSL) increased with consumption of low angle boundary (LAGB). In addition, possible transformations between different grain boundaries are observed here.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, Kun; Bannister, Mark E.; Meyer, Fred W.

Here, in a magnetic fusion energy (MFE) device, the plasma-facing materials (PFMs) will be subjected to tremendous fluxes of ions, heat, and neutrons. The response of PFMs to the fusion environment is still not well defined. Tungsten metal is the present candidate of choice for PFM applications such as the divertor in ITER. However, tungsten's microstructure will evolve in service, possibly to include recrystallization. How tungsten's response to plasma exposure evolves with changes in microstructure is presently unknown. In this work, we have exposed hot-worked and recrystallized tungsten to an 80 eV helium ion beam at a temperature of 900more » °C to fluences of 2 × 10 23 or 20 × 10 23 He/m 2. This resulted in a faceted surface structure at the lower fluence or short but well-developed nanofuzz structure at the higher fluence. There was little difference in the hot-rolled or recrystallized material's near-surface (≤50 nm) bubbles at either fluence. At higher fluence and deeper depth, the bubble populations of the hot-rolled and recrystallized were different, the recrystallized being larger and deeper. This may explain previous high-fluence results showing pronounced differences in recrystallized material. The deeper penetration in recrystallized material also implies that grain boundaries are traps, rather than high-diffusivity paths.« less

High temperature microstructural stability and recrystallization mechanisms in 14YWT alloys

DOE PAGES

Aydogan, E.; El-Atwani, O.; Takajo, S.; ...

2018-02-09

In-situ neutron diffraction experiments were performed on room temperature compressed 14YWT nanostructured ferritic alloys at 1100°C and 1150°C to understand their thermally activated static recrystallization mechanisms. The existence of high density of Y-Ti-O rich nano-oxides (<5 nm) shift the recrystallization temperature up due to Zener pinning of the grain boundaries, making these materials attractive for high temperature applications. This study serves to quantify the texture evolution in-situ and understand the effect of particles on the recrystallization mechanisms in 14YWT alloys. We have shown, both experimentally and theoretically, that there is considerable recovery in the 20% compressed sample after 6.5 hmore » annealing at 1100°C while recrystallization occurs within an hour of annealing at 1100°C and 1150°C in the 60% compressed samples. Moreover, the 60% compressed samples show {112}<110> and {112}<111> texture components during annealing, in contrast to the conventional recrystallization textures in body centered cubic alloys. Furthermore, nano-oxide size, shape, density and distribution are considerably different in unrecrystallized and abnormally grown grains. Transmission electron microscopy analysis shows that oxide particles having a size between 5 and 30 nm play a critical role for recrystallization mechanisms in 14YWT nanostructured ferritic alloys.« less

High temperature microstructural stability and recrystallization mechanisms in 14YWT alloys

DOE Office of Scientific and Technical Information (OSTI.GOV)

Aydogan, E.; El-Atwani, O.; Takajo, S.

In-situ neutron diffraction experiments were performed on room temperature compressed 14YWT nanostructured ferritic alloys at 1100°C and 1150°C to understand their thermally activated static recrystallization mechanisms. The existence of high density of Y-Ti-O rich nano-oxides (<5 nm) shift the recrystallization temperature up due to Zener pinning of the grain boundaries, making these materials attractive for high temperature applications. This study serves to quantify the texture evolution in-situ and understand the effect of particles on the recrystallization mechanisms in 14YWT alloys. We have shown, both experimentally and theoretically, that there is considerable recovery in the 20% compressed sample after 6.5 hmore » annealing at 1100°C while recrystallization occurs within an hour of annealing at 1100°C and 1150°C in the 60% compressed samples. Moreover, the 60% compressed samples show {112}<110> and {112}<111> texture components during annealing, in contrast to the conventional recrystallization textures in body centered cubic alloys. Furthermore, nano-oxide size, shape, density and distribution are considerably different in unrecrystallized and abnormally grown grains. Transmission electron microscopy analysis shows that oxide particles having a size between 5 and 30 nm play a critical role for recrystallization mechanisms in 14YWT nanostructured ferritic alloys.« less

Recrystallization and grain growth behavior of rolled tungsten under VDE-like short pulse high heat flux loads

NASA Astrophysics Data System (ADS)

Yuan, Y.; Greuner, H.; Böswirth, B.; Krieger, K.; Luo, G.-N.; Xu, H. Y.; Fu, B. Q.; Li, M.; Liu, W.

2013-02-01

Short pulse heat loads expected for vertical displacement events (VDEs) in ITER were applied in the high heat flux (HHF) test facility GLADIS at IPP-Garching onto samples of rolled W. Pulsed neutral beams with the central heat flux of 23 MW/m2 were applied for 0.5, 1.0 and 1.5 s, respectively. Rapid recrystallization of the adiabatically loaded 3 mm thick samples was observed when the pulse duration was up to 1.0 s. Grains grew markedly following recrystallization with increasing pulse length. The recrystallization temperature and temperature dependence of the recrystallized grain size were also investigated. The results showed that the recrystallization temperature of the W grade was around 2480 °C under the applied heat loading condition, which was nearly 1150 °C higher than the conventional recrystallization temperature, and the grains were much finer. A linear relationship between the logarithm of average grain size (ln d) and the inverse of maximum surface temperature (1/Tmax) was found and accordingly the activation energy for grain growth in temperature evolution up to Tmax in 1.5 s of the short pulse HHF load was deduced to be 4.1 eV. This provided an effective clue to predict the structure evolution under short pulse HHF loads.

The risk of recrystallization: changes to the toxicity and morphology of pyrimethamine.

PubMed

Perold, Zak; Caira, Mino R; Brits, Marius

2014-01-01

Pyrimethamine, an anti-malarial agent known to exhibit solid state polymorphism, may be purified by means of recrystallization. Recrystallization may alter the solid state chemistry of pharmaceuticals, which may impact the toxicity and/or manufacturability thereof. We evaluated the risks associated with the recrystallization of pyrimethamine. Pyrimethamine was recrystallized using several organic solvents. X-ray diffraction, thermal analysis, infra-red spectroscopy, microscopy, flowability -, solubility and dissolution testing as well as computational work were employed to evaluate the recrystallized products. A toxic solvatomorph of pyrimethamine (Pyr-MeOH) was found to be the product from methanol recrystallization. The elucidation of - and the elaboration on the unique characteristics of Pyr-MeOH provides the pharmaceutical industry with several means to identify Pyr-MeOH and to distinguish it from the pharmaceutically preferred anhydrous form (Pyr). Thermal methods of analysis found that the toxicity of Pyr-MeOH may be reversed by overcoming a desolvation activation energy of 148 kJ/mol. In addition it was found that recrystallization altered the morphology of Pyr. Angle of repose and tapped density determinations identified that the different morphologies of Pyr displayed differences in powder flow and compressibility behaviour and In Silico calculations were successful in rendering morphologies resembling that found experimentally. We present a solvatomorph of pyrimethamine and provide several characteristic means to identify this unwanted toxic form and quantified the energy required to overcome its toxicity. In addition we describe that Pyr may present in different morphologies and show how it may impact the manufacturability thereof.

Analysis of Particle-Stimulated Nucleation (PSN)-Dominated Recrystallization for Hot-Rolled 7050 Aluminum Alloy

NASA Astrophysics Data System (ADS)

Adam, Khaled F.; Long, Zhengdong; Field, David P.

2017-04-01

In 7xxx series aluminum alloys, the constituent large and small second-phase particles present during deformation process. The fraction and spatial distribution of these second-phase particles significantly influence the recrystallized structure, kinetics, and texture in the subsequent treatment. In the present work, the Monte Carlo Potts model was used to model particle-stimulated nucleation (PSN)-dominated recrystallization and grain growth in high-strength aluminum alloy 7050. The driving force for recrystallization is deformation-induced stored energy, which is also strongly affected by the coarse particle distribution. The actual microstructure and particle distribution of hot-rolled plate were used as an initial point for modeling of recrystallization during the subsequent solution heat treatment. Measurements from bright-field TEM images were performed to enhance qualitative interpretations of the developed microstructure. The influence of texture inhomogeneity has been demonstrated from a theoretical point of view using pole figures. Additionally, in situ annealing measurements in SEM were performed to track the orientational and microstructural changes and to provide experimental support for the recrystallization mechanism of PSN in AA7050.

Facile synthesis of hollow zeolite microspheres through dissolution–recrystallization procedure in the presence of organosilanes

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tao, Haixiang; Ren, Jiawen; Liu, Xiaohui

2013-04-15

Hollow zeolite microspheres have been hydrothermally synthesized in the presence of organosilanes via a dissolution–recrystallization procedure. In the presence of organosilanes, zeolite particles with a core/shell structure formed at the first stage of hydrothermal treatment, then the core was consumed and recrystallized into zeolite framework to form the hollow structure during the second hydrothermal process. The influence of organosilanes was discussed, and a related dissolution–recrystallization mechanism was proposed. In addition, the hollow zeolite microspheres exhibited an obvious advantage in catalytic reactions compared to conventional ZSM-5 catalysts, such as in the alkylation of toluene with benzyl chloride. - Graphical abstract: Hollowmore » zeolite spheres with aggregated zeolite nanocrystals were synthesized via a dissolution–recrystallization procedure in the presence of organosiline. Highlights: ► Hollow zeolite spheres with aggregated zeolite nanocrystals were synthesized via a dissolution–recrystallization procedure. ► Organosilane influences both the morphology and hollow structure of zeolite spheres. ► Hollow zeolite spheres showed an excellent catalytic performance in alkylation of toluene with benzyl chloride.« less

Progressive deformation of ultramafic rocks accompanied with deflection of layered structure and mylonitization culminating into a pseudotachylyte-bearing seismogenic fault - a field evidence of plastic instability

NASA Astrophysics Data System (ADS)

Ueda, T.; Obata, M.

2011-12-01

Plastic instability leading to rupture nucleation and propagetion (e.g. Hobbs et al.1986, Kelemen and Hirth, 2007) is an attractive hypothesis for deep earthquakes but lacked clear field evidences. 1D across-fault shear localization observed in some places (e.g. Jin et al.1998) is not clear if the deformation is directly related with seismicity. We present a clear field evidence of plastic instability as guided by pyroxenite/peridotite layering deflection structure (hereafter called LD structure, see figure) accompanied with mylonitization in spinel(Sp)-peridotite facies (P>~1GPa) in Balmuccia peridotite, Ivrea-Verbano Zone, Italy. The studied area contains abundant PST-bearing faults and N-S trending primary pyroxenite layers. Many faults in the area cut pyroxenite layers, but LD structure is found only in one place presented here. Many PSTs in the area have been (re)crystallized in Sp-peridotite facies, and have typically ultramylonitic texture (Ueda et al., 2008) with some injection veins. The fault with LD structure is situated in a fault system, which has two dominant attitudes with regional N-S extension. The shear strain of LD structure measured on outcrop surface is ~2.0. Near the fault, elongated Opx porphyroclasts (ellipses in figure) oblique to local layering are visible in peridotite. The dominant deformation textures are dynamic recrystallization in peridotite and kinking or undulatory extinction in pyroxenite. The mineral assemblages of the mylonite neoblast in the peridotite and the pyroxenite are Ol+Opx+Cpx+Sp+hornblende(Hbl), Cpx+Opx+Sp, respectively. Hbl typically occur only in neoblast. In the vicinity (several hundreds of micron) of the fault, dolomite(Dol) also occur in equilibrium with the assemblage above. The recrystallized grain sizes are 20-50 microns in peridotite and 10-30 microns in pyroxenite. The rarity of LD structure is consistent with general conception that deformation processes which lead to dynamic rupture initiation ought to be recorded in limited area on a resultant fault surface. The N-S extensional arrangement of the fault system including the fault of LD structure, the depth of PST (re)crystallization and mylonitization, all indicate that the rupture nucleation occurred in extensional tectonics (Souquiere and Fabbri , 2010). The occurrence of Dol in the vicinity of the PST fault suggests that this is the very place where plastic instability accompanied with fluid chemistry evolution (from H2O-rich to CO2-rich, caused by mylonitization and hydration) of Ueda et al. (2008.) had taken place.

Effect of Prestraining of Recrystallization Temperature and Mechanical Properties of Commercial, Sintered, Wrought Molybdenum

NASA Technical Reports Server (NTRS)

Dike, Kenneth C; Long, Roger A

1953-01-01

Given three presumably identical lots of commercial, sintered, wrought molybdenum, the 1-hour recrystallization temperature of one lot remained above 2900 F by limiting the amount of effective restraining to 35 percent or less. Different recrystallization temperatures were obtained in various atmospheres, the highest in argon and the lowest in hydrogen. Metal thus fabricated and then stress-relieved possessed an ultimate tensile strength at room temperature within 10 percent of metal swaged 99 percent and also possessed equivalent ductility. At 1800 F, equivalent strength and ductility was obtained irrespective of the amount of swaging over the range of 10 to 99 percent. The amount of swaging greatly influenced the recrystallized grain size but the difference in grain size is not the major controlling factor which determines whether recrystallized molybdenum is ductile or brittle at room temperature.

Optimum rolling ratio for obtaining {001}<110> recrystallization texture in Ti-Nb-Al biomedical shape memory alloy.

PubMed

Inamura, T; Shimizu, R; Kim, H Y; Miyazaki, S; Hosoda, H

2016-04-01

The rolling rate (r) dependence of textures was investigated in the Ti-26Nb-3Al (mol%) alloy to reveal the conditions required to form the {001}<110> recrystallization texture, which is a desirable orientation for the β-titanium shape memory alloy. {001}<110> was the dominant cold-rolling texture when r=90% and it was transferred to the recrystallization texture without forming {112}<110>, which is detrimental for the isotropic mechanical properties of the rolled sheet. A further increase in r resulted in the formation of {112}<110> in both rolling and recrystallization textures. Therefore, r should be controlled to form only the {001}<110> rolling texture, because the {112}<110> texture can overwhelm the {001}<110> texture during recrystallization. Copyright © 2016 Elsevier B.V. All rights reserved.

Effect of starting microstructure on helium plasma-materials interaction in tungsten

DOE PAGES

Wang, Kun; Bannister, Mark E.; Meyer, Fred W.; ...

2016-11-24

Here, in a magnetic fusion energy (MFE) device, the plasma-facing materials (PFMs) will be subjected to tremendous fluxes of ions, heat, and neutrons. The response of PFMs to the fusion environment is still not well defined. Tungsten metal is the present candidate of choice for PFM applications such as the divertor in ITER. However, tungsten's microstructure will evolve in service, possibly to include recrystallization. How tungsten's response to plasma exposure evolves with changes in microstructure is presently unknown. In this work, we have exposed hot-worked and recrystallized tungsten to an 80 eV helium ion beam at a temperature of 900more » °C to fluences of 2 × 10 23 or 20 × 10 23 He/m 2. This resulted in a faceted surface structure at the lower fluence or short but well-developed nanofuzz structure at the higher fluence. There was little difference in the hot-rolled or recrystallized material's near-surface (≤50 nm) bubbles at either fluence. At higher fluence and deeper depth, the bubble populations of the hot-rolled and recrystallized were different, the recrystallized being larger and deeper. This may explain previous high-fluence results showing pronounced differences in recrystallized material. The deeper penetration in recrystallized material also implies that grain boundaries are traps, rather than high-diffusivity paths.« less

Study of Improved Aluminum Materials for Vehicular Armor

DTIC Science & Technology

1977-04-07

and along cell walls. Dislocations generated during deformation cf the 17 -------------- recrystallized structure interacted with the grain...unrecrystallized (HR) 7475 plate containing dislocations within subgrains and along cell walls. Hot rolling the recrystallized structure at 750OF produced...a structure after solution heat treatment that consisted of elongated recrystallized grains containing polygonized cells . This structure developed

Combined Effect of Heating Rate and Microalloying Elements on Recrystallization During Annealing of Dual-Phase Steels

NASA Astrophysics Data System (ADS)

Bellavoine, Marion; Dumont, Myriam; Drillet, Josée; Hébert, Véronique; Maugis, Philippe

2018-05-01

Adjusting ferrite recrystallization kinetics during annealing is a way to control the final microstructure and thus the mechanical properties of advanced cold-rolled high-strength steels. Two strategies are commonly used for this purpose: adjusting heating rates and/or adding microalloying elements. The present work investigates the effect of heating rate and microalloying elements Ti, Nb, and Mo on recrystallization kinetics during annealing in various cold-rolled Dual-Phase steel grades. The use of combined experimental and modeling approaches allows a deeper understanding of the separate influence of heating rate and the addition of microalloying elements. The comparative effect of Ti, Nb, and Mo as solute elements and as precipitates on ferrite recrystallization is also clarified. It is shown that solute drag has the largest delaying effect on recrystallization in the present case and that the order of solute drag effectiveness of microalloying elements is Nb > Mo > Ti.

Combined Effect of Heating Rate and Microalloying Elements on Recrystallization During Annealing of Dual-Phase Steels

NASA Astrophysics Data System (ADS)

Bellavoine, Marion; Dumont, Myriam; Drillet, Josée; Hébert, Véronique; Maugis, Philippe

2018-07-01

Adjusting ferrite recrystallization kinetics during annealing is a way to control the final microstructure and thus the mechanical properties of advanced cold-rolled high-strength steels. Two strategies are commonly used for this purpose: adjusting heating rates and/or adding microalloying elements. The present work investigates the effect of heating rate and microalloying elements Ti, Nb, and Mo on recrystallization kinetics during annealing in various cold-rolled Dual-Phase steel grades. The use of combined experimental and modeling approaches allows a deeper understanding of the separate influence of heating rate and the addition of microalloying elements. The comparative effect of Ti, Nb, and Mo as solute elements and as precipitates on ferrite recrystallization is also clarified. It is shown that solute drag has the largest delaying effect on recrystallization in the present case and that the order of solute drag effectiveness of microalloying elements is Nb > Mo > Ti.

Recrystallization kinetics of warm-rolled tungsten in the temperature range 1150-1350 °C

NASA Astrophysics Data System (ADS)

Alfonso, A.; Juul Jensen, D.; Luo, G.-N.; Pantleon, W.

2014-12-01

Pure tungsten is a potential candidate material for the plasma-facing first wall and the divertor of fusion reactors. Both parts have to withstand high temperatures during service. This will alter the microstructure of the material by recovery, recrystallization and grain growth and will cause degradation in material properties as a loss in mechanical strength and embrittlement. The thermal stability of a pure tungsten plate warm-rolled to 67% thickness reduction was investigated by long-term isothermal annealing in the temperature range between 1150 °C and 1350 °C up to 2200 h. Changes in the mechanical properties during annealing are quantified by Vickers hardness measurements. They are described concisely by classical kinetic models for recovery and recrystallization. The observed time spans for recrystallization and the obtained value for the activation energy of the recrystallization process indicate a sufficient thermal stability of the tungsten plate during operation below 1075 °C.

Boundary migration in a 3D deformed microstructure inside an opaque sample

DOE PAGES

Zhang, Y. B.; Budai, J. D.; Tischler, J. Z.; ...

2017-06-30

How boundaries surrounding recrystallization grains migrate through the 3D network of dislocation boundaries in deformed crystalline materials is unknown and critical for the resulting recrystallized crystalline materials. Furthermore, by using X-ray Laue diffraction microscopy, we show for the first time the migration pattern of a typical recrystallization boundary through a well-characterized deformation matrix. The data provide a unique possibility to investigate effects of both boundary misorientation and plane normal on the migration, information which cannot be accessed with any other techniques. Our results show that neither of these two parameters can explain the observed migration behavior. Instead we suggest thatmore » the subdivision of the deformed microstructure ahead of the boundary plays the dominant role. Our experimental observations challenge the assumptions of existing recrystallization theories, and set the stage for determination of mobilities of recrystallization boundaries.« less

Improvement of seawater salt quality by hydro-extraction and re-crystallization methods

NASA Astrophysics Data System (ADS)

Sumada, K.; Dewati, R.; Suprihatin

2018-01-01

Indonesia is one of the salt producing countries that use sea water as a source of raw materials, the quality of salt produced is influenced by the quality of sea water. The resulting average salt quality contains 85-90% NaCl. The Indonesian National Standard (SNI) for human salt’s consumption sodium chloride content is 94.7 % (dry base) and for industrial salt 98,5 %. In this study developed the re-crystallization without chemical and hydro-extraction method. The objective of this research to choose the best methods based on efficiency. The results showed that re-crystallization method can produce salt with NaCl content 99,21%, while hydro-extraction method content 99,34 % NaCl. The salt produced through both methods can be used as a consumption and industrial salt, Hydro-extraction method is more efficient than re-crystallization method because re-crystallization method requires heat energy.

Effect of Boron on the Hot Ductility of Resulfurized Low-Carbon Free-Cutting Steel

NASA Astrophysics Data System (ADS)

Liu, Hai-tao; Chen, Wei-qing

2015-09-01

The hot ductility of resulfurized low-carbon free-cutting steel with boron additives is studied in the temperature range 850 - 1200°C with the help of a Gleeble-1500 thermomechanical simulator. The introduction of boron increases hot ductility, especially at 900 - 1050°C. In the single-phase austenitic region, this effect is caused by segregation of boron over grain boundaries, acceleration of dynamic recrystallization, and solid-solution softening of deformed austenite.

Towards the determination of deformation rates - pinch-and-swell structures as a natural and simulated paleo-strain rate gage

NASA Astrophysics Data System (ADS)

Peters, Max; Poulet, Thomas; Karrech, Ali; Regenauer-Lieb, Klaus; Herwegh, Marco

2014-05-01

Layered rocks deformed under viscous deformation conditions frequently show boudinage, a phenomenon that results from differences in effective viscosity between the involved layers. In the case of continuous necking of a mechanically stiffer layer embedded in a weaker matrix, symmetric boudins are interpreted as the result of dominant visco-plastic deformation (Goscombe et al., 2004). However, information on the physical conditions, material properties and deformation processes are yet unknown. Natural samples deformed under low-grade (T<350°C) metamorphic conditions were studied in detail in the Dent de Morcles and Doldenhorn nappes of the Helvetic Alps in order to accurately simulate their deformation styles by numerical models. In these samples, monomineralic calcite (Cc) veins were repeatedly boudinaged on cm- to µm-scale. Remnants of incompletely recrystallized original vein Cc grains in the swells indicate a sequence of deformation twinning, followed by progressive dynamic recrystallization along former twin planes up to complete recrystallization in the pinches (Schmalholz and Maeder, 2012). This sequence suggests dislocation creep to be active as important deformation mechanism. In contrast to the pinch-and-swell structures, the grain size of the Cc in the surrounding matrix is much finer-grained due to pinning by secondary particles, forcing the matrix to deform under viscous granular creep, i.e. by diffusion accommodated grain boundary sliding. The deformation processes observed in the natural samples were incorporated into a numerical model in order to evaluate the rheology of both layer and matrix, using an extension to a user material subroutine (Karrech et al., 2011a) for the finite element solver ABAQUS. We implemented thermo-mechanical coupling allowing elastic, viscous and plastic deformation of Cc (Herwegh et al., in press). We simulate a pure-shear box using finite elements, each representing a grain size distribution, which undergo layer-parallel extension. The box is built up by 3 layers, consisting of a central layer of coarse-grained populations, surrounded by finer-grained populations on bottom and top. The rheology evolves from transient stages (elasticity and strain hardening) to composite viscous flow (GSI & GSS) with increasing shear strain. The small grain sizes in top and bottom layers are strain-invariant and limited in their growth (comparable to Zener pinning) forcing the matrix to deform by exclusively by GSS creep. In contrast, the initially coarse grain sizes of the central layer are allowed to adapt to the physical deformation conditions by either grain growth or grain size reduction following the Paleowattmeter of Austin and Evans (2007) combined with the thermodynamic approach of Regenauer-Lieb and Yuen (2004). Depending on the dissipated energy, grain sizes in these domains vary substantially in space and time. While low strain rates (low stresses) in the swells favor grain growth and GSI dominated deformation, high strain rates in the pinches provoke dramatic grain size reduction with an increasing contribution of GSS as a function of decreasing grain size. The development of symmetric necks observed in nature thus seems to coincide with the transition from dislocation to diffusion creep dominated flow with continuous grain size reduction and growth from swell to neck at relatively high extensional strains. REFERENCES Austin, N. and Evans, B. (2007). Paleowattmeters: A scaling relation for dynamically recrystallized grain size. Geology, 35. Goscombe, B.D., Passchier, C.W. and Hand, M. (2004). Boudinage classification: End-member boudin types and modified boudin structures, Journal of Structural Geology, 26. Herwegh, M., Poulet, T., Karrech, A. and Regenauer-Lieb, K. (in press). From transient to steady state deformation and grain size: A thermodynamic approach using elasto-visco-plastic numerical modeling. Journal of Geophysical Research. Karrech, A., Regenauer-Lieb, K. and Poulet, T. (2011a). A Damaged visco-plasticity model for pressure and temperature sensitive geomaterials. Journal of Engineering Science 49. Regenauer-Lieb, K. and Yuen, D. (2004). Positive feedback of interacting ductile faults from coupling of equation of state, rheology and thermal-mechanics. Physics of the Earth and Planetary Interiors, 142. Schmalholz, S.M. and Maeder, X. (2012). Pinch-and-swell structure and shear zones in viscoplastic layers. Journal of Structural Geology, 34.

Cellular monotectic model solidification

NASA Technical Reports Server (NTRS)

Kaukler, William F.

1987-01-01

Succinonitrile (sn) was purified to a superior level using a fractional recrystallization method. The melting point of the best twice recrystallized sn was not raised by following with double distillation. This was tested using differential scanning calorimetry. The peak shape on melting also proved that double distillation after double recrystallization did not improve the quality. Stability and phase diagrams for succinonitrile and glycerol are presented.

Effect of one-step recrystallization on the grain boundary evolution of CoCrFeMnNi high entropy alloy and its subsystems.

PubMed

Chen, Bo-Ru; Yeh, An-Chou; Yeh, Jien-Wei

2016-02-29

In this study, the grain boundary evolution of equiatomic CoCrFeMnNi, CoCrFeNi, and FeCoNi alloys after one-step recrystallization were investigated. The special boundary fraction and twin density of these alloys were evaluated by electron backscatter diffraction analysis. Among the three alloys tested, FeCoNi exhibited the highest special boundary fraction and twin density after one-step recrystallization. The special boundary increment after one-step recrystallization was mainly affected by grain boundary velocity, while twin density was mainly affected by average grain boundary energy and twin boundary energy.

High-quality Silicon Films Prepared by Zone-melting Recrystallization

NASA Technical Reports Server (NTRS)

Chen, C. K.; Geis, M. W.; Tsaur, B. Y.; Fan, J. C. C.

1984-01-01

The graphite strip heater zone melting recrystallization (ZMR) technique is described. The material properties of the ZMR films, and SOI device results are reviewed. Although our ZMR work is primarily motivated by integrated circuit applications, this work evolved in part from earlier research on laser crystallization of thick amorphous GaAs and Si films, which was undertaken with the goal of producing low cost photovoltaic materials. The ZMR growth process and its effect on the properties of the recrystallized films may contribute some insight to a general understanding of the rapid recrystallization of Si for solar cells. Adaptation of ZMR for solar cell fabrication is considered.

Effect of Scandium on the Interaction of Concurrent Precipitation and Recrystallization in Commercial AA3003 Aluminum Alloy

NASA Astrophysics Data System (ADS)

Tu, Yiyou; Qian, Huan; Zhou, Xuefeng; Jiang, Jianqing

2014-04-01

In the current study, the effect of Sc addition on the interaction of concurrent precipitation and recrystallization in commercial AA3003 aluminum alloy was investigated using optical microscopy, scanning electron microscopy, and transmission electron microscopy. In case of AA3003 alloy, which was cold rolled to a true strain of 2.20 and heated at a heating rate of 150 K/s, the onset of precipitation and ending of recrystallization are signified by the critical temperature, T C ~740 K (467 °C). There is a change in the shape of the recrystallized grains from pancake-like to equiaxed shape, as the annealing temperature increases greater than T C. In case of AA3003 alloy microalloyed with 0.4 wt pct of Sc, the high no. density precipitation of coherent Al3Sc precipitates always occurs before recrystallization because of the small nucleation barrier and high rate of decomposition. This leads to extremely coarse pancake-like recrystallization grains with high fraction of low-angle grain boundaries in the entire annealing temperature range, even at a high brazing temperature of 883 K (610 °C).

Incorporation of Eu(III) into Calcite under Recrystallization conditions.

PubMed

Hellebrandt, S E; Hofmann, S; Jordan, N; Barkleit, A; Schmidt, M

2016-09-13

The interaction of calcite with trivalent europium under recrystallization conditions was studied on the molecular level using site-selective time-resolved laser fluorescence spectroscopy (TRLFS). We conducted batch studies with a reaction time from seven days up to three years with three calcite powders, which differed in their specific surface area, recrystallization rates and impurities content. With increase of the recrystallization rate incorporation of Eu(3+) occurs faster and its speciation comes to be dominated by one species with its excitation maximum at 578.8 nm, so far not identified during previous investigations of this process under growth and phase transformation conditions. A long lifetime of 3750 μs demonstrates complete loss of hydration, consequently Eu must have been incorporated into the bulk crystal. The results show a strong dependence of the incorporation kinetics on the recrystallization rate of the different calcites. Furthermore the investigation of the effect of different background electrolytes (NaCl and KCl) demonstrate that the incorporation process under recrystallization conditions strongly depends on the availability of Na(+). These findings emphasize the different retention potential of calcite as a primary and secondary mineral e.g. in a nuclear waste disposal site.

Inhibiting ice recrystallization and optimization of cell viability after cryopreservation.

PubMed

Chaytor, Jennifer L; Tokarew, Jacqueline M; Wu, Luke K; Leclère, Mathieu; Tam, Roger Y; Capicciotti, Chantelle J; Guolla, Louise; von Moos, Elisabeth; Findlay, C Scott; Allan, David S; Ben, Robert N

2012-01-01

The ice recrystallization inhibition activity of various mono- and disaccharides has been correlated with their ability to cryopreserve human cell lines at various concentrations. Cell viabilities after cryopreservation were compared with control experiments where cells were cryopreserved with dimethylsulfoxide (DMSO). The most potent inhibitors of ice recrystallization were 220 mM solutions of disaccharides; however, the best cell viability was obtained when a 200 mM d-galactose solution was utilized. This solution was minimally cytotoxic at physiological temperature and effectively preserved cells during freeze-thaw. In fact, this carbohydrate was just as effective as a 5% DMSO solution. Further studies indicated that the cryoprotective benefit of d-galactose was a result of its internalization and its ability to mitigate osmotic stress, prevent intracellular ice formation and/or inhibit ice recrystallization. This study supports the hypothesis that the ability of a cryoprotectant to inhibit ice recrystallization is an important property to enhance cell viability post-freeze-thaw. This cryoprotective benefit is observed in three different human cell lines. Furthermore, we demonstrated that the ability of a potential cryoprotectant to inhibit ice recrystallation may be used as a predictor of its ability to preserve cells at subzero temperatures.

Incorporation of Eu(III) into Calcite under Recrystallization conditions

PubMed Central

Hellebrandt, S. E.; Hofmann, S.; Jordan, N.; Barkleit, A.; Schmidt, M.

2016-01-01

The interaction of calcite with trivalent europium under recrystallization conditions was studied on the molecular level using site-selective time-resolved laser fluorescence spectroscopy (TRLFS). We conducted batch studies with a reaction time from seven days up to three years with three calcite powders, which differed in their specific surface area, recrystallization rates and impurities content. With increase of the recrystallization rate incorporation of Eu3+ occurs faster and its speciation comes to be dominated by one species with its excitation maximum at 578.8 nm, so far not identified during previous investigations of this process under growth and phase transformation conditions. A long lifetime of 3750 μs demonstrates complete loss of hydration, consequently Eu must have been incorporated into the bulk crystal. The results show a strong dependence of the incorporation kinetics on the recrystallization rate of the different calcites. Furthermore the investigation of the effect of different background electrolytes (NaCl and KCl) demonstrate that the incorporation process under recrystallization conditions strongly depends on the availability of Na+. These findings emphasize the different retention potential of calcite as a primary and secondary mineral e.g. in a nuclear waste disposal site. PMID:27618958

Anisotropic Morphological Changes in Goethite during Fe(2+)-Catalyzed Recrystallization.

PubMed

Joshi, Prachi; Gorski, Christopher A

2016-07-19

When goethite is exposed to aqueous Fe(2+), rapid and extensive Fe atom exchange can occur between solid-phase Fe(3+) and aqueous Fe(2+) in a process referred to as Fe(2+)-catalyzed recrystallization. This process can lead to the structural incorporation or release of trace elements, which has important implications for contaminant remediation and nutrient biogeochemical cycling. Prior work found that the process did not cause major changes to the goethite structure or morphology. Here, we further investigated if and how goethite morphology and aggregation behavior changed temporally during Fe(2+)-catalyzed recrystallization. On the basis of existing literature, we hypothesized that Fe(2+)-catalyzed recrystallization of goethite would not result in changes to individual particle morphology or interparticle interactions. To test this, we reacted nanoparticulate goethite with aqueous Fe(2+) at pH 7.5 over 30 days and used transmission electron microscopy (TEM), cryogenic TEM, and (55)Fe as an isotope tracer to observe changes in particle dimensions, aggregation, and isotopic composition over time. Over the course of 30 days, the goethite particles substantially recrystallized, and the particle dimensions changed anisotropically, resulting in a preferential increase in the mean particle width. The temporal changes in goethite morphology could not be completely explained by a single mineral-transformation mechanism but rather indicated that multiple transformation mechanisms occurred concurrently. Collectively, these results demonstrate that the morphology of goethite nanoparticles does change during recrystallization, which is an important step toward identifying the driving force(s) of recrystallization.

Mechanism of Martensitic to Equiaxed Microstructure Evolution during Hot Deformation of a Near-Alpha Ti Alloy

NASA Astrophysics Data System (ADS)

Shams, Seyed Amir Arsalan; Mirdamadi, Shamsoddin; Abbasi, Seyed Mahdi; Kim, Daehwan; Lee, Chong Soo

2017-06-01

In this study, mechanisms of microstructural evolution during hot deformation of Ti-1100 were investigated by EBSD analysis. Misorientation angle distribution of initial microstructure showed that diffusionless martensitic phase transformation in Ti-1100 obeys Burgers orientation relationship, and most of the high-angle-grain boundaries consist of angles of 60 and 63 deg. Calculated activation energy of hot deformation ( 338 kJ/mol) and EBSD grain boundary maps revealed that continuous dynamic recrystallization (CDRX) is the dominant mechanism during hot compression at 1073 K (800 °C) and strain rate of 0.005 s-1. At a temperature range of 1073 K to 1173 K (800 °C to 900 °C), not only the array of variants lying perpendicular to compression axis but also CDRX contributes to flow softening. Increasing the rolling temperature from 1123 K to 1273 K (850 °C to 1000 °C) brought about changes in spheroidization mechanism from CDRX to conventional boundary splitting and termination migration correlated with the higher volume fraction of beta phase at higher temperatures.

Abnormal grain growth in AISI 304L stainless steel

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shirdel, M., E-mail: mshirdel1989@ut.ac.ir; Mirzadeh, H., E-mail: hmirzadeh@ut.ac.ir; Advanced Metalforming and Thermomechanical Processing Laboratory, School of Metallurgy and Materials Engineering, University of Tehran, Tehran

2014-11-15

The microstructural evolution during abnormal grain growth (secondary recrystallization) in 304L stainless steel was studied in a wide range of annealing temperatures and times. At relatively low temperatures, the grain growth mode was identified as normal. However, at homologous temperatures between 0.65 (850 °C) and 0.7 (900 °C), the observed transition in grain growth mode from normal to abnormal, which was also evident from the bimodality in grain size distribution histograms, was detected to be caused by the dissolution/coarsening of carbides. The microstructural features such as dispersed carbides were characterized by optical metallography, X-ray diffraction, scanning electron microscopy, energy dispersivemore » X-ray analysis, and microhardness. Continued annealing to a long time led to the completion of secondary recrystallization and the subsequent reappearance of normal growth mode. Another instance of abnormal grain growth was observed at homologous temperatures higher than 0.8, which may be attributed to the grain boundary faceting/defaceting phenomenon. It was also found that when the size of abnormal grains reached a critical value, their size will not change too much and the grain growth behavior becomes practically stagnant. - Highlights: • Abnormal grain growth (secondary recrystallization) in AISI 304L stainless steel • Exaggerated grain growth due to dissolution/coarsening of carbides • The enrichment of carbide particles by titanium • Abnormal grain growth due to grain boundary faceting at very high temperatures • The stagnancy of abnormal grain growth by annealing beyond a critical time.« less

The threshold effects of Nd and Ho: YAG laser-induced surface modification on demineralization of dentin surfaces.

PubMed

Kinney, J H; Haupt, D L; Balooch, M; White, J M; Bell, W L; Marshall, S J; Marshall, G W

1996-06-01

Laser irradiation alters the structure of dentin and produces surface layers that give the appearance of being more enamel-like. The laser-modified surface may be more resistant to demineralization; hence, many investigators are proposing continued development of the laser as a possible preventive treatment for caries. The purpose of this study was to explore the morphological changes that occur in dentin when treated at threshold illuminance with two clinically interesting laser wavelengths, and to evaluate the effectiveness of the laser-treated surface at resisting demineralization in an acid-gel solution. The Nd: YAG laser (wavelength 1060 nm) produced significant recrystallization and grain growth of the apatite, without the formation of second phases such as beta-tricalcium phosphate. This recrystallized surface layer showed resistance to demineralization; however, the layer did not provide protection of the underlying dentin from demineralization because of cracks and macroscopic voids that allowed for penetration of the demineralizing gel. The Ho: YAG laser-treated surface (wavelength 2100 nm) did not show significant evidence of recrystallization and grain growth, and only a trace amount of an acid-resistant layer was observed with demineralization. It is speculated that the Ho:YAG laser is coupling with absorbed water, and that the heat transfer from the water to the mineral phase is inefficient. For the purposes of creating a demineralization-resistant layer, threshold illuminance with both Nd: YAG and Ho: YAG was ineffective.

Modeling the microstructural changes during hot tandem rolling of AA5 XXX aluminum alloys: Part I. Microstructural evolution

NASA Astrophysics Data System (ADS)

Wells, M. A.; Samarasekera, I. V.; Brimacombe, J. K.; Hawbolt, E. B.; Lloyd, D. J.

1998-06-01

A comprehensive mathematical model of the hot tandem rolling process for aluminum alloys has been developed. Reflecting the complex thermomechanical and microstructural changes effected in the alloys during rolling, the model incorporated heat flow, plastic deformation, kinetics of static recrystallization, final recrystallized grain size, and texture evolution. The results of this microstructural engineering study, combining computer modeling, laboratory tests, and industrial measurements, are presented in three parts. In this Part I, laboratory measurements of static recrystallization kinetics and final recrystallized grain size are described for AA5182 and AA5052 aluminum alloys and expressed quantitatively by semiempirical equations. In Part II, laboratory measurements of the texture evolution during static recrystallization are described for each of the alloys and expressed mathematically using a modified form of the Avrami equation. Finally, Part III of this article describes the development of an overall mathematical model for an industrial aluminum hot tandem rolling process which incorporates the microstructure and texture equations developed and the model validation using industrial data. The laboratory measurements for the microstructural evolution were carried out using industrially rolled material and a state-of-the-art plane strain compression tester at Alcan International. Each sample was given a single deformation and heat treated in a salt bath at 400 °C for various lengths of time to effect different levels of recrystallization in the samples. The range of hot-working conditions used for the laboratory study was chosen to represent conditions typically seen in industrial aluminum hot tandem rolling processes, i.e., deformation temperatures of 350 °C to 500 °C, strain rates of 0.5 to 100 seconds and total strains of 0.5 to 2.0. The semiempirical equations developed indicated that both the recrystallization kinetics and the final recrystallized grain size were dependent on the deformation history of the material i.e., total strain and Zener-Hollomon parameter ( Z), where Z = dot \\varepsilon exp left( {{Q_{def} }/{RT_{def }}} right) and time at the recrystallization temperature.

Monte Carlo modeling of recrystallization processes in α-uranium

DOE PAGES

Steiner, M. A.; McCabe, R. J.; Garlea, E.; ...

2017-08-01

In this study, starting with electron backscattered diffraction (EBSD) data obtained from a warm clock-rolled α-uranium deformation microstructure, a Potts Monte Carlo model was used to simulate static site-saturated recrystallization while testing a number of different conditions for the assignment of recrystallized nuclei within the microstructure. The simulations support observations that recrystallized nuclei within α-uranium form preferentially on non-twin high-angle grain boundary sites at 450 °C, and demonstrate that the most likely nucleation sites on these boundaries can be identified by the surrounding degree of Kernel Average Misorientation (KAM), which may be considered as a proxy for the local geometricallymore » necessary dislocation (GND) density.« less

Characterization of thermoplastic polyimide NEW-TPI

NASA Technical Reports Server (NTRS)

Hou, T. H.; Reddy, R. M.

1991-01-01

Thermal and rheological properties of a commercial thermoplastic polyimide, NEW-TPI, were characterized. The as-received material possesses initially a transient crystallite form with a bimodal distribution in peak melting temperatures. After the meltings of the initial crystallite structures, the sample can be recrystallized by various thermal treatments. A bimodal or single-modal melting peak distribution is formed for annealing temperatures below or above 360 C, respectively. The recrystallized crystallinities are all transient in nature. The polymers are unable to be recrystallized after being subjected to elevated temperature annealing above 450 C. The recrystallization mechanism was postulated, and a simple kinetics model was found to describe the behavior satisfactorily under conditions of prolonged thermal annealing.

Effect of one-step recrystallization on the grain boundary evolution of CoCrFeMnNi high entropy alloy and its subsystems

PubMed Central

Chen, Bo-Ru; Yeh, An-Chou; Yeh, Jien-Wei

2016-01-01

In this study, the grain boundary evolution of equiatomic CoCrFeMnNi, CoCrFeNi, and FeCoNi alloys after one-step recrystallization were investigated. The special boundary fraction and twin density of these alloys were evaluated by electron backscatter diffraction analysis. Among the three alloys tested, FeCoNi exhibited the highest special boundary fraction and twin density after one-step recrystallization. The special boundary increment after one-step recrystallization was mainly affected by grain boundary velocity, while twin density was mainly affected by average grain boundary energy and twin boundary energy. PMID:26923713

Effect of friction stir processing on tribological properties of Al-Si alloys

NASA Astrophysics Data System (ADS)

Aktarer, S. M.; Sekban, D. M.; Yanar, H.; Purçek, G.

2017-02-01

As-cast Al-12Si alloy was processed by single-pass friction stir processing (FSP), and its effect on mainly friction and wear properties of processed alloy was studied in detail. The needle-shaped eutectic silicon particles were fragmented by intense plastic deformation and dynamic recrystallization during FSP. The fragmented and homogenously distributed Si particles throughout the improve the mechanical properties and wear behavior of Al-12Si alloy. The wear mechanisms for this improvement were examined and the possible reasons were discussed.

Computational Analysis of Material Flow During Friction Stir Welding of AA5059 Aluminum Alloys

DTIC Science & Technology

2011-01-01

tool material (AISI H13 tool steel ) is modeled as an isotropic linear-elastic material. Within the analysis, the effects of some of the FSW key process...threads/m; (b) tool 598 material = AISI H13 tool steel ; (c) workpiece material = 599 AA5059; (d) tool rotation speed = 500 rpm; (e) tool travel 600 speed...the strain-hardening term is augmented to take into account for the effect of dynamic recrystallization) while the FSW tool material (AISI H13

The Role of Solvent Reorganization Dynamics in Electron-Transfer Processes. Theory-Experiment Comparisons for Electrochemical and Homogeneous Electron Exchange Involving Metallocene Redox Couples

DTIC Science & Technology

1985-08-01

Kodak) by crystallization from acetone; it was recrystallized twice from ethanol and dried in a vacuum oven. Tetraethylamonium perchlorate (TEAP) (G...the electrooxidation of in(Cp’) 2 , which yielded significantly smaller reverse (cathodic) currents in the most strongly coordinating solvents (DMX...DM50) at slower scan rates (< 0.5 V sec-1). Nevertheless, satisfactory a.c. polarograms were obtained for each of these system=. 5 4 Temperature

The effect of precipitation on the evolution of recrystallization textures in an AA 8011 aluminum alloy sheet

NASA Astrophysics Data System (ADS)

Ryu, Jong-Ho; Lee, Yoon-Soo; Lee, Dong Nyung

2001-06-01

The texture of an AA 8011 aluminum alloy sheet cold rolled by 95% showed a typical β-fiber, which runs from the copper orientation [C={112}<111>] over S [{123}<634>] to brass [B={011}<112>]. The development of annealing textures depended on annealing temperatures due to the interaction between precipitation and recrystallization. Upon annealing at a low temperature of 275°C, precipitation took place before recrystallization. This led to a weak recrystallization texture consisting of {011}<122>, {001˜<100>, and {hk0}<001>, among which the {011}<122> orientation developed near large FeAl3 particles as the main orientation and the cube [{001}<100>] orientation originating from the matrix was relatively weak. After annealing at 350 and 500°C, a strong cube texture developed along with a weak {011}<122> orientation. When the cube orientation developed, the copper orientation disappeared most rapidly. These results were discussed based on the interaction between precipitation and recrystallization.

Microstructure evolution and texture development of hot form-quench (HFQ) AZ31 twin roll cast (TRC) magnesium alloy

NASA Astrophysics Data System (ADS)

Alias, J.; Zhou, X.; Das, Sanjeev; El-Fakir, Omer; Thompson, G. E.

2017-12-01

The present study on the microstructure evolution of hot form-quench (HFQ) AZ31 twin roll cast magnesium alloy attempt to provide an understanding on the grain structure and heterogeneous intermetallic phase formation in the alloy and texture development following the HFQ process. Grain recrystallization and partial dissolution of eutectic β-Mg17Al12 phase particles were occurred during the solution heat treatment at 450°C, leaving the alloy consists of recrystallized grains and discontinuous or random β-Mg17Al12 phase particles distribution with small volume fraction. The particles act as effective nucleation sites for new grains during recrystallization and variation of recrystallization occurrence contributed to texture alteration. The partial or full β-Mg17Al12 phase dissolution following the HFQ induces void formation that act as fracture nucleation site and the corresponding texture alteration in the recrystallized grains led to poor formability in TRC alloy.

Recrystallization texture in nickel heavily deformed by accumulative roll bonding

NASA Astrophysics Data System (ADS)

Mishin, O. V.; Zhang, Y. B.; Godfrey, A.

2017-07-01

The recrystallization behavior of Ni processed by accumulative roll bonding to a total accumulated von Mises strain of 4.8 has been examined, and analyzed with respect to heterogeneity in the deformation microstructure. The regions near the bonding interface are found to be more refined and contain particle deformation zones around fragments of the steel wire brush used to prepare the surface for bonding. Sample-scale gradients are also observed, manifested as differences between the subsurface, intermediate and central layers, where the distributions of texture components are different. These heterogeneities affect the progress of recrystallization. While the subsurface and near-interface regions typically contain lower frequencies of cube-oriented grains than anywhere else in the sample, a strong cube texture forms in the sample during recrystallization, attributed to both a high nucleation rate and fast growth rate of cube-oriented grains. The observations highlight the sensitivity of recrystallization to heterogeneity in the deformation microstructure and demonstrate the importance of characterizing this heterogeneity over several length scales.

The Influence of Interfacial Roughness on Fiber Sliding in Oxide Composites with La-Monazite Interphases

NASA Technical Reports Server (NTRS)

Davis, J. B.; Hay, R. S.; Marshall, D. B.; Morgan, P. E. D.; Sayir, A.; Gray, Hugh R. (Technical Monitor); Farmer, Serene C. (Technical Monitor)

2002-01-01

Room temperature debonding and sliding of La-Monazite coated fibers is assessed using a composite with a polycrystalline alumina matrix and fibers of several different single crystal (mullite, sapphire) and directionally solidified eutectic (Al2O3/Y3Al5O12 and Al2O3/Y-ZrO2) compositions. These fibers provide a range of residual stresses and interfacial roughnesses. Sliding occurred over a debond crack at the fiber-coating interface when the sliding displacement and surface roughness were relatively small. At large sliding displacements with relatively rough interfaces, the monazite coatings were deformed extensively by fracture, dislocations and occasional twinning, whereas the fibers were undamaged. Dense, fine-grained (10 nm) microstructures suggestive of dynamic recrystallization were also observed in the coatings. Frictional heating during sliding is assessed. The possibility of low temperature recrystallization is discussed in the light of the known resistance of monazite to radiation damage. The ability of La-Monazite to undergo plastic deformation relatively easily at low temperatures may be enabling for its use as a composite interface.

Dislocation loop formation by swift heavy ion irradiation of metals.

PubMed

Khara, Galvin S; Murphy, Samuel T; Duffy, Dorothy M

2017-07-19

A coupled two-temperature, molecular dynamics methodology is used to simulate the structural evolution of bcc metals (Fe and W) and fcc metals (Cu and Ni) following irradiation by swift heavy ions. Electronic temperature dependent electronic specific heat capacities and electron-phonon coupling strengths are used to capture the full effects of the variation in the electronic density of states. Tungsten is found to be significantly more resistant to damage than iron, due both to the higher melting temperature and the higher thermal conductivity. Very interesting defect structures, quite different from defects formed in cascades, are found to be created by swift heavy ion irradiation in the bcc metals. Isolated vacancies form a halo around elongated interstitial dislocation loops that are oriented along the ion path. Such configurations are formed by rapid recrystallization of the molten cylindrical region that is created by the energetic ion. Vacancies are created at the recrystallization front, resulting in excess atoms at the core which form interstitial dislocation loops on completion of crystallization. These unique defect structures could, potentially, be used to create metal films with superior mechanical properties and interesting nanostructures.

Dislocation loop formation by swift heavy ion irradiation of metals

NASA Astrophysics Data System (ADS)

Khara, Galvin S.; Murphy, Samuel T.; Duffy, Dorothy M.

2017-07-01

A coupled two-temperature, molecular dynamics methodology is used to simulate the structural evolution of bcc metals (Fe and W) and fcc metals (Cu and Ni) following irradiation by swift heavy ions. Electronic temperature dependent electronic specific heat capacities and electron-phonon coupling strengths are used to capture the full effects of the variation in the electronic density of states. Tungsten is found to be significantly more resistant to damage than iron, due both to the higher melting temperature and the higher thermal conductivity. Very interesting defect structures, quite different from defects formed in cascades, are found to be created by swift heavy ion irradiation in the bcc metals. Isolated vacancies form a halo around elongated interstitial dislocation loops that are oriented along the ion path. Such configurations are formed by rapid recrystallization of the molten cylindrical region that is created by the energetic ion. Vacancies are created at the recrystallization front, resulting in excess atoms at the core which form interstitial dislocation loops on completion of crystallization. These unique defect structures could, potentially, be used to create metal films with superior mechanical properties and interesting nanostructures.

Microstructure Characterization and Stress Corrosion Evaluation of Autogenous and Hybrid Friction Stir Welded Al-Cu-Li 2195 Alloy

NASA Technical Reports Server (NTRS)

Li, Zhixian; Arbegast, William J.; Meletis, Efstathios I.

1997-01-01

Friction stir welding process is being evaluated for application on the Al-Cu-Li 2195 Super-Light Weight External Tank of the Space Transportation System. In the present investigation Al-Cu-Li 2195 plates were joined by autogenous friction stir welding (FSW) and hybrid FSW (friction stir welding over existing variable polarity plasma arc weld). Optical microscopy and transmission electron microscopy (TEM) were utilized to characterize microstructures of the weldments processed by both welding methods. TEM observations of autogenous FSW coupons in the center section of the dynamically-recrystallized zone showed an equiaxed recrystallized microstructure with an average grain size of approx. 3.8 microns. No T(sub 1), precipitates were present in the above-mentioned zone. Instead, T(sub B) and alpha precipitates were found in this zone with a lower population. Alternate immersion, anodic polarization, constant load, and slow strain tests were carried out to evaluate the general corrosion and stress-corrosion properties of autogenous and hybrid FSW prepared coupons. The experimental results will be discussed.

Microstructure Evolution and Flow Stress Model of a 20Mn5 Hollow Steel Ingot during Hot Compression.

PubMed

Liu, Min; Ma, Qing-Xian; Luo, Jian-Bin

2018-03-21

20Mn5 steel is widely used in the manufacture of heavy hydro-generator shaft due to its good performance of strength, toughness and wear resistance. However, the hot deformation and recrystallization behaviors of 20Mn5 steel compressed under high temperature were not studied. In this study, the hot compression experiments under temperatures of 850-1200 °C and strain rates of 0.01/s-1/s are conducted using Gleeble thermal and mechanical simulation machine. And the flow stress curves and microstructure after hot compression are obtained. Effects of temperature and strain rate on microstructure are analyzed. Based on the classical stress-dislocation relation and the kinetics of dynamic recrystallization, a two-stage constitutive model is developed to predict the flow stress of 20Mn5 steel. Comparisons between experimental flow stress and predicted flow stress show that the predicted flow stress values are in good agreement with the experimental flow stress values, which indicates that the proposed constitutive model is reliable and can be used for numerical simulation of hot forging of 20Mn5 hollow steel ingot.

Quantifying the effect of diagenetic recrystallization on the Mg isotopic composition of marine carbonates

NASA Astrophysics Data System (ADS)

Chanda, Piyali; Fantle, Matthew S.

2017-05-01

The Mg and Sr isotopic compositions (δ26Mg and 87Sr/86Sr) of pore fluids and bulk carbonates from Ocean Drilling Project Site 1171 (South Tasman Rise; 2148.2 m water depth) are reported, in order to evaluate the potential of diagenesis to alter carbonate-based geochemical proxies in an open marine system. Given the trace amounts of Mg in marine carbonates relative to coexisting pore fluids, diagenesis can alter carbonate δ26Mg, a promising proxy for seawater δ26Mg that may help elucidate long-term changes in the global Mg cycle. Constraints on the effect of diagenetic recrystallization on carbonate δ26Mg are therefore critical for accurate proxy interpretations. This study provides context for assessing the fidelity of geochemical proxy-reconstructions using the primary components (i.e., foraminiferal tests and nannofossils) of bulk carbonate sediments. We find that pore fluid δ26Mg values (on the DSM3 scale) at Site 1171 increase systematically with depth (from -0.72‰ to -0.39‰ in the upper ∼260 m), while the δ26Mg of bulk carbonates decrease systematically with depth (from -2.23‰ to -5.00‰ in the upper ∼260 m). This variability is ascribed primarily to carbonate recrystallization, with a small proportion of the variability due to down-hole changes in nannofossil and foraminiferal species composition. The inferred effect of diagenesis on bulk carbonate δ26Mg correlates with down-core changes in Mg/Ca, Sr/Ca, Na/Ca, and 87Sr/86Sr. A depositional reactive-transport model is employed to validate the hypothesis that calcite recrystallization in this system can generate sizeable shifts in carbonate δ26Mg. Model fits to the data suggest a fractionation factor and a partition coefficient that are consistent with previous work, assuming calcite recrystallization rates of ⩽7%/Ma constrained by Sr geochemistry. In addition, either partial dissolution or a distinctly different previous diagenetic regime must be invoked in order to explain aspects of the elemental chemistry and 87Sr/86Sr of relatively deep sediments from Holes A and C. This study indicates that the dynamics of a given sedimentary system can significantly alter bulk carbonate geochemistry, and presents a framework for considering the potential impact of such alteration on picked archives such as foraminiferal tests and nannofossils. Ultimately, this study contributes to the development of δ26Mg as a proxy for seawater δ26Mg by quantifying the susceptibility of carbonate δ26Mg to diagenetic alteration, particularly in sediments in open marine systems. This study suggests that because of the sensitivity of carbonate δ26Mg to diagenetic recrystallization, it can, in certain systems, be used to quantify the impact of diagenesis on carbonate-based geochemical proxies.

Photoacoustic Imaging.

DTIC Science & Technology

1983-12-01

recrystallization is currently an active area of research. Much effort has been made to grow large grain polysilicon with grain sizes of 100 microns from fine grain... polysilicon using laser recrystallization. The recrystallization process is inherently traumatic, producing large changes in temperature in short...temperature distribution above as the source term in the acoustic field equation, we ol fain r where B1)jwP) The general solution to this equation is given by

A quasi-in-situ EBSD observation of the transformation from rolling texture to recrystallization texture in V-4Cr-4Ti alloy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Peng, Lixia

Recrystallization texture evolution of rolled V-4Cr-4Ti alloy has been investigated by quasi-in-situ EBSD (electron back-scattering diffraction) method. Concurrently, the precipitates were characterized by SEM (Scanning Electron Microscopy). It was found that both the initial rolling textures and the distribution of the precipitates affected the formation of the recrystallization texture. It was revealed that the texture transformations of (558) 〈110〉 + (665) 〈110〉 to (334) 〈483〉 + (665) 〈1 1 2.4〉 were possibly attributed to the selective drag induced by the sparsely dispersed Ti-rich precipitates. While the densely distributed Ti-rich precipitates were responsible for the randomized recrystallization texture. Finally, when themore » precipitates were absent, the orientation changes from (112) 〈110〉 and (558) 〈110〉 to (111) 〈112〉 and (001) <110> to (001) <520> were observed. - Highlights: • Micro recrystallization texture evolution in V-4Cr-4Ti alloys is reported for the first time. • The volume fraction of Ti-rich precipitates has significant effect on the recrystallization texture evolution. • The dissolution of the Ti-rich precipitates above 1100 °C induces the strengthening of (111) <112> texture.« less

In-situ observation of recrystallization in an AlMgScZr alloy using confocal laser scanning microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Taendl, J., E-mail: johannes.taendl@tugraz.atl; Nambu, S.; Orthacker, A.

2015-10-15

In this work we present a novel in-situ approach to study the recrystallization behavior of age hardening alloys. We use confocal laser scanning microscopy (CLSM) at 400 °C to investigate the static recrystallization of an AlMg4Sc0.4Zr0.12 alloy in-situ. The results are combined with electron backscatter diffraction (EBSD) and transmission electron microscopy (TEM) analyses. It was found that CLSM is a powerful tool to visualize both the local initiation and temporal sequence of recrystallization. After fast nucleation and initial growth, the grain growth rate decreases and the grain boundary migration stops after some minutes due to Zener pinning from Al{sub 3}(Sc,Zr)more » precipitates produced during the heat treatment. EBSD and TEM analyses confirm both the boundary movements and the particle-boundary interactions. - Highlights: • First time that CLSM is used to study recrystallization in-situ. • The start and end of recrystallization can be directly observed. • The procedure is easy to apply and requires only simple data interpretation. • In-situ observations on the surface correlate to modifications inside the bulk. • In-situ observations correlate to EBSD and EFTEM analyses.« less

Cube texture formation during the early stages of recrystallization of Al-1%wt.Mn and AA1050 aluminium alloys

NASA Astrophysics Data System (ADS)

Miszczyk, M. M.; Paul, H.

2015-08-01

The cube texture formation during primary recrystallization was analysed in plane strain deformed samples of a commercial AA1050 alloy and an Al-1%wt.Mn model alloy single crystal of the Goss{110}<001> orientation. The textures were measured with the use of X-ray diffraction and scanning electron microscopy equipped with an electron backscattered diffraction facility. After recrystallization of the Al-1%wt.Mn single crystal, the texture of the recrystallized grains was dominated by four variants of the S{123}<634> orientation. The cube grains were only sporadically detected by the SEM/EBSD system. Nevertheless, an increased density of <111> poles corresponding to the cube orientation was observed. The latter was connected with the superposition of four variants of the S{123}<634> orientation. This indicates that the cube texture after the recrystallization was a ‘compromise texture’. In the case of the recrystallized AA1050 alloy, the strong cube texture results from both the increased density of the particular <111> poles of the four variants of the S orientation and the ∼40°(∼< 111>)-type rotation. The first mechanism transforms the Sdef-oriented areas into Srex ones, whereas the second the near S-oriented, as-deformed areas into near cube-oriented grains.

Influence of Heating Rate on Ferrite Recrystallization and Austenite Formation in Cold-Rolled Microalloyed Dual-Phase Steels

NASA Astrophysics Data System (ADS)

Philippot, C.; Bellavoine, M.; Dumont, M.; Hoummada, K.; Drillet, J.; Hebert, V.; Maugis, P.

2018-01-01

Compared with other dual-phase (DP) steels, initial microstructures of cold-rolled martensite-ferrite have scarcely been investigated, even though they represent a promising industrial alternative to conventional ferrite-pearlite cold-rolled microstructures. In this study, the influence of the heating rate (over the range of 1 to 10 K/s) on the development of microstructures in a microalloyed DP steel is investigated; this includes the tempering of martensite, precipitation of microalloying elements, recrystallization, and austenite formation. This study points out the influence of the degree of ferrite recrystallization prior to the austenite formation, as well as the importance of the cementite distribution. A low heating rate giving a high degree of recrystallization, leads to the formation of coarse austenite grains that are homogenously distributed in the ferrite matrix. However, a high heating rate leading to a low recrystallization degree, results in a banded-like structure with small austenite grains surrounded by large ferrite grains. A combined approach, involving relevant multiscale microstructural characterization and modeling to rationalize the effect of the coupled processes, highlights the role of the cold-worked initial microstructure, here a martensite-ferrite mixture: recrystallization and austenite formation commence in the former martensite islands before extending in the rest of the material.

Investigation of the Atypical Glass Transition and Recrystallization Behavior of Amorphous Prazosin Salts

PubMed Central

Kumar, Lokesh; Popat, Dharmesh; Bansal, Arvind K.

2011-01-01

This manuscript studied the effect of counterion on the glass transition and recrystallization behavior of amorphous salts of prazosin. Three amorphous salts of prazosin, namely, prazosin hydrochloride, prazosin mesylate and prazosin tosylate were prepared by spray drying, and characterized by optical-polarized microscopy, differential scanning calorimetry and powder X-ray diffraction. Modulated differential scanning calorimetry was used to determine the glass transition and recrystallization temperature of amorphous salts. Glass transition of amorphous salts followed the order: prazosin mesylate > prazosin tosylate ∼ prazosin hydrochloride. Amorphous prazosin mesylate and prazosin tosylate showed glass transition, followed by recrystallization. In contrast, amorphous prazosin hydrochloride showed glass transition and recrystallization simultaneously. Density Functional Theory, however, suggested the expected order of glass transition as prazosin hydrochloride > prazosin mesylate > prazosin tosylate. The counterintuitive observation of amorphous prazosin hydrochloride having lower glass transition was explained in terms of its lower activation energy (206.1 kJ/mol) for molecular mobility at Tg, compared to that for amorphous prazosin mesylate (448.5 kJ/mol) and prazosin tosylate (490.7 kJ/mol), and was further correlated to a difference in hydrogen bonding strength of the amorphous and the corresponding recrystallized salts. This study has implications in selection of an optimal amorphous salt form for pharmaceutical development. PMID:24310595

Investigation of the atypical glass transition and recrystallization behavior of amorphous prazosin salts.

PubMed

Kumar, Lokesh; Popat, Dharmesh; Bansal, Arvind K

2011-08-25

This manuscript studied the effect of counterion on the glass transition and recrystallization behavior of amorphous salts of prazosin. Three amorphous salts of prazosin, namely, prazosin hydrochloride, prazosin mesylate and prazosin tosylate were prepared by spray drying, and characterized by optical-polarized microscopy, differential scanning calorimetry and powder X-ray diffraction. Modulated differential scanning calorimetry was used to determine the glass transition and recrystallization temperature of amorphous salts. Glass transition of amorphous salts followed the order: prazosin mesylate > prazosin tosylate ~ prazosin hydrochloride. Amorphous prazosin mesylate and prazosin tosylate showed glass transition, followed by recrystallization. In contrast, amorphous prazosin hydrochloride showed glass transition and recrystallization simultaneously. Density Functional Theory, however, suggested the expected order of glass transition as prazosin hydrochloride > prazosin mesylate > prazosin tosylate. The counterintuitive observation of amorphous prazosin hydrochloride having lower glass transition was explained in terms of its lower activation energy (206.1 kJ/mol) for molecular mobility at Tg, compared to that for amorphous prazosin mesylate (448.5 kJ/mol) and prazosin tosylate (490.7 kJ/mol), and was further correlated to a difference in hydrogen bonding strength of the amorphous and the corresponding recrystallized salts. This study has implications in selection of an optimal amorphous salt form for pharmaceutical development.

Inhibition of Recrystallization of Amorphous Lactose in Nanocomposites Formed by Spray-Drying.

PubMed

Hellrup, Joel; Alderborn, Göran; Mahlin, Denny

2015-11-01

This study aims at investigating the recrystallization of amorphous lactose in nanocomposites. In particular, the focus is on the influence of the nano- to micrometer length scale nanofiller arrangement on the amorphous to crystalline transition. Further, the relative significance of formulation composition and manufacturing process parameters for the properties of the nanocomposite was investigated. Nanocomposites of amorphous lactose and fumed silica were produced by co-spray-drying. Solid-state transformation of the lactose was studied at 43%, 84%, and 94% relative humidity using X-ray powder diffraction and microcalorimetry. Design of experiments was used to analyze spray-drying process parameters and nanocomposite composition as factors influencing the time to 50% recrystallization. The spray-drying process parameters showed no significant influence. However, the recrystallization of the lactose in the nanocomposites was affected by the composition (fraction silica). The recrystallization rate constant decreased as a function of silica content. The lowered recrystallization rate of the lactose in the nanocomposites could be explained by three mechanisms: (1) separation of the amorphous lactose into discrete compartments on a micrometer length scale (compartmentalization), (2) lowered molecular mobility caused by molecular interactions between the lactose molecules and the surface of the silica (rigidification), and/or (3) intraparticle confinement of the amorphous lactose. © 2015 Wiley Periodicals, Inc. and the American Pharmacists Association.

Preparation and recrystallization behavior of spray-dried co-amorphous naproxen-indomethacin.

PubMed

Beyer, Andreas; Radi, Lydia; Grohganz, Holger; Löbmann, Korbinian; Rades, Thomas; Leopold, Claudia S

2016-07-01

To improve the dissolution properties and the physical stability of amorphous active pharmaceutical ingredients, small molecule stabilizing agents may be added to prepare co-amorphous systems. The objective of the study was to investigate if spray-drying allows the preparation of co-amorphous drug-drug systems such as naproxen-indomethacin and to examine the influence of the process conditions on the resulting initial sample crystallinity and the recrystallization behavior of the drug(s). For this purpose, the process parameters inlet temperature and pump feed rate were varied according to a 2(2) factorial design and the obtained samples were analyzed with X-ray powder diffractometry and Fourier-transformed infrared spectroscopy. Evaluation of the data revealed that the preparation of fully amorphous samples could be achieved depending on the process conditions. The resulting recrystallization behavior of the samples, such as the total recrystallization rate, the individual recrystallization rates of naproxen and indomethacin as well as the polymorphic form of indomethacin that was formed were influenced by these process conditions. For initially amorphous samples, it was found that naproxen and indomethacin recrystallized almost simultaneously, which supports the theory of formation of drug-drug heterodimers in the co-amorphous phase. Copyright © 2016 Elsevier B.V. All rights reserved.

Effects of rolling conditions on recrystallization microstructure and texture in magnetostrictive Fe-Ga-Al rolled sheets

NASA Astrophysics Data System (ADS)

Li, Jiheng; Liu, Yangyang; Li, Xiaojuan; Mu, Xing; Bao, Xiaoqian; Gao, Xuexu

2018-07-01

The effects of different rolling conditions on the microstructure and texture of primary and secondary recrystallization in magnetostrictive Fe82Ga9Al9+0.1at%NbC alloy sheets were investigated. After the primary recrystallization annealing at 850 °C for 5 min, the as-rolled sheets prepared by warm-cold rolling with an intermediate annealing, can be fully recrystallized, and obtain the homogeneous matrix in which the fine dispersed NbC precipitate particles are distributed. The primary recrystallization textures of sheets with different rolling conditions consist mostly of strong {1 0 0} textures, γ-fiber textures, {4 1 1}〈1 4 8〉 texture and weak Goss texture. In the primary recrystallized sheets prepared by warm-cold rolling with an intermediate annealing, the high energy grain boundaries and ∑9 boundaries have the highest proportion. After high temperature annealing, the secondary recrystallizations of Goss grains in these sheets are more complete, and the size of abnormal grown Goss grain is up to several centimeters, which results in the strongest Goss texture. Correspondingly, the largest magnetostriction of 183 ppm is observed. The sample prepared by warm-cold rolling with an intermediate annealing, has homogeneous primary matrix, special texture components and grain boundary distribution, all of which provide a better surrounding for the abnormal growth of Goss grains. This work indicates that the control of rolling conditions of Fe-Ga-Al alloy sheets is necessary to achieve the strong Goss texture and obtain a possible high magnetostriction if other appropriate conditions (stress, domain structure) are achieved.

Improvement of physicomechanical properties of carbamazepine by recrystallization at different pH values.

PubMed

Javadzadeh, Yousef; Mohammadi, Ameneh; Khoei, Nazaninossadat Seyed; Nokhodchi, Ali

2009-06-01

The morphology of crystals has an appreciable impact role on the physicochemical properties of drugs. Drug properties such as flowability, dissolution, hardness and bioavailability may be affected by crystallinity behaviours of drugs. The objective of this study was to achieve an improved physicomechanical property of carbamazepine powder through recrystallization from aqueous solutions at different pH values. For this purpose, carbamazapine was recrystallized from aqueous solutions at different pH values (1, 7, 11). The morphology of crystals was investigated using scanning electron microscopy; X-ray powder diffraction (XRPD) was used to identify polymorphism; thermodynamic properties were analyzed using differential scanning calorimetery (DSC). Dissolution rate was determined using USP dissolution apparatus. Mechanical behavior of recrystallized carbamazepine powders was investigated by making tablets under different compaction pressure and measuring their hardness. SEM studies showed that the carbamazepine crystallization in different media affected the morphology and size of carbamazepine crystals. The shape of carbamazepine crystals changed from flaky or thin plate-like to needle shape. XRPD and DSC results ruled out any crystallinity changes occurring due to the temperature during recrystallization procedure or pH of crystallization media. The crushing strength of tablets indicated that all of the recrystallized carbamazepine samples had better compactiblity than the original carbamazepine powder. In vitro dissolution studies of carbamazepine samples showed a higher dissolution rate for carbamazepine crystals obtained from media with pH 11 and 1. Carbamazepine particles recrystallized from aqueous solutions of different pH values (all media) appeared to have superior mechanical properties to those of the original carbamazepine sample.

Two-step recrystallization of water in concentrated aqueous solution of poly(ethylene glycol).

PubMed

Gemmei-Ide, Makoto; Motonaga, Tetsuya; Kasai, Ryosuke; Kitano, Hiromi

2013-02-21

Crystallization behavior of water in a concentrated aqueous solution of poly(ethylene glycol) (PEG) with a water content of 37.5 wt % was investigated by temperature variable mid-infrared (mid-IR) spectroscopy in a temperature range of 298-170 K. The mid-IR spectrum of water at 298 K showed that a large water cluster was not formed and that most of the water molecules were associated with the PEG chain. Ice formation, however, occurred as found in previous studies by differential scanning calorimetory. Ice formations were grouped into three types: crystallization at 231 K during cooling, that at 198 K during heating, and that at 210 K during heating. The latter two were just recrystallization. These ice formations were the direct transition from hydration species to ice without condensation regardless of crystallization or recrystallization. This means that the recrystallized water in the present system was not generated from low-density amorphous solid water. At a low cooling rate, nearly complete crystallization at 231 K during cooling and no recrystallization were observed. At a high cooling rate, no crystallization and two-step recrystallization at 198 and 210 K were observed. The former and latter recrystallizations were found to be generated from water associated with the PEG chains with ttg (the sequence -O-CH(2)-CH(2)-O- having a trans (t) conformation about the -C-O- bond and a gauche (g) conformation about the -C-C- bond) and random conformations, respectively. These results indicate that recrystallizable water does not have a single specific water structure.

Deformation Mechanism and Recrystallization Relationships in Galfenol Single Crystals: On the Origin of Goss and Cube Orientations

NASA Astrophysics Data System (ADS)

Na, Suok-Min; Smith, Malcolm; Flatau, Alison B.

2018-06-01

In this work, deformation mechanism related to recrystallization behavior in single-crystal disks of Galfenol (Fe-Ga alloy) was investigated to gain insights into the influence of crystal orientations on structural changes and selective grain growth that take place during secondary recrystallization. We started with the three kinds of single-crystal samples with (011)[100], (001)[100], and (001)[110] orientations, which were rolled and annealed to promote the formation of different grain structures and texture evolutions. The initial Goss-oriented (011)[100] crystal mostly rotated into {111}<112> orientations with twofold symmetry and shear band structures by twinning resulted in the exposure of rolled surface along {001}<110> orientation during rolling. In contrast, the Cube-oriented (001)[100] single crystal had no change in texture during rolling with the thickness reduction up to 50 pct. The {123}<111> slip systems were preferentially activated in these single crystals during deformation as well as {112}<111> slip systems that are known to play a role in primary slip of body-centered cubic (BCC) materials such as α-iron and Fe-Si alloys. After annealing, the deformed Cube-oriented single crystal had a small fraction (<10 pct) of recrystallized Goss-oriented grains. The weak Goss component remained in the shear bands of the 50 pct rolled Goss-oriented single crystal, and it appeared to be associated with coalescence of subgrains inside shear band structures during primary recrystallization. Rolling of the (001)[110] single crystal led to the formation of a tilted (001)[100] component close to the <120> orientation, associated with {123}<111> slip systems as well. This was expected to provide potential sites of nucleation for secondary recrystallization; however, no Goss- and Cube-oriented components actually developed in this sample during secondary recrystallization. Those results illustrated how the recrystallization behavior can be influenced by deformed structure and the slip systems.

Evolution of microstructure and grain boundary character distribution of a tin bronze annealed at different temperatures

DOE Office of Scientific and Technical Information (OSTI.GOV)

Huang, Weijiu; Chongqing Municipal Key Laboratory of Institutions of Higher Education for Mould Technology, Chongqing University of Technology, Chongqing 400054; Chai, Linjiang, E-mail: chailinjiang@cqut.edu.cn

2016-04-15

Specimens cut from a rolled tin bronze sheet were annealed at 400–800 °C for 1 h and evolution of their microstructures was then characterized in details by electron channeling contrast imaging and electron backscatter diffraction techniques. Particularly, statistics on special boundaries (SBs) with Σ ≤ 29 and network connectivity of random high angle boundaries (HABs) in the annealed specimens were examined to probe optimization potentials of grain boundary character distribution (GBCD) for this material. Results show that the deformed microstructure in the as-received material begins to be recrystallized when the annealing temperature increase to 500 °C and average grain sizesmore » surge with further increasing temperatures. As a result of the recrystallization, a large number of annealing twins (with Σ3 misorientation) are produced, leading to remarkably increased fractions of SBs (f{sub SBs}). Thanks to preexisting dense low angle boundaries, the majority of SBs in the 500 °C specimen with only partial recrystallization are Σ3{sub ic} (incoherent) boundaries, which effectively disrupt connectivity of random HABs network. Although the f{sub SBs} can be further increased (up to 72.5%) in specimens with full recrystallization (at higher temperatures), the Σ3{sub ic} boundaries would be replaced to some extent by Σ3{sub c} (coherent) boundaries which do not contribute directly to optimizing the GBCD. This work should be able to provide clear suggestions on applying the concept of grain boundary engineering to tin bronze alloys. - Highlights: • The rolled tin bronze begins to be recrystallized as temperature increases to 500 °C. • A lot of SBs are produced after recrystallization and the highest f{sub SBs} is 72.5%. • Partially recrystallized specimen has the optimum GBCD due to more Σ3{sub ic} boundaries. • The Σ3{sub ic} boundaries are replaced by Σ3{sub c} boundaries after full recrystallization.« less

User-independent EBSD parameters to study the progress of recovery and recrystallization in Cu-Zn alloy during in situ heating.

PubMed

Sharma, N K; Shekhar, S

2016-12-01

Microstructural evolution of cold-rolled Cu-5%Zn alloy during in situ heating inside field-emission scanning electron microscope was utilized to obtain user-independent parameters in order to trace the progress of static recovery and recrystallization. Electron back-scattered diffraction (EBSD)-based orientation imaging microscopy was used to obtain micrographs at various stages of in situ heating. It is shown that unlike the pre-existing methods, additional EBSD-based parameter can be used to trace the progress of recovery and recrystallization, which is not dependent on user input and hence less prone to error. True strain of 0.3 was imposed during cold rolling of alloy sample. Rolled sample was subjected to in situ heating from room temperature to 500°C (∼0.58 Tm) with soaking time of 10 min, at each of the intermediate temperatures viz. 100, 200, 300, 400 and 450°C. After reaching 500°C, the sample was kept at this temperature for a maximum duration of around 15 h. The sample showed clear signs of recovery for temperature up to 450°C, and at 500°C, recrystallization started to take place. Recrystallization kinetics was moderate, and full recrystallization was achieved in approximately 120 min. We found that EBSD parameter, namely, band contrast intensity can be used as an extra handle to map out the progress of recrystallization occurring in the sample. By contrast, mean angular deviation can be used to understand the evolution of recovery in samples. The parameters mentioned in the current study, unlike other pre-existing methods, can also be used for mapping local microstructural transformations due to recovery and recrystallization. We discuss the benefits and limitations in using these additional handles in understanding the changes taking place in the material during in situ heating. © 2016 The Authors Journal of Microscopy © 2016 Royal Microscopical Society.

Effect of Aluminum on the Microstructure and Properties of Two Refractory High-Entropy Alloys (Postprint)

DTIC Science & Technology

2014-04-01

The chemical compositions of the recrystallized ic release; distribution unlimited. Fig. 5. (a) Equiaxed grain structure of the annealed...deformation bands crossing a grain boundary; (c) fine recrystallized grains formed at grain boundaries; (d) a higher magnification image shows the...presence of nano-precipitates at the boundaries of the recrystallized grains. 220 O.N. Senkov et al. / Acta Materialia 68 (2014) 214–228and non

Research and Process-Optimization on Mixed Crystal Caused Uneven-Performance of High-strength Structural Car Steel QStE500TM

NASA Astrophysics Data System (ADS)

Jian-wen, Li; Hong-yan, Liu

Handan Iron and Steel production of high-strength structural car steel QStE500TM thin gauge products using Nb + Ti composite strengthening, with a small amount of Cr element to improve its hardenability, the process parameter control is inappropriate with Nb + Ti complex steel, it is easy to produce in the mixed crystal phenomenon, resulting in decreasing the toughness and uneven performance. In this paper, Gleeble 3500 thermal simulation testing machine for high-strength structural steel car QStE500TM product deformation austenite recrystallization behavior research, determined completely recrystallized, partial recrystallization and non-recrystallization region, provide theoretical basis and necessary data for reasonable controlled rolling process for production.

Ice-Active Substances from the Infective Juveniles of the Freeze Tolerant Entomopathogenic Nematode, Steinernema feltiae.

PubMed

Ali, Farman; Wharton, David A

2016-01-01

Steinernema feltiae is a moderately freezing tolerant nematode, that can withstand intracellular ice formation. We investigated recrystallization inhibition, thermal hysteresis and ice nucleation activities in the infective juveniles of S. feltiae. Both the splat cooling assay and optical recrystallometry indicate the presence of ice active substances that inhibit recrystallization in the nematode extract. The substance is relatively heat stable and largely retains the recrystallization inhibition activity after heating. No thermal hysteresis activity was detected but the extract had a typical hexagonal crystal shape when grown from a single seed crystal and weak ice nucleation activity. An ice active substance is present in a low concentration, which may be involved in the freezing survival of this species by inhibiting ice recrystallization.

Electron backscatter diffraction study of deformation and recrystallization textures of individual phases in a cross-rolled duplex steel

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zaid, Md; Bhattacharjee, P.P., E-mail: pinakib@iith.ac.in

2014-10-15

The evolution of microstructure and texture during cross-rolling and annealing was investigated by electron backscatter diffraction in a ferritic–austenitic duplex stainless steel. For this purpose an alloy with nearly equal volume fraction of the two phases was deformed by multi-pass cross-rolling process up to 90% reduction in thickness. The rolling and transverse directions were mutually interchanged in each pass by rotating the sample by 90° around the normal direction. In order to avoid deformation induced phase transformation and dynamic strain aging, the rolling was carried out at an optimized temperature of 898 K (625 °C) at the warm-deformation range. Themore » microstructure after cross warm-rolling revealed a lamellar structure with alternate arrangement of the bands of two phases. Strong brass and rotated brass components were observed in austenite in the steel after processing by cross warm-rolling. The ferrite in the cross warm-rolling processed steel showed remarkably strong RD-fiber (RD//< 011 >) component (001)< 011 >. The development of texture in the two phases after processing by cross warm-rolling could be explained by the stability of the texture components. During isothermal annealing of the 90% cross warm-rolling processed material the lamellar morphology was retained before collapse of the lamellar structure to the mutual interpenetration of the phase bands. Ferrite showed recovery resulting in annealing texture similar to the deformation texture. In contrast, the austenite showed primary recrystallization without preferential orientation selection leading to the retention of deformation texture. The evolution of deformation and annealing texture in the two phases of the steel was independent of one another. - Highlights: • Effect of cross warm-rolling on texture formation is studied in duplex steel. • Brass texture in austenite and (001)<110 > in ferrite are developed. • Ferrite shows recovery during annealing retaining the (001)<110 > component. • Austenite shows recrystallization during annealing retaining the deformation texture. • The deformation of recrystallization of two phases is independent of one other.« less

Pressure Dependence of Magnesite Flow Strength

NASA Astrophysics Data System (ADS)

Millard, J. W.; Holyoke, C. W., III; McDaniel, C.; Raterron, P.; Kronenberg, A. K.; Tokle, L.

2017-12-01

Recent experiments by Holyoke et al. (2014) indicate that magnesite is weak compared with olivine, leading to strain localization into magnesite-bearing horizons of downgoing subducting slabs, potentially leading to intermediate (200-400 km) deep focus earthquakes DFEs. Flow strengths (σ) of magnesite were determined as functions of strain rate and temperature (T), but not of pressure (P). In order to determine the pressure dependence of magnesite deforming by dislocation creep and low temperature plasticity (LTP), we performed triaxial deformation experiments on natural, coarse-grained (80 μm) magnesite aggregates at T = 900oC, strain rate of 2*10-5/s and P from 3.2 to 7.9 GPa in the D-DIA at Beamline 6-BMB at the Advanced Photon Source at Argonne National Lab. Strengths of magnesite aggregates increase as a function of pressure, from σ=0.85 GPa (at P = 3.2 GPa) to 1.69 GPa (at P = 7.9 GPa). Microstructures developed at P ≤ 6.2 GPa include grain flattening and sweeping undulatory extinction, and dynamic recrystallization at grain boundaries (by bulge nucleation), consistent with dislocation creep. Microstructures generated at P ≥ 6.7 GPa include some twins and kink bands, grain flattening and patchy undulatory extinction, and bulging recrystallization at grain boundaries. These microstructures indicate contributions to strain of both LTP and dislocation creep mechanisms. The pressure dependence can be described by a thermally activated enthalpy, where s increases with P by way of an activation volume V*. Based on both D-DIA and Griggs apparatus results (of Holyoke et al., 2014), V* = 8.5 (± 0.5) × 10-6 m3 mol-1. This value is comparable to V* determined for creep of olivine (9.5 (± 7) × 10-6 m3 mol-1 Durham et al., 2009), indicating that the strength difference between magnesite and olivine will continue to be significant at high pressures, and lead to strain localization at all subduction zone depths.

Reconstruction of 3d grain boundaries from rock thin sections, using polarised light

NASA Astrophysics Data System (ADS)

Markus Hammes, Daniel; Peternell, Mark

2016-04-01

Grain boundaries affect the physical and chemical properties of polycrystalline materials significantly by initiating reactions and collecting impurities (Birchenall, 1959), and play an essential role in recrystallization (Doherty et al. 1997). In particular, the shape and crystallographic orientation of grain boundaries reveal the deformation and annealing history of rocks (Kruhl and Peternell 2002, Kuntcheva et al. 2006). However, there is a lack of non-destructive and easy-to-use computer supported methods to determine grain boundary geometries in 3D. The only available instrument using optical light to measure grain boundary angles is still the polarising microscope with attached universal stage; operated manually and time-consuming in use. Here we present a new approach to determine 3d grain boundary orientations from 2D rock thin sections. The data is recorded by using an automatic fabric analyser microscope (Peternell et al., 2010). Due to its unique arrangement of 9 light directions the highest birefringence colour due to each light direction and crystal orientation (retardation) can be determined at each pixel in the field of view. Retardation profiles across grain boundaries enable the calculation of grain boundary angle and direction. The data for all positions separating the grains are combined and further processed. In combination with the lateral position of the grain boundary, acquired using the FAME software (Hammes and Peternell, in review), the data is used to reconstruct a 3d grain boundary model. The processing of data is almost fully automatic by using MATLAB®. Only minor manual input is required. The applicability was demonstrated on quartzite samples, but the method is not solely restricted on quartz grains and other birefringent polycrystalline materials could be used instead. References: Birchenall, C.E., 1959: Physical Metallurgy. McGraw-Hill, New York. Doherty, R.D., Hughes, D.A., Humphreys, F.J., Jonas, J.J., Juul Jensen, D., Kassner, M.E., King, W.E., McNelley, T.R., McQueen, H.J., Rollett, A.D., 1997: Current issues in recrystallization: a review. Materials Science and Engineering A 238, 219-274. Hammes, D.M., Peternell, M., in review. FAME: Software for analysing rock microstructures. Computers & Geoscience. Kruhl, J.H., Peternell, M., 2002. The equilibration of high-angle grain boundaries in dynamically recrystallized quartz: the effect of crystallography and temperature. Journal of Structural Geology 24, 1125-1137. Kuntcheva, B., Kruhl, J.H. & Kunze, K., 2006. Crystallographic orientation of high-angle grain boundaries in dynamically recrystallized quartz: First results. Tectonophysics 421, 331-346. Peternell, M., Hasalová, P., Wilson, J.L., Piaziolo, S., Schulmann, K., 2010. Evaluating quartz crystallographic preferred orientations and the role of deformation partitioning using EBSD and fabric analyser techniques. Journal of Structural Geology 32, 803-817.

Deformation Enhanced Recrystallization of Titanite: Insight from the Western Gneiss Region Ultrahigh-Pressure Terrane

NASA Astrophysics Data System (ADS)

Gordon, S. M.; Reddy, S. M.; Blatchford, H.; Whitney, D. L.; Kirkland, C. L.; Teyssier, C.; Evans, N. J.; McDonald, B.

2017-12-01

Titanite readily recrystallizes due to metamorphism, deformation, and/or fluids making it an ideal chronometer for tracking the exhumation of high-grade rocks. The Western Gneiss Region (WGR), Norway, is a giant UHP terrane exhumed as a fairly coherent slab. Parts of the WGR underwent little deformation during exhumation; however, meters-scale shear zones, located across the WGR, deformed over a range of pressures, from (U)HP to amphibolite facies. Titanite from quartzofeldpathic gneiss within, directly adjacent to, and 300 m away from a mylonitic shear zone within the southern WGR have been analyzed to track exhumation and investigate effects of deformation on recrystallization and trace-element mobility. EBSD was used to characterize the microstructural evolution of the gneisses, and trace-element concentrations and timing of recrystallization were estimated by split-stream LA-ICPMS. Titanite grain size decreases from outside (>200) to inside (<75 µm) the shear zone. Gneiss in and directly adjacent to the shear zone contain partially to completely recrystallized grains, with 207-corrected 206Pb/238U ages of <405 Ma. Gneiss within the shear zone shows a greater percentage of recrystallized grains. EBSD data indicate that some titanite comprises multiple subgrains within an optically coherent single grain. Subgrains in titanite cores show evidence of inherited radiogenic Pb, whereas subgrains in rims and tails of deformed sigma grains were recrystallized. In a gneiss directly adjacent to the shear zone, optically coherent grains are zoned, with increasing Sr and decreasing Zr from core to rim; titanite subgrains within the shear-zone gneiss are too small to analyze. In comparison, titanite from the gneiss outside the shear zone does not show any internal microstructures or evidence for Scandian recrystallization and has low U and high 204Pb. These results show that most trace elements are unaffected by deformation of titanite; however, Pb is mobile. Deformation thus plays an important role in resetting U-Pb systematics and allows the timing of shear zone development to be linked to the early stages of eclogite exhumation at ca. 405 Ma. Atom-probe analyses of adjacent subgrains, one that has recrystallized and one with an inherited age, will provide insight into trace-element mobility on the nm-scale.

[Comporison Sduty of Microstructure by Metallographicalk on the Polarized Light and Texture by XRD of CC 5083 and CC 5182 Aluminium Alloy after Cold Rolling and Recrystallization].

PubMed

Chen, Ming-biao; Li, Yong-wei; Tan, Yuan-biao; Ma, Min; Wang, Xue-min; Liu, Wen-chang

2015-03-01

At present the study of relation between microstructure, texture and performance of CC 5083 aluminium alloy after cold tolling and recrystallization processes is still finitude. So that the use of the CC 5083 aluminium alloy be influenced. Be cased into electrical furnace, hot up with unlimited speed followed the furnace hot up to different temperature and annealed 2h respectively, and be cased into salt-beth furnace, hot up quickly to different temperature and annealed 30 min respectively for CC 5083 and CC 5182 aluminum alloy after cold roling with 91.5% reduction. The microstructure be watched use metallographic microscope, the texture be inspected by XRD. The start temperature of recrystallization and grain grow up temperature within annealing in the electric furnace of CC 5083 aluminum alloy board is 343 degrees C, and the shap of grain after grow up with long strip (the innovation point ); The start temperature of recrystallization within annealling in the salt bath furnace of CC 5083 is 343 degrees C. The start temperature and end temperature of recrystallization within annealling of CC 5083 and CC 5182 aluminum alloy is 371 degrees C. The grain grow up outstanding of cold rooled CC 5152 aluminum alloy after annealed with 454 degrees C in the electric furnace and salt bath furnace. The start temperature of grain grow up of CC 5083 alluminurn alloy annealed in the electric furnace and salt bath furnace respectively is higher than the start temperature of grain grow up of CC 5182 alluminum alloy annealed in the electric furnace and salt bath furnace respectively. The strat temperature of recrystallization grain grow up is higher than which annealled with other three manner annealing process. The recrystallization temperature of CC 5182 annealed in the salt bath furnace is higher than which annealed in the electric furnace. The recrystallization temperature of the surface layer of CC 5083 and CC 5182 aluminum alloy is higher than the inner layer (the innovation point). There is a difference each other of the structure and the texture of the four manner annealing aluminum alloy (the innovation point). There is a little difference at the recrystallization processes course reflectived by the observe results of structure transform and by the examination results of texture transmission.

Deformation Enhanced Recrystallization of Titanite: Insight from the Western Gneiss Region Ultrahigh-Pressure Terrane

NASA Astrophysics Data System (ADS)

Gordon, S. M.; Reddy, S. M.; Blatchford, H.; Whitney, D. L.; Kirkland, C. L.; Teyssier, C.; Evans, N. J.; McDonald, B.

2016-12-01

Titanite readily recrystallizes due to metamorphism, deformation, and/or fluids making it an ideal chronometer for tracking the exhumation of high-grade rocks. The Western Gneiss Region (WGR), Norway, is a giant UHP terrane exhumed as a fairly coherent slab. Parts of the WGR underwent little deformation during exhumation; however, meters-scale shear zones, located across the WGR, deformed over a range of pressures, from (U)HP to amphibolite facies. Titanite from quartzofeldpathic gneiss within, directly adjacent to, and 300 m away from a mylonitic shear zone within the southern WGR have been analyzed to track exhumation and investigate effects of deformation on recrystallization and trace-element mobility. EBSD was used to characterize the microstructural evolution of the gneisses, and trace-element concentrations and timing of recrystallization were estimated by split-stream LA-ICPMS. Titanite grain size decreases from outside (>200) to inside (<75 µm) the shear zone. Gneiss in and directly adjacent to the shear zone contain partially to completely recrystallized grains, with 207-corrected 206Pb/238U ages of <405 Ma. Gneiss within the shear zone shows a greater percentage of recrystallized grains. EBSD data indicate that some titanite comprises multiple subgrains within an optically coherent single grain. Subgrains in titanite cores show evidence of inherited radiogenic Pb, whereas subgrains in rims and tails of deformed sigma grains were recrystallized. In a gneiss directly adjacent to the shear zone, optically coherent grains are zoned, with increasing Sr and decreasing Zr from core to rim; titanite subgrains within the shear-zone gneiss are too small to analyze. In comparison, titanite from the gneiss outside the shear zone does not show any internal microstructures or evidence for Scandian recrystallization and has low U and high 204Pb. These results show that most trace elements are unaffected by deformation of titanite; however, Pb is mobile. Deformation thus plays an important role in resetting U-Pb systematics and allows the timing of shear zone development to be linked to the early stages of eclogite exhumation at ca. 405 Ma. Atom-probe analyses of adjacent subgrains, one that has recrystallized and one with an inherited age, will provide insight into trace-element mobility on the nm-scale.

Magnetic resonance diffusion and relaxation characterization of water in the unfrozen vein network in polycrystalline ice and its response to microbial metabolic products

NASA Astrophysics Data System (ADS)

Brown, Jennifer R.; Brox, Timothy I.; Vogt, Sarah J.; Seymour, Joseph D.; Skidmore, Mark L.; Codd, Sarah L.

2012-12-01

Polycrystalline ice, as found in glaciers and the ice sheets of Antarctica, is a low porosity porous media consisting of a complicated and dynamic pore structure of liquid-filled intercrystalline veins within a solid ice matrix. In this work, Nuclear Magnetic Resonance measurements of relaxation rates and molecular diffusion, useful for probing pore structure and transport dynamics in porous systems, were used to physically characterize the unfrozen vein network structure in ice and its response to the presence of metabolic products produced by V3519-10, a cold tolerant microorganism isolated from the Vostok ice core. Recent research has found microorganisms that can remain viable and even metabolically active within icy environments at sub-zero temperatures. One potential mechanism of survival for V3519-10 is secretion of an extracellular ice binding protein that binds to the prism face of ice crystals and inhibits ice recrystallization, a coarsening process resulting in crystal growth with ice aging. Understanding the impact of ice binding activity on the bulk vein network structure in ice is important to modeling of frozen geophysical systems and in development of ice interacting proteins for biotechnology applications, such as cryopreservation of cell lines, and manufacturing processes in food sciences. Here, we present the first observations of recrystallization inhibition in low porosity ice containing V3519-10 extracellular protein extract as measured with Nuclear Magnetic Resonance and Magnetic Resonance Imaging.

Effects of V addition on recrystallization resistance of 7150 aluminum alloy after simulative hot deformation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lai, Jing; Shi, Cangji; Chen, X.-Grant, E-mail: xgrant_chen@uqac.ca

2014-10-15

The effects of different V contents (0.01 to 0.19 wt.%) on the recrystallization resistance of 7150 aluminum alloys during post-deformation heat treatment were investigated. The microstructural evolutions at as-cast, as-homogenized conditions and after post-deformation annealing were studied using optical, scanning electron and transmission electron microscopes and using the electron backscattered diffraction technique. The precipitation of Al{sub 21}V{sub 2} dispersoids was observed in alloys containing 0.11 to 0.19 wt.% V after homogenization. The dispersoids were mainly distributed in the dendrite cells, and the precipitate-free zones occurred in the interdendritic regions and near grain boundaries. V addition could significantly enhance the recrystallizationmore » resistance during post-deformation annealing, particularly in the presence of a great number of Al{sub 21}V{sub 2} dispersoids. Recrystallized grain growth was effectively restricted because of the dispersoid pinning effect. The alloy containing 0.15 wt.% V exhibited the highest recrystallization resistance amongst all V-containing alloys studied. - Highlights: • Investigated the effect of V level on microstructure and flow stress of 7150 alloys • Characterized microstructures using optical microscopy, SEM, TEM and EBSD • Described the precipitation behavior of V-dispersoids in the dendritic structure • Studied the V effect on recrystallization resistance during post heat treatment • V addition greatly enhanced the recrystallization resistance during annealing.« less

Recrystallization and grain growth phenomena in a particle-reinforced aluminum composite

NASA Astrophysics Data System (ADS)

van Aken, D. C.; Krajewski, P. E.; Vyletel, G. M.; Allison, J. E.; Jones, J. W.

1995-06-01

Recrystallization and grain growth in a 2219/TiC/15p composite were investigated as functions of the amount of deformation and deformation temperature. Both cold and hot deformed samples were annealed at the normal solution treatment temperature of 535 °C. It was shown that large recrystallized grain diameters, relative to the interparticle spacing, could be produced in a narrow range of deformation for samples cold-worked and those hot-worked below 450 °C. For cold-worked samples, between 4 to 6 pct deformation, the recrystallized grain diameters varied from 530 to 66 μm as the amount of deformation increased. Subsequent grain growth was not observed in these recrystallized materials and noncompact grain shapes were observed. For deformations greater than 15 pct, recrystallized grain diameters less than the interparticle spacing were observed and subsequent grain growth produced a pinned grain diameter of 27 μm. The pinned grain diameter agreed well with an empirical model based on three dimensional (3-D) Monte Carlo simulations of grain growth and particle pinning in a two-phase material. Tensile properties were determined as a function of grain size, and it was shown that grain size had a weak influence on yield strength. A maximum in the yield strength was observed at a grain size larger than the normal grain growth and particle-pinned diameter.

[Investigation of the recrystallization of trehalose as a good glass-former excipient].

PubMed

Katona, Gábor; Orsolya, Jójártné Laczkovich; Szabóné, Révész Piroska

2014-01-01

An amorphous form of trehalose is easy to prepare by using a solvent method. The recrystallization kinetics can be followed well, which is important because of the occurrence of polymorphic forms of trehalose. This is especially significant in the case of dry powder inhalers. Spray-drying was used as a preparation method this being one of the most efficient technologies with which to obtain an amorphous form. This method can result in the required particle size and a monodisperse distribution with excellent flowability and with moreover considerable amorphization. In our work, trehalose was applied as a technological auxiliary agent, and literature data relating to the spray-drying technology of trehalose were collected. Studies were made of the influence of the spraying process on the amorphization of trehalose and on the recrystallization of amorphous trehalose during storage. Amorphous samples were investigated under 3 different conditions during 3 months. The recrystallization process was followed by differential scanning calorimetry and X-ray powder diffraction. The results demonstrated the perfect amorphization of trehalose during the spray-drying process. The glass transition temperature was well measurable in the samples and proved to be the same as the literature data. Recrystallization under normal conditions was very slow but at high relative humidity the process was accelerated greatly. Amorphous trehalose gave rise to dihydrate forms (gamma- and h-trehaloses) during recrystallization, and beta-trehalose was also identified as an anhydrous form.

Composite Magnetite and Protein Containing CaCO3 Crystals. External Manipulation and Vaterite → Calcite Recrystallization-Mediated Release Performance.

PubMed

Sergeeva, Alena; Sergeev, Roman; Lengert, Ekaterina; Zakharevich, Andrey; Parakhonskiy, Bogdan; Gorin, Dmitry; Sergeev, Sergey; Volodkin, Dmitry

2015-09-30

Biocompatibility and high loading capacity of mesoporous CaCO3 vaterite crystals give an option to utilize the polycrystals for a wide range of (bio)applications. Formation and transformations of calcium carbonate polymorphs have been studied for decades, aimed at both basic and applied research interests. Here, composite multilayer-coated calcium carbonate polycrystals containing Fe3O4 magnetite nanoparticles and model protein lysozyme are fabricated. The structure of the composite polycrystals and vaterite → calcite recrystallization kinetics are studied. The recrystallization results in release of both loaded protein and Fe3O4 nanoparticles (magnetic manipulation is thus lost). Fe3O4 nanoparticles enhance the recrystallization that can be induced by reduction of the local pH with citric acid and reduction of the polycrystal crystallinity. Oppositely, the layer-by-layer assembled poly(allylamine hydrochloride)/poly(sodium styrenesulfonate) polyelectrolyte coating significantly inhibits the vaterite → calcite recrystallization (from hours to days) most likely due to suppression of the ion exchange giving an option to easily tune the release kinetics for a wide time scale, for example, for prolonged release. Moreover, the recrystallization of the coated crystals results in formulation of multilayer capsules keeping the feature of external manipulation. This study can help to design multifunctional microstructures with tailor-made characteristics for loading and controlled release as well as for external manipulation.

Influence of processing parameters and alloying additions on the mechanically determined no-recrystallization temperature in niobium microalloyed steels

NASA Astrophysics Data System (ADS)

Homsher-Ritosa, Caryn Nicole

Microalloying elements are added to plate steels to improve the mechanical properties through grain refinement and precipitation strengthening. In industrial practice, such refinement is obtained by controlling the rolling near critical temperatures in austenite. Generally, a large amount of hot deformation is desired below the no-recrystallization temperature (TNR) to increase the grain boundary area to promote fine ferrite grains upon transformation during cooling. Ideally, a high TNR is desired for increased deformation below TNR at minimal rolling loads and minimal loss of productivity. To increase TNR, microalloying elements such as Nb, V, and Ti are used. The primary purpose of the current study was to determine the effect of multiple microalloying elements on the mechanically determined via torsion testing no-recrystallization temperature (TNR_Tor) in Nb-bearing plate steel. This project focused on the influence of alloying elements and deformation parameters on TNR_Tor. The main objective was to experimentally determine the TNR_Tor for various laboratory-grade steels with systematically varying amounts of Nb, V, and Ti, with C and N held constant. The synergistic effects of these microalloying elements were evaluated. Another objective was to determine the TNR_Tor with systematically varied deformation parameters for the same set of steels. Comparisons of the measured TNR through two different mechanical tests were conducted. Finally, a microstructural evaluation around the mechanically determined TNR_Tor via multistep hot torsion testing was made. To accomplish these objectives six Nb-bearing steels were laboratory produced with 0.065 wt pct C, 0.044 wt pct N, and varying amounts of Nb, V, and Ti. Multistep hot torsion tests were conducted using the GleebleRTM 3500 thermomechanical simulator between the temperatures of 1200 and 750 °C. The mean flow stress was calculated for each deformation step and plotted against the inverse absolute temperature. The TNR_Tor was determined by finding the intersection point of two linear regressions fit to the data. The TNR_Tor values were compared with measured TNR values from double-hit compression tests and with predicted values using empirical equations from the literature. Light optical micrographs and electron backscatter diffraction scans were examined for samples quenched from just above and just below the experimentally determined values of TNR_Tor for the high Nb, low Ti, and commercially produced 10V45 alloys to help verify the prior austenite grain morphology. For all processing conditions, the low Nb alloy was the least effective in increasing TNR_Tor and the high additions of Ti were the most effective at increasing TNR_Tor. The additions of V were not significantly effective in altering TNR_Tor and it is believed the Nb overpowered any influence the V additions may have had on TNR_Tor. An increase in strain or an increase strain rate decreased TNR_Tor. The T NR values measured from multistep hot torsion testing were lower than the TNR values measured from double-hit compression tests. The use of the mean flow stress versus inverse temperature curve to determine TNR_Tor does not correlate to the microstructural meaning of T NR (i.e. no recrystallization). The transition from completely recrystallized grains to less than complete recrystallization is not properly modeled by the intersection of two linear regions and is more gradual than the mechanical test implies. From the microstructural analysis of a10V45 steel, there is evidence of recrystallization at temperatures 200 °C below the measured TNR_Tor. The slope change on the mean flow stress versus inverse temperature curves is believed to be, in part, accumulated strain as well as refinement of continuously recrystallized grains causing a Hall-Petch type strength increase.

Recrystallization in Si upon ion irradiation at room temperature in Co/Si(111) thin film systems

NASA Astrophysics Data System (ADS)

Banu, Nasrin; Satpati, B.; Dev, B. N.

2018-04-01

After several decades of research it was concluded that for a constant flux recrystallization in Si upon ion irradiation is possible only at high temperature. At low temperature or at room temperature only amorphization can take place. However we have observed recrystallization in Si upon ion irradiation at room temperature in a Co/Si thin film system. The Co/Si sample was prepared by deposition of 25 nm Co on clean Si(111) substrate. An oxide layer (˜ 2nm) of cobalt at the top of the film due to air exposure. The ion irradiation was done at room temperature under high vacuum with 1MeV Si+ ion with low beam current < 400 nA. Earlier we have shown similar ion induced recrystallization in Si(100) substrate which had a sandwich Si/Ni/Si structure. This system had an epitaxial buffer Si layer on Si substrate. This study also shows that the phenomenon is independent of substrate orientation and buffer layer. We have used transmission electron microscopy (TEM) to study the recrystallization behavior.

Purification and crystal growth of NPB via imidazolium based ionic liquids

NASA Astrophysics Data System (ADS)

Oh, Yong-Taeg; Shin, Dong-Chan

2018-04-01

Here we report the production of high purity and crystallinity organic electronic material of NPB (N,N‧-Di-[(1-naphthyl)-N,N‧-diphenyl]-1,1‧-biphenyl-4,4‧-diamine (C44H32N2) through solution recrystallization within imidazolium based ionic liquids. When low purity NPB was recrystallized at 170 °C within C8MIM[TFSI], its purity was drastically improved from 82% to 99.92%. These recrystallized NPB crystals showed 0.040° FWHM (Full Width Half Maximum) of X-ray (1 1 1) diffraction peak. Such small FWHM angle indicates single-crystal like crystallinity. Initial NPB powder was dissolved at 100 °C and recrystallized at temperature above 110 °C. At higher temperature of 170 °C, a small number of bigger crystals were formed compared to those at 110 °C. This can be well explained by the classical nucleation and growth theory. Therefore, solution recrystallization process using ionic liquid might be promising for mass production of organic electronic materials by replacing the widely-used sublimation purification method.

Microstructural Evolution During Cold Rolling and Subsequent Annealing in Low-Carbon Steel with Different Initial Microstructures

NASA Astrophysics Data System (ADS)

Ogawa, Toshio; Dannoshita, Hiroyuki; Maruoka, Kuniaki; Ushioda, Kohsaku

2017-08-01

Microstructural evolution during cold rolling and subsequent annealing of low-carbon steel with different initial microstructures was investigated from the perspective of the competitive phenomenon between recrystallization of ferrite and reverse phase transformation from ferrite to austenite. Three kinds of hot-rolled sheet specimens were prepared. Specimen P consisted of ferrite and pearlite, specimen B consisted of bainite, and specimen M consisted of martensite. The progress of recovery and recrystallization of ferrite during annealing was more rapid in specimen M than that in specimens P and B. In particular, the recrystallized ferrite grains in specimen M were fine and equiaxed. The progress of ferrite-to-austenite phase transformation during intercritical annealing was more rapid in specimen M than in specimens P and B. In all specimens, the austenite nucleation sites were mainly at high-angle grain boundaries, such as those between recrystallized ferrite grains. The austenite distribution was the most uniform in specimen M. Thus, we concluded that fine equiaxed recrystallized ferrite grains were formed in specimen M, leading to a uniform distribution of austenite.

Cryogenic strength improvement by utilizing room-temperature deformation twinning in a partially recrystallized VCrMnFeCoNi high-entropy alloy

PubMed Central

Jo, Y. H.; Jung, S.; Choi, W. M.; Sohn, S. S.; Kim, H. S.; Lee, B. J.; Kim, N. J.; Lee, S.

2017-01-01

The excellent cryogenic tensile properties of the CrMnFeCoNi alloy are generally caused by deformation twinning, which is difficult to achieve at room temperature because of insufficient stress for twinning. Here, we induced twinning at room temperature to improve the cryogenic tensile properties of the CrMnFeCoNi alloy. Considering grain size effects on the critical stress for twinning, twins were readily formed in the coarse microstructure by cold rolling without grain refinement by hot rolling. These twins were retained by partial recrystallization and played an important role in improving strength, allowing yield strengths approaching 1 GPa. The persistent elongation up to 46% as well as the tensile strength of 1.3 GPa are attributed to additional twinning in both recrystallized and non-recrystallization regions. Our results demonstrate that non-recrystallized grains, which are generally avoided in conventional alloys because of their deleterious effect on ductility, can be useful in achieving high-strength high-entropy alloys. PMID:28604656

Ice-Active Substances from the Infective Juveniles of the Freeze Tolerant Entomopathogenic Nematode, Steinernema feltiae

PubMed Central

Ali, Farman; Wharton, David A.

2016-01-01

Steinernema feltiae is a moderately freezing tolerant nematode, that can withstand intracellular ice formation. We investigated recrystallization inhibition, thermal hysteresis and ice nucleation activities in the infective juveniles of S. feltiae. Both the splat cooling assay and optical recrystallometry indicate the presence of ice active substances that inhibit recrystallization in the nematode extract. The substance is relatively heat stable and largely retains the recrystallization inhibition activity after heating. No thermal hysteresis activity was detected but the extract had a typical hexagonal crystal shape when grown from a single seed crystal and weak ice nucleation activity. An ice active substance is present in a low concentration, which may be involved in the freezing survival of this species by inhibiting ice recrystallization. PMID:27227961

Pairing Heterocyclic Cations with closo-Icosahedral Borane and Carborane Anions. II. Benchtop Alternative Synthetic Methodologies for Binary Triazolium and Tetrazolium Salts with Significant Water Solubility

DTIC Science & Technology

2010-04-01

produced from eutectic melts. Nat. Mater. 2008, 7, 626-630. 9. Any attempt at recrystallizing the 1:1 mixture of cations in (12) is likely to afford... recrystallizations . So, rather than recrystallizing each individual adduct, we concentrated on performing a careful spectroscopic examination of the...suggested. [1] While it is well-known that an admixture of two neutral compounds often affords eutectic behavior, we wondered whether or not the same

Ostwald ripening of clays and metamorphic minerals

USGS Publications Warehouse

Eberl, D.D.; Srodon, J.; Kralik, M.; Taylor, B.E.; Peterman, Z.E.

1990-01-01

Analyses of particle size distributions indicate that clay minerals and other diagenetic and metamorphic minerals commonly undergo recrystallization by Ostwald ripening. The shapes of their particle size distributions can yield the rate law for this process. One consequence of Ostwald ripening is that a record of the recrystallization process is preserved in the various particle sizes. Therefore, one can determine the detailed geologic history of clays and other recrystallized minerals by separating, from a single sample, the various particle sizes for independent chemical, structural, and isotopic analyses.

Orientation filtering for crystalline films

DOEpatents

Smith, Henry I.; Atwater, Harry A.; Thompson, Carl V.; Geis, Michael W.

1986-12-30

A substrate is coated with a film to be recrystallized. A pattern of crystallization barriers is created in the film, for example, by etching voids in the film. An encapsulation layer is generally applied to protect the film, fill the voids and otherwise enhance a recrystallization process. Recrystallization is carried out such that certain orientations pass preferentially through the barrier, generally as a result of growth-velocity anisotropy. The result is a film of a specific predetermined crystallographic orientation, a range of orientations or a set of discrete orientations.

Microstructural variation in the transport direction of a large-scale mid-crustal thrust (Woodroffe Thrust, Central Australia)

NASA Astrophysics Data System (ADS)

Wex, Sebastian; Mancktelow, Neil S.; Hawemann, Friedrich; Pennacchioni, Giorgio; Camacho, Alfredo

2016-04-01

The over ˜600 km long E-W trending mid-crustal Woodroffe Thrust is one the most prominent structures of a range of large-scale shear zones that developed in the Musgrave Ranges region in Central Australia. During the Petermann Orogeny around 550 Ma the Woodroffe Thrust placed 1.2 Ga granulites onto similarly-aged amphibolite and granulite facies gneisses along a south-dipping plane with a top-to-north shear sense. Due to late-stage open folding of the thrust plane, a nearly continuous N-S profile of 60 km length in the direction of thrusting could be studied for variation in microstructure. The regional P/T variations in the mylonitized footwall (600 to 500 °C at ~ 0.8 GPa from S to N) indicate that the original angle of dip was shallow (~ 10°) towards the south. Along the profile, evidence for fluid-present conditions are effectively absent in the more southerly areas and only present on a local scale in the north, characterizing the regional conditions to be "dry". This is indicated by: 1) only rare syntectonic quartz veins in the footwall; 2) very little sericitization of plagioclase; 3) breakdown of plagioclase to kyanite + garnet, rather than kyanite + clinozoisite; and 4) variable presence of hydrothermally introduced calcite. These changes in P/T conditions and fluid availability are associated with corresponding changes in mineral assemblage and microstructure. Mylonitized dolerites consists of a syn-kinematic assemblage (decreasing modal amounts from left to right) of Pl + Cpx + Grt + Ky + Rt + Ilm ± Opx ± Amp ± Qz in the central/southern areas and Pl + Bt + Amp + Chl + Ilm ± Kfs ± Mag ± Ap in the north. The amount of newly grown garnet decreases towards the north and garnet is generally absent in the northernmost exposures of the Woodroffe Thrust. Mylonitized felsic granulites and granitoids consist of syn-kinematic assemblages of Qz + Pl + Kfs + Grt + Cpx + Ky + Ilm + Rt ± Bt ± Amp ± Opx ± Ap in the south and Qz + Pl + Kfs + Bt + Czo + Grt + Ilm ± Mag + Ttn ± Ms ± Amp ± Ap in the north. Plagioclase and K-feldspar dynamically recrystallized (grainsize < 10 μm) along the entire 60 km N-S transect, but with an increasing degree in the more southern exposures. Over the entire area dynamically recrystallized quartz aggregates in mylonites show polygonal, strain-free, equigranular grains, with a morphology indicating SGR recrystallization, under temperatures usually considered typical for GBM, which could potentially be due to the relatively "dry" conditions. Quartz grainsizes are on average 24 μm and 44 μm in the southern and northern areas, respectively. The increase in grain size towards the north correlates well with the increasing influx of fluids, but is in contrast to the trend of higher metamorphic grade towards the south. This suggests that fluid, rather than temperature, may be the main factor controlling the rheology of such "dry" middle crust.

Effects of annealing and additions on dynamic mechanical properties of SnSb quenched alloy

NASA Astrophysics Data System (ADS)

El-Bediwi, A. B.

2004-08-01

The elastic modulus, internal friction and stiffness values of quenched SnSb bearing alloy have been evaluated using the dynamic resonance technique. Annealing for 2 and 4 h at 120, 140 and 160degreesC caused variations in the elastic modulus. internal friction and stiffness values. This is due to structural changes in the SnSb matrix during isothermal annealing such as coarsening in the phases (Sn, Sb or intermetallic compounds), recrystallization and stress relief. In addition, adding a small amount (1 wt.%) of Cu or Ag improved the bearing mechanical properties of the SnSb bearing alloy. The SnSbCu1 alloy has the best bearing mechanical properties with thermo-mechanical stability for long time at high temperature.

Rapid trench initiated recrystallization and stagnation in narrow Cu interconnect lines

DOE Office of Scientific and Technical Information (OSTI.GOV)

O'Brien, Brendan B.; Rizzolo, Michael; Prestowitz, Luke C.

2015-10-26

Understanding and ultimately controlling the self-annealing of Cu in narrow interconnect lines has remained a top priority in order to continue down-scaling of back-end of the line interconnects. Recently, it was hypothesized that a bottom-up microstructural transformation process in narrow interconnect features competes with the surface-initiated overburden transformation. Here, a set of transmission electron microscopy images which captures the grain coarsening process in 48 nm lines in a time resolved manner is presented, supporting such a process. Grain size measurements taken from these images have demonstrated that the Cu microstructural transformation in 48 nm interconnect lines stagnates after only 1.5 h atmore » room temperature. This stubborn metastable structure remains stagnant, even after aggressive elevated temperature anneals, suggesting that a limited internal energy source such as dislocation content is driving the transformation. As indicated by the extremely low defect density found in 48 nm trenches, a rapid recrystallization process driven by annihilation of defects in the trenches appears to give way to a metastable microstructure in the trenches.« less

Behavior of sheets from Ti-alloys by rolling and heat treatment

NASA Astrophysics Data System (ADS)

Isaenkova, M.; Perlovich, Yu.; Fesenko, V.; Gritskevich, M.; Stolbov, S.; Zaripova, M.

2017-10-01

Sheets from single- and two-phase Ti-alloys (VT1-0, Ti-22Nb-9%Zr and VT-16) were rolled at the room temperature up to various deformation degrees and annealed at temperatures 500-900 °C. The regularities of texture formation in both phases were established. In the technically pure Ti (VT1-0) with the single α-Ti phase the final stable texture component is (0001)±30-40°ND-TD<101 ¯0>. In the two-phase alloy the reorientation of basal axes of α-Ti occurs by the same trajectories as in the single phase alloy. However, in the case of two-phase alloy texture development in α-Ti stops at the intermediate stage, when this texture consists of components with rolling planes (0001)±15-20°ND-RD and (0001)±30-40°ND-TD. The stability of the first components can be provided both by the mutually balanced operation of pyramidal and basal slip systems, activity of which remains at the high deformation degree of two-phase alloy, and by the dynamic α↔β phase transformations, taking place in the distorted structures of α- and β-phases in the course of its cold rolling. At recrystallization of technically pure Ti the basal component disappears in its texture. At the same time, prismatic axes turn by angles 20÷30° depending on the heating rate of the rolled sheet and annealing temperature. At recrystallization of the two-phase Ti-alloy prismatic axes of its α-grains doesn't turn relative to their positions in the rolling texture, as it occurs in the single-phase alloy. This fact indicates to some alternative mode of arising new recrystallized grains in two-phase alloys.

Effects of warming rate, temperature, and antifreeze proteins on the survival of mouse spermatozoa frozen at an optimal rate.

PubMed

Koshimoto, Chihiro; Mazur, Peter

2002-08-01

We have recently reported that the survival of mouse spermatozoa is decreased when they are warmed at a suboptimal rate after being frozen at an optimal rate. We proposed that this drop in survival is caused by physical damage derived from the recrystallization of extracellular ice during slow warming. The first purpose of the present study was to determine the temperatures over which the decline in survival occurs during slow warming and the kinetics of the decline at fixed subzero temperatures. The second purpose was to examine the effects of antifreeze proteins (AFP) on the survival of slowly warmed mouse spermatozoa, the rationale being that AFP have the property of inhibiting ice recrystallization. With respect to the first point, a substantial loss in motility occurred when slow warming was continued to higher than -50 degrees C and the survival of the sperm decreased with an increase in the temperature at which slow warming was terminated. In contrast, the motility of sperm that were warmed rapidly to these temperatures remained high initially but dropped with increased holding time. At -30 degrees C, most of the drop occurred in 5 min. These results are consistent with the hypothesis that damage develops as a consequence of the recrystallization of the external ice. AFP ought to inhibit such recrystallization, but we found that the addition of AFP-I, AFP-III, and an antifreeze glycoprotein at concentrations of 1-100 microg/ml did not protect the frozen-thawed cells; rather it led to a decrease in survival that was proportional to the concentration. There was no decrease in survival from exposure to the AFP in the absence of freezing. AFP are known to produce changes in the structure and habit of ice crystals, and some have reported deleterious consequences associated with those structural changes. We suggest that such changes may be the basis of the adverse effects of AFP on the survival of the sperm, especially since mouse sperm are exquisitely sensitive to a variety of mechanical stresses.

Geochemistry of speleothems affected by aragonite to calcite recrystallization - Potential inheritance from the precursor mineral

NASA Astrophysics Data System (ADS)

Domínguez-Villar, David; Krklec, Kristina; Pelicon, Primož; Fairchild, Ian J.; Cheng, Hai; Edwards, Lawrence R.

2017-03-01

Formerly aragonite speleothems recrystallized to calcite result from solutions subsaturated in aragonite and supersaturated in calcite that infiltrate into the speleothem through the interconnected porosity. In most cases, the crystal replacement takes place through a thin solution film. This diagenetic process can occur under open or semi-closed geochemical conditions. Thus, secondary calcite crystals record the composition of the fluid at the time of diagenesis affected by calcite partition coefficients and fractionation factors (open system) or partly inherit the composition of the primary aragonite (semi-closed system). So, whether or not recrystallized aragonite speleothems can record reliable geochemical signals from the time of speleothem primary deposition still is an open debate. We studied a stalagmite from Eagle Cave (Spain) predominantly composed of secondary calcite that replaced aragonite, although a core of primary aragonite extending 45 mm along the growth direction was preserved at the base of the sample. We obtained Mg and Sr compositional maps, paired U-Th dating and δ18O and δ13C profiles across the diagenetic front. Additionally, two parallel isotope records were obtained along the speleothem growth direction in the aragonite and calcite sectors. Our results support that recrystallization of this speleothem took place in open system conditions for δ18O, δ13C, Mg and Sr, but in semi-closed system conditions for U and Th. The recrystallization of this sample took place during one or several events, likely after the Younger Dryas as a result of climate change influencing drip water composition. Based on compositional zoned patterns, we suggest that the advance of diagenetic fronts in this speleothem had an average rate of 50 ± 45 μm/yr. Such recrystallization rate can transform any aragonite speleothem into calcite within a few centuries. We suggest that the volume of water interacting with the speleothem at the time of recrystallization is of critical importance for inheritance of different elements. The volume of solution is controlled by (1) the discharge of water passing through the sample and (2) the lapse time between aragonite dissolution and calcite precipitation. Hydrology and hydrochemistry of the interacting solution, together with the mineralogy and texture of the speleothem are the essential controls for the diagenesis of the speleothem. Recrystallization of aragonite speleothems does not follow stratigraphical levels of the sample but occurs along sites with preferential flow paths in any sector of the speleothem. In these cases the relationship between age and distance from base is not preserved. However, alternation of periods of recrystallization with periods of aragonite precipitation causing speleothem accretion can result in recrystallized speleothems with coherent distance from the base-age relationship. Thus, early diagenesis of speleothems affected by seasonal or inter-annual oscillation of drip waters supersaturated and subsaturated in aragonite may provide best-scenario conditions for dating and preservation of paleoenvironmental records along recrystallized speleothems. However, even in this scenario, the variable discharge and the diagenetic rate control the geochemical inheritance from the primary aragonite crystals.

Microstructure and Mechanical Properties of Welds of Al - Mg - Si Alloys After Different Modes of Impulse Friction Stir Welding

NASA Astrophysics Data System (ADS)

Kondrat'ev, S. Yu.; Morozova, Yu. N.; Golubev, Yu. A.; Hantelmann, C.; Naumov, A. A.; Mikhailov, V. G.

2018-03-01

Welded joints of aluminum alloy 6082-T6 formed by the method of impulse friction stir welding are studied. The effect of the power and frequency of the pulses on the microstructure and mechanical properties of the welded joints is determined. Application of an additional pulse during the welding affects the surface quality and the shape of the weld, the distribution of the oxide layer and of particles of the hardening phase, and the grain size in the zone of dynamic recrystallization.

REX3DV1.0

DOE Office of Scientific and Technical Information (OSTI.GOV)

Holm, Elizabeth A.

2002-03-28

This code is a FORTRAN code for three-dimensional Monte Carol Potts Model (MCPM) Recrystallization and grain growth. A continuum grain structure is mapped onto a three-dimensional lattice. The mapping procedure is analogous to color bitmapping the grain structure; grains are clusters of pixels (sites) of the same color (spin). The total system energy is given by the Pott Hamiltonian and the kinetics of grain growth are determined through a Monte Carlo technique with a nonconserved order parameter (Glauber dynamics). The code can be compiled and run on UNIX/Linux platforms.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hu, Shenyang; Lavender, Curt A.; Joshi, Vineet V.

Recrystallization plays an important role in swelling kinetics of irradiated metallic nuclear fuels. This talk will present a three-dimensional microstructure-dependent swelling model by integrating the evolution of intra-and inter- granular gas bubbles, dislocation loop density, and recrystallization.

Recrystallization characteristics and interfacial oxides on the compression bonding interface

NASA Astrophysics Data System (ADS)

Xie, Bijun; Sun, Mingyue; Xu, Bin; Li, Dianzhong

2018-05-01

Up to now, the mechanism of interface bonding is still not fully understood. This work presents interfacial characteristics of 316LN stainless steel bonding joint after cold compression bonding with subsequent annealing. EBSD analysis shows that fine recrystallization grains preferentially appear near the bonding interface and grow towards both sides of the interface. Transmission electron microscopy reveals that initial cold compression bonding disintegrates the native oxide scales and brings pristine metal from both sides of the interface come into intimate contact, while the broken oxide particles are remained at the original interface. The results indicate that partial bonding can be achieved by cold compression bonding with post-annealing treatment and recrystallization firstly occurs along the bonding interface. However, the interfacial oxides impede the recrystallization grains step over the interface and hinder the complete healing of the bonding interface.

Recrystallization characteristics of oxide dispersion strengthened nickel-base alloys

NASA Technical Reports Server (NTRS)

Hotzler, R. K.; Glasgow, T. K.

1980-01-01

Electron microscopy was employed to study the process of recrystallization in two oxide dispersion strengthened (ODS) mechanically alloyed nickel-base alloys, MA 754 and MA 6000E. MA 754 contained both fine, uniformly dispersed particles and coarser oxides aligned along the working direction. Hot rolled MA 754 had a grain size of 0.5 microns and high dislocation densities. After partial primary recrystallization, the fine grains transformed to large elongated grains via secondary (or abnormal) grain growth. Extruded and rolled MA 6000E contained equiaxed grains of 0.2 micron diameter. Primary recrystallization occurring during working eliminated virtually all dislocations. Conversion from fine to coarse grains was triggered by gamma prime dissolution; this was also a process of secondary or abnormal grain growth. Comparisons were made to conventional and oxide dispersion strengthened nickel-base alloys.

Nuclear magnetic resonance analysis and activation energy spectrum of the irreversible structural relaxation of amorphous zirconium tungstate

NASA Astrophysics Data System (ADS)

Miotto, F.; Rech, G. L.; Turatti, A. M.; Catafesta, J.; Zorzi, J. E.; Pereira, A. S.; Perottoni, C. A.

2018-03-01

Zirconium tungstate undergoes a sequence of phase transitions from cubic (α -ZrW2O8 ) to orthorhombic (γ -ZrW2O8 ) to amorphous (a -ZrW2O8 ) upon increasing pressure at room temperature. The amorphous phase is known to undergo anomalous endothermic recrystallization into a high-temperature β -ZrW2O8 phase above 600∘C at ambient pressure (and back to α -ZrW2O8 when brought to room temperature). The endothermic recrystallization of a -ZrW2O8 is preceded by an irreversible exothermic structural relaxation. New W-O bonds are formed upon amorphization, continuing a tendency of increasing W coordination number in going from α to γ -ZrW2O8 . In fact, contrarily to α -ZrW2O8 , in which one-quarter of the oxygen atoms are bonded only to one W (terminal oxygens), previous works found no evidence of single-bonded oxygen atoms in a -ZrW2O8 . It thus could be argued that the irreversible character of the structural relaxation of a -ZrW2O8 is due to W-O bond breaking upon annealing of the amorphous phase. To test this hypothesis, x-ray diffraction, 17O magic-angle spinning NMR, Raman, and far-infrared analyses were performed on samples of amorphous zirconium tungstate previously annealed to increasingly higher temperatures, looking for any evidence of features that could be assigned to the presence of terminal oxygen atoms. No evidence of single-bonded oxygen was found before the onset of recrystallization. Furthermore, the kinetics of the structural relaxation of a -ZrW2O8 is consistent with a continuous spectrum of activation energy, spanning all the range from 1 to 2.5 eV . These findings suggest that the structural relaxation of amorphous zirconium tungstate, however irreversible, is not accompanied by W-O bond breaking, but most probably characterized by a succession of (mostly) irreversible local atomic rearrangements.

BHQ revisited (1) - Looking at grain size

NASA Astrophysics Data System (ADS)

Heilbronner, Renée; Kilian, Rüdiger; Tullis, Jan

2016-04-01

Black Hills Quartzite (BHQ) has been used extensively in experimental rock deformation for numerous studies. Coaxial and general shear experiments have been carried out, for example, to define the dislocation creep regimes of quartz (Hirth & Tullis, 1992), to determine the effect of annealing (Heilbronner & Tullis, 2002) or to study the development of texture and microstructure with strain (Heilbronner & Tullis, 2006). BHQ was also used to determine the widely used quartz piezometer by Stipp & Tullis (2003). Among the microstructure analyses that were performed in those original papers, grain size was usually determined using CIP misorientation images. However, the CIP method (= computer-integrated polarization microscopy, details in Heilbronner and Barrett, 2014) is only capable of detecting the c-axis orientation of optically uniaxial materials and hence is only capable of detecting grain boundaries between grains that differ in c-axis orientation. One of the puzzling results we found (Heilbronner & Tullis, 2006) was that the recrystallized grain size seemed to depend on the crystallographic preferred orientation of the domain. In other words the grain size did not only depend on the flow stress but also on the orientation of the c-axis w/r to the shear direction. At the time, no EBSD analysis (electron back scatter diffraction) was carried out and hence the full crystallographic orientation was not known. In principle it is therefore possible that we missed some grain boundaries (between grains with parallel c-axes) and miscalculated our grain sizes. In the context of recent shear experiments on quartz gouge at the brittle-viscous transition (see Richter et al., this conference), where EBSD is used to measure the recrystallized grain size, we wanted to re-measure the CIP grain sizes of our 2006 samples (deformed in regime 1, 2 and 3 of dislocation) in exactly the same way. In two companion posters we use EBSD orientation imaging to repeat, refine and expand the microstructure and texture analysis of Heilbronner & Tullis (2006). Here, in poster (1), we focus on the recrystallized grain size with the aim of (a) comparing CIP- and EBSD derived grain size measurements, (b) of comparing the recrystallized grain size of coaxially deformed and sheared BHQ and (c) in order to confirm that the quartz piezometer indeed depends on texture, and (d) to test if it also depends on the type of deformation (irrotational versus rotational deformation). References cited: Heilbronner, R., and S.D. Barrett (2014) Image Analysis in Earth Sciences, Springer. Heilbronner, R., and J. Tullis (2002), The effect of static annealing on micro- structure and crystallographic preferred orientations of quartzites experimentally deformed in axial compression and shear, Geol. Soc. Spec. Publ., 200, 191 - 218. Heilbronner, R., and J. Tullis (2006), Evolution of c axis pole figures and grain size during dynamic recrystallization: Results from experimentally sheared quartzite. JGR, 111, B10202, doi:10.1029/2005JB004194, 2006 Hirth, G., and J. Tullis (1992), Dislocation creep regimes in quartz aggregates, JSG, 14, 145-159. Stipp, M., and J. Tullis (2003), The recrystallized grain size piezometer for quartz, Geophys. Res. Lett., 30(21), 2088, doi:10.1029/2003GL018444.

Dynamic deformation of volcanic ejecta from the Toba caldera: possible relevance to Cretaceous/Tertiary boundary phenomena

DOE Office of Scientific and Technical Information (OSTI.GOV)

Carter, N.L.; Officer, C.B.; Chesner, C.A.

1986-05-01

Plagioclase and biotite phenocrysts in ignimbrites erupted from the Toba caldera, Sumatra, show microstructures and textures indicative of shock stress levels higher than 10 GPa. Strong dynamic deformation has resulted in intense kinking in biotite and, with increasing shock intensity, the development of plagioclase of planar features, shock mosaicism, incipient recrystallization, and possible partial melting. Microstructures in quartz indicative of strong shock deformation are rare, however, and many shock lamellae, if formed, may have healed during post-shock residence in the hot ignimbrite; they might be preserved in ash falls. Peak shock stresses from explosive silicic volcanism and other endogenous processesmore » may be high and if so would obviate the need for extraterrestrial impacts to produce all dynamically deformed structures, possibly including shock features observed near the Cretaceous/Tertiary boundary. 38 references, 3 figures.« less

Recrystallization and grain growth induced by ELMs-like transient heat loads in deformed tungsten samples

NASA Astrophysics Data System (ADS)

Suslova, A.; El-Atwani, O.; Sagapuram, D.; Harilal, S. S.; Hassanein, A.

2014-11-01

Tungsten has been chosen as the main candidate for plasma facing components (PFCs) due to its superior properties under extreme operating conditions in future nuclear fusion reactors such as ITER. One of the serious issues for PFCs is the high heat load during transient events such as ELMs and disruption in the reactor. Recrystallization and grain size growth in PFC materials caused by transients are undesirable changes in the material, since the isotropic microstructure developed after recrystallization exhibits a higher ductile-to-brittle transition temperature which increases with the grain size, a lower thermal shock fatigue resistance, a lower mechanical strength, and an increased surface roughening. The current work was focused on careful determination of the threshold parameters for surface recrystallization, grain growth rate, and thermal shock fatigue resistance under ELM-like transient heat events. Transient heat loads were simulated using long pulse laser beams for two different grades of ultrafine-grained tungsten. It was observed that cold rolled tungsten demonstrated better power handling capabilities and higher thermal stress fatigue resistance compared to severely deformed tungsten. Higher recrystallization threshold, slower grain growth, and lower degree of surface roughening were observed in the cold rolled tungsten.

Effect of alloying elements and coiling temperature on the recrystallization behavior and the bainitic transformation in TRIP steels

NASA Astrophysics Data System (ADS)

Han, Seongho; Seong, Hwangoo; Ahn, Yeonsang; Garcia, C. I.; DeArdo, A. J.; Kim, Inbae

2009-08-01

The effects of alloying elements and coiling temperature on recrystallization behavior and bainitic transformation were investigated based on 0.07C-Mn-Cr-Nb steel with a low carbon equivalent. Based on the ferrite recrystallization behavior, the proper intercritical annealing temperature of all studied steels was suggested to produce TRIP steel with good strength and elongation balance. All steels coiled at 550 °C showed much faster ferrite recrystallization behavior than steels coiled at 700 °C. In addition to the coiling temperature, the effect of increasing carbon content on the ferrite recrystallization was minor at a coiling temperature of 550 °C, but much more prominent at a coiling temperature of 700 °C. The highest Mo added steel showed the best strength and elongation balance, and the highest carbon and Mo added steel showed the highest tensile strength at a coiling temperature of 550 °C. The steel containing a higher amount of elemental Al (0.7 wt.% Al) exhibited much better elongation than the lower Al added steel (0.04 wt.% Al) in TS 780 MPa grade, about 24 % and 19 %, respectively.

Solid dispersion of acetaminophen and poly(ethylene oxide) prepared by hot-melt mixing.

PubMed

Yang, Min; Wang, Peng; Huang, Chien-Yueh; Ku, M Sherry; Liu, Huiju; Gogos, Costas

2010-08-16

In this study, a model drug, acetaminophen (APAP), was melt mixed with poly(ethylene oxide) (PEO) using a Brabender mixer. APAP was found to recrystallize upon cooling to room temperature for all the drug loadings investigated. Higher drug loading leads to faster recrystallization rate. However, the morphology of the recrystallized drug crystals is identical in samples with different drug loadings and does not change with the storage time. To adjust the drug's dissolution rate, nanoclay Cloisite 15A and 30B were added into the binary mixture. The presence of either of the nanoclay dramatically accelerates the drug's recrystallization rate and slows down the drug's releasing rate. The drop of the releasing rate is mainly due to the decrease of wettability, as supported by the contact angle data. Data analysis of the dissolution results suggests that the addition of nanoclays changes the drug's release mechanism from erosion dominant to diffusion dominant. This study suggests that nanoclays may be utilized to tailor the drug's releasing rate and to improve the dosage form's stability by dramatically shortening the lengthy recrystallization process. Copyright (c) 2010 Elsevier B.V. All rights reserved.

Recrystallization and grain growth induced by ELMs-like transient heat loads in deformed tungsten samples

PubMed Central

Suslova, A.; El-Atwani, O.; Sagapuram, D.; Harilal, S. S.; Hassanein, A.

2014-01-01

Tungsten has been chosen as the main candidate for plasma facing components (PFCs) due to its superior properties under extreme operating conditions in future nuclear fusion reactors such as ITER. One of the serious issues for PFCs is the high heat load during transient events such as ELMs and disruption in the reactor. Recrystallization and grain size growth in PFC materials caused by transients are undesirable changes in the material, since the isotropic microstructure developed after recrystallization exhibits a higher ductile-to-brittle transition temperature which increases with the grain size, a lower thermal shock fatigue resistance, a lower mechanical strength, and an increased surface roughening. The current work was focused on careful determination of the threshold parameters for surface recrystallization, grain growth rate, and thermal shock fatigue resistance under ELM-like transient heat events. Transient heat loads were simulated using long pulse laser beams for two different grades of ultrafine-grained tungsten. It was observed that cold rolled tungsten demonstrated better power handling capabilities and higher thermal stress fatigue resistance compared to severely deformed tungsten. Higher recrystallization threshold, slower grain growth, and lower degree of surface roughening were observed in the cold rolled tungsten. PMID:25366885

Recrystallization of water in non-water-soluble (meth)acrylate polymers is not rare and is not devitrification.

PubMed

Gemmei-Ide, Makoto; Ohya, Atsushi; Kitano, Hiromi

2012-02-16

Change in the state of water sorbed into four kinds of non-water-soluble poly(meth)acrylates with low water content by temperature (T) perturbation was examined on the basis of T variable mid-infrared (MIR) spectroscopy. Many studies using differential scanning calorimetry suggested that there was no change in the state. T dependence of their MIR spectra, however, clearly demonstrated various changes in the state. Furthermore, recrystallization, which was crystallization during heating, was observed in all four polymers. The recrystallization observed in this study was not devitrification, which is the change in the state from glassy water to crystalline water, but vapor deposition during heating (vapor re-deposition). There were only two reports about recrystallization of water in a non-water-soluble polymer before this report; therefore, it might be considered to be a rare phenomenon. However, as demonstrated in this study, it is not a rare phenomenon. Recrystallization (vapor re-deposition) of water in the polymer matrices is related to a balance between flexibility and strength of the electrostatic interaction sites of polymer matrices but might not be related to the biocompatibility of polymers.

Recrystallization and grain growth induced by ELMs-like transient heat loads in deformed tungsten samples.

PubMed

Suslova, A; El-Atwani, O; Sagapuram, D; Harilal, S S; Hassanein, A

2014-11-04

Tungsten has been chosen as the main candidate for plasma facing components (PFCs) due to its superior properties under extreme operating conditions in future nuclear fusion reactors such as ITER. One of the serious issues for PFCs is the high heat load during transient events such as ELMs and disruption in the reactor. Recrystallization and grain size growth in PFC materials caused by transients are undesirable changes in the material, since the isotropic microstructure developed after recrystallization exhibits a higher ductile-to-brittle transition temperature which increases with the grain size, a lower thermal shock fatigue resistance, a lower mechanical strength, and an increased surface roughening. The current work was focused on careful determination of the threshold parameters for surface recrystallization, grain growth rate, and thermal shock fatigue resistance under ELM-like transient heat events. Transient heat loads were simulated using long pulse laser beams for two different grades of ultrafine-grained tungsten. It was observed that cold rolled tungsten demonstrated better power handling capabilities and higher thermal stress fatigue resistance compared to severely deformed tungsten. Higher recrystallization threshold, slower grain growth, and lower degree of surface roughening were observed in the cold rolled tungsten.

Dynamic Grain Growth in Forsterite Aggregates Experimentally Deformed to High Strain

NASA Astrophysics Data System (ADS)

Kellermann Slotemaker, A.; de Bresser, H.; Spiers, C.; Drury, M.

2004-12-01

The dynamics of the outer Earth are largely controlled by olivine rheology. From previous work it has become clear that if olivine rocks are deformed to high strain, substantial weakening may occur before steady state mechanical behaviour is approached. This weakening appears directly related to progressive modification of the grain size distribution through competing effects of dynamic recrystallization and syn-deformational grain growth. However, most of our understanding of these processes in olivine comes from tests on coarse-grained materials that were reduced in grain size during straining by grain size insensitive (dislocation) creep mechanisms. The aim of the present study was to investigate microstructure evolution of fine-grained olivine rocks that coarsen in grain size while deforming by grain size sensitive (GSS) creep. We used fine-grained (~1 μ m) olivine aggregates (i.e., forsterite/Mg2SiO4), containing ~0.5 wt% water and 10 vol% enstatite (MgSiO3). Two types of experiments were carried out: 1) Hot isostatic pressing (HIP) followed by axial compression to varying strains up to a maximum of ~45%, at 600 MPa confining pressure and a temperature of 950°C, 2) HIP treatment without axial deformation. Microstructures were characterized by analyzing full grain size distributions and texture using SEM/EBSD. Our stress-strain curves showed continuous hardening. When samples were temporally unloaded for short time intervals, no difference in flow stress was observed before and after the interruption in straining. Strain rate sensitivity analysis showed a low value of ~1.5 for the stress exponent n. Measured grain sizes show an increase with strain up to a value twice that of the starting value. HIP-only samples showed only minor increase in grain size. A random LPO combined with the low n ~1.5 suggests dominant GSS creep controlled by grain boundary sliding. These results indicate that dynamic grain growth occurs in forsterite aggregates deforming by GSS creep, and we relate the continuous strain hardening to this process. A dynamic grain growth model involving an increase in cellular defect fraction seems best applicable to the grain growth observed in this study. We suggest that the employment of this model to fine-grained olivine rocks can further improve our understanding of the microstructural evolution of this material and related rheological behaviour.

Orientation filtering for crystalline films

DOEpatents

Smith, H.I.; Atwater, H.A.; Thompson, C.V.; Geis, M.W.

1986-12-30

A substrate is coated with a film to be recrystallized. A pattern of crystallization barriers is created in the film, for example, by etching voids in the film. An encapsulation layer is generally applied to protect the film, fill the voids and otherwise enhance a recrystallization process. Recrystallization is carried out such that certain orientations pass preferentially through the barrier, generally as a result of growth-velocity anisotropy. The result is a film of a specific predetermined crystallographic orientation, a range of orientations or a set of discrete orientations. 7 figs.

Strong Surface Diffusion Mediated Glancing-Angle Deposition: Growth, Recrystallization and Reorientation of Tin Nanorods

NASA Astrophysics Data System (ADS)

Wang, Huan-Hua; Shi, Yi-Jian; William, Chu; Yigal, Blum

2008-01-01

Different from usual glancing-angle deposition where low surface diffusion is necessary to form nanorods, strong surface diffusion mediated glancing-angle deposition is exemplified by growing tin nanorod films on both silicon and glass substrates simultaneously via thermal evaporation. During growth, the nanorods were simultaneously baked by the high-temperature evaporator, and therefore re-crystallized into single crystals in consequence of strong surface diffusion. The monocrystalline tin nanorods have a preferred orientation perpendicular to the substrate surface, which is quite different from the usual uniformly oblique nanorods without recrystallization.

Role of the Double-Layer Cation on the Potential-Dependent Stretching Frequencies and Binding Geometries of Carbon Monoxide at Platinum-Nonaqueous Interfaces

DTIC Science & Technology

1992-02-01

were recrystallized twice from water, or water, and then ethanol , and methanol/water, respectively, and dried at 100"C under vacuum for 24 hours. The...hexafluorophosphate, and recrystallized twice from absolute ethanol . The alkali perchlorates (LiCIO4, NaCl0 4, KCIO 4, from G.F. Smith) were recrystallized twice from...which a Ag/AgCl (3M KCI) reference electrode was used. All measurements were made at room 5 temperature , 23 ± VC. RESULTS In our earlier preliminary

Optically induced melting of colloidal crystals and their recrystallization.

PubMed

Harada, Masashi; Ishii, Masahiko; Nakamura, Hiroshi

2007-04-15

Colloidal crystals melt by applying focused light of optical tweezers and recrystallize after removing it. The disturbed zone by the light grows radially from the focus point and the ordering starts from the interface with the crystal. Although the larger disturbed zone is observed for the higher power optical tweezers, a master curve is extracted by normalization of the disturbed zone. The temporal changes of the normalized disturbed zone are well described with exponential functions, indicating that the melting and recrystallization process is governed by a simple relaxation mechanism.

Annealing effects in plated-wire memory elements. II - Recrystallization in Permalloy films.

NASA Technical Reports Server (NTRS)

Marquardt, S. J.; Kench, J. R.

1971-01-01

Results of grain-size measurements in Permalloy platings suggest that recrystallization is possible at temperatures as low as 200 C, but that it is an extremely heterogeneous process. No worthwhile correlation was found to exist between observed grain size and magnetic dispersion in samples aged in the temperature range from 180 to 230 C. It is suggested that the magnetic aging which occurs under these conditions may be due to some other diffusion-controlled process than recrystallization; a process such as chemical homogenization is tentatively preferred.

Hot Deformation Behavior and a Two-Stage Constitutive Model of 20Mn5 Solid Steel Ingot during Hot Compression

PubMed Central

Liu, Min; Ma, Qing-Xian; Luo, Jian-Bin

2018-01-01

20Mn5 steel is widely used in the manufacture of heavy hydro-generator shaft forging due to its strength, toughness, and wear resistance. However, the hot deformation and recrystallization behaviors of 20Mn5 steel compressed under a high temperature were not studied. For this article, hot compression experiments under temperatures of 850–1200 °C and strain rates of 0.01 s−1–1 s−1 were conducted using a Gleeble-1500D thermo-mechanical simulator. Flow stress-strain curves and microstructure after hot compression were obtained. Effects of temperature and strain rate on microstructure are analyzed. Based on the classical stress-dislocation relationship and the kinetics of dynamic recrystallization, a two-stage constitutive model is developed to predict the flow stress of 20Mn5 steel. Comparisons between experimental flow stress and predicted flow stress show that the predicted flow stress values are in good agreement with the experimental flow stress values, which indicates that the proposed constitutive model is reliable and can be used for numerical simulation of hot forging of 20Mn5 solid steel ingot. PMID:29547570

Microstructure Evolution and Flow Stress Model of a 20Mn5 Hollow Steel Ingot during Hot Compression

PubMed Central

Liu, Min; Ma, Qing-Xian; Luo, Jian-Bin

2018-01-01

20Mn5 steel is widely used in the manufacture of heavy hydro-generator shaft due to its good performance of strength, toughness and wear resistance. However, the hot deformation and recrystallization behaviors of 20Mn5 steel compressed under high temperature were not studied. In this study, the hot compression experiments under temperatures of 850–1200 °C and strain rates of 0.01/s–1/s are conducted using Gleeble thermal and mechanical simulation machine. And the flow stress curves and microstructure after hot compression are obtained. Effects of temperature and strain rate on microstructure are analyzed. Based on the classical stress-dislocation relation and the kinetics of dynamic recrystallization, a two-stage constitutive model is developed to predict the flow stress of 20Mn5 steel. Comparisons between experimental flow stress and predicted flow stress show that the predicted flow stress values are in good agreement with the experimental flow stress values, which indicates that the proposed constitutive model is reliable and can be used for numerical simulation of hot forging of 20Mn5 hollow steel ingot. PMID:29561826

Dynamic Recrystallization Model for Whisker and Hillock Growth

DOE Office of Scientific and Technical Information (OSTI.GOV)

Vianco, Paul T.; Neilsen, Michael K.

2015-07-01

Tin (Sn) whiskers are not a recent development. Studies in the late 1930’s investigated thin filaments that grew spontaneously from Sn coatings used for the corrosion protection of electronic hardware. It was soon recognized that these Sn filaments,or whiskers, could create short circuits in the same electronic equipment. Figure 1a illustrates whisker growth in the hole of a printed circuit board having an immersion Sn surface finish. The engineering solution was to contaminate the Sn with > 3wt.% of lead (Pb). The result was that whisker growth was replaced with hillock formation (Fig. 1b) that posed a minimal reliability concerntomore » electrical circuits. Today, Pb-containing finishes are being replaced with pure Sn coatings to meet environmental restrictions on Pb use. The same short-circuit concerns have been raised, once again, with respect to Sn whiskers. The present authors have taken the approach that, in order to develop more widely applicable, first-principles strategies to mitigate Sn whisker formation, it is necessary to understand the fundamental mechanism(s) and rate kinetics underlying their development. Numerous mechanisms have been proposed by other authors to describe whisker growth, including static recrystallization by Boguslavsky and Bush.« less

Effects of Static Recrystallization and Precipitation on Mechanical Properties of 00Cr12 Ferritic Stainless Steel

NASA Astrophysics Data System (ADS)

Shao, Yi; Liu, Chenxi; Yue, Tengxiao; Liu, Yongchang; Yan, Zesheng; Li, Huijun

2018-05-01

The 00Cr12 ferritic stainless steel samples were isothermally held at different temperatures in the range of 700 °C to 1000 °C to investigate the effect of static recrystallization and precipitation on mechanical properties, such as microhardness, tensile strength, and yield strength. The results show that the formation of the fine recrystallized grain, as well as precipitation, coarsening, and dissolution of the second-phase particles, influences the mechanical properties remarkably. The fine recrystallized grain can provide a positive grain boundary-strengthening effect in the sample under a relatively high holding temperature. Coarsening and dissolution of M23C6 result in partial depletion of precipitate hardening. In contrast, the size and number density of MX particles are almost constant, regardless of the holding temperature; therefore, it can provide a better precipitation-hardening effect.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Deibler, Lisa Anne; Brown, Arthur; Puskar, Joseph D.

Drawn 304L stainless steel tubing was subjected to 42 different annealing heat treatments with the goal of initializing a microstructural model to select a heat treatment to soften the tubing from a hardness of 305 Knoop to 225–275 Knoop. The amount of recrystallization and grain size caused by 18 heat treatments were analyzed via optical microscopy and image analysis, revealing the full range of recrystallization from 0 to 100%. The formation of carbides during the longer duration and higher-temperature heat treatments was monitored via transmission electron microscope evaluation. The experimental results informed a model which includes recovery, recrystallization, and grainmore » growth to predict microstructure and hardness. After initialization of the model, it was able to predict hardness with a R 2 value of 0.95 and recrystallization with an R 2 value of 0.99. As a result, the model was then utilized in the design and testing of a heat treatment to soften the tubing.« less

A comparative study on the direct deposition of μc-Si:H and plasma-induced recrystallization of a-Si:H: Insight into Si crystallization in a high-density plasma

NASA Astrophysics Data System (ADS)

Zhou, H. P.; Xu, M.; Xu, S.; Feng, Y. Y.; Xu, L. X.; Wei, D. Y.; Xiao, S. Q.

2018-03-01

Deep insight into the crystallization mechanism of amorphous silicon is of theoretical and technological significance for the preparation of high-quality microcrystalline/polycrystalline silicon. In this work, we intensively compare the present two plasma-involved routes, i.e., the direct deposition and recrystallization of precursor amorphous silicon (a-Si) films, to fabricate microcrystalline silicon. Both the directly deposited and recrystallized samples show multi-layered structures as revealed by electronic microscopy. High-density hydrogen plasma involved recrystallization process, which is mediated by the hydrogen diffusion into the deep region of the precursor a-Si film, displays significantly different nucleation configuration, interface properties, and crystallite shape. The underlying mechanisms are analyzed in combination with the interplay of high-density plasma and growing or treated surface.

FEM study of recrystallized tungsten under ELM-like heat loads

NASA Astrophysics Data System (ADS)

Du, J.; Yuan, Y.; Wirtz, M.; Linke, J.; Liu, W.; Greuner, H.

2015-08-01

FEM thermal analysis has been performed on rolled tungsten plate loaded with heat load of 23 MW/m2 for 1.5 s. Gradient temperature field is generated due to the Gaussian shape beam profile. Recrystallization and grain growth of various scales were found at different areas of the sample depending on the localized thermal field. FEM thermal-mechanical analyses have been performed on the recrystallized tungsten exposed to ELMs-like heat loads. The analyzed load conditions were 0.38 and 1.14 GW/m2 with different base temperatures. Material deterioration due to recrystallization was implemented by adopting decreased yield stress, tangent modulus, strength coefficient and ductility coefficients. Life time predicted by adopting strain life criterion indicates grain growth from 5 μm to 100 μm causes the life decrease of 80%. This result is gained by pure mathematical calculation based on the empiric assumptions of material properties.

Thermoplastic polyimide NEW-TPI (trademark)

NASA Technical Reports Server (NTRS)

Hou, Tan-Hung; Reddy, Rakasi M.

1990-01-01

Thermal and rheological properties of a commercial thermoplastic polyimide, NEW-TPI (trademark), were characterized. The as-received material possesses initially a transient crystallite form with a bimodal distribution in peak melting temperatures. After the melting of the initial crystallite structure, the sample can be recrystallized by various thermal treatments. A bimodal or single modal melting peak distribution is formed for annealing temperatures below or above 360 C, respectively. The recrystallized crystallinities are all transient in nature. The polymers are unable to be recrystallized after being subjected to elevated temperature annealing above 450 C. The recrystallization mechanism was postulated, and a simple kinetics model was found to describe the behavior rather satisfactory under the conditions of prolonged thermal annealing. Rheological measurements made in the linear viscoelastic range support the evidence observed in the thermal analysis. Furthermore, the measurements sustain the manufacturer's recommended processing window of 400 to 420 C for this material.

A study of the oxide dispersion and recrystallization in NiCrAl prepared from preoxidized powder

NASA Technical Reports Server (NTRS)

Glasgow, T. K.

1975-01-01

The SAP technique of dispersion strengthening (formation of an oxide dispersion by preoxidation of metal powders) was applied to atomized powder of the alloy Ni-17Cr-5Al-0.2 Y. SAP-NiCrAl was worked by extrusion and rod rolling at 1205 C and by swaging at 760 C. A variety of annealing treatments were applied after working to determine the recrystallization response. NiCrAlY, similarly prepared from atomized powder, but without a preoxidation treatment, was examined for comparison. The SAP-NiCrAl of this study exhibited oxide particle size and spacing much larger than that usually observed in oxide dispersion strengthened alloys; nonetheless, it was possible to achieve abnormal (secondary) recrystallization in the SAP-NiCrAl as has been reported for other oxide dispersion strengthened alloys. In contrast, unoxidized NiCrAlY exhibited only primary recrystallization.

Recrystallization-induced self-assembly for the growth of Cu₂O superstructures.

PubMed

Shang, Yang; Shao, Yi-Ming; Zhang, Dong-Feng; Guo, Lin

2014-10-20

The assembly of inorganic nanoparticles (NPs) into 3D superstructures with defined morphologies is of particular interest. A novel strategy that is based on recrystallization-induced self-assembly (RISA) for the construction of 3D Cu2O superstructures and employs Cu2O mesoporous spheres with diameters of approximately 300 nm as the building blocks has now been developed. Balancing the hydrolysis and recrystallization rates of the CuCl precursors through precisely adjusting the experimental parameters was key to success. Furthermore, the geometry of the superstructures can be tuned to obtain either cubes or tetrahedra and was shown to be dependent on the growth behavior of bulk CuCl. The overall strategy extends the applicability of recrystallization-based processes for the guided construction of assemblies and offers unique insights for assembling larger particles into complicated 3D superstructures. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Copper Refinement from Anode to Cathode and then to Wire Rod: Effects of Impurities on Recrystallization Kinetics and Wire Ductility.

PubMed

Helbert, Anne-Laure; Moya, Alice; Jil, Tomas; Andrieux, Michel; Ignat, Michel; Brisset, François; Baudin, Thierry

2015-10-01

In this paper, the traceability of copper from the anode to the cathode and then the wire rod has been studied in terms of impurity content, microstructure, texture, recrystallization kinetics, and ductility. These characterizations were obtained based on secondary ion mass spectrometry, differential scanning calorimetry (DSC), X-ray diffraction, HV hardness, and electron backscattered diffraction. It is shown that the recrystallization was delayed by the total amount of impurities. From tensile tests performed on cold drawn and subsequently annealed wires for a given time, a simplified model has been developed to link tensile elongation to the chemical composition. This model allowed quantification of the contribution of some additional elements, present in small quantity, on the recrystallization kinetics. The proposed model adjusted for the cold-drawn wires was also validated on both the cathode and wire rod used for the study of traceability.

A method for the monitoring of metal recrystallization based on the in-situ measurement of the elastic energy release using neutron diffraction.

PubMed

Christien, F; Telling, M T F; Knight, K S; Le Gall, R

2015-05-01

A method is proposed for the monitoring of metal recrystallization using neutron diffraction that is based on the measurement of stored energy. Experiments were performed using deformed metal specimens heated in-situ while mounted at the sample position of the High Resolution Powder Diffractometer, HRPD (ISIS Facility), UK. Monitoring the breadth of the resulting Bragg lines during heating not only allows the time-dependence (or temperature-dependence) of the stored energy to be determined but also the recrystallized fraction. The analysis method presented here was developed using pure nickel (Ni270) specimens with different deformation levels from 0.29 to 0.94. In situ temperature ramping as well as isothermal annealing was undertaken. The method developed in this work allows accurate and quantitative monitoring of the recrystallization process. The results from neutron diffraction are satisfactorily compared to data obtained from calorimetry and hardness measurements.

Microstructure and yield strength effects on hydrogen and tritium induced cracking in HERF (high-energy-rate-forged) stainless steel

DOE Office of Scientific and Technical Information (OSTI.GOV)

Morgan, M J; Tosten, M H

1989-01-01

Rising-load J-integral measurements and falling-load threshold stress intensity measurements were used to characterize hydrogen and tritium induced cracking in high-energy-rate-forged (HERF) 21-6-9 stainless steel. Samples having yield strengths in the range 517--930 MPa were thermally charged with either hydrogen or tritium and tested at room temperature in either air or high-pressure hydrogen gas. In general, the hydrogen isotopes reduced the fracture toughness by affecting the fracture process. Static recrystallization in the HERF microstructures affected the material's fracture toughness and its relative susceptibility to hydrogen and tritium induced fracture. In hydrogen-exposed samples, the reduction in fracture toughness was primarily dependent onmore » the susceptibility of the microstructure to intergranular fracture and only secondarily affected by strength in the range of 660 to 930 MPa. Transmission-electron microscopy observations revealed that the microstructures least susceptible to hydrogen-induced intergranular cracking contained patches of fully recrystallized grains. These grains are surrounded by highly deformed regions containing a high number density of dislocations. The microstructure can best be characterized as duplex'', with soft recrystallized grains embedded in a hard, deformed matrix. The microstructures most susceptible to hydrogen-induced intergranular fracture showed no well-developed recrystallized grains. The patches of recrystallized grains seemed to act as crack barriers to hydrogen-induced intergranular fracture. In tritium-exposed-and-aged samples, the amount of static recrystallization also affected the fracture toughness properties but to a lesser degree. 7 refs., 25 figs.« less

Evolution of grain boundary character distributions in alloy 825 tubes during high temperature annealing: Is grain boundary engineering achieved through recrystallization or grain growth?

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bai, Qin; Zhao, Qing

Grain boundary engineering (GBE) of nickel-based alloy 825 tubes was carried out with different cold drawing deformations by using a draw-bench on a factory production line and subsequent annealing at various temperatures. The microstructure evolution of alloy 825 during thermal-mechanical processing (TMP) was characterized by means of the electron backscatter diffraction (EBSD) technique to study the TMP effects on the grain boundary network and the evolution of grain boundary character distributions during high temperature annealing. The results showed that the proportion of ∑ 3{sup n} coincidence site lattice (CSL) boundaries of alloy 825 tubes could be increased to > 75%more » by the TMP of 5% cold drawing and subsequent annealing at 1050 °C for 10 min. The microstructures of the partially recrystallized samples and the fully recrystallized samples suggested that the proportion of low ∑ CSL grain boundaries depended on the annealing time. The frequency of low ∑ CSL grain boundaries increases rapidly with increasing annealing time associating with the formation of large-size highly-twinned grains-cluster microstructure during recrystallization. However, upon further increasing annealing time, the frequency of low ∑ CSL grain boundaries decreased markedly during grain growth. So it is concluded that grain boundary engineering is achieved through recrystallization rather than grain growth. - Highlights: •The grain boundary engineering (GBE) is applicable to 825 tubes. •GBE is achieved through recrystallization rather than grain growth. •The low ∑ CSL grain boundaries in 825 tubes can be increased to > 75%.« less

Physical stability and recrystallization kinetics of amorphous ibipinabant drug product by fourier transform raman spectroscopy.

PubMed

Sinclair, Wayne; Leane, Michael; Clarke, Graham; Dennis, Andrew; Tobyn, Mike; Timmins, Peter

2011-11-01

The solid-state physical stability and recrystallization kinetics during storage stability are described for an amorphous solid dispersed drug substance, ibipinabant, at a low concentration (1.0%, w/w) in a solid oral dosage form (tablet). The recrystallization behavior of the amorphous ibipinabant-polyvinylpyrrolidone solid dispersion in the tablet product was characterized by Fourier transform (FT) Raman spectroscopy. A partial least-square analysis used for multivariate calibration based on Raman spectra was developed and validated to detect less than 5% (w/w) of the crystalline form (equivalent to less than 0.05% of the total mass of the tablet). The method provided reliable and highly accurate predictive crystallinity assessments after exposure to a variety of stability storage conditions. It was determined that exposure to moisture had a significant impact on the crystallinity of amorphous ibipinabant. The information provided by the method has potential utility for predictive physical stability assessments. Dissolution testing demonstrated that the predicted crystallinity had a direct correlation with this physical property of the drug product. Recrystallization kinetics was measured using FT Raman spectroscopy for the solid dispersion from the tablet product stored at controlled temperature and relative humidity. The measurements were evaluated by application of the Johnson-Mehl-Avrami (JMA) kinetic model to determine recrystallization rate constants and Avrami exponent (n = 2). The analysis showed that the JMA equation could describe the process very well, and indicated that the recrystallization kinetics observed was a two-step process with an induction period (nucleation) followed by rod-like crystal growth. Copyright © 2011 Wiley-Liss, Inc.

Effects of Roughing on Finish Rolling Simulations in Microalloyed Strip Steels

NASA Astrophysics Data System (ADS)

Chalimba, S. A. J.; Mostert, R. J.; Stumpf, W. E.; Siyasiya, C. W.; Banks, K. M.

2017-11-01

The effects of a roughing pass in hot rolling simulations were assessed in VN and Nb-Ti steels. Continuous cooling phase transformation temperatures, flow curves, softening mechanisms (dynamic transformation DT and dynamic recrystallization DRX), and deformed microstructure morphologies were analyzed. The application of one or more roughing passes eliminates the effects of prior microstructural history and ensures that all stock material experiences equivalent hot working conditions and state of the microalloying elements. It has been shown that roughing in hot simulation has the following positive influences: (1) provide more reliable flow stress data; (2) give greater consistencies and accuracy in analysis of softening mechanisms giving three distinct regimes (DT regime at temperatures below 800 °C, DT/DRX inter-mode regime between 800 and 950 °C and DRX regime for temperatures above 950 °C for VN steel); (3) promotion of softening mechanisms as evidence by low critical strains (ɛ_{{{c} {DT}}} was within the range 0.08-0.12, while for finishing-only pass, the ɛ_{{{c} {DT}}} was in the range of 0.11-0.14 at \\dot{ɛ } = 0.1 s-1); (4) for roughing and finishing schedules, DT was verified to occur at temperatures 117 and 133 °C above Ae3 for VN steel and Nb-Ti steel, respectively, compared to the F-only schedules which showed that DT can only occur at temperatures below the Ae3; (5) RF schedules promoted uniform microstructural morphologies compared to inhomogeneous microstructures realized in F-only schedules.

Some chemical aspects of diagenetic carbonates from the Miocene of Sitakund, Bangladesh

DOE Office of Scientific and Technical Information (OSTI.GOV)

Akhter, S.H.; Chowdhury, S.Q.; Kandaker, N.I.

1990-05-01

A preliminary chemical and petrological study was done of the Miocene limestone and its comparison with surrounding and overlying marine shales. The material for these studies was obtained from the Miocene Surma sediments exposed in Sitakund region, Cluttagong, Bangladesh. These limestones occur in a predominantly marine shale sequence and show an apparent angular structural relationship with respect to the host marine shales. Three types of carbonates are recognized: banded limestone, dark laminated limestone, and argillaceous limestone. These are devoid of any skeletal remains and often show recrystallization phenomena. Carbonate mineral phases included calcite, aragonite, dolomite, and more rarely magnesite andmore » ankerite. Noncarbonate fraction shows quartz, although very fine grained, is intricately intergrown, indicating that it is at least recrystallized, if not authigenic. Petrographic study of these carbonates show a great variability in terms of texture and composition and suggest a complex multistep and presumably continuous diagenesis. Relatively high REE (rare earth elements) abundances in these carbonates are most likely due to diagenesis and incorporation of mobile REE from local detrital phases into diagenetic carbonates. The anomalously low abundances of cerium in all the carbonates indicates a predominantly marine source for the REE. Recrystallization of carbonate resulted in the extensive exchange of Sr and O between carbonate and diagenetic fluid, the latter being low in REE/Ca ratios. Associated marine shales have quite dissimilar trace-element signatures. This may reflect uncommon crustal sources of REE for the carbonates and clastics. The enrichment of Ni and Zn in marine shales are related to the proximality of local bedrock source areas and clay minerals in the marine sediments.« less

High-pressure metamorphism in the southern New England Orogen: Implications for long-lived accretionary orogenesis in eastern Australia

NASA Astrophysics Data System (ADS)

Phillips, G.; Offler, R.; Rubatto, D.; Phillips, D.

2015-09-01

New geochemical, metamorphic, and isotopic data are presented from high-pressure metamorphic rocks in the southern New England Orogen (eastern Australia). Conventional and optimal thermobarometry are augmented by U-Pb zircon and 40Ar/39Ar phengite dating to define pressure-temperature-time (P-T-t) histories for the rocks. The P-T-t histories are compared with competing geodynamic models for the Tasmanides, which can be summarized as (i) a retreating orogen model, the Tasmanides formed above a continuous, west dipping, and eastward retreating subduction zone, and (ii) a punctuated orogen model, the Tasmanides formed by several arc accretion, subduction flip, and/or transference events. Whereas both scenarios are potentially supported by the new data, an overlap between the timing of metamorphic recrystallization and key stages of Tasmanides evolution favors a relationship between a single, long-lived subduction zone and the formation, exhumation, and exposure of the high-pressure rocks. By comparison with the retreating orogen model, the following links with the P-T-t histories emerge: (i) exhumation and underplating of oceanic eclogite during the Delamerian Orogeny, (ii) recrystallization of underplated and exhuming high-pressure rocks at amphibolite facies conditions coeval with a period of rollback, and (iii) selective recrystallization of high-pressure rocks at blueschist facies conditions, reflecting metamorphism in a cooled subduction zone. The retreating orogen model can also account for the anomalous location of the Cambrian-Ordovician high-pressure rocks in the Devonian-Carboniferous New England Orogen, where sequential rollback cycles detached and translated parts of the leading edge of the overriding plate to the next, younger orogenic cycle.

Molecular dynamics study of the melting of a supported 887-atom Pd decahedron.

PubMed

Schebarchov, D; Hendy, S C; Polak, W

2009-04-08

We employ classical molecular dynamics simulations to investigate the melting behaviour of a decahedral Pd(887) cluster on a single layer of graphite (graphene). The interaction between Pd atoms is modelled with an embedded-atom potential, while the adhesion of Pd atoms to the substrate is approximated with a Lennard-Jones potential. We find that the decahedral structure persists at temperatures close to the melting point, but that just below the melting transition, the cluster accommodates to the substrate by means of complete melting and then recrystallization into an fcc structure. These structural changes are in qualitative agreement with recently proposed models, and they verify the existence of an energy barrier preventing softly deposited clusters from 'wetting' the substrate at temperatures below the melting point.

Atomistic potentials based energy flux integral criterion for dynamic adiabatic shear banding

NASA Astrophysics Data System (ADS)

Xu, Yun; Chen, Jun

2015-02-01

The energy flux integral criterion based on atomistic potentials within the framework of hyperelasticity-plasticity is proposed for dynamic adiabatic shear banding (ASB). System Helmholtz energy decomposition reveals that the dynamic influence on the integral path dependence is originated from the volumetric strain energy and partial deviatoric strain energy, and the plastic influence only from the rest part of deviatoric strain energy. The concept of critical shear banding energy is suggested for describing the initiation of ASB, which consists of the dynamic recrystallization (DRX) threshold energy and the thermal softening energy. The criterion directly relates energy flux to the basic physical processes that induce shear instability such as dislocation nucleations and multiplications, without introducing ad-hoc parameters in empirical constitutive models. It reduces to the classical path independent J-integral for quasi-static loading and elastic solids. The atomistic-to-continuum multiscale coupling method is used to simulate the initiation of ASB. Atomic configurations indicate that DRX induced microstructural softening may be essential to the dynamic shear localization and hence the initiation of ASB.

Stress in recrystallized quartz by electron backscatter diffraction mapping

NASA Astrophysics Data System (ADS)

Llana-Fúnez, S.

2017-07-01

The long-term state of stress at middle and lower crustal depths can be estimated through the study of the microstructure of exhumed rocks from active and/or ancient shear zones. Constitutive equations for deformation mechanisms in experimentally deformed rocks relate differential stress to the size of recrystallized grains. Cross et al. (2017) take advantage of electron backscatter diffraction mapping to systematically separate new recrystallized grains from host grains on the basis of the measurable lattice distorsion within the grains. They produce the first calibrated piezometer for quartz with this technique, reproducing within error a previous calibration based on optical microscopy.

Application of two-level factorial design to investigate the effect of process parameters on the sonocrystallization of sulfathiazole

NASA Astrophysics Data System (ADS)

Kuo, Peng-Hsuan; Zhang, Bo-Cong; Su, Chie-Shaan; Liu, Jun-Jen; Sheu, Ming-Thau

2017-08-01

In this study, cooling sonocrystallization was used to recrystallize an active pharmaceutical ingredient, sulfathiazole, using methanol as the solvent. The effects of three operating parameters-sonication intensity, sonication duration, and solution concentration-on the recrystallization were investigated by using a 2k factorial design. The solid-state properties of sulfathiazole, including the mean particle size, crystal habit, and polymorphic form, were analyzed. Analysis of variance showed that the effect of the sonication intensity, cross-interaction effect of sonication intensity/sonication duration, and cross-interaction effect of sonication intensity/solution concentration on the recrystallization were significant. The results obtained using the 2k factorial design indicated that a combination of high sonication intensity and long sonication duration is not favorable for sonocrystallization, especially at a high solution concentration. A comparison of the solid-state properties of the original and the recrystallized sulfathiazole revealed that the crystal habit of the recrystallized sulfathiazole was more regular and that its mean particle size could be reduced to approximately 10 μm. Furthermore, the analytical results obtained using the PXRD, DSC, and FTIR spectroscopy indicated that the polymorphic purity of sulfathiazole improved from the original Form III/IV mixture to Form III after sonocrystallization.

Microstructure study of a severely plastically deformed Mg-Zn-Y alloy by application of low angle annular dark field diffraction contrast imaging.

PubMed

Basha, Dudekula Althaf; Rosalie, Julian M; Somekawa, Hidetoshi; Miyawaki, Takashi; Singh, Alok; Tsuchiya, Koichi

2016-01-01

Microstructural investigation of extremely strained samples, such as severely plastically deformed (SPD) materials, by using conventional transmission electron microscopy techniques is very challenging due to strong image contrast resulting from the high defect density. In this study, low angle annular dark field (LAADF) imaging mode of scanning transmission electron microscope (STEM) has been applied to study the microstructure of a Mg-3Zn-0.5Y (at%) alloy processed by high pressure torsion (HPT). LAADF imaging advantages for observation of twinning, grain fragmentation, nucleation of recrystallized grains and precipitation on second phase particles in the alloy processed by HPT are highlighted. By using STEM-LAADF imaging with a range of incident angles, various microstructural features have been imaged, such as nanoscale subgrain structure and recrystallization nucleation even from the thicker region of the highly strained matrix. It is shown that nucleation of recrystallized grains starts at a strain level of revolution [Formula: see text] (earlier than detected by conventional bright field imaging). Occurrence of recrystallization of grains by nucleating heterogeneously on quasicrystalline particles is also confirmed. Minimizing all strain effects by LAADF imaging facilitated grain size measurement of [Formula: see text] nm in fully recrystallized HPT specimen after [Formula: see text].

Modeling the microstructural changes during hot tandem rolling of AA5 XXX aluminum alloys: Part II. Textural evolution

NASA Astrophysics Data System (ADS)

Wells, M. A.; Samarasekera, I. V.; Brimacombe, J. K.; Hawbolt, E. B.; Lloyd, D. J.

1998-06-01

In Part II of this article, the experimental work undertaken to measure the effect of deformation parameters (temperature, strain, and strain rate) on the texture formation during hot deformation and the evolution during subsequent recrystallization is described. In addition, the isothermal kinetics of development of individual texture components were also determined. A neutron diffractometer was used to measure the texture in the as-hot-deformed aluminum samples, and the samples were then heat treated in a 400 °C salt bath for various lengths of time, with the texture being remeasured at various stages in the recrystallization process. Using data from the experimental program, the texture evolution during recrystallization was modeled by applying a modified form of the Avrami equation. Results indicated that, of the deformation parameters studied, textural development was most sensitive to the deformation temperature for both alloys. In addition, modeling results revealed that the Cu component ({112} <111>) was the first to recrystallize, typically followed by the S ({123} <634>) and Bs ({110} <112>) components. This is in agreement with earlier work which indicated that the Bs component was the hardest to recrystallize, possibly because it is able to deform on very few slip systems and, hence, the dislocation interaction may be low.

Measurement of process-dependent material properties of pharmaceutical solids by nanoindentation.

PubMed

Liao, Xiangmin; Wiedmann, Timothy Scott

2005-01-01

The purpose of this work was to evaluate nanoindentation as a means to characterize the material properties of pharmaceutical solids. X-ray diffraction of potassium chloride and acetaminophen showed that samples prepared by cooling a melt to a crystalline sample as opposed to slow recrystallization had the same crystal structure. With analysis of the force-displacement curves, the KCl quenched samples had a hardness that was 10 times higher than the recrystallized KCl, while acetaminophen quenched samples were 25% harder than the recrystallized samples. The elastic moduli of the quenched samples were also much greater than that observed for the recrystallized samples. Although the elasticity was independent of load, the hardness increased with load for acetaminophen. With each sample, the flow at constant load increased with applied load. Etching patterns obtained by atomic force microscopy showed that the KCl quenched sample had a higher dislocation density than the recrystallized sample, although there was no evident difference in the acetaminophen samples. Overall, the differences in the observed sample properties may be related to the dislocation density. Thus, nanoindentation has been shown to be a sensitive method for determining a processed-induced change in the hardness, creep, and elasticity of KCl and acetaminophen. (c) 2004 Wiley-Liss, Inc.

Prediction of recrystallization behavior of troglitazone/polyvinylpyrrolidone solid dispersion by solid-state NMR.

PubMed

Ito, Atsutoshi; Watanabe, Tomoyuki; Yada, Shuichi; Hamaura, Takeshi; Nakagami, Hiroaki; Higashi, Kenjirou; Moribe, Kunikazu; Yamamoto, Keiji

2010-01-04

The purpose of this study was to elaborate the relationship between the (13)C CP/MAS NMR spectra and the recrystallization behavior during the storage of troglitazone solid dispersions. The solid dispersions were prepared by either the solvent method or by co-grinding. The recrystallization behavior under storage conditions at 40 degrees C/94% RH was evaluated by the Kolmogorov-Johnson-Mehl-Avrami (KJMA) equation. Solid dispersions prepared by the solvent method or by prolonged grinding brought about inhibition of the nucleation and the nuclei growth at the same time. No differences in the PXRD profiles were found in the samples prepared by the co-grinding and solvent methods, however, (13)C CP/MAS NMR showed significant differences in the spectra. The correlation coefficients using partial least square regression analysis between the PXRD profiles and the apparent nuclei-growth constant or induction period to nucleation were 0.1305 or 0.6350, respectively. In contrast, those between the (13)C CP/MAS NMR spectra and the constant or the period were 0.9916 or 0.9838, respectively. The (13)C CP/MAS NMR spectra had good correlation with the recrystallization kinetic parameters evaluated by the KJMA equation. Consequently, solid-state NMR was judged to be a useful tool for the prediction of the recrystallization behavior of solid dispersions.

Recrystallization Behavior in Mixed Solder Joints of BGA Components during Thermal Shock

NASA Astrophysics Data System (ADS)

Tan, Shihai; Han, Jing; Guo, Fu

2018-03-01

Sn-37Pb and Sn-3.0Ag-0.5Cu solder pastes printed onto a board were attached to ball grid array (BGA) samples using Sn-3.0Ag-0.5Cu solder balls. Before thermal shock, the initial grain orientations on the cross-section were obtained by scanning electron microscopy equipped with an electron backscattered diffraction system. Three mixed solder joints (two from the corner and another from the middle of the BGA component) and three lead-free solder joints (at the same positions) were selected to investigate the recrystallization behavior under thermal shock (TS) cycling conditions. All of the mixed and lead-free solder joints were initially single crystal. The results showed that recrystallization occurred in both the mixed and lead-free solder joints after 200 TS. For the mixed solder joints, more recrystallization was observed and the location of samples had a significant influence on their recrystallization behavior, while location was not as important for the lead-free samples after 200 TS in this study. Both the mixed and lead-free solder joints at the corner of BGA components showed the poorest reliability. According to misorientation distribution maps and subgrain rotation behaviors, the reliability of mixed solder joints was much poorer than that of lead-free solder joints.

Effect of cold deformation on the recrystallization behavior of FePd alloy at the ordering temperature using electron backscatter diffraction

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lin, Hung-Pin; Chen, Yen-Chun; Chen, Delphic

2014-08-15

In this study, the evolution of the recrystallization texture and microstructure was investigated after annealing of 50% and 90% cold-rolled FePd alloy at 530 °C. The FePd alloy was produced by vacuum arc melting in an atmosphere of 97% Ar and 3% H{sub 2}. The specimens were cold rolled to achieve 50% and 90% reduction in thickness. Electron backscatter diffraction measurements were performed on the rolling direction–normal direction section. With increased deformation from 50% to 90%, recrystallized texture transition occurs. For the 50% cold-rolled alloy, the preferred orientation is (0 1 0) [11 0 1], which is close to themore » cubic orientation after 400 h of annealing. For the 90% cold-rolled alloy, the orientation changes to (0 5 4) [22–4 5] after 16 h of annealing. - Highlights: • Texture and microstructure in cold-rolled FePd alloy was investigated during annealing using EBSD. • The recrystallized texture of 50% cold-rolled FePd is (0 1 0) [11 0 1] at 530 °C for 400 hours. • The recrystallized texture of 90% cold-rolled FePd is changed to (0 5 4) [22–4 5] at 530 °C after 16 hours.« less

Modeling High Temperature Deformation Behavior of Large-Scaled Mg-Al-Zn Magnesium Alloy Fabricated by Semi-continuous Casting

NASA Astrophysics Data System (ADS)

Li, Jianping; Xia, Xiangsheng

2015-09-01

In order to improve the understanding of the hot deformation and dynamic recrystallization (DRX) behaviors of large-scaled AZ80 magnesium alloy fabricated by semi-continuous casting, compression tests were carried out in the temperature range from 250 to 400 °C and strain rate range from 0.001 to 0.1 s-1 on a Gleeble 1500 thermo-mechanical machine. The effects of the temperature and strain rate on the hot deformation behavior have been expressed by means of the conventional hyperbolic sine equation, and the influence of the strain has been incorporated in the equation by considering its effect on different material constants for large-scaled AZ80 magnesium alloy. In addition, the DRX behavior has been discussed. The result shows that the deformation temperature and strain rate exerted remarkable influences on the flow stress. The constitutive equation of large-scaled AZ80 magnesium alloy for hot deformation at steady-state stage (ɛ = 0.5) was The true stress-true strain curves predicted by the extracted model were in good agreement with the experimental results, thereby confirming the validity of the developed constitutive relation. The DRX kinetic model of large-scaled AZ80 magnesium alloy was established as X d = 1 - exp[-0.95((ɛ - ɛc)/ɛ*)2.4904]. The rate of DRX increases with increasing deformation temperature, and high temperature is beneficial for achieving complete DRX in the large-scaled AZ80 magnesium alloy.

Biosignatures in the Recrystallized Shock Melt Pocket of ALH-77005 Shergottite — Clues to Martian Life

NASA Astrophysics Data System (ADS)

Gyollai, I.; Polgári, M.; Bérczi, Sz.; Gucsik, A.; Pál-Molnár, E.

2017-11-01

In the spinifex textured, recrystallized shock melt portion in ALH 77005 shergottite mineralized microbially produced texture (MMPT) - in form of pearl necklace-like, vermiform inner signatures - was measured, which we propose to have Martian origin.

Effects of two-step homogenization on precipitation behavior of Al{sub 3}Zr dispersoids and recrystallization resistance in 7150 aluminum alloy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Guo, Zhanying; Key Laboratory for Anisotropy and Texture of Materials, Northeastern University, Shenyang 110819, China,; Zhao, Gang

2015-04-15

The effect of two-step homogenization treatments on the precipitation behavior of Al{sub 3}Zr dispersoids was investigated by transmission electron microscopy (TEM) in 7150 alloys. Two-step treatments with the first step in the temperature range of 300–400 °C followed by the second step at 470 °C were applied during homogenization. Compared with the conventional one-step homogenization, both a finer particle size and a higher number density of Al{sub 3}Zr dispersoids were obtained with two-step homogenization treatments. The most effective dispersoid distribution was attained using the first step held at 300 °C. In addition, the two-step homogenization minimized the precipitate free zonesmore » and greatly increased the number density of dispersoids near dendrite grain boundaries. The effect of two-step homogenization on recrystallization resistance of 7150 alloys with different Zr contents was quantitatively analyzed using the electron backscattered diffraction (EBSD) technique. It was found that the improved dispersoid distribution through the two-step treatment can effectively inhibit the recrystallization process during the post-deformation annealing for 7150 alloys containing 0.04–0.09 wt.% Zr, resulting in a remarkable reduction of the volume fraction and grain size of recrystallization grains. - Highlights: • Effect of two-step homogenization on Al{sub 3}Zr dispersoids was investigated by TEM. • Finer and higher number of dispersoids obtained with two-step homogenization • Minimized the precipitate free zones and improved the dispersoid distribution • Recrystallization resistance with varying Zr content was quantified by EBSD. • Effectively inhibit the recrystallization through two-step treatments in 7150 alloy.« less

Dissolution enhancement of gliclazide using pH change approach in presence of twelve stabilizers with various physico-chemical properties.

PubMed

Talari, Roya; Varshosaz, Jaleh; Mostafavi, Seyed Abolfazl; Nokhodchi, Ali

2009-01-01

The micronization using milling process to enhance dissolution rate is extremely inefficient due to a high energy input, and disruptions in the crystal lattice which can cause physical or chemical instability. Therefore, the aim of the present study is to use in situ micronization process through pH change method to produce micron-size gliclazide particles for fast dissolution hence better bioavailability. Gliclazide was recrystallized in presence of 12 different stabilizers and the effects of each stabilizer on micromeritic behaviors, morphology of microcrystals, dissolution rate and solid state of recrystallized drug particles were investigated. The results showed that recrystallized samples showed faster dissolution rate than untreated gliclazide particles and the fastest dissolution rate was observed for the samples recrystallized in presence of PEG 1500. Some of the recrystallized drug samples in presence of stabilizers dissolved 100% within the first 5 min showing at least 10 times greater dissolution rate than the dissolution rate of untreated gliclazide powders. Micromeritic studies showed that in situ micronization technique via pH change method is able to produce smaller particle size with a high surface area. The results also showed that the type of stabilizer had significant impact on morphology of recrystallized drug particles. The untreated gliclazide is rod or rectangular shape, whereas the crystals produced in presence of stabilizers, depending on the type of stabilizer, were very fine particles with irregular, cubic, rectangular, granular and spherical/modular shape. The results showed that crystallization of gliclazide in presence of stabilizers reduced the crystallinity of the samples as confirmed by XRPD and DSC results. In situ micronization of gliclazide through pH change method can successfully be used to produce micron-sized drug particles to enhance dissolution rate.

Predicting the Kinetics of Ice Recrystallization in Aqueous Sugar Solutions

PubMed Central

2018-01-01

The quality of stored frozen products such as foods and biomaterials generally degrades in time due to the growth of large ice crystals by recrystallization. While there is ample experimental evidence that recrystallization within such products (or model systems thereof) is often dominated by diffusion-limited Ostwald ripening, the application of Ostwald-ripening theories to predict measured recrystallization rates has only met with limited success. For a model system of polycrystalline ice within an aqueous solution of sugars, we here show recrystallization rates can be predicted on the basis of Ostwald ripening theory, provided (1) the theory accounts for the fact the solution can be nonideal, nondilute and of different density than the crystals, (2) the effect of ice-phase volume fraction on the diffusional flux of water between crystals is accurately described, and (3) all relevant material properties (involving binary Fick diffusion coefficients, the thermodynamic factor of the solution, and the surface energy of ice) are carefully estimated. To enable calculation of material properties, we derive an alternative formulation of Ostwald ripening in terms of the Maxwell–Stefan instead of the Fick approach to diffusion. First, this leads to a cancellation of the thermodynamic factor (a measure for the nonideality of a solution), which is a notoriously difficult property to obtain. Second, we show that Maxwell–Stefan diffusion coefficients can to a reasonable approximation be related to self-diffusion coefficients, which are relatively easy to measure or predict in comparison to Fick diffusion coefficients. Our approach is validated for a binary system of water and sucrose, for which we show predicted recrystallization rates of ice compare well to experimental results, with relative deviations of at most a factor of 2. PMID:29651228

Predicting the Kinetics of Ice Recrystallization in Aqueous Sugar Solutions.

PubMed

van Westen, Thijs; Groot, Robert D

2018-04-04

The quality of stored frozen products such as foods and biomaterials generally degrades in time due to the growth of large ice crystals by recrystallization. While there is ample experimental evidence that recrystallization within such products (or model systems thereof) is often dominated by diffusion-limited Ostwald ripening, the application of Ostwald-ripening theories to predict measured recrystallization rates has only met with limited success. For a model system of polycrystalline ice within an aqueous solution of sugars, we here show recrystallization rates can be predicted on the basis of Ostwald ripening theory, provided (1) the theory accounts for the fact the solution can be nonideal, nondilute and of different density than the crystals, (2) the effect of ice-phase volume fraction on the diffusional flux of water between crystals is accurately described, and (3) all relevant material properties (involving binary Fick diffusion coefficients, the thermodynamic factor of the solution, and the surface energy of ice) are carefully estimated. To enable calculation of material properties, we derive an alternative formulation of Ostwald ripening in terms of the Maxwell-Stefan instead of the Fick approach to diffusion. First, this leads to a cancellation of the thermodynamic factor (a measure for the nonideality of a solution), which is a notoriously difficult property to obtain. Second, we show that Maxwell-Stefan diffusion coefficients can to a reasonable approximation be related to self-diffusion coefficients, which are relatively easy to measure or predict in comparison to Fick diffusion coefficients. Our approach is validated for a binary system of water and sucrose, for which we show predicted recrystallization rates of ice compare well to experimental results, with relative deviations of at most a factor of 2.

Glass fiber processing for the Moon/Mars program: Center director's discretionary fund final report

NASA Technical Reports Server (NTRS)

Tucker, D. S.; Ethridge, E.; Curreri, P.

1992-01-01

Glass fiber has been produced from two lunar soil simulants. These two materials simulate lunar mare soil and lunar highland soil compositions, respectively. Short fibers containing recrystallized areas were produced from the as-received simulants. Doping the highland simulant with 8 weight percent B2-O3 yielded a material which could be spun continuously. The effects of lunar gravity on glass fiber formation were studied utilizing NASA's KC-135 aircraft. Gravity was found to play a major role in final fiber diameter.

Monitoring processing properties of high performance thermoplastics using frequency dependent electromagnetic sensing

NASA Technical Reports Server (NTRS)

Kranbuehl, D. E.; Delos, S. E.; Hoff, M. S.; Weller, L. W.; Haverty, P. D.

1987-01-01

An in situ NDE dielectric impedance measurement method has been developed for ascertaining the cure processing properties of high temperature advanced thermoplastic and thermosetting resins, using continuous frequency-dependent measurements and analyses of complex permittivity over 9 orders of magnitude and 6 decades of frequency at temperatures up to 400 C. Both ionic and Debye-like dipolar relaxation processes are monitored. Attention is given to LARC-TPI, PEEK, and poly(arylene ether) resins' viscosity, glass transition temperature, recrystallization, and residual solvent content and evolution properties.

Characterization of the Micro Textures in a Friction Stir Weld

NASA Technical Reports Server (NTRS)

Schneider, Judy; Nunes, Arthur C.

2004-01-01

In friction stir welding (FSW), a rotating threaded pin tool is inserted into a weld seam and literally stirs the edges of the seam together. The Dynamically-Recrystallized-Zone (DXZ) of a polished and etched FSW cross-section exhibits contrasting bands (the "onion-ring" structure), the origins of which are unclear. An orientation image mapping (OIM) study suggests that the corresponding bands may correspond respectively to a "straight-through" current of metal bypassing the pin tool in a single rotation or less and a "maelstrom" current rotating a number of times around the pin tool.

Metadynamic and static recrystallization softening behavior of a bainite steel

NASA Astrophysics Data System (ADS)

Li, Lixin; Zheng, Liangyu; Ye, Ben; Tong, Zeqiong

2018-01-01

The metadynamic recrystallization (MDRX) and static recrystallization (SRX) softening behavior of a bainite steel was investigated by two-pass isothermal compression experiments at temperatures of 1173, 1273, 1373, and 1473 K and strain rates of 0.01, 0.1, 1, and 10 s-1 with inter-pass times of 1, 5, 10, and 30 s on a Gleeble-1500 thermo-mechanical simulator. Kinetic equations were developed to evaluate the softening fractions caused by MDRX and SRX. A comparison between the experimental and predicted softening fractions showed that the proposed kinetic equations can provide a precise estimation of the MDRX and SRX behavior of the studied steel. The results based on the kinetic equations indicated that the MDRX and SRX softening fraction increases with the increase in strain rate, deformation temperature, inter-pass time, and pre-strain; the activation energy of MDRX is much smaller than that of SRX; and the no-recrystallization temperature of the investigated steel is 1179.4 K.

Fabric and texture at Siple Dome, Antarctica

USGS Publications Warehouse

Diprinzio, C.L.; Wilen, Lawrence A.; Alley, R.B.; Fitzpatrick, J.J.; Spencer, M.K.; Gow, A.J.

2005-01-01

Preferred c-axis orientations are present in the firn at Siple Dome, West Antarctica, and recrystallization begins as shallow as 200 m depth in ice below -20??C, based on digital analysis of c-axis fabrics, grain-sizes and other characteristics of 52 vertical thin sections prepared in the field from the kilometer-long Siple Dome ice core. The shallowest section analyzed, from 22 m, shows clustering of c axes toward the vertical. By 200 m depth, girdle fabric and other features of recrystallized ice are evident in layers (or regions), separated by layers (regions) of typically finer-grained ice lacking evidence of recrystallization. Ice from about 700-780 m depth, which was deposited during the last ice age, is especially fine-grained, with strongly vertical c axes, but deeper ice shows much larger crystals and strong evidence of recrystallization. Azimuthal asymmetry of some c-axis fabrics, trends in grain-size, and other indicators reveal additional information on processes and history of ice flow at Siple Dome.

Effect of Thermomechanical Processing on Texture and Superelasticity in Fe-Ni-Co-Al-Ti-B Alloy

NASA Astrophysics Data System (ADS)

Lee, Doyup; Omori, Toshihiro; Han, Kwangsik; Hayakawa, Yasuyuki; Kainuma, Ryosuke

2018-03-01

The texture and superelasticity were investigated in austenitic Fe-Ni-Co-Al-Ti-B alloy with various reduction ratios of cold rolling and heating ratios in annealing. The rolled sheets show the {110} <112> deformation texture at a reduction ratio higher than 80%, while the texture hardly changes in the primary recrystallization at 1000 °C. The β (B2) precipitates inhibit the grain growth at this temperature, but they dissolve during heating, and secondary recrystallization occurs due to decreased pinning force at temperatures higher than 1100 °C, resulting in texture change to {210} <001> . The recrystallization texture is more strongly developed when the reduction ratio and heating rate are high and slow, respectively. The 90% cold-rolled and slowly heated sheet shows the recrystallization texture and high fraction of low-angle boundaries. As a result, ductility and superelasticity can be drastically improved in the 90% cold-rolled sheet, although superelasticity was previously obtained only in thin sheets with 98.5% reduction.

A study of the oxide dispersion and recrystallization in NiCrAl prepared from preoxidized powder

NASA Technical Reports Server (NTRS)

Glasgow, T. K.

1975-01-01

The sintered aluminum powder (SAP) technique of dispersion strengthening (formation of an oxide dispersion by preoxidation of metal powders) was applied to atomized powder of a nickel alloy containing, by weight, 17% Cr, 5% Al, and 0.2% Y. The SAP-NiCrAl alloy (without the ytterbium removed by oxdation) was worked by extrusion and rod rolling at 1205 C and by swaging at 760 C. Annealing treatments were applied after working to determine the recrystallization response. The NiCrAlY alloy, similarly prepared from atomized powder, but without a preoxidation treatment, was examined for comparison. The SAP-NiCrAl alloy exhibited oxide particle size and spacing much larger than that usually observed in oxide dispersion strengthened alloys; nonetheless, it was possible to achieve abnormal (secondary) recrystallization in the SAP-NiCrAl alloy as has been reported for other oxide dispersion strengthened alloys. In contrast, the unoxidized NiCrAlY alloy exhibited only primary recrystallization.

Effects of Laves phase particles on recovery and recrystallization behaviors of Nb-containing FeCrAl alloys

DOE PAGES

Sun, Zhiqian; Edmondson, Philip D.; Yamamoto, Yukinori

2017-11-15

The microstructures and mechanical properties of deformed and annealed Nb-containing FeCrAl alloys were investigated. Fine dispersion of Fe 2Nb-type Laves phase particles was observed in the bcc-Fe matrix after applying a thermomechanical treatment, especially along grain/subgrain boundaries, which effectively stabilized the recovered and recrystallized microstructures compared with the Nb-free FeCrAl alloy. The stability of recovered areas increased with Nb content up to 1 wt%. The recrystallized grain structure in Nb-containing FeCrAl alloys consisted of elongated grains along the rolling direction with a weak texture when annealed below 1100 °C. An abnormal relationship between recrystallized grain size and annealing temperature wasmore » found. Microstructural inhomogeneity in the deformed and annealed states was explained based on the Taylor factor. Annealed Nb-containing FeCrAl alloys showed a good combination of strength and ductility, which is desirable for their application as fuel cladding in light-water reactors.« less

Experiments and modeling to characterize microstructure and hardness in 304L

DOE PAGES

Deibler, Lisa Anne; Brown, Arthur; Puskar, Joseph D.

2017-01-12

Drawn 304L stainless steel tubing was subjected to 42 different annealing heat treatments with the goal of initializing a microstructural model to select a heat treatment to soften the tubing from a hardness of 305 Knoop to 225–275 Knoop. The amount of recrystallization and grain size caused by 18 heat treatments were analyzed via optical microscopy and image analysis, revealing the full range of recrystallization from 0 to 100%. The formation of carbides during the longer duration and higher-temperature heat treatments was monitored via transmission electron microscope evaluation. The experimental results informed a model which includes recovery, recrystallization, and grainmore » growth to predict microstructure and hardness. After initialization of the model, it was able to predict hardness with a R 2 value of 0.95 and recrystallization with an R 2 value of 0.99. As a result, the model was then utilized in the design and testing of a heat treatment to soften the tubing.« less

A method for the monitoring of metal recrystallization based on the in-situ measurement of the elastic energy release using neutron diffraction

DOE Office of Scientific and Technical Information (OSTI.GOV)

Christien, F., E-mail: frederic.christien@univ-nantes.fr; Le Gall, R.; Telling, M. T. F.

2015-05-15

A method is proposed for the monitoring of metal recrystallization using neutron diffraction that is based on the measurement of stored energy. Experiments were performed using deformed metal specimens heated in-situ while mounted at the sample position of the High Resolution Powder Diffractometer, HRPD (ISIS Facility), UK. Monitoring the breadth of the resulting Bragg lines during heating not only allows the time-dependence (or temperature-dependence) of the stored energy to be determined but also the recrystallized fraction. The analysis method presented here was developed using pure nickel (Ni270) specimens with different deformation levels from 0.29 to 0.94. In situ temperature rampingmore » as well as isothermal annealing was undertaken. The method developed in this work allows accurate and quantitative monitoring of the recrystallization process. The results from neutron diffraction are satisfactorily compared to data obtained from calorimetry and hardness measurements.« less

Shock-induced fine-grained recrystallization of olivine - Evidence against subsolidus reduction of Fe/2+/

NASA Technical Reports Server (NTRS)

Ahrens, T. J.; Tsay, F.-D.; Live, D. H.

1976-01-01

Electron spin resonance (ESR) studies have been carried out on three single grains of terrestrial olivine (Fo90) shock loaded along the 010 line to peak pressures of 280, 330, and 440 kbar. The results indicate that neither metallic Fe similar to that observed in returned lunar soils nor paramagnetic Fe(3+) caused by oxidation of Fe(2+) has been produced in these shock experiments. Trace amounts of Mn (2+) have been detected in both shocked and unshocked olivine. The ESR signals of Mn(2+) show spectral features which are found to correlate with the degree of shock-induced recrystallization observed petrographically. The increasing mass fraction of recrystallized olivine correlates with increasing shock pressures. This phenomenon is modelled assuming it results from the progressive effect of the shock-induced transformation of the olivine to a yet unknown high-pressure phase and its subsequent reversion to the low-pressure olivine phase. The mass fraction of recrystallized material is predicted to be nearly linear with shock pressure.

Control of fault shearing on the fabric of a syn-tectonic granite : magnetic fabric and crystallographic preferred orientation (CPO) of quartz input

NASA Astrophysics Data System (ADS)

Walter, Bastien; Géraud, Yves; Diraison, Marc; Oliot, Emilien

2013-04-01

The late-Miocene monzogranitic pluton of Porto Azzurro (PA) on Elba Island (Italy), was emplaced in the footwall of the N-S striking Zuccale Fault (ZF), a Low-Angle Normal Fault (LANF). In the Barbarossa outcrop, this poorly exposed pluton shows few NNE-SSW and WNW-ESE striking shear bands, respectively moderately dipping eastward and steeply dipping northward, which appear to be associated to the brittle fracturation, and no clear relationship between all these structures and the ZF is described. In order to get information about possible relationship between these shear bands, brittle structures and prior fabric of this igneous stock, and about the timing of formation of these ductile deformations relative to the pluton emplacement, rock fabrics were studied on samples taken both inside and outside of one of these shear bands. The magnetic fabric was analyzed with anisotropy of magnetic susceptibility measurements (AMS), and the crystallographic preferred orientations of dynamically recrystallized quartz were measured with the electron back-scattered diffraction (EBSD) method. Quartz CPOs are directly compared, after EBSD data processing, with the macroscopic ductile structures orientation, according to the geographical North. The pooling of data of these two methods reveals two distinct petrofabrics within the Barbarossa monzogranite. The first fabric, with a low dip angle, is identified only on samples taken outside of the influence of the shear bands. Orientation of paramagnetic minerals, with biotite as the main magnetic mineral carrier, and quartz CPOs are consistent, pervasive within the whole outcrop and are linked to the eastward extension produced by the LANF Zuccale Fault. This fabric suggests that the dynamic of the magmatic supplies during emplacement of the pluton of PA was controlled by the LANF's extension, and confirms this magmatic intrusion to be likely syn-tectonic. The second fabric is identified close or within the studied shear bands with a similar orientation to them. Our data show that these ductile structures impose a local new tectonic fabric overprinting the pre-existing one. The common re-orientation of the magnetic minerals, of the recrystallized quartz and of the brittle structures suggest a strain localization and a continuous strain process localized along stain bands from late-magmatic flowing, highlighted by biotite orientation, then during shear bands activation, at temperature around 350-400° C. Finally, these structures would have remained active through the ductile-brittle transition, leading to the localized intense fracturation of the Barbarossa outcrop.

Intragranular Recrystallization and Lattice Reorientation of Calcite Grains in Experimentally Deformed Crinoids and Trilobites

NASA Astrophysics Data System (ADS)

Kim, N.; Takahashi, M.; Shigematsu, N.; Ree, J. H.; Jung, H.

2017-12-01

Intragranular recrystallization, including subgrain-rotation-recrystallization (SGR) and nucleation (and growth) of new grains along boundaries of deformation twins and bands, is an important process leading to grain-size reduction and causing rheological change depending on deformation condition. Despite of its importance, the detailed processes of intragranular recrystallization are still somewhat unclear. We deformed a limestone using triaxial testing machine at AIST of Japan at temperature of 500 700 °, strain rate of 10-4 10-5 s-1, confining pressure of 200 MPa and strain of up to 30%, to explore intragranular recrystallization processes of calcite. The limestone contains two abundant fossils, crinoid and trilobite. The crinoids are mono- or poly-crystalline. We focus on the monocrystalline crinoids with a coarser grain size ( 700 μm). The trilobites are polycrystalline and much finer-grained ( 7 μm) with initially a strong c-axis preferred orientation. At a lower temperature condition, subgrains develop both in twin and host domains of crinoids and evolve into new grains by SGR. At a higher temperature, recrystallized grains have irregular grain boundaries and bimodal grain-size distribution, implying grain-boundary migration (GBM) recrystallization. At a lower temperature, new grains nucleating and growing along twin boundaries inherit lattice orientation of twin domain, and with the nucleation site and usually a smaller grain size, they can be distinguished from new grains by SGR. At a higher temperature, however, the distinction is difficult at present due to extensive GBM. For the trilobites, there is only local GBM with no significant change in grain size, and flattening of grains reflects the bulk strain at a lower temperature. At a higher temperature, individual grains of the trilobites are equi-axed with weakened LPO, although the strain of trilobites is higher than bulk strain. These microfabrics suggest that the dominant deformation mechanism of the trilobites is diffusion creep. Although the initial LPO of the trilobites is weakened, the LPO is still preserved up to strain of 30%. This implies that even if the grain size of trilobites and matrix is similar in naturally deformed limestones, the lattice orientation map may be useful in recognizing trilobite fossils.

Recrystallization and Grain Growth Kinetics in Binary Alpha Titanium-Aluminum Alloys

NASA Astrophysics Data System (ADS)

Trump, Anna Marie

Titanium alloys are used in a variety of important naval and aerospace applications and often undergo thermomechanical processing which leads to recrystallization and grain growth. Both of these processes have a significant impact on the mechanical properties of the material. Therefore, understanding the kinetics of these processes is crucial to being able to predict the final properties. Three alloys are studied with varying concentrations of aluminum which allows for the direct quantification of the effect of aluminum content on the kinetics of recrystallization and grain growth. Aluminum is the most common alpha stabilizing alloying element used in titanium alloys, however the effect of aluminum on these processes has not been previously studied. This work is also part of a larger Integrated Computational Materials Engineering (ICME) effort whose goal is to combine both computational and experimental efforts to develop computationally efficient models that predict materials microstructure and properties based on processing history. The static recrystallization kinetics are measured using an electron backscatter diffraction (EBSD) technique and a significant retardation in the kinetics is observed with increasing aluminum concentration. An analytical model is then used to capture these results and is able to successfully predict the effect of solute concentration on the time to 50% recrystallization. The model reveals that this solute effect is due to a combination of a decrease in grain boundary mobility and a decrease in driving force with increasing aluminum concentration. The effect of microstructural inhomogeneities is also experimentally quantified and the results are validated with a phase field model for recrystallization. These microstructural inhomogeneities explain the experimentally measured Avrami exponent, which is lower than the theoretical value calculated by the JMAK model. Similar to the effect seen in recrystallization, the addition of aluminum also significantly slows downs the grain growth kinetics. This is generally attributed to the solute drag effect due to segregation of solute atoms at the grain boundaries, however aluminum segregation is not observed in these alloys. The mechanism for this result is explained and is used to validate the prediction of an existing model for solute drag.

Evolution of quartz microstructure and c-axis crystallographic preferred orientation within ductilely deformed granitoids (Arolla unit, Western Alps)

NASA Astrophysics Data System (ADS)

Menegon, Luca; Pennacchioni, Giorgio; Heilbronner, Renee; Pittarello, Lidia

2008-11-01

We have studied quartz microstructures and the c-axis crystallographic preferred orientations (CPOs) in four granitoid samples representative of increasing ductile shear deformation, from a weakly deformed granitoid (stage 1) to a mylonitic granitoid (stage 4). The quartz c-axis CPO measured in the mylonitic granitoid has been compared with the one observed in a fully recrystallized quartz mylonite from the same area. All the samples belong to the Austroalpine Arolla unit (Western Alps) and were deformed at greenschist facies conditions. The quartz c-axis CPO was analyzed using a U-stage and the optical orientation imaging technique. The magmatic plagioclase, forming more than 50% of the volume of the granitoid, is extensively replaced by a mica-rich aggregate even in weakly deformed samples of stage 1. These aggregates flow to form an interconnected weak matrix with increasing deformation, wrapping relatively less strained quartz grains that undergo dominantly coaxial strain. Recrystallization of quartz ranges from less than 1% in the weakly deformed granitoid to up to 85% in the mylonitic granitoid, with average grain strain of 41% and 64%, respectively. With increasing strain and recrystallization, quartz grains in the granitoids show a sequence of transient microstructures and CPOs. Crystal plastic deformation is initially accomplished by dislocation glide with limited recovery, and at 50% grain strain it results in a CPO consistent with dominantly basal < a> slip. At 60% grain strain, recrystallization is preferentially localized along shear bands, which appear to develop along former intragranular cracks, and the recrystallized grains develop a strong c-axis CPO with maxima orthogonal to the shear band boundaries and independent of the host grain orientation. Within the granitoid mylonite, at an average quartz grain strain of 64%, recrystallization is extensive and the c-axis CPO of new grains displays maxima overlapping the host c-axis orientation and, therefore, unrelated to the bulk sense of shear. The host-controlled CPO is inferred to reflect pervasive recrystallization by progressive subgrain rotation. The switch from 'shear band-control' to 'host-control' on c-axis CPO occurred between 40% and 70% of recrystallization. In the quartz mylonite, the quartz c-axis CPO develops an asymmetric single girdle consistent with the bulk sense of shear and the synkinematic greenschist facies conditions. This study indicates that the CPO evolution of quartz may significantly differ in cases of polymineralic vs. monomineralic rocks under the same deformation conditions, if quartz in the polymineralic rock behaves as a 'strong' phase.

Ca. 400 Ma Recrystallization of Norwegian Ultrahigh-pressure Eclogites: an ion Microprobe and Chemical Abrasion Study

NASA Astrophysics Data System (ADS)

Root, D. B.; Mattinson, J. M.; Hacker, B. R.; Wooden, J. L.

2002-12-01

Understanding the formation and exhumation of the ultrahigh-pressure (UHP) rocks of western Norway hinges on precise determination of the time of eclogite recrystallization. Our study consists of SHRIMP analysis, in conjunction with CL imagery, of zircon from four UHP and high-pressure (HP) eclogites; and detailed TIMS analysis of zircon from two samples subjected to combined thermal annealing and multi-step chemical abrasion (CA). SHRIMP analyses of the Otnheim and Langenes eclogites yield Caledonian spot ages of ca. 400 Ma from zircon rims. CL imagery and Th/U ratios from the Langenes eclogite indicate formation of rims by recrystallization of inherited zircon. SHRIMP analysis of the UHP Flatraket eclogite yielded a broad range of apparently concordant Caledonian ages. CA analyses of two fractions yielded moderate Pb loss from the first (lowest T) steps; possible minor Pb loss or minor growth at 400 Ma from the second steps; and a 407-404 Ma cluster of slightly discordant 206Pb/238U ages, most likely free from Pb loss, from the remaining steps. We interpret the latter to reflect recrystallization of inherited zircon, with possible new growth, at ca. 400-395 Ma. Alternatively, the high-temperature CA steps could represent growth at 407-404 Ma, with apparent discordance due to intermediate daughter product effects. HP/UHP zircon recrystallization in the Flatraket eclogite is inferred from three lines of evidence: i) zircon occurs as inclusions in garnet, omphacite, breunnerite, dolomite, and quartz, as well as in symplectites after phengite and omphacite; ii) association of zircon with rutile implies zircon formation during HP breakdown of Zr-ilmenite; and iii) chondrite-normalized ICP-MS analyses of the CA steps reveal small Eu anomalies and shallow HREE profiles, indicating zircon recrystallization in the presence of garnet. CA analysis of the Verpeneset eclogite yielded distinctly discordant step ages from two steps comprising <90% of the sample, with 206Pb/238U ages of 408 and 414 Ma. CL imagery indicates incomplete recrystallization of inherited igneous zircon, in keeping with steep HREE profiles determined from chondrite-normalized ICP-MS analyses. Our zircon age of ca. 400-395 Ma for the Flatraket eclogite is significantly younger than the 425 Ma age often cited for western Norway eclogite recrystallization, implying, in conjunction with 390-385 Ma 40Ar/39Ar white mica cooling ages, faster rates of exhumation (ca. 15 km/m.y.), and weakening the link between UHP metamorphism and ophiolite emplacement at 430-425 Ma.

Factors controlling in vitro recrystallization of the Caulobacter crescentus paracrystalline S-layer.

PubMed Central

Nomellini, J F; Kupcu, S; Sleytr, U B; Smit, J

1997-01-01

The S-layer of Caulobacter is a two-dimensional paracrystalline array on the cell surface composed of a single protein, RsaA. We have established conditions for preparation of stable, soluble protein and then efficient in vitro recrystallization of the purified protein. Efficient recrystallization and long range order could not be obtained with pure protein only, though it was apparent that calcium was required for crystallization. Recrystallization was obtained when lipid vesicles were provided, but only when the vesicles contained the specific species of Caulobacter smooth lipopolysaccharide (SLPS) that previous studies implicated as a requirement for attaching the S-layer to the cell surface. The specific type of phospholipids did not appear critical; phospholipids rather different from those present in Caulobacter membranes or archaebacterial tetraether lipids worked equally well. The source of LPS was critical; rough and smooth variants of Salmonella typhimurium LPS as well as the rough form of Caulobacter LPS were ineffective. The requirement for calcium ions for recrystallization was further evaluated; strontium ions could substitute for calcium, and to a lesser extent, cobalt, barium, manganese and magnesium ions also stimulated crystallization. On the other hand, nickel and cadmium provided only weak crystallization stimulation, and zinc, copper, iron, aluminum ions, and the monovalent potassium, sodium, and lithium ions were ineffective. The recrystallization could also be reproduced with Langmuir-Blodgett lipid monolayers at an air-water interface. As with the vesicle experiments, this was only successful when SLPS was incorporated into the lipid mix. The best method for RsaA preparation, leading to apparently monomeric protein that was stable for many months, was an extraction with a low pH aqueous solution. We also achieved recrystallization, albeit at lower efficiency, using RsaA protein solubilized by 8 M urea, a method which allows retrieval of protein from inclusions, when expressed as heterologous protein in Escherichia coli or when retrieved as shed, precipitated protein from certain mutant caulobacters. In summary, the clarification of recrystallization methods has confirmed the requirement of SLPS as a surface attachment component and suggests that its presence in a membrane-like structure greatly stimulates the extent and quality of S-layer formation. The in vitro approach allowed the demonstration that specific ions are capable of participating in crystallization and now provides an assay for the crystallization potential of modified S-layer proteins, whether they were produced in or can be secreted by caulobacters. PMID:9335282

Calcium phosphates recovery from digester supernatant by fast precipitation and recrystallization

NASA Astrophysics Data System (ADS)

Vasenko, Liubov; Qu, Haiyan

2018-01-01

Conditional solubility of dicalcium phosphate dihydrate (DCPD) and hydroxyapatite (HAp) in digester supernatant was determined as a function of pH and was compared to its conditional solubility in distilled water. Conditional solubility of both substances in digester supernatant at pH >5-6 was higher than their conditional solubility in pure water due to the presence of impurities, and this influence is more significant for HAp. Amorphous CaP was precipitated through a fast precipitation process from digester supernatant with initial total phosphate concentration 0.008 mol/L and 0.015 mol/L and Ca/P ratios 2 and 5. The amorphous CaP can be subsequently recrystallized into crystalline CaP. Obtained amorphous products have Ca/P ratio > 1, which allow performing the recrystallization process without further Ca dosing into the system. Batch recrystallization of the amorphous products resulted in crystallization of HAp, DCPD or their mixture depending on the conditions of the process. Maximum achieved P-recovery was 69.5%. The increase of phosphate concentration and the addition of seeding decreased the yield of the process but promoted crystallization of DCPD. The increase of Ca/P ratio had a positive effect on the total P-recovery. Compared with the direct batch crystallization of CaP from digester supernatant, the two-step process with fast precipitation and recrystallization significantly improved the color of the obtained products.

Solid-state characterization of nevirapine.

PubMed

Sarkar, Mahua; Perumal, O P; Panchagnula, R

2008-09-01

The purpose of this investigation is to characterize nevirapine from commercial samples and samples crystallized from different solvents under various conditions. The solid-state behavior of nevirapine samples was investigated using a variety of complementary techniques such as microscopy (optical, polarized, hot stage microscopy), differential scanning calorimeter, thermogravimetric analysis, Fourier transform infrared spectroscopy and powder X-ray diffractometry. The commercial samples of nevirapine had the same polymorphic crystalline form with an anhedral crystal habit. Intrinsic dissolution of nevirapine was similar for both the commercial batches. Powder dissolution showed pH dependency, with maximum dissolution in acidic pH and there was no significant effect of particle size. The samples recrystallized from different solvent systems with varying polarity yielded different crystal habits. Stirring and degrees of supersaturation influenced the size and shape of the crystals. The recrystallized samples did not produce any new polymorphic form, but weak solvates with varying crystal habit were produced. Recrystallized samples showed differences in the x-ray diffractograms. However, all the samples had the same internal crystal lattice as revealed from their similar melting points and heat of fusion. The intrinsic dissolution rate of recrystallized samples was lower than the commercial sample. It was found that the compression pressure resulted in desolvation and partial conversion of the crystal form. After compression, the recrystallized samples showed similar x-ray diffractograms to the commercial sample. Amorphous form showed slightly higher aqueous solubility than the commercial crystalline form.

Ice Recrystallization in a Solution of a Cryoprotector and Its Inhibition by a Protein: Synchrotron X-Ray Diffraction Study.

PubMed

Zakharov, Boris; Fisyuk, Alexander; Fitch, Andy; Watier, Yves; Kostyuchenko, Anastasia; Varshney, Dushyant; Sztucki, Michael; Boldyreva, Elena; Shalaev, Evgenyi

2016-07-01

Ice formation and recrystallization is a key phenomenon in freezing and freeze-drying of pharmaceuticals and biopharmaceuticals. In this investigation, high-resolution synchrotron X-ray diffraction is used to quantify the extent of disorder of ice crystals in binary aqueous solutions of a cryoprotectant (sorbitol) and a protein, bovine serum albumin. Ice crystals in more dilute (10 wt%) solutions have lower level of microstrain and larger crystal domain size than these in more concentrated (40 wt%) solutions. Warming the sorbitol-water mixtures from 100 to 228 K resulted in partial ice melting, with simultaneous reduction in the microstrain and increase in crystallite size, that is, recrystallization. In contrast to sorbitol solutions, ice crystals in the BSA solutions preserved both the microstrain and smaller crystallite size on partial melting, demonstrating that BSA inhibits ice recrystallization. The results are consistent with BSA partitioning into quasi-liquid layer on ice crystals but not with a direct protein-ice interaction and protein sorption on ice surface. The study shows for the first time that a common (i.e., not-antifreeze) protein can have a major impact on ice recrystallization and also presents synchrotron X-ray diffraction as a unique tool for quantification of crystallinity and disorder in frozen aqueous systems. Copyright © 2016 American Pharmacists Association®. Published by Elsevier Inc. All rights reserved.

A Behavioral Analysis of the Laboratory Learning Process: Redesigning a Teaching Unit on Recrystallization.

ERIC Educational Resources Information Center

Mulder, T.; Verdonk, A. H.

1984-01-01

Reports on a project in which observations of student and teaching assistant behavior were used to redesign a teaching unit on recrystallization. Comments on the instruction manual, starting points for teaching the unit, and list of objectives with related tasks are included. (JN)

The Effect of Welding Energy on the Microstructural and Mechanical Properties of Ultrasonic-Welded Copper Joints

PubMed Central

Yang, Jingwei; Cao, Biao; Lu, Qinghua

2017-01-01

The effects of welding energy on the mechanical and microstructural characteristics of ultrasonic-welded pure copper plates were investigated. Complex dynamic recrystallization and grain growth occurred inside the weld zone during ultrasonic welding. At a low welding energy, a thin band of straight weld interfaces was observed and had an ultra-fine grain structure. With an increase in welding energy, the weld interface progressively changed from flat to sinusoidal, and eventually turned into a convoluted wavy pattern, bearing similarities to shear instabilities, as observed in fluid dynamics. The lap shear load of the joints initially increased and then remained stable as the welding energy increased. The tensile characteristics of the joints significantly depended on the development of plastic deformation at the interface. The influence of the microstructure on the hardness was also discussed. PMID:28772553

Dynamic creation and evolution of gradient nanostructure in single-crystal metallic microcubes

NASA Astrophysics Data System (ADS)

Thevamaran, Ramathasan; Lawal, Olawale; Yazdi, Sadegh; Jeon, Seog-Jin; Lee, Jae-Hwang; Thomas, Edwin L.

2016-10-01

We demonstrate the dynamic creation and subsequent static evolution of extreme gradient nanograined structures in initially near-defect-free single-crystal silver microcubes. Extreme nanostructural transformations are imposed by high strain rates, strain gradients, and recrystallization in high-velocity impacts of the microcubes against an impenetrable substrate. We synthesized the silver microcubes in a bottom-up seed-growth process and use an advanced laser-induced projectile impact testing apparatus to selectively launch them at supersonic velocities (~400 meters per second). Our study provides new insights into the fundamental deformation mechanisms and the effects of crystal and sample-shape symmetries resulting from high-velocity impacts. The nanostructural transformations produced in our experiments show promising pathways to developing gradient nanograined metals for engineering applications requiring both high strength and high toughness—for example, in structural components of aircraft and spacecraft.

The Effect of Welding Energy on the Microstructural and Mechanical Properties of Ultrasonic-Welded Copper Joints.

PubMed

Yang, Jingwei; Cao, Biao; Lu, Qinghua

2017-02-16

The effects of welding energy on the mechanical and microstructural characteristics of ultrasonic-welded pure copper plates were investigated. Complex dynamic recrystallization and grain growth occurred inside the weld zone during ultrasonic welding. At a low welding energy, a thin band of straight weld interfaces was observed and had an ultra-fine grain structure. With an increase in welding energy, the weld interface progressively changed from flat to sinusoidal, and eventually turned into a convoluted wavy pattern, bearing similarities to shear instabilities, as observed in fluid dynamics. The lap shear load of the joints initially increased and then remained stable as the welding energy increased. The tensile characteristics of the joints significantly depended on the development of plastic deformation at the interface. The influence of the microstructure on the hardness was also discussed.

Deformation Behavior and Microstructure Evolution of As-Cast 42CrMo Alloy in Isothermal and Non-isothermal Compression

NASA Astrophysics Data System (ADS)

Qin, Fangcheng; Li, Yongtang; Qi, Huiping; Lv, Zhenhua

2016-11-01

The isothermal and non-isothermal multi-pass compression tests of centrifugal casting 42CrMo steel were conducted on a Gleeble-3500 thermal simulation machine. The effects of compression passes and finishing temperatures on deformation behavior and microstructure evolution were investigated. It is found that the microstructure is homogeneous with equiaxed grains, and the flow stress does not show significant change with the increase in passes, while the peak softening coefficient increases first and then decreases during inter-pass. Moreover, the dominant mechanisms of controlled temperature and accumulated static recrystallization for grain refinement and its homogeneous distribution are found after 5 passes deformation. As the finishing temperature increases, the flow stress decreases gradually, but the dynamic recrystallization accelerates and softening effect increases, resulting in the larger grain size and homogeneous microstructure. The microhardness decreases sharply because the sufficient softening occurs in microstructure. When the finishing temperature is 890 °C, the carbide particles are precipitated in the vicinity of the grain boundaries, thus inhibiting the dislocation motion. Thus, the higher finishing temperature (≥970 °C) for centrifugal casting 42CrMo alloy should be avoided in non-isothermal multi-pass deformation, which is beneficial to grain refinement and properties improvement.

Fluid-rock interactions related to metamorphic reducing fluid flow in meta-sediments: example of the Pic-de-Port-Vieux thrust (Pyrenees, Spain)

NASA Astrophysics Data System (ADS)

Trincal, Vincent; Buatier, Martine; Charpentier, Delphine; Lacroix, Brice; Lanari, Pierre; Labaume, Pierre; Lahfid, Abdeltif; Vennemann, Torsten

2017-09-01

In orogens, shortening is mainly accommodated by thrusts, which constitute preferential zones for fluid-rock interactions. Fluid flow, mass transfer, and mineralogical reactions taking place along thrusts have been intensely investigated, especially in sedimentary basins for petroleum and uranium research. This study combines petrological investigations, mineralogical quantifications, and geochemical characterizations with a wide range of analytical tools with the aim of defining the fluid properties (nature, origin, temperature, and redox) and fluid-host rock interactions (mass transfers, recrystallization mechanisms, and newly formed synkinematic mineralization) in the Pic-de-Port-Vieux thrust fault zone (Pyrenees, Spain). We demonstrate that two geochemically contrasted rocks have been transformed by fluid flow under low-grade metamorphism conditions during thrusting. The hanging-wall Triassic red pelite was locally bleached, while the footwall Cretaceous dolomitic limestone was mylonitized. The results suggest that thrusting was accompanied by a dynamic calcite recrystallization in the dolomitic limestone as well as by leaching of iron via destabilization of iron oxides and phyllosilicate crystallization in the pelite. Geochemical and physical changes highlighted in this study have strong implications on the understanding of the thrust behavior (tectonic and hydraulic), and improve our knowledge of fluid-rock interactions in open fluid systems in the crust.

Dry Sliding Wear Behavior and Subsurface Microstructure Evolution of Mg97Zn1Y2 Alloy in a Wide Sliding Speed Range

NASA Astrophysics Data System (ADS)

An, J.; Xuan, X. H.; Zhao, J.; Sun, W.; Liang, C.

2016-12-01

The wear properties of Mg97Zn1Y2 alloy were investigated using the pin-on-disk wear machine within a load range of 20-380 N and a sliding speed range of 0.2-4.0 m/s. Analysis of worn surfaces using scanning electron microscope and energy-dispersive x-ray spectrometer revealed that wear mechanisms including abrasion + oxidation, delamination accompanied by heavy surface oxidation and delamination operated in mild wear regime, while wear mechanisms such as severe plastic deformation, severe plastic deformation accompanied by spallation of oxidation layer and surface melting prevailed in severe wear regime. The microstructural evolution and hardness change in subsurfaces were examined by optical microscopy and hardness tester. The transformation of surface material from the deformed into dynamic recrystallization (DRX) microstructure was observed before and after mild-to-severe transition. The reason for mild-to-severe wear transition was identified as the transformation of strain hardening to DRX softening in subsurface. Mg97Zn1Y2 alloy has a superior mild-to-severe wear transition resistance to AZ alloys because of its higher recrystallization temperature. A novel model for evaluating the critical surface temperature of mild-to-severe wear transition was established using DRX kinetics.

Hot deformation behavior of microstructural constituents in a duplex stainless steel during high-temperature straining

NASA Astrophysics Data System (ADS)

Momeni, Amir; Kazemi, Shahab; Bahrani, Ali

2013-10-01

The hot deformation characteristics of 1.4462 duplex stainless steel (DSS) were analyzed by considering strain partitioning between austenite and ferrite constituents. The individual behavior of ferrite and austenite in microstructure was studied in an iso-stress condition. Hot compression tests were performed at temperatures of 800-1100°C and strain rates of 0.001-1 s-1. The flow stress was modeled by a hyperbolic sine constitutive equation, the corresponding constants and apparent activation energies were determined for the studied alloys. The constitutive equation and law of mixture were used to measure the contribution factor of each phase at any given strain. It is found that the contribution factor of ferrite exponentially declines as the Zener-Hollomon parameter ( Z) increases. On the contrary, the austenite contribution polynomially increases with the increase of Z. At low Z values below 2.6.×1015 (ln Z=35.5), a negative contribution factor is determined for austenite that is attributed to dynamic recrystallization. At high Z values, the contribution factor of austenite is about two orders of magnitude greater than that of ferrite, and therefore, austenite can accommodate more strain. Microstructural characterization via electron back-scattered diffraction (EBSD) confirms the mechanical results and shows that austenite recrystallization is possible only at high temperature and low strain rate.

EBSD Study on Grain Boundary and Microtexture Evolutions During Friction Stir Processing of A413 Cast Aluminum Alloy

NASA Astrophysics Data System (ADS)

Shamanian, Morteza; Mostaan, Hossein; Safari, Mehdi; Szpunar, Jerzy A.

2016-07-01

The as-cast Al alloys contain heterogeneous distributions of non-deforming particles due to non-equilibrium solidification effects. Therefore, these alloys have poor tribological and mechanical behaviors. It is well known that using friction stir processing (FSP), very fine microstructure is created in the as-cast Al alloys, while their wear resistance can be improved. In this research work, FSP is used to locally refine a surface layer of the coarse as-cast microstructure of cast A413 Al alloy. The main objective of this study is to investigate the effect of FSP on microstructure and microtexture evolutions in A413 cast Al alloy. The grain boundary character distribution, grain structure, and microtexture evolutions in as-cast and friction stir processed A413 Al alloy are analyzed by electron back scatter diffraction technique. It is found that with the FSP, the fraction of low ∑boundary such as ∑3, 7, and 9 are increased. The obtained results show that there are no deformation texture components in the structure of friction stir processed samples. However, some of the main recrystallization texture components such as BR and cubeND are formed during FSP which indicate the occurrence of dynamic recrystallization phenomenon due to the severe plastic deformation induced by the rotation of tool.

Modeling and Finite Element Analysis for the Dynamic Recrystallization Behavior of Ti-5Al-5Mo-5V-3Cr-1Zr Near β Titanium Alloy During Hot Deformation

NASA Astrophysics Data System (ADS)

Lv, Ya-ping; Li, Shao-jun; Zhang, Xiao-yong; Li, Zhi-you; Zhou, Ke-chao

2018-04-01

Evolution for the dynamic recrystallization (DRX) volume fraction of Ti-5Al-5Mo-5V-3Cr-1Zr near β titanium alloy during hot deformation was characterized by using the Johnson-Mehl-Avrami-Kolmogorov (JMAK) equation. To determine the equation parameters, a series of thermal simulation experiments at the temperature of 1023-1098 K and strain rate of 0.001-1 s‒1 to the true strain of 0.7 were conducted to obtain the essential data about stress σ and strain ɛ. By further transforming the relationship of σ versus ɛ into the relationship of strain hardening rate dσ/dɛ versus σ, two characteristic strains at the beginning of DRX (critical strain ɛc) and at the peak stress (peak strain ɛp) were identified from the dσ/dɛ-σ curves. Sequentially, the parameters in the JMAK equation were determined from the linear fitting of the different relationships among critical strain ɛc, peak strain ɛp and deformation conditions (including temperature T, strain rate \\dot ɛ and strain ɛ). The as-obtained JMAK equation was expressed as XDRX=1-exp[-0.0053((ɛ-ɛc)/ɛc)2.1], where ɛc=0.6053ɛp and ɛp=0.0031 \\dot ɛ .0081exp(28,781/RT). Finally, the JMAK equation was implanted into finite element program to simulate the hot compression of thermal simulation experiments. The simulation predictions and experimental results about the DRX volume fraction distribution showed a good consistency.

Experimental constraints and theoretical bases for microstructural damage in plate boundary shear zones

NASA Astrophysics Data System (ADS)

Skemer, P. A.; Cross, A. J.; Bercovici, D.

2016-12-01

(Ultra)mylonites from plate boundary shear zones are characterized by severe grain-size reduction and well-mixed mineral phases. The evolution from relatively undeformed tectonite protoliths to highly deformed (ultra)mylonites via the formation of new grain and phase boundaries is described as microstructural `damage.' Microstructural damage is important for two reasons: grain-size reduction is thought to result in significant rheological weakening, while phase mixing inhibits mechanical recovery and preserves the zone of weakness to be reactivated repeatedly throughout the tectonic cycle. Grain-size reduction by dynamic recrystallization has been studied extensively in both geologic and engineered materials, yet the progressive mixing of mineral phases during high pressure/temperature shear - the other essential element of damage or mylonitization - is not well understood. In this contribution we present new experimental results and theory related to two distinct phase mixing processes. First, we describe high strain torsion experiments on calcite and anhydrite mixtures and a simple geometric mixing model related to the stretching and thinning of monophase domains. Second, we describe a grain-switching mechanism that is driven by the surface-tension driven migration of newly formed interphase triple junctions. Unlike dynamic recrystallization, which occurs at relatively small strains, both phase mixing mechanisms described here appear to require extremely large strains, a prediction that is consistent with geologic observations. These data suggest that ductile shear zones experience long, transient intervals of microstructural evolution during which rheology is not at steady state. Microstructural damage may be interpreted as the product of several interconnected physical processes, which are collectively essential to the preservation of long-lived, Earth-like plate tectonics.

Petrofabrics of high-pressure rocks exhumed at the slab-mantle interface from the "point of no return" in a subduction zone (Sivrihisar, Turkey)

NASA Astrophysics Data System (ADS)

Whitney, Donna L.; Teyssier, Christian; Seaton, Nicholas C. A.; Fornash, Katherine F.

2014-12-01

The highest pressure recorded by metamorphic rocks exhumed from oceanic subduction zones is 2.5 GPa, corresponding to the maximum decoupling depth (MDD) (80 ± 10 km) identified in active subduction zones; beyond the MDD (the "point of no return") exhumation is unlikely. The Sivrihisar massif (Turkey) is a coherent terrane of lawsonite eclogite and blueschist facies rocks in which assemblages and fabrics record P-T-fluid-deformation conditions during exhumation from 80 to 45 km. Crystallographic fabrics and other features of high-pressure metasedimentary and metabasaltic rocks record transitions during exhumation. In quartzite, microstructures and crystallographic fabrics record deformation in the dislocation creep regime, including dynamic recrystallization during decompression, and a transition from prism slip to activation of rhomb and basal slip that may be related to a decrease in water fugacity during decompression ( 2.5 to 1.5 GPa). Phengite, lawsonite, and omphacite or glaucophane in quartzite and metabasalt remained stable during deformation, and omphacite developed an L-type crystallographic fabric. In marble, aragonite developed columnar textures with strong crystallographic fabrics that persisted during partial to complete dynamic recrystallization that was likely achieved in the stability field of aragonite (P > 1.2 GPa). Results of kinematic vorticity analysis based on lawsonite shape fabrics are consistent with shear criteria in quartzite and metabasalt and indicate a large component of coaxial deformation in the exhuming channel beneath a simple shear dominated interface. This large coaxial component may have multiplied the exhuming power of the subduction channel and forced deeply subducted rocks to flow back from the point of no return.

A two-stage constitutive model of X12CrMoWVNbN10-1-1 steel during elevated temperature

NASA Astrophysics Data System (ADS)

Zhu, Luobei; He, Jianli; Zhang, Ying

2018-02-01

In order to clarify the competition between work hardening (WH) caused by dislocation movements and the dynamic softening result from dynamic recovery (DRV) and dynamic recrystallization (DRX), a new two-stage flow stress model of X12CrMoWVNbN10-1-1 (X12) ferrite heat-resistant steel was established to describe the whole hot deformation behavior. And the parameters were determined by the experimental data operated on a Gleeble-3800 thermo- mechanical simulation. In this constitutive model, a single internal variable dislocation density evolution model is used to describe the influence of WH and DRV to flow stress. The DRX kinetic dynamic model can express accurately the contribution of DRX to the decline of flow stress, which was established on the Avrami equation. Furthermore, The established new model was compared with Fields-Bachofen (F-B) model and experimental data. The results indicate the new two-stage flow stress model can more accurately represent the hot deformation behavior of X12 ferrite heat-resistant steel, and the average error is only 0.0995.

Composition-dependent metallic glass alloys correlate atomic mobility with collective glass surface dynamics.

PubMed

Nguyen, Duc; Zhu, Zhi-Guang; Pringle, Brian; Lyding, Joseph; Wang, Wei-Hua; Gruebele, Martin

2016-06-22

Glassy metallic alloys are richly tunable model systems for surface glassy dynamics. Here we study the correlation between atomic mobility, and the hopping rate of surface regions (clusters) that rearrange collectively on a minute to hour time scale. Increasing the proportion of low-mobility copper atoms in La-Ni-Al-Cu alloys reduces the cluster hopping rate, thus establishing a microscopic connection between atomic mobility and dynamics of collective rearrangements at a glass surface made from freshly exposed bulk glass. One composition, La60Ni15Al15Cu10, has a surface resistant to re-crystallization after three heating cycles. When thermally cycled, surface clusters grow in size from about 5 glass-forming units to about 8 glass-forming units, evidence of surface aging without crystal formation, although its bulk clearly forms larger crystalline domains. Such kinetically stable glass surfaces may be of use in applications where glassy coatings stable against heating are needed.

In Situ XRD Studies of the Process Dynamics During Annealing in Cold-Rolled Copper

NASA Astrophysics Data System (ADS)

Dey, Santu; Gayathri, N.; Bhattacharya, M.; Mukherjee, P.

2016-12-01

The dynamics of the release of stored energy during annealing along two different crystallographic planes, i.e., {111} and {220}, in deformed copper have been investigated using in situ X-ray diffraction measurements at 458 K and 473 K (185 °C and 200 °C). The study has been carried out on 50 and 80 pct cold-rolled Cu sheets. The microstructures of the rolled samples have been characterized using optical microscopy and electron backscattered diffraction measurements. The microstructural parameters were evaluated from the X-ray diffractogram using the Scherrer equation and the modified Rietveld method. The stored energy along different planes was determined using the modified Stibitz formula from the X-ray peak broadening, and the bulk stored energy was evaluated using differential scanning calorimetry. The process dynamics of recovery and recrystallization as observed through the release of stored energy have been modeled as the second-order and first-order processes, respectively.

In situ imaging of the dynamics of photo-induced structural phase transition at high pressures by picosecond acoustic interferometry

NASA Astrophysics Data System (ADS)

Kuriakose, Maju; Chigarev, Nikolay; Raetz, Samuel; Bulou, Alain; Tournat, Vincent; Zerr, Andreas; Gusev, Vitalyi E.

2017-05-01

Picosecond acoustic interferometry is used to monitor in time the motion of the phase transition boundary between two water ice phases, VII and VI, coexisting at a pressure of 2.15 GPa when compressed in a diamond anvil cell at room temperature. By analyzing the time-domain Brillouin scattering signals accumulated for a single incidence direction of probe laser pulses, it is possible to access ratios of sound velocity values and of the refractive indices of the involved phases, and to distinguish between the structural phase transition and a recrystallization process. Two-dimensional spatial imaging of the phase transition dynamics indicates that it is initiated by the pump and probe laser pulses, preferentially at the diamond/ice interface. This method should find applications in three-dimensional monitoring with nanometer spatial resolution of the temporal dynamics of low-contrast material inhomogeneities caused by phase transitions or chemical reactions in optically transparent media.

Texture Development in a Friction Stir Lap-Welded AZ31B Magnesium Alloy

NASA Astrophysics Data System (ADS)

Naik, B. S.; Chen, D. L.; Cao, X.; Wanjara, P.

2014-09-01

The present study was aimed at characterizing the microstructure, texture, hardness, and tensile properties of an AZ31B-H24 Mg alloy that was friction stir lap welded (FSLWed) at varying tool rotational rates and welding speeds. Friction stir lap welding (FSLW) resulted in the presence of recrystallized grains and an associated hardness drop in the stir zone (SZ). Microstructural investigation showed that both the AZ31B-H24 Mg base metal (BM) and SZ contained β-Mg17Al12 and Al8Mn5 second phase particles. The AZ31B-H24 BM contained a type of basal texture (0001)<110> with the (0001) plane nearly parallel to the rolled sheet surface and <110> directions aligned in the rolling direction. FSLW resulted in the formation of another type of basal texture (0001)<100> in the SZ, where the basal planes (0001) became slightly tilted toward the transverse direction, and the prismatic planes (100) and pyramidal planes (101) exhibited a 30 deg + ( n - 1) × 60 deg rotation ( n = 1, 2, 3, …) with respect to the rolled sheet normal direction, due to the shear plastic flow near the pin surface that occurred from the intense local stirring. With increasing tool rotational rate and decreasing welding speed, the maximum intensity of the basal poles (0001) in the SZ decreased due to a higher degree of dynamic recrystallization that led to a weaker or more random texture. The tool rotational rate and welding speed had a strong effect on the failure load of FSLWed joints. A combination of relatively high welding speed (20 mm/s) and low tool rotational rate (1000 rpm) was observed to be capable of achieving a high failure load. This was attributed to the relatively small recrystallized grains and high intensity of the basal poles in the SZ arising from the low heat input as well as the presence of a small hooking defect.

Copper phthalocyanine films deposited by liquid-liquid interface recrystallization technique (LLIRCT).

PubMed

Patil, K R; Sathaye, S D; Hawaldar, R; Sathe, B R; Mandale, A B; Mitra, A

2007-11-15

The simple recrystallization process is innovatively used to obtain the nanoparticles of copper phthalocyanine by a simple method. Liquid-liquid interface recrystallization technique (LLIRCT) has been employed successfully to produce small sized copper phthalocyanine nanoparticles with diameter between 3-5 nm. The TEM-SAED studies revealed the formation of 3-5 nm sized with beta-phase dominated mixture of alpha and beta copper phthalocyanine nanoparticles. The XRD, SEM, and the UV-vis studies were further carried out to confirm the formation of copper phthalocyanine thin films. The cyclic voltametry (CV) studies conclude that redox reaction is totally reversible one electron transfer process. The process is attributed to Cu(II)/Cu(I) redox reaction.

Analysis of Semiconductor Structures by Nuclear and Electrical Techniques.

DTIC Science & Technology

temperatures well below the Si-Al eutectic (577C), fine grained polycrystalline Si in contact with Al films recrystallizes in the Al matrix. The... recrystallization can be deferred or suppressed by placing a buffer layer of V or Ti between the Al film and poly Si. (2) When annealing Pt films deposited on Si

Manufacturing process to reduce large grain growth in zirconium alloys

DOEpatents

Rosecrans, Peter M.

1987-01-01

A method of treating cold-worked zirconium alloys to reduce large grain gth during thermal treatment at temperatures above the recrystallization temperature of the alloy comprising heating the cold-worked alloy between about 1300.degree.-1350.degree. F. for 1 to 3 hours prior to treatment above its recrystallization temperature.

Gold Nanoparticle Aggregation as a Probe of Antifreeze (Glyco) Protein-Inspired Ice Recrystallization Inhibition and Identification of New IRI Active Macromolecules

NASA Astrophysics Data System (ADS)

Mitchell, Daniel E.; Congdon, Thomas; Rodger, Alison; Gibson, Matthew I.

2015-10-01

Antifreeze (glyco)proteins are found in polar fish species and act to slow the rate of growth of ice crystals; a property known as ice recrystallization inhibition. The ability to slow ice growth is of huge technological importance especially in the cryopreservation of donor cells and tissue, but native antifreeze proteins are often not suitable, nor easily available. Therefore, the search for new materials that mimic this function is important, but currently limited by the low-throughout assays associated with the antifreeze properties. Here 30 nm gold nanoparticles are demonstrated to be useful colorimetric probes for ice recrystallization inhibition, giving a visible optical response and is compatible with 96 well plates for high-throughout studies. This method is faster, requires less infrastructure, and has easier interpretation than the currently used ‘splat’ methods. Using this method, a series of serum proteins were identified to have weak, but specific ice recrystallization inhibition activity, which was removed upon denaturation. It is hoped that high-throughput tools such as this will accelerate the discovery of new antifreeze mimics.

Plasma deposited stability enhancement coating for amorphous ketoprofen.

PubMed

Bosselmann, Stephanie; Owens, Donald E; Kennedy, Rachel L; Herpin, Matthew J; Williams, Robert O

2011-05-01

A hydrophobic fluorocarbon coating deposited onto amorphous ketoprofen via pulsed plasma-enhanced chemical vapor deposition (PPECVD) significantly prolonged the onset of recrystallization compared to uncoated drug. Rapid freezing (RF) employed to produce amorphous ketoprofen was followed by PPECVD of perfluorohexane. The effect of coating thickness on the recrystallization and dissolution behavior of ketoprofen was investigated. Samples were stored in open containers at 40°C and 75% relative humidity, and the onset of recrystallization was monitored by DSC. An increase in coating thickness provided enhanced stability against recrystallization for up to 6 months at accelerated storage conditions (longest time of observation) when compared to three days for uncoated ketoprofen. Results from XPS analysis demonstrated that an increase in coating thickness was associated with improved surface coverage thus enabling superior protection. Dissolution testing showed that at least 80% of ketoprofen was released in buffer pH 6.8 from all coated samples. Overall, an increase in coating thickness resulted in a more complete drug release due to decreased adhesion of the coating to the substrate. Copyright © 2010 Elsevier B.V. All rights reserved.

Gold Nanoparticle Aggregation as a Probe of Antifreeze (Glyco) Protein-Inspired Ice Recrystallization Inhibition and Identification of New IRI Active Macromolecules

PubMed Central

Mitchell, Daniel E.; Congdon, Thomas; Rodger, Alison; Gibson, Matthew I.

2015-01-01

Antifreeze (glyco)proteins are found in polar fish species and act to slow the rate of growth of ice crystals; a property known as ice recrystallization inhibition. The ability to slow ice growth is of huge technological importance especially in the cryopreservation of donor cells and tissue, but native antifreeze proteins are often not suitable, nor easily available. Therefore, the search for new materials that mimic this function is important, but currently limited by the low-throughout assays associated with the antifreeze properties. Here 30 nm gold nanoparticles are demonstrated to be useful colorimetric probes for ice recrystallization inhibition, giving a visible optical response and is compatible with 96 well plates for high-throughout studies. This method is faster, requires less infrastructure, and has easier interpretation than the currently used ‘splat’ methods. Using this method, a series of serum proteins were identified to have weak, but specific ice recrystallization inhibition activity, which was removed upon denaturation. It is hoped that high-throughput tools such as this will accelerate the discovery of new antifreeze mimics. PMID:26499135

Devitrification and recrystallization of nanoparticle-containing glycerol and PEG-600 solutions.

PubMed

Lv, Fukou; Liu, Baolin; Li, Weijie; Jaganathan, Ganesh K

2014-02-01

Nanoparticles in solution offer unique electrical, mechanical and thermal properties due to their physical presence and interaction with the state of dispersion. This work is aimed to study the effects of hydroxyapatite (HA) nanoparticles on the devitrification and recrystallization events of two important cryoprotective solutions used in cell and tissue preservation namely glycerol (60%w/w) and PEG-600 (50%w/w). HA nanoparticles (20, 40 or 60 nm) were incorporated into solutions at the content of 0.1% or 0.5%(w/w), and were studied by differential scanning calorimeter (DSC) and cryomicroscopy. The presence of nanoparticles does not change the glass transition temperatures and melting temperatures of quenched solutions, but significantly affects the behavior of devitrification and recrystallization upon warming. Cryomicroscopic investigation showed the complex interactions among solution type, nanoparticle size and nanoparticle content, which apparently influence ice crystal growth or recrystallization in the quenched dispersions. These findings have significant implications for biomaterial cryopreservation, cryosurgery, and food manufacturing. The complexity of ice crystal growth kinetics in nanoparticle-containing dispersions remains to be poorly understood at the moment. Copyright © 2013 Elsevier Inc. All rights reserved.

Gold Nanoparticle Aggregation as a Probe of Antifreeze (Glyco) Protein-Inspired Ice Recrystallization Inhibition and Identification of New IRI Active Macromolecules.

PubMed

Mitchell, Daniel E; Congdon, Thomas; Rodger, Alison; Gibson, Matthew I

2015-10-26

Antifreeze (glyco)proteins are found in polar fish species and act to slow the rate of growth of ice crystals; a property known as ice recrystallization inhibition. The ability to slow ice growth is of huge technological importance especially in the cryopreservation of donor cells and tissue, but native antifreeze proteins are often not suitable, nor easily available. Therefore, the search for new materials that mimic this function is important, but currently limited by the low-throughout assays associated with the antifreeze properties. Here 30 nm gold nanoparticles are demonstrated to be useful colorimetric probes for ice recrystallization inhibition, giving a visible optical response and is compatible with 96 well plates for high-throughout studies. This method is faster, requires less infrastructure, and has easier interpretation than the currently used 'splat' methods. Using this method, a series of serum proteins were identified to have weak, but specific ice recrystallization inhibition activity, which was removed upon denaturation. It is hoped that high-throughput tools such as this will accelerate the discovery of new antifreeze mimics.

Tensile Properties of Molybdenum and Tungsten from 2500 to 3700 F

NASA Technical Reports Server (NTRS)

Hall, Robert W.; Sikora, Paul F.

1959-01-01

Specimens of commercially pure sintered tungsten, arc-cast unalloyed molybdenum, and two arc-cast molybdenum-base alloys (one with 0.5 percent titanium, the other with 0.46 percent titanium and 0.07 percent zirconium) were fabricated from 1/2-inch-diameter rolled or swaged bars. All specimens were evaluated in short-time tensile tests in the as-received condition, and all except the molybdenum-titanium-zirconium alloy were tested after a 30-minute recrystallization anneal at 3800 F in a vacuum of approximately 0.1 micron. Results showed that the tungsten was considerably stronger than either the arc-cast unalloyed molybdenum or the molybdenum-base alloys over the 2500 to 3700 F temperature range. Recrystallization of swaged tungsten at 3800 F considerably reduced its tensile strength at 2500 F. However, above 3100 F, the as-swaged tungsten specimens recrystallized during testing, and had about the same strength as when recrystallized at 3800 F before evaluation. The ductility of molybdenum-base materials was very high at all test temperatures; the ductility of tungsten decreased sharply above about 3120 F.

Crystal doping aided by rapid expansion of supercritical solutions.

PubMed

Vemavarapu, Chandra; Mollan, Matthew J; Needham, Thomas E

2002-01-01

The purpose of this study was to test the utility of rapid expansion of supercritical solution (RESS) based cocrystallizations in inducing polymorph conversion and crystal disruption of chlorpropamide (CPD). CPD crystals were recrystallized by the RESS process utilizing supercritical carbon dioxide as the solvent. The supercritical region investigated for solute extraction ranged from 45 to 100 degrees C and 2000 to 8000 psi. While pure solute recrystallization formed stage I of these studies, stage II involved recrystallization of CPD in the presence of urea (model impurity). The composition, morphology, and crystallinity of the particles thus produced were characterized utilizing techniques such as microscopy, thermal analysis, x-ray powder diffractometry, and high-performance liquid chromatography. Also, comparative evaluation between RESS and evaporative crystallization from liquid solvents was performed. RESS recrystallizations of commercially available CPD (form A) resulted in polymorph conversion to metastable forms C and V, depending on the temperature and pressure of the recrystallizing solvent. Cocrystallization studies revealed the formation of eutectic mixtures and solid solutions of CPD + urea. Formation of the solid solutions resulted in the crystal disruption of CPD and subsequent amorphous conversion at urea levels higher than 40% wt/wt. Consistent with these results were the reductions in melting point (up to 9 degrees C) and in the DeltaH(f) values of CPD (up to 50%). Scanning electron microscopy revealed a particle size reduction of up to an order of magnitude upon RESS processing. Unlike RESS, recrystallizations from liquid organic solvents lacked the ability to affect polymorphic conversions. Also, the incorporation of urea into the lattice of CPD was found to be inadequate. In providing the ability to control both the particle and crystal morphologies of active pharmaceutical ingredients, RESS proved potentially advantageous to crystal engineering. Rapid crystallization kinetics were found vital in making RESS-based doping superior to conventional solvent-based cocrystallizations.

Evolution of microstructure, texture and inhibitor along the processing route for grain-oriented electrical steels using strip casting

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liu, Hai-Tao, E-mail: liuht@ral.neu.edu.cn; Institute of Research of Iron and Steel, Shasteel, Zhangjiagang 215625, Jiangsu; Yao, Sheng-Jie

2015-08-15

In the present work, a regular grade GO sheet was produced successively by strip casting, hot rolling, normalizing annealing, two-stage cold rolling with intermediate annealing, primary recrystallization annealing, secondary recrystallization annealing and purification. The aim of this paper was to characterize the evolution of microstructure, texture and inhibitor along the new processing route by comprehensive utilization of optical microscopy, X-ray diffraction and transmission electron microscopy. It was found that a fine microstructure with the ferrite grain size range of 7–12 μm could be obtained in the primary recrystallization annealed sheet though a very coarse microstructure was produced in the initialmore » as-cast strip. The main finding was that the “texture memory” effect on Goss texture started on the through-thickness intermediate annealed strip after first cold rolling, which was not similar to the “texture memory” effect on Goss texture starting on the surface layers of the hot rolled strip in the conventional production route. As a result, the origin of Goss nuclei capable of secondary recrystallization lied in the grains already presented in Goss orientation in the intermediate annealed strip after first cold rolling. Another finding was that fine and dispersive inhibitors (mainly AlN) were easy to be produced in the primary recrystallization microstructure due to the initial rapid solidification during strip casting and the subsequent rapid cooling, and the very high temperature reheating usually used before hot rolling in the conventional production route could be avoided. - Highlights: • A regular grade grain-oriented electrical steel was produced. • Evolution of microstructure, texture and inhibitor was characterized. • Origin of Goss nuclei lied in the intermediate annealed strip. • A fine primary recrystallization microstructure could be produced. • Effective inhibitors were easy to be obtained in the new processing route.« less

Content of toxic and essential metals in recrystallized and washed table salt in Shiraz, Iran

PubMed Central

2014-01-01

Background Table salt is the most commonly used food additive. Since most of the salt consumed in Iran comes from mines, contamination with heavy metals is a health concern. The commonest salt purification method in Iran is washing with water. But recently, some industries have turned to recrystallization method. The present study aimed to determine the level of essential and non-essential heavy metals in the table salt refined with recrystallization and washing methods. Methods Thirty eight pre-packed salt samples were directly collected from retail market in Shiraz (22 samples refined with recrystallization method and 16 with washing method). The level of lead, cadmium, copper, zinc, nickel and cobalt was determined using Voltammetric method. Daily intakes of lead and cadmium as well as their weekly intakes were calculated. Results The levels of lead, cadmium, copper, zinc, nickel and cobalt in recrystallized samples were 0. 30 ± 0.26, 0.02 ± 0.02, 0.11 ± 0.06, 0.34 ± 0.22, 0.15 ± 0.19 and 0.008 ± 0.007 μg/g, respectively, and also 0.37 ± 0.27, 0.017 ± 0.021, 0.19 ± 0.18, 0.37 ± 0.20, 0.13 ± 0.23 and 0.037 ± 0.06 μg/g in washed salt samples. The calculated weekly intake of lead and cadmium was 0.216 and 0.014 μg/kg, respectively for the recrystallized and 0.2653 and 0.0119 μg/kg for the washed salts. Conclusion All values for toxic metals were lower than the permitted maximum for human consumption as prescribed by Codex and Institute of Standards and Industrial Research of Iran. Only 0.8652-1.0612% of lead and 0.17-0.2% of cadmium PTWIs are received via salt consumption weekly. PMID:24398299

Crystallographic control and texture inheritance during mylonitization of coarse grained quartz veins

NASA Astrophysics Data System (ADS)

Ceccato, Alberto; Pennacchioni, Giorgio; Menegon, Luca; Bestmann, Michel

2017-10-01

Quartz veins within Rieserferner pluton underwent deformation during post-magmatic cooling at temperature around 450 °C. Different crystallographic orientations of cm-sized quartz vein crystals conditioned the evolution of microstructures and crystallographic preferred orientations (CPO) during vein-parallel simple shear up to high shear strains (γ ≈ 10). For γ < 2, crystals stretched to ribbons of variable aspect ratios. The highest aspect ratios resulted from {m} glide in ribbons with c-axis sub-parallel to the shear zone vorticity Y-axis. Ribbons with c-axis orthogonal to Y (XZ-type ribbons) were stronger and hardened more quickly: they show lower aspect ratios and fine (grain size 10-20 μm) recrystallization along sets of microshear zones (μSZs) exploiting crystallographic planes. Distortion of XZ-type ribbons and recrystallization preferentially exploited the slip systems with misorientation axis close to Y. New grains of μSZs initiated by subgrain rotation recrystallization (SGR) and thereupon achieved high angle misorientations by a concurrent process of heterogeneous rigid grain rotation around Y associated with the confined shear within the μSZ. Dauphiné twinning occurred pervasively, but did not play a dominant role on μSZ nucleation. Recrystallization became widespread at γ > 2 and pervasive at γ ≈ 10. Ultramylonitic quartz veins are fine grained ( 10 μm, similar to new grains of μSZ) and show a CPO banding resulting in a bulk c-axis CPO with a Y-maximum, as part of a single girdle about orthogonal to the foliation, and orientations at the pole figure periphery at moderate to high angle to the foliation. This bulk CPO derives from steady-state SGR associated with preferential activity, in the different CPO bands, of slip systems generating subgrain boundaries with misorientation axes close to Y. The CPO of individual recrystallized bands is largely inherited from the original crystallographic orientation of the ribbons (and therefore vein crystals) from which they derived. High strain and pervasive recrystallization were not enough to reset the initial crystallographic heterogeneity and this CPO memory is explained by the dominance of SGR. This contrast with experimental observation of a rapid erasure of a pristine CPO by cannibalism from grains with the most favourably oriented slip system under dominant grain boundary migration recrystallization.

Strain Amount Dependent Grain Size and Orientation Developments during Hot Compression of a Polycrystalline Nickel Based Superalloy

PubMed Central

He, Guoai; Tan, Liming; Liu, Feng; Huang, Lan; Huang, Zaiwang; Jiang, Liang

2017-01-01

Controlling grain size in polycrystalline nickel base superalloy is vital for obtaining required mechanical properties. Typically, a uniform and fine grain size is required throughout forging process to realize the superplastic deformation. Strain amount occupied a dominant position in manipulating the dynamic recrystallization (DRX) process and regulating the grain size of the alloy during hot forging. In this article, the high-throughput double cone specimen was introduced to yield wide-range strain in a single sample. Continuous variations of effective strain ranging from 0.23 to 1.65 across the whole sample were achieved after reaching a height reduction of 70%. Grain size is measured to be decreased from the edge to the center of specimen with increase of effective strain. Small misorientation tended to generate near the grain boundaries, which was manifested as piled-up dislocation in micromechanics. After the dislocation density reached a critical value, DRX progress would be initiated at higher deformation region, leading to the refinement of grain size. During this process, the transformations from low angle grain boundaries (LAGBs) to high angle grain boundaries (HAGBs) and from subgrains to DRX grains are found to occur. After the accomplishment of DRX progress, the neonatal grains are presented as having similar orientation inside the grain boundary. PMID:28772514

An electron microscopy examination of primary recrystallization in TD-nickel.

NASA Technical Reports Server (NTRS)

Petrovic, J. J.; Ebert, L. J.

1972-01-01

Primary recrystallization in TD-nickel 1 in. bar has previously been regarded as the process by which the initial fine grain structure is converted to a coarse grain size (increases in grain size by 500 times) under suitable deformation and annealing conditions. This process is dependent on deformation mode. While it occurs readily after rolling transverse to the bar axis and annealing (800 C), it is completely inhibited by longitudinal rolling and swaging deformations, even for very high (1320 C) annealing temperatures. A transmission electron microscopy examination of deformation and annealing substructures indicates that primary recrystallization in TD-nickel 1 in. bar actually occurs on the sub-light optical level, to produce a grain structure similar in size to the initial fine grained state.

Facially Amphipathic Glycopolymers Inhibit Ice Recrystallization.

PubMed

Graham, Ben; Fayter, Alice E R; Houston, Judith E; Evans, Rachel C; Gibson, Matthew I

2018-05-02

Antifreeze glycoproteins (AFGPs) from polar fish are the most potent ice recrystallization (growth) inhibitors known, and synthetic mimics are required for low-temperature applications such as cell cryopreservation. Here we introduce facially amphipathic glycopolymers that mimic the three-dimensional structure of AFGPs. Glycopolymers featuring segregated hydrophilic and hydrophobic faces were prepared by ring-opening metathesis polymerization, and their rigid conformation was confirmed by small-angle neutron scattering. Ice recrystallization inhibition (IRI) activity was reduced when a hydrophilic oxo-ether was installed on the glycan-opposing face, but significant activity was restored by incorporating a hydrophobic dimethylfulvene residue. This biomimetic strategy demonstrates that segregated domains of distinct hydrophilicity/hydrophobicity are a crucial motif to introduce IRI activity, which increases our understanding of the complex ice crystal inhibition processes.

Magma-assisted strain localization in an orogen-parallel transcurrent shear zone of southern Brazil

NASA Astrophysics Data System (ADS)

Tommasi, AndréA.; Vauchez, Alain; Femandes, Luis A. D.; Porcher, Carla C.

1994-04-01

In a lithospheric-scale, orogen-parallel transcurrent shear zone of the Pan-African Dom Feliciano belt of southern Brazil, two successive generations of magmas, an early calc-alkaline and a late peraluminous, have been emplaced during deformation. Microstructures show that these granitoids experienced a progressive deformation from magmatic to solid state under decreasing temperature conditions. Magmatic deformation is indicated by the coexistence of aligned K-feldspar, plagioclase, micas, and/or tourmaline with undeformed quartz. Submagmatic deformation is characterized by strain features, such as fractures, lattice bending, or replacement reactions affecting only the early crystallized phases. High-temperature solid-state deformation is characterized by extensive grain boundary migration in quartz, myrmekitic K-feldspar replacement, and dynamic recrystallization of both K-feldspar and plagioclase. Decreasing temperature during solid-state deformation is inferred from changes in quartz crystallographic fabrics, decrease in grain size of recrystallized feldspars, and lower Ti amount in recrystallized biotites. Final low-temperature deformation is characterized by feldspar replacement by micas. The geochemical evolution of the synkinematic magmatism, from calc-alkaline metaluminous granodiorites with intermediate 87Sr/86Sr initial ratio to peraluminous granites with very high 87Sr/86Sr initial ratio, suggests an early lower crustal source or a mixed mantle/crustal source, followed by a middle to upper crustal source for the melts. Shearing in lithospheric faults may induce partial melting in the lower crust by shear heating in the upper mantle, but, whatever the process initiating partial melting, lithospheric transcurrent shear zones may collect melt at different depths. Because they enhance the vertical permeability of the crust, these zones may then act as heat conductors (by advection), promoting an upward propagation of partial melting in the crust. Synkinematic granitoids localize most, if not all, deformation in the studied shear zone. The regional continuity and the pervasive character of the magmatic fabric in the various synkinematic granitic bodies, consistently displaying similar plane and direction of flow, argue for accommodation of large amounts of orogen-parallel movement by viscous deformation of these magmas. Moreover, activation of high-temperature deformation mechanisms probably allowed a much easier deformation of the hot synkinematic granites than of the colder country rock and, consequently, contributed significantly to the localization of deformation. Finally, the small extent of the low-temperature deformation suggests that the strike-slip deformation ended approximately synchronously with the final cooling of the peraluminous granites. The evolution of the deformation reflects the strong influence of synkinematic magma emplacement and subsequent cooling on the thermomechanical evolution of the shear zone. Magma intrusion in an orogen-scale transcurrent shear zone deeply modifies the rheological behavior of the continental crust. It triggers an efficient thermomechanical softening localized within the fault that may subsist long enough for large displacements to be accommodated. Therefore the close association of deformation and synkinematic magmatism probably represents an important factor controlling the mechanical response of continental plates in collisional environments.

Progressive softening of brittle-ductile transition due to interplay between chemical and deformation processes

NASA Astrophysics Data System (ADS)

Jeřábek, Petr; Bukovská, Zita; Morales, Luiz F. G.

2017-04-01

The micro-scale shear zones (shear bands) in granitoids from the South Armorican Shear Zone reflect localization of deformation and progressive weakening in the conditions of brittle-ductile transition. We studied microstructures in the shear bands with the aim to establish their P-T conditions and to derive stress and strain rates for specific deformation mechanisms. The evolving microstructure within shear bands documents switches in deformation mechanisms related to positive feedbacks between deformation and chemical processes and imposes mechanical constraints on the evolution of the brittle-ductile transition in the continental transform fault domains. The metamorphic mineral assemblage present in the shear bands indicate their formation at 300-350 ˚ C and 100-400 MPa. Focusing on the early development of shear bands, we identified three stages of shear band evolution. The early stage I associated with initiation of shear bands occurs via formation of microcracks with possible yielding differential stress of up to 250 MPa (Diamond and Tarantola, 2015). Stage II is associated with subgrain rotation recrystallization and dislocation creep in quartz and coeval dissolution-precipitation creep of microcline. Recrystallized quartz grains in shear bands show continual increase in size, and decrease in stress and strain rates from 94 MPa to 17-26 MPa (Stipp and Tullis, 2003) and 3.8*10-12 s-1- 1.8*10-14 s-1 (Patterson and Luan, 1990) associated with deformation partitioning into weaker microcline layer and shear band widening. The quartz mechanical data allowed us to set some constrains for coeval dissolution-precipitation of microcline which at our estimated P-T conditions suggests creep at 17-26 MPa differential stress and 3.8*10-13 s-1 strain rate. Stage III is characterized by localized slip along interconnected white mica bands accommodated by dislocation creep at strain rate 3.8*10-12 s-1 and stress 9.36 MPa (Mares and Kronenberg, 1993). The studied example documents a competition between shear zone widening and narrowing mechanisms, i.e. distributed and localized deformation, depending on the specific mineral phase and deformation mechanism active in each moment of the shear zone evolution. In addition, our mechanical data point to dynamic evolution of the studied brittle-ductile transition characterized by major weakening to strengths ˜10 MPa. Such non-steady-state evolution may be common in crustal shear zones especially when phase transformations are involved. References: Diamond, L. W., and A. Tarantola (2015), Interpretation of fluid inclusions in quartz deformed by weak ductile shearing: Reconstruction of differential stress magnitudes and pre-deformation fluid properties, Earth Planet. Sci. Lett., 417, 107-119. Mares, V. M., and A. K. Kronenberg (1993), Experimental deformation of muscovite, J. Struct. Geol., 15(9), 1061-1075. Paterson, M. S., and F. C. Luan (1990), Quartzite rheology under geological conditions, Geol. Soc. London, Spec. Publ., 54(1), 299-307. Stipp, M., and J. Tullis (2003), The recrystallized grain size piezometer for quartz, Geophys. Res. Lett., 30(21), 1-5.

Modeling ductile metals under large strain, pressure and high strain rate incorporating damage and microstructure evolution

NASA Astrophysics Data System (ADS)

Iannitti, Gianluca; Bonora, Nicola; Ruggiero, Andrew; Dichiaro, Simone

2012-03-01

In this work, a constitutive modeling that couples plasticity, grain size evolution (due to plastic deformation and dynamic recrystallization) and ductile damage has been developed. The effect of grain size on the material yield stress (Hall-Petch) and on the melting temperature has been considered. The model has been used to investigate computationally the behavior of high purity copper in dynamic tensile extrusion test (DTE). An extensive numerical simulation work, using implicit finite element code with direct integration, has been performed and the results have been compared with available experimental data. The major finding is that the proposed model is capable to predict most of the observed features such as the increase of material ductility with the decreasing average grain size, the overall number and size of fragments and the average grain size distribution in the fragment trapped into the dime.

Modeling ductile metals under large strain, pressure and high strain rates incorporating damage and microstructure evolution

NASA Astrophysics Data System (ADS)

Iannitti, Gianluca; Bonora, Nicola; Ruggiero, Andrew; Dichiaro, Simone

2011-06-01

In this work, a constitutive modeling that couples plasticity, grain size evolution (due to plastic deformation and dynamic recrystallization) and ductile damage has been developed. The effect of grain size on the material yield stress (Hall-Petch) and on the melting temperature has been considered. The model has been used to investigate computationally the behaviour of high purity copper in dynamic tensile extrusion test (DTE). An extensive numerical simulation work, using implicit finite element code with direct integration, has been performed and the results have been compared with available experimental data. The major finding is that the proposed model is capable to predict most of the observed features such as the increase of material ductility with the decreasing average grain size, the overall number and size of fragments and the average grain size distribution in the fragment trapped into the dime.

Investigation on Hot Workability of Homogenized Al-Zn-Mg-Cu Alloy Based on Activation Energy and Processing Map

NASA Astrophysics Data System (ADS)

Peng, Xiaoyan; Su, Wusen; Xiao, Dan; Xu, Guofu

2018-06-01

Hot deformation behaviors of the homogenized Al-Zn-Mg-Cu alloy were studied by uniaxial compression tests carried out at 623-743 K and strain rates of 0.01-10 s-1. The constitutive equation was developed for the activation energy, and thus the activation energy map was constructed. During the hot deformation, the dominated softening mechanisms were the dynamic recovery and dynamic recrystallization, which were most likely to be driven with increasing temperature and decreasing activation energy. Based on the superposition of the activation energy map and the processing map, together with the microstructure characteristics, the optimized hot workability of the alloy was proposed at the domain (670-743 K and 0.01-0.16 s-1), where the peak efficiency was 0.39 and the activation energy range was 196-260 kJ mol-1.

Dynamic creation and evolution of gradient nanostructure in single-crystal metallic microcubes.

PubMed

Thevamaran, Ramathasan; Lawal, Olawale; Yazdi, Sadegh; Jeon, Seog-Jin; Lee, Jae-Hwang; Thomas, Edwin L

2016-10-21

We demonstrate the dynamic creation and subsequent static evolution of extreme gradient nanograined structures in initially near-defect-free single-crystal silver microcubes. Extreme nanostructural transformations are imposed by high strain rates, strain gradients, and recrystallization in high-velocity impacts of the microcubes against an impenetrable substrate. We synthesized the silver microcubes in a bottom-up seed-growth process and use an advanced laser-induced projectile impact testing apparatus to selectively launch them at supersonic velocities (~400 meters per second). Our study provides new insights into the fundamental deformation mechanisms and the effects of crystal and sample-shape symmetries resulting from high-velocity impacts. The nanostructural transformations produced in our experiments show promising pathways to developing gradient nanograined metals for engineering applications requiring both high strength and high toughness-for example, in structural components of aircraft and spacecraft. Copyright © 2016, American Association for the Advancement of Science.

Analysing the strength of friction stir welded dissimilar aluminium alloys using Sugeno Fuzzy model

NASA Astrophysics Data System (ADS)

Barath, V. R.; Vaira Vignesh, R.; Padmanaban, R.

2018-02-01

Friction stir welding (FSW) is a promising solid state joining technique for aluminium alloys. In this study, FSW trials were conducted on two dissimilar plates of aluminium alloy AA2024 and AA7075 by varying the tool rotation speed (TRS) and welding speed (WS). Tensile strength (TS) of the joints were measured and a Sugeno - Fuzzy model was developed to interconnect the FSW process parameters with the tensile strength. From the developed model, it was observed that the optimum heat generation at WS of 15 mm.min-1 and TRS of 1050 rpm resulted in dynamic recovery and dynamic recrystallization of the material. This refined the grains in the FSW zone and resulted in peak tensile strength among the tested specimens. Crest parabolic trend was observed in tensile strength with variation of TRS from 900 rpm to 1200 rpm and TTS from 10 mm.min-1 to 20 mm.min-1.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Myers, M.A.; LaSalvia, J.C.; Hoke, D.

Combustion synthesis followed by densification was utilized in producing monolithic TiC and TiB2 materials, and TiC-Ni, TiB2-Ni, TiB2-Al2O3, and TiB2SiC ceramic composites. Static and dynamic densification equipments were developed with the loading applied immediately after the synthesis reaction was completed and the ceramic/composite was ductile. All the ceramics exhibited an equiaxed grain structure with alternating regions at high and low dislocation densities, indicating that recovery/recrystallization mechanisms are prevalent. The grain boundaries were, as far as could be established, devoid of impurities and second phases. Quasi-static and dynamic mechanical testing were performed and revealed that the materials exhibited strength levels comparablemore » to conventionally produced materials. Instrumented densification experiments were conducted and a temperature-dependent consitutive model was applied for plastic deformation of the porous combustion synthesis product.« less

Simulation of possible regolith optical alteration effects on carbonaceous chondrite meteorites

NASA Technical Reports Server (NTRS)

Clark, Beth E.; Fanale, Fraser P.; Robinson, Mark S.

1993-01-01

As the spectral reflectance search continues for links between meteorites and their parent body asteroids, the effects of optical surface alteration processes need to be considered. We present the results of an experimental simulation of the melting and recrystallization that occurs to a carbonaceous chondrite meteorite regolith powder upon heating. As done for the ordinary chondrite meteorites, we show the effects of possible parent-body regolith alteration processes on reflectance spectra of carbonaceous chondrites (CC's). For this study, six CC's of different mineralogical classes were obtained from the Antarctic Meteorite Collection: two CM meteorites, two CO meteorites, one CK, and one CV. Each sample was ground with a ceramic mortar and pestle to powders with maximum grain sizes of 180 and 90 microns. The reflectance spectra of these powders were measured at RELAB (Brown University) from 0.3 to 2.5 microns. Following comminution, the 90 micron grain size was melted in a nitrogen controlled-atmosphere fusion furnace at an approximate temperature of 1700 C. The fused sample was immediately held above a flow of nitrogen at 0 C for quenching. Following melting and recrystallization, the samples were reground to powders, and the reflectance spectra were remeasured. The effects on spectral reflectance for a sample of the CM carbonaceous chondrite called Murchison are shown.

Tension-controlled single-crystallization of copper foils for roll-to-roll synthesis of high-quality graphene films

NASA Astrophysics Data System (ADS)

Jo, Insu; Park, Subeom; Kim, Dongjin; San Moon, Jin; Park, Won Bae; Kim, Tae Hyeong; Hyoun Kang, Jin; Lee, Wonbae; Kim, Youngsoo; Lee, Dong Nyung; Cho, Sung-Pyo; Choi, Hyunchul; Kang, Inbyeong; Park, Jong Hyun; Lee, Jeong Soo; Hong, Byung Hee

2018-04-01

It has been known that the crystalline orientation of Cu substrates plays a crucial role in chemical vapor deposition (CVD) synthesis of high-quality graphene. In particular, Cu (1 1 1) surface showing the minimum lattice mismatch with graphene is expected to provide an ideal catalytic reactivity that can minimize the formation of defects, which also induces larger single-crystalline domain sizes of graphene. Usually, the Cu (1 1 1) substrates can be epitaxially grown on single-crystalline inorganic substrates or can be recrystallized by annealing for more than 12 h, which limits the cost and time-effective synthesis of graphene. Here, we demonstrate a new method to optimize the crystalline orientations of vertically suspended Cu foils by tension control during graphene growth, resulting in large-area recrystallization into Cu (1 1 1) surface as the applied tension activates the grain boundary energy of Cu and promotes its abnormal grain growth to single crystals. In addition, we found a clue that the formation of graphene cooperatively assists the recrystallization into Cu (1 1 1) by minimizing the surface energy of Cu. The domain sizes and charge carrier mobility of graphene grown on the single-crystalline Cu (1 1 1) are 5 times and ~50% increased, respectively, in comparison with those of graphene from Cu (1 0 0), indicating that the less lattice mismatch and the lower interaction energy between Cu (1 1 1) and graphene allows the growth of larger single-crystalline graphene with higher charge carrier mobility. Thus, we believe that our finding provides a crucial idea to design a roll-to-roll (R2R) graphene synthesis system where the tension control is inevitably involved, which would be of great importance for the continuous production of high-quality graphene in the future.

Recrystallization of Manganite (γ-MnOOH) and Implications for Trace Element Cycling.

PubMed

Hens, Tobias; Brugger, Joël; Cumberland, Susan A; Etschmann, Barbara; Frierdich, Andrew J

2018-02-06

The recrystallization of Mn(III,IV) oxides is catalyzed by aqueous Mn(II) (Mn(II) aq ) during (bio)geochemical Mn redox cycling. It is poorly understood how trace metals associated with Mn oxides (e.g., Ni) are cycled during such recrystallization. Here, we use X-ray absorption spectroscopy (XAS) to examine the speciation of Ni associated with Manganite (γ-Mn(III)OOH) suspensions in the presence or absence of Mn(II) aq under variable pH conditions (pH 5.5 and 7.5). In a second set of experiments, we used a 62 Ni isotope tracer to quantify the amount of dissolved Ni that exchanges with Ni incorporated in the Manganite crystal structure during reactions in 1 mM Mn(II) aq and in Mn(II)-free solutions. XAS spectra show that Ni is initially sorbed on the Manganite mineral surface and is progressively incorporated into the mineral structure over time (13% after 51 days) even in the absence of dissolved Mn(II). The amount of Ni incorporation significantly increases to about 40% over a period of 51 days when Mn(II) aq is present in solution. Similarly, Mn(II) aq promotes Ni exchange between Ni-substituted Manganite and dissolved Ni(II), with around 30% of Ni exchanged at pH 7.5 over the duration of the experiment. No new mineral phases are detected following recrystallization as determined by X-ray diffraction and XAS. Our results reveal that Mn(II)-catalyzed mineral recrystallization partitions Ni between Mn oxides and aqueous fluids and can therefore affect Ni speciation and mobility in the environment.

Internal Shear Forging Processes for Missile Primary Structures.

DTIC Science & Technology

1981-07-20

received condition. The as-received micro- structure displayed elongated recrystallized grains interspersed with particles of precipitate phases. SEM...re- crystallization regime for this alloy, and rolled specimens were reheated to 3160 C between passes, some recrystallization and grain size changes...experiment revealed that the actual solution treatment temperature was probably higher than 5000C. This resulted in melting of the eutectic and solid

Chemical Characterization of Dimethylsulfoxide (DMSO) Munitions Recrystallization Process Samples.

DTIC Science & Technology

1984-10-01

position unless so designated by other aulthorized documents. Disposition Destroy this report when it is no longer needed. Do riot return it to the... DESTRIBUTION LIST ....... ........... ... ................................. -12 rABLES 1. HPLC Analyses of Munitions from DMS0 Recrystallization Process...characterization and identification of any trace organics present in addition to the nitramines. Portions of the two samples, designated as evaporator

Effect of Post-deformation Annealing Treatment on the Microstructural Evolution of a Cold-Worked Corrosion-Resistant Superalloy (CRSA) Steel

NASA Astrophysics Data System (ADS)

Mirzaei, A.; Zarei-Hanzaki, A.; Mohamadizadeh, A.; Lin, Y. C.

2018-03-01

The post-deformation annealing treatments of a commercial cold-worked corrosion-resistant superalloy steel (Sanicro 28 steel) were carried out at different temperatures in the range of 900-1100 °C for different holding durations of 5, 10, and 15 min. The effects of post-deformation annealing time and temperature on the microstructural evolution and subsequent mechanical properties of the processed Sanicro 28 steel were investigated. The observations indicated that twin-twin hardening in cold deformation condition mainly correlates with abundant nucleation of mechanical twins in multiple directions resulting in considerable strain hardening behavior. Microstructural investigations showed that the static recrystallization takes place after isothermal holding at 900 °C for 5 min. Increasing the annealing temperature from 900 to 1050 °C leads to recrystallization development and grain refinement in the as-recrystallized state. In addition, an increase in annealing duration from 5 to 15 min leads to subgrain coarsening and subsequently larger recrystallized grains size. The occurrence of large proportion of the grain refinement, which is achieved in the first annealing stage at 1050 °C after 5 min, is considered as the main factor for the maximum elongation at this stage.

Ice recrystallization kinetics in the presence of synthetic antifreeze glycoprotein analogues using the framework of LSW theory.

PubMed

Budke, C; Heggemann, C; Koch, M; Sewald, N; Koop, T

2009-03-05

The Ostwald ripening of polycrystalline ice in aqueous sucrose solutions was investigated experimentally. The kinetics of this ice recrystallization process was studied at temperatures between -6 and -10 degrees C and varying ice volume fractions. Using the theory of Lifshitz, Slyozov, and Wagner (LSW), the diffusion-limited rate constant for ice recrystallization was determined. Also, the effects of synthetic analogues of natural antifreeze glycoproteins (AFGP) were studied. These analogues synAFGPmi (i = 3-5) contained monosaccharide side groups instead of disaccharide side groups that occur in natural AFGP. In order to account for the inhibition effect of the synAFGPmi, we have modified classical LSW theory, allowing for the derivation of inhibition rate constants. It was found that the investigated synAFGPmi inhibit ice recrystallization at concentrations down to approximately 3 microg mL(-1) or, equivalently, approximately 1 micromol L(-1) for the largest synAFGPmi investigated: synAFGPm5. Hence, our new method is capable of quantitatively assessing the efficiency of very similar AFGP with a sensitivity that is at least 2 orders of magnitude larger than that typical for quantitative thermal hysteresis measurements.

Influence of phosphate glass recrystallization on the stability of a waste matrix to leaching

NASA Astrophysics Data System (ADS)

Yudintsev, S. V.; Pervukhina, A. M.; Mokhov, A. V.; Malkovsky, V. I.; Stefanovsky, S. V.

2017-04-01

In Russia, highly radioactive liquid wastes from recycling of spent fuel of nuclear reactors are solidified into Na-Al-P glass for underground storage. The properties of the matrix including the radionuclide fixation will change with time due to crystallization. This is supported by the results of study of the interaction between glassy matrices, products of their crystallization, and water. The concentration of Cs in a solution at the contact of a recrystallized sample increased by three orders of magnitude in comparison with an experiment with glass. This difference is nearly one order of magnitude for Sr, Ce, and Nd (simulators of actinides) and U due to their incorporation into phases with low solubility in water. Based on data on the compositional change of solutions after passing through filters of various diameters, it is concluded that Cs occurs in the dissolved state in runs with a glass and recrystallized matrix. At the same time, Sr, lanthanides, and U occur in the dissolved state and in the composition of colloids in runs with glass, and mostly in colloid particles after contact with the recrystallized sample. These results should be regarded for substantiation of safety for geological waste storage.

Small molecule ice recrystallization inhibitors mitigate red blood cell lysis during freezing, transient warming and thawing

NASA Astrophysics Data System (ADS)

Briard, Jennie G.; Poisson, Jessica S.; Turner, Tracey R.; Capicciotti, Chantelle J.; Acker, Jason P.; Ben, Robert N.

2016-03-01

During cryopreservation, ice recrystallization is a major cause of cellular damage. Conventional cryoprotectants such as dimethyl sulfoxide (DMSO) and glycerol function by a number of different mechanisms but do not mitigate or control ice recrystallization at concentrations utilized in cryopreservation procedures. In North America, cryopreservation of human red blood cells (RBCs) utilizes high concentrations of glycerol. RBC units frozen under these conditions must be subjected to a time-consuming deglycerolization process after thawing in order to remove the glycerol to <1% prior to transfusion thus limiting the use of frozen RBC units in emergency situations. We have identified several low molecular mass ice recrystallization inhibitors (IRIs) that are effective cryoprotectants for human RBCs, resulting in 70-80% intact RBCs using only 15% glycerol and slow freezing rates. These compounds are capable of reducing the average ice crystal size of extracellular ice relative to a 15% glycerol control validating the positive correlation between a reduction in ice crystal size and increased post-thaw recovery of RBCs. The most potent IRI from this study is also capable of protecting frozen RBCs against the large temperature fluctuations associated with transient warming.

S-Isovaline Contained in Meteorites, Induces Enantiomeric Excess in D,L-glutamic Acid During Recrystallization

NASA Astrophysics Data System (ADS)

Kojo, Shosuke

2015-06-01

S-Isovaline (S-Iva: 6.7 mmol) and D,L-glutamic acid (Glu: 2 mmol) were dissolved in 10 ml of hot water, and the resulting solution was divided in 5 vessels. After recrystallization, the crystals were collected from each vessel, and the enantiomeric excess (ee) of Glu was determined with chemical derivatization using 1-fluoro-2,4-dinitrophenyl- 5-L-leucinamide followed by high-performance liquid chromatography. Ten crystallizations provided all D-rich Glu with ee values of 2.69 % ± 0.81 % (mean ± standard deviation), and those using R-Iva provided all L-rich Glu with ee values of 6.24 % ± 2.20 %. Five recrystallizations of D,L-Glu alone provided ee values of 0.474 % ± 0.33 %. The differences among these three ee values were statistically significant, showing that S-Iva, which was present in meteorites caused a significant induction of ee in this physiological amino acid. This is the first outcome that S-Iva induced ee changes in a physiological amino acid. S-Iva did not induce any ee changes in D,L-asparagine, leucine, valine, methionine, phenylalanine, tryptophan, glutamine, tyrosine, aspartic acid, or histidine under similar recrystallizations.

Effects of Al3(Sc,Zr) and Shear Band Formation on the Tensile Properties and Fracture Behavior of Al-Mg-Sc-Zr Alloy

NASA Astrophysics Data System (ADS)

Huang, Hongfeng; Jiang, Feng; Zhou, Jiang; Wei, Lili; Qu, Jiping; Liu, Lele

2015-11-01

The mechanical properties and microstructures of Al-6Mg-0.25Sc-0.1Zr alloy (wt.%) during annealing were investigated by means of uniaxial tensile testing, optical microscope, scanning electron microscope, transmission electron microscope, and high-resolution transmission electron microscope. The results show that a large number of micro and grain-scale shear bands form in this alloy after cold rolling. As the tensile-loading force rises, strain softening would generate in shear bands, resulting in the occurrence of shear banding fracture in cold-rolled Al-Mg-Sc-Zr alloys. Recrystallization takes place preferentially in shear bands during annealing. Due to the formation of coarse-grain bands constructed by new subgrains, recrystallization softening tends to occur in these regions. During low-temperature annealing, recrystallization is inhibited by nano-scale Al3(Sc,Zr) precipitates which exert significant coherency strengthening and modulus hardening. However, the strengthening effect of Al3(Sc,Zr) decreases with the increasing of particle diameter at elevated annealing temperature. The mechanical properties of the recrystallized Al-Mg-Sc-Zr alloy decrease to a minimum level, and the fracture plane exhibits pure ductile fracture characteristics.

Small molecule ice recrystallization inhibitors mitigate red blood cell lysis during freezing, transient warming and thawing

PubMed Central

Briard, Jennie G.; Poisson, Jessica S.; Turner, Tracey R.; Capicciotti, Chantelle J.; Acker, Jason P.; Ben, Robert N.

2016-01-01

During cryopreservation, ice recrystallization is a major cause of cellular damage. Conventional cryoprotectants such as dimethyl sulfoxide (DMSO) and glycerol function by a number of different mechanisms but do not mitigate or control ice recrystallization at concentrations utilized in cryopreservation procedures. In North America, cryopreservation of human red blood cells (RBCs) utilizes high concentrations of glycerol. RBC units frozen under these conditions must be subjected to a time-consuming deglycerolization process after thawing in order to remove the glycerol to <1% prior to transfusion thus limiting the use of frozen RBC units in emergency situations. We have identified several low molecular mass ice recrystallization inhibitors (IRIs) that are effective cryoprotectants for human RBCs, resulting in 70–80% intact RBCs using only 15% glycerol and slow freezing rates. These compounds are capable of reducing the average ice crystal size of extracellular ice relative to a 15% glycerol control validating the positive correlation between a reduction in ice crystal size and increased post-thaw recovery of RBCs. The most potent IRI from this study is also capable of protecting frozen RBCs against the large temperature fluctuations associated with transient warming. PMID:27021850

Effect of storage conditions on the recrystallization of drugs in solid dispersions with crospovidone.

PubMed

Shibata, Yusuke; Fujii, Makiko; Suzuki, Ayako; Koizumi, Naoya; Kanada, Ken; Yamada, Masaki; Watanabe, Yoshiteru

2014-06-01

The physical stability of amorphous solid dispersions (SDs) is influenced by their storage conditions. The goal of this work was to investigate the factors affecting the recrystallization of drugs in SDs after storage under conditions of high temperature and high humidity. SDs of three drugs (dipyridamole, nifedipine and indomethacin) with different functional groups (amino, carbonyl and hydroxyl) and onset times for crystallization of the amorphous state were prepared using crospovidone (CrosPVP). All of the drugs in the SDs remained in an amorphous state at 25 °C/50% relative humidity (RH) in closed glass bottles for at least six months. Under conditions of high temperature (40 °C/75%RH/closed and 60 °C/open), differences in interactions between the hydrogen bond donors of the drugs and the amide carbonyl group of CrosPVP are essential factors for recrystallization of the drugs in the SDs. On the other hand, under condition of high humidity (40 °C/75%RH/open), in addition to the difference in the interaction between the drug and CrosPVP, the rate of increase in moisture content affects their recrystallization in SDs.

Reduced graphene oxide-induced recrystallization of NiS nanorods to nanosheets and the improved Na-storage properties.

PubMed

Pan, Qin; Xie, Jian; Zhu, Tiejun; Cao, Gaoshao; Zhao, Xinbing; Zhang, Shichao

2014-04-07

Preparation of two-dimensional (2D) graphene-like materials is currently an emerging field in materials science since the discovery of single-atom-thick graphene prepared by mechanical cleavage. In this work, we proposed a new method to prepare 2D NiS, where reduced graphene oxide (rGO) was found to induce the recrystallization of NiS from nanorods to nanosheets in a hydrothermal process. The process and mechanism of recrystallization have been clarified by various characterization techniques, including scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive X-ray spectroscopy (EDS) mapping, and X-ray photoelectron spectroscopy (XPS). The characterization of ex situ NiS/rGO products by SEM and EDS mapping indicates that the recrystallization of NiS from nanorods to nanosheets is realized actually through an exfoliation process, while the characterization of in situ NiS/rGO products by SEM, TEM, and EDS mapping reveals the exfoliation process. The XPS result demonstrates that hydrothermally assisted chemical bonding occurs between NiS and rGO, which induces the exfoliation of NiS nanorods into nanosheets. The obtained NiS/rGO composite shows promising Na-storage properties.

Small molecule ice recrystallization inhibitors mitigate red blood cell lysis during freezing, transient warming and thawing.

PubMed

Briard, Jennie G; Poisson, Jessica S; Turner, Tracey R; Capicciotti, Chantelle J; Acker, Jason P; Ben, Robert N

2016-03-29

During cryopreservation, ice recrystallization is a major cause of cellular damage. Conventional cryoprotectants such as dimethyl sulfoxide (DMSO) and glycerol function by a number of different mechanisms but do not mitigate or control ice recrystallization at concentrations utilized in cryopreservation procedures. In North America, cryopreservation of human red blood cells (RBCs) utilizes high concentrations of glycerol. RBC units frozen under these conditions must be subjected to a time-consuming deglycerolization process after thawing in order to remove the glycerol to <1% prior to transfusion thus limiting the use of frozen RBC units in emergency situations. We have identified several low molecular mass ice recrystallization inhibitors (IRIs) that are effective cryoprotectants for human RBCs, resulting in 70-80% intact RBCs using only 15% glycerol and slow freezing rates. These compounds are capable of reducing the average ice crystal size of extracellular ice relative to a 15% glycerol control validating the positive correlation between a reduction in ice crystal size and increased post-thaw recovery of RBCs. The most potent IRI from this study is also capable of protecting frozen RBCs against the large temperature fluctuations associated with transient warming.

Microstructural analysis of the thermal annealing of ice-Ih using EBSD

NASA Astrophysics Data System (ADS)

Hidas, Károly; Tommasi, Andréa; Mainprice, David; Chauve, Thomas; Barou, Fabrice; Montagnat, Maurine

2017-04-01

Rocks deformed in the middle crust and deeper in the Earth typically remain at high temperature for extended time spans after the cessation of deformation. This results in annealing of the deformation microstructure by a series of thermally activated, diffusion-based processes, namely: recovery and static recrystallization, which may also modify the crystal preferred orientation (CPO) or texture. Understanding the effects of annealing on the microstructure and CPO is therefore of utmost importance for the interpretation of the microstructures and for the estimation of the anisotropy of physical properties of lower crustal and mantle rocks. Ice-Ih -the typical form of water ice on the Earth's surface, with hexagonal crystal symmetry- deforms essentially by glide of dislocations on the basal plane [1], thus it has high viscoplastic anisotropy, which induces strong heterogeneity of stresses and strains at both the intra- and intergranular scales [2-3]. This behavior makes ice-Ih an excellent analog material for silicate minerals that compose the Earth. In situ observations of the evolution of the microstructures and CPO during annealing enable the study of the interplay between the various physical processes involved in annealing (recovery, nucleation, grain growth). They also allow the analysis of the impact of the preexisting deformation microstructures on the microstructural and CPO evolution during annealing. Here we studied the evolution of the microstructure of ice-Ih during static recrystallization by stepwise annealing experiments. We alternated thermal annealing and electron backscatter diffraction (EBSD) analyses on polycrystalline columnar ice-Ih pre-deformed in uniaxial compression at temperature of -7 °C to strains of 3.0-5.2. Annealing experiments were carried out at -5 °C and -2 °C up to a maximum of 3.25 days, typically in 5-6 steps. EBSD crystal orientation maps obtained after each annealing step permit the description of microstructural changes. Decrease in average intragranular misorientation at the sample scale and modification of the misorientation across subgrain boundaries provide evidence for recovery from the earliest stages of annealing. This evolution is similar for all studied samples irrespective of their initial strain or annealing temperature. After an incubation period up to 2 hours, recovery is accompanied by recrystallization (nucleation and grain boundary migration). Grain growth proceeds at the expense of domains with high intra-granular misorientations and its kinetics fits the parabolic growth law. Deformation-induced microstructures (tilt boundaries and kink bands) are stable features during early stages of static recrystallization and locally slow down grain boundary migration, pinning grain growth. REFERENCES 1. Duval, P., Ashby, M.F., Anderman, I., 1983. Rate-controlling processes in the creep of polycrystalline ice. Journal of Physical Chemistry 87, 4066-4074. 2. Grennerat, F., Montagnat, M., Castelnau, O., Vacher, P., Moulinec, H., Suquet, P., Duval, P., 2012. Experimental characterization of the intragranular strain field in columnar ice during transient creep. Acta Materialia 60, 3655-3666. 3. Chauve, T., Montagnat, M., Vacher, P., 2015. Strain field evolution during dynamic recrystallization nucleation: A case study on ice. Acta Materialia 101, 116-124. Funding: Research leading to these results was funded by the EU-FP7 Marie Curie postdoctoral grant PIEF-GA-2012-327226 to K.H.

Static Recovery Modeling of Dislocation Density in a Cold Rolled Clad Aluminum Alloy

NASA Astrophysics Data System (ADS)

Penlington, Alex

Clad alloys feature one or more different alloys bonded to the outside of a core alloy, with non-equilibrium, interalloy interfaces. There is limited understanding of the recovery and recrystallization behaviour of cold rolled clad aluminum alloys. In order to optimize the properties of such alloys, new heat treatment processes may be required that differ from what is used for the monolithic alloys. This study examines the recovery behaviour of a cold rolled Novelis Fusion(TM) alloy containing an AA6XXX core with an AA3003 cladding on one side. The bond between alloys appears microscopically discrete and continuous, but has a 30 microm wide chemical gradient. The as-deformed structure at the interalloy region consists of pancaked sub-grains with dislocations at the misorientation boundaries and a lower density organized within the more open interiors. X-ray line broadening was used to extract the dislocation density from the interalloy region and an equivalently deformed AA6XXX following static annealing using a modified Williamson-Hall analysis. This analysis assumed that Gaussian broadening contributions in a pseudo-Voigt function corresponded only to strain from dislocations. The kinetics of the dislocation density evolution to recrystallization were studied isothermally at 2 minute intervals, and isochronally at 175 and 205°C. The data fit the Nes model, in which the interalloy region recovered faster than AA6XXX at 175°C, but was slower at 205°C. This was most likely caused by change in texture and chemistry within this region such as over-aging of AA6XXX . Simulation of a continuous annealing and self homogenization process both with and without pre-recovery indicates a detectable, though small change in the texture and grain size in the interalloy region.

A re-evaluation of the mechanism of SIBM

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bate, P.; Hutchinson, B.

The process for creating a new recrystallized grain by the bulging out of an existing grain boundary within the deformed structure was recognized by Beck and Sperry and described as strain induced boundary migration, often now as SIBM. For many years SIBM seemed to be accorded less significance than the subgrain growth models for nucleation of recrystallization. However, the importance of SIBM is increasingly recognized, for example in the case of cube texture development in aluminum alloys. There is increasing evidence that high angle boundaries in deformed metals are not only residues of the prior grain structure but may alsomore » be generated by the deformation itself. These also participate in the nucleation of recrystallization on annealing and must do so by some form of SIBM mechanism.« less

Etude de la texture des rubans EPR de silicium polycristallin photovoltaïque

NASA Astrophysics Data System (ADS)

Chibani, A.; Gauthier, R.; Pinard, P.; Andonov, P.

1991-09-01

EPR polysilicon ribbons are obtained from a 5N-6N purity grade silicon powder melting followed by a recrystallization step. Being assigned to the photocell manufacture, we study the texture by X-ray diffraction method to reveal the majority of the crystal orientations and prove the eventual existence of specific orientations adapted to the best photovoltaic conversion efficiencies such as (100), (110) or (111). Moreover, we tested the possibility to induce the (111) orientation with a monocrystalline seed having this orientation. It appears that the crystal growth is essentially anisotropic and that only the orientation of the grains with their (331) planes parallel to the ribbon surface may be considered as dominant after the recrystallization step; finally, the (111) starting seed has an effect only at the recrystallization onset.

High-Temperature Tensile Behaviors of Base Metal and Electron Beam-Welded Joints of Ni-20Cr-9Mo-4Nb Superalloy

NASA Astrophysics Data System (ADS)

Gupta, R. K.; Anil Kumar, V.; Sukumaran, Arjun; Kumar, Vinod

2018-05-01

Electron beam welding of Ni-20Cr-9Mo-4Nb alloy sheets was carried out, and high-temperature tensile behaviors of base metal and weldments were studied. Tensile properties were evaluated at ambient temperature, at elevated temperatures of 625 °C to 1025 °C, and at strain rates of 0.1 to 0.001 s-1. Microstructure of the weld consisted of columnar dendritic structure and revealed epitaxial mode of solidification. Weld efficiency of 90 pct in terms of strength (UTS) was observed at ambient temperature and up to an elevated temperature of 850 °C. Reduction in strength continued with further increase of test temperature (up to 1025 °C); however, a significant improvement in pct elongation is found up to 775 °C, which was sustained even at higher test temperatures. The tensile behaviors of base metal and weldments were similar at the elevated temperatures at the respective strain rates. Strain hardening exponent `n' of the base metal and weldment was 0.519. Activation energy `Q' of base metal and EB weldments were 420 to 535 kJ mol-1 determined through isothermal tensile tests and 625 to 662 kJ mol-1 through jump-temperature tensile tests. Strain rate sensitivity `m' was low (< 0.119) for the base metal and (< 0.164) for the weldment. The δ phase was revealed in specimens annealed at 700 °C, whereas, twins and fully recrystallized grains were observed in specimens annealed at 1025 °C. Low-angle misorientation and strain localization in the welds and the HAZ during tensile testing at higher temperature and strain rates indicates subgrain formation and recrystallization. Higher elongation in the weldment (at Test temperature > 775 °C) is attributed to the presence of recrystallized grains. Up to 700 °C, the deformation is through slip, where strain hardening is predominant and effect of strain rate is minimal. Between 775 °C to 850 °C, strain hardening is counterbalanced by flow softening, where cavitation limits the deformation (predominantly at lower strain rate). Above 925 °C, flow softening is predominant resulting in a significant reduction in strength. Presence of precipitates/accumulated strain at high strain rate results in high strength, but when the precipitates were coarsened at lower strain rates or precipitates were dissolved at a higher temperature, the result was a reduction in strength. Further, the accumulated strain assisted in recrystallization, which also resulted in a reduction in strength.

Deformation in the hanging wall of Cretaceous HP rocks (Austroalpine Ötztal-Stubai Complex, European Eastern Alps): constraints on timing, conditions and kinematics

NASA Astrophysics Data System (ADS)

Habler, Gerlinde; Thöni, Martin; Grasemann, Bernhard; Sölva, Helmuth; Cotza, Gianluca

2010-05-01

The position and nature of the tectonic boundary between the Cretaceous eclogite facies metamorphic Texel Complex (Sölva et al. 2005, TC) and the Ötztal-Stubai Complex sensu stricto (OSC) with predominantly pre-Cretaceous tectonometamorphic imprint remained a matter of discussion (Fügenschuh et al. 2009). Sölva et al (2005) described the Cretaceous Schneeberg Normal Fault Zone (SNFZ) as the major tectonic boundary between the exhuming TC and the OSC, where the major portion of ductile deformation was partitioned into the rheologically weak Schneeberg/Monteneve Unit (SMU). In contrast, other authors proposed a model of a coherent vertical crustal section in the southern OSC (Schmid and Haas 1989), which was rotated and exhumed by erosion due to Oligocene large scale refolding (Fügenschuh et al. 2009). Here, new Rb-Sr data of muscovite and biotite from para- and orthogneisses from the Ferwalltal and Timmelsjoch areas (Austria/Italy) were correlated with mineral chemical and structural data in order to constrain the age and kinematics of the predominant deformational imprint in the OSC representing the hanging wall of the SNFZ. In the Ferwalltal the undisturbed OSC/SMU boundary is exposed. Above that boundary an amphibolite facies mylonitic foliation (Sc1) represented by the compositional layering of coarse grained Qtz, Bt and dynamically recrystallized Pl interferes with an overprinting mylonitic foliation (Sc2) with spatially heterogeneous intensity. Sc1-planes were syn-tectonically overgrown by euhedral Grt with single phase continuous prograde chemical zoning and Bt-porphyroblasts. Dc2 postdated garnet growth and caused the formation of SCC' fabrics in Bt-Pl gneisses. Still Qtz recrystallized dynamically, whereas Ms and Bt newly crystallized during Dc2. In the study area, the lithological boundaries in the OSC mainly are subparallel to the predominant foliation Sc1. These planes dip with 45-50° to the NW-NNW and show a WNW-plunging stretching lineation (LSc1) of dynamically recrystallized plagioclase and quartz. Shear kinematics of Dc1 alternate between Top to WNW or ESE. Sc2 foliation planes and the lithological-tectonic OSC/SMU boundary dip with intermediate angles towards N - NNW but also bear a W-plunging stretching lineation (LSc2). Dc2 structures consistently indicate W-directed shear kinematics. Due to the angular relationship of Sc1 and Sc2 the lithological boundaries of the OSC are truncated at the boundary with the SMU. Cretaceous Rb-Sr isochrons were obtained from Bt-granite-gneiss about 400m structurally above the OSC/SMU boundary. Fine-grained muscovite forming part of the major foliation Sc1 yielded a Rb-Sr Ms-WR age of 86.1 ± 0.9 Ma interpreted as a crystallization age constraining the timing of Dc1. The evidence of isotopic equilibration was supported by the homogeneous major element Ms composition. Rb-Sr Bt-WR data from the same material yielded 80.8±0.8 Ma interpreted to reflect cooling below c. 300°C. Several Rb-Sr Bt-WR data obtained from the Ferwalltal area gave age-results between 80.0 and 84.7 Ma and thus range among numerous Bt-WR Rb-Sr ages available from the wider study area (Thöni and Hoinkes 1987). Both deformation stages Dc1 and Dc2 predate this cooling period, as the Qtz-mica-fabrics demand significantly higher T-conditions. Subsequent deformation covers strongly partitioned brittle-ductile shear zones dipping with 50 - 60° to NW, as well as ultra-cataclasites bearing pseudotachylites, which reactivated Sc1- or Sc2 planes about 50 - 70 meters above the OSC/SMU boundary. Both brittle-ductile and brittle structures showed W-directed kinematics of normal faulting. The continuation of consistent shear kinematics to the brittle regime, as well as the extensive database of mica ages indicating cooling to below c. 300°C in the OSC adjacent to the SMU between 85 - 80 Ma (Thöni and Hoinkes 1987, with references) contradict a model of Oligocene ductile refolding. References: Fügenschuh B, Flöss D, Speckbacher R (2009) In Alpine Workshop Cogne. Schmid SM, Haas R (1989) Tectonics 8: 697-718. Sölva H, Grasemann B, Thöni M, Thiede RC, Habler G (2005) Tectonophysics 401: 143-166. Thöni M, Hoinkes G (1987) In Geodynamics of the Eastern Alps, pp. 200-213. Edited by Flügel HW and Faupl P. Vienna: Deuticke.

Textural and Rb-Sr isotopic evidence for late Paleozoic mylonitization within the Honey Hill fault zone southeastern Connecticut

DOE Office of Scientific and Technical Information (OSTI.GOV)

O'Hara, K.D.; Gromet, L.P.

A petrographic and Rb-Sr isotopic study of rocks within and near the Honey Hill fault zone places important constraints on its history of movement. Rb-Sr apparent ages for micas and plagioclase from these rocks have been reset and range from Permian to Triassic, considerably younger than the minimum stratigraphic age (Ordovician) of the rocks studied or of Acadian (Devonian) regional metamorphism. Permian Rb-Sr ages of dynamically recrystallized muscovite date the development of mylonite fabric. An older age is precluded by the excellent preservation of unrecovered quartz, which indicates that these rocks did not experience temperatures high enough to anneal quartzmore » or thermally reset Rb-Sr isotopic systems in muscovite since the time of mylonitization. Metamorphic mineral assemblages and mineral apparent ages in rocks north of the fault zone indicate recrystallization under similar upper greenschist-lower amphibolite grade conditions during Permian to Triassic time. Collectively these results indicate that the Honey Hill fault zone was active during the Late Paleozoic and that ductile deformation and metamorphism associated with the Alleghanian orogeny extend well into southern Connecticut. An Alleghanian age for mylonitization within the Honey Hill fault zone suggests it should be considered as a possible site for the major Late Paleozoic strike-slip displacements inferred from paleomagnetic studies for parts of coastal New England and maritime Canada.« less

Improving significantly the failure strain and work hardening response of LPSO-strengthened Mg-Y-Zn-Al alloy via hot extrusion speed control

NASA Astrophysics Data System (ADS)

Tan, Xinghe; Chee, Winston; Chan, Jimmy; Kwok, Richard; Gupta, Manoj

2017-07-01

The effect of hot extrusion speed on the microstructure and mechanical properties of MgY1.06Zn0.76Al0.42 (at%) alloy strengthened by the novel long-period stacking ordered (LPSO) phase was systematically investigated. Increase in the speed of extrusion accelerated dynamic recrystallization of α-Mg via particle-stimulated nucleation and grain growth in the alloy. The intensive recrystallization and grain growth events weakened the conventional basal texture and Hall-Petch strengthening in the alloy which led to significant improvement in its failure strain from 4.9% to 19.6%. The critical strengthening contribution from LPSO phase known for attributing high strength to the alloy was observed to be greatly undermined by the parallel competition from texture weakening and the adverse Hall-Petch effect when the alloy was extruded at higher speed. Absence of work hardening interestingly observed in the alloy extruded at lower speed was discussed in terms of its ultra-fine grained microstructure which promoted the condition of steady-state defect density in the alloy; where dislocation annihilation balances out the generation of new dislocations during plastic deformation. One approach to improve work hardening response of the alloy to prevent unstable deformation and abrupt failure in service is to increase the grain diameter in the alloy by judiciously increasing the extrusion speed.

Exploration of crystal simulation potential by fluconazole isomorphism and its application in improvement of pharmaceutical properties

NASA Astrophysics Data System (ADS)

Thakur, Amitha; Kumar, Dinesh; Thipparaboina, Rajesh; Shastri, Nalini R.

2014-11-01

Control of crystal morphology during crystallization is a paramount challenge in pharmaceutical processing. Hence, there is need to introduce computational methods for morphology prediction to manage production cost of drugs and improve related pharmaceutical and biopharmaceutical properties. Layer docking approach with molecular dynamics opens a new avenue for crystal habit prediction in presence of solvent. In the present study, attempts were made to correlate predicted and experimental crystal habits of fluconazole considering solvent interactions using layer docking approach. Simulated results from layer docking approach with methanol as solvent gave two dominant facets (0 1 1) and (1 0 1) with a surface area 22.43% and 19.82% respectively, which were in agreement with the experimental results. Experimentally grown modified crystal habit of fluconazole in methanol showed enhanced dissolution rate (p<0.05) when compared to plain drug. This was attributed to the increased surface area on the specified facets caused by interactions with the solvent. Furthermore, Differential Scanning Calorimetry, Fourier Transform Infrared (FTIR) Spectroscopy and powder X-ray Diffraction of recrystallized samples confirmed only a habit change and absence of any polymorphs, hydrates or solvates. Flow and compressibility of fluconazole recrystallized in methanol was significantly improved when compared to plain drug. This study demonstrates a methodical approach using computational tools for prediction and modification of crystal habit, to enhance dissolution of poorly soluble drugs, for future pharmaceutical applications.

The response of fabric variations to simple shear and migration recrystallization

DOE PAGES

Kennedy, Joseph H.; Pettit, Erin C.

2015-06-01

The observable microstructures in ice are the result of many dynamic and competing processes. These processes are influenced by climate variables in the firn. Layers deposited in different climate regimes may show variations in fabric which can persist deep into the ice sheet; fabric may 'remember' these past climate regimes. In this paper, we model the evolution of fabric variations below the firn–ice transition and show that the addition of shear to compressive-stress regimes preserves the modeled fabric variations longer than compression-only regimes, because shear drives a positive feedback between crystal rotation and deformation. Even without shear, the modeled icemore » retains memory of the fabric variation for ~200 ka in typical polar ice-sheet conditions. Our model shows that temperature affects how long the fabric variation is preserved, but only affects the strain-integrated fabric evolution profile when comparing results straddling the thermal-activation-energy threshold (~–10°C). Even at high temperatures, migration recrystallization does not eliminate the modeled fabric's memory under most conditions. High levels of nearest-neighbor interactions will, however, eliminate the modeled fabric's memory more quickly than low levels of nearest-neighbor interactions. Finally, our model predicts that fabrics will retain memory of past climatic variations when subject to a wide variety of conditions found in polar ice sheets.« less