Microstructure evolution and dynamic recrystallization behavior of a powder metallurgy Ti-22Al-25Nb alloy during hot compression

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

Jia, Jianbo

The flow behavior of a powder metallurgy (P/M) Ti-22Al-25Nb alloy during hot compression tests has been investigated at a strain rate of 0.01 s{sup −1} and a temperature range of 980–1100 °C up to various true strains from 0.1 to 0.9. The effects of deformation temperature and strain on microstructure characterization and nucleation mechanisms of dynamic recrystallization (DRX) were assessed by means of Optical microscope (OM), electron backscatter diffraction (EBSD) and transmission electron microscope (TEM) techniques, respectively. The results indicated that the process of DRX was promoted by increasing deformation temperature and strain. By regression analysis, a power exponent relationshipmore » between peak stresses and sizes of stable DRX grains was developed. In addition, it is suggested that the discontinuous dynamic recrystallization (DDRX) and continuous dynamic recrystallization (CDRX) controlled nucleation mechanisms for DRX grains operated simultaneously during the whole hot process, and which played the leading role varied with hot process parameters of temperature and strain. It was further demonstrated that the CDRX featured by progressive subgrain rotation was weakened by elevating deformation temperatures. - Highlights: •Flow behavior of a P/M Ti-22Al-25Nb is studied by hot compression tests. •Microstructure evolution of alloy is affected by deformation temperature and strain. •The relationship between peak stress and stable DRX grain size was developed. •The process of DRX was promoted by increasing deformation temperature and strain. •Nucleation mechanisms of DRX were identified by EBSD analysis and TEM observation.« less

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.

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.

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.

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.

Effect of the Rate of Hot Compressive Deformation on the Kinetics of Dynamic and Static Recrystallization of Novel Medium-Carbon Medium-Alloy Steel

NASA Astrophysics Data System (ADS)

Khlusova, E. I.; Zisman, A. A.; Knyazyuk, T. V.; Novoskol'tsev, N. N.

2018-03-01

Dynamic and static recrystallization occurring under hot deformation at a rate of 1 and 100 sec - 1 in high-strength medium-carbon wear-resistant steels developed at CRISM "Prometey" for die forming of parts of driven elements of tillage machines is studied. The critical strain of dynamic recrystallization and the threshold temperatures and times of finish of static recrystallization are determined for the studied deformation rates at various temperatures.

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.

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.

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.

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.

Effect of strain on evolution of dynamic recrystallization in Nb-1 wt%Zr-0.1 wt%C alloy at 1500 and 1600 °C

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

Behera, A.N.

Uniaxial compression tests were carried out on Nb-1 wt%Zr-0.1 wt%C alloy at temperature of 1500 and 1600 °C and strain rate of 0.1 s{sup −1} to study the evolution of dynamic recrystallization with strain. Electron back scatter diffraction was used to quantify the microstructural evolution. Nb-1Zr-0.1C alloy showed a necklace structure at a strain of 0.9 when deformed at 1500 °C and at strain of 0.6 when deformed at 1600 °C, both at strain rate of 0.1 s{sup −1}. This suggested the occurrence of dynamic recrystallization. At 1500 °C and strain of 0.9 the local average misorientation and the grainmore » orientation spread was low confirming the presence of dynamic recrystallization at this deformation condition. At both 1500 and 1600 °C and all measured strains the recrystallized grains had a strong fiber component of <001>. - Highlights: • Necklace formation of dynamically recrystallized grains occurred at strain of 0.6 and 0.9 for 1500 and 1600 °C, respectively. • Equiaxed microstructures were seen with increase in strain for both 1500 and 1600 °C. • At large strains the predominant recrystallized texture evolved to <001> pole.« less

Microstructural Characteristic of the Al-Fe-Cu Alloy During High-Speed Repetitive Continuous Extrusion Forming

NASA Astrophysics Data System (ADS)

Hu, Jiamin; Teng, Jie; Ji, Xiankun; Kong, Xiangxin; Jiang, Fulin; Zhang, Hui

2016-11-01

High-speed repetitive continuous extrusion forming process (R-Conform process) was performed on the Al-Fe-Cu alloy. The microstructural evolution and mechanical properties were studied by x-ray diffraction, electron backscatter diffraction, transmission electron microscopy and tensile testing. The results show that a significant improvement of tensile ductility concurs with a considerable loss of tensile strength before four passes, after that the process on mechanical properties variation tends to be steady, indicating an accelerated mechanical softening occurs when comparing to low-speed R-Conform process. Microstructure characterization indicates that the accumulated strain promotes the transformation of low angle boundaries to high angle boundaries, thus leading to the acceleration of continuous dynamic recrystallization process, and the precipitates are broken, spheroidized and homogeneously distribute in Al matrix as increasing R-Conform passes. Massive microshear bands are observed after initial passes of R-Conform process, which may promote continuous dynamic recrystallization and further grain refinement during high-speed R-Conform process.

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.

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).

Dynamic Recrystallization Behavior and Corrosion Resistance of a Dual-Phase Mg-Li Alloy

PubMed Central

Liu, Gang; Xie, Wen; Wei, Guobing; Yang, Yan; Liu, Junwei; Xu, Tiancai; Xie, Weidong; Peng, Xiaodong

2018-01-01

The hot deformation and dynamic recrystallization behavior of the dual-phase Mg-9Li-3Al-2Sr-2Y alloy had been investigated using a compression test. The typical dual-phase structure was observed, and average of grain size of as-homogenized alloy is about 110 µm. It mainly contains β-Li, α-Mg, Al4Sr and Al2Y phases. The dynamic recrystallization (DRX) kinetic was established based on an Avrami type equation. The onset of the DRX process occurred before the peak of the stress–strain flow curves. It shows that the DRX volume fraction increases with increasing deformation temperature or decreasing strain rate. The microstructure evolution during the hot compression at various temperatures and strain rates had been investigated. The DRX grain size became larger with the increasing testing temperature or decreasing strain rate because the higher temperature or lower strain rate can improve the migration of DRX grain boundaries. The fully recrystallized microstructure can be achieved in a small strain due to the dispersed island-shape α-Mg phases, continuous the Al4Sr phases and spheroidal Al2Y particles, which can accelerate the nucleation. The continuous Al4Sr phases along the grain boundaries are very helpful for enhancing the corrosion resistance of the duplex structured Mg-Li alloy, which can prevent the pitting corrosion and filiform corrosion. PMID:29522473

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

Dynamic Recrystallization Behavior and Corrosion Resistance of a Dual-Phase Mg-Li Alloy.

PubMed

Liu, Gang; Xie, Wen; Wei, Guobing; Yang, Yan; Liu, Junwei; Xu, Tiancai; Xie, Weidong; Peng, Xiaodong

2018-03-09

The hot deformation and dynamic recrystallization behavior of the dual-phase Mg-9Li-3Al-2Sr-2Y alloy had been investigated using a compression test. The typical dual-phase structure was observed, and average of grain size of as-homogenized alloy is about 110 µm. It mainly contains β-Li, α-Mg, Al₄Sr and Al₂Y phases. The dynamic recrystallization (DRX) kinetic was established based on an Avrami type equation. The onset of the DRX process occurred before the peak of the stress-strain flow curves. It shows that the DRX volume fraction increases with increasing deformation temperature or decreasing strain rate. The microstructure evolution during the hot compression at various temperatures and strain rates had been investigated. The DRX grain size became larger with the increasing testing temperature or decreasing strain rate because the higher temperature or lower strain rate can improve the migration of DRX grain boundaries. The fully recrystallized microstructure can be achieved in a small strain due to the dispersed island-shape α-Mg phases, continuous the Al₄Sr phases and spheroidal Al₂Y particles, which can accelerate the nucleation. The continuous Al₄Sr phases along the grain boundaries are very helpful for enhancing the corrosion resistance of the duplex structured Mg-Li alloy, which can prevent the pitting corrosion and filiform corrosion.

Dynamic recrystallization behavior of an as-cast TiAl alloy during hot compression

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

Li, Jianbo, E-mail: lijianbo1205@163.com; Liu, Yong, E-mail: yonliu@csu.edu.cn; Wang, Yan, E-mail: wangyan@csu.edu.cn

2014-11-15

High temperature compressive deformation behaviors of as-cast Ti–43Al–4Nb–1.4W–0.6B alloy were investigated at temperatures ranging from 1050 °C to 1200 °C, and strain rates from 0.001 s{sup −1} to 1 s{sup −1}. Electron back scattered diffraction technique, scanning electron microscopy and transmission electron microscopy were employed to investigate the microstructural evolutions and nucleation mechanisms of the dynamic recrystallization. The results indicated that the true stress–true strain curves show a dynamic flow softening behavior. The dependence of the peak stress on the deformation temperature and the strain rate can well be expressed by a hyperbolic-sine type equation. The activation energy decreases withmore » increasing the strain. The size of the dynamically recrystallized β grains decreases with increasing the value of the Zener–Hollomon parameter (Z). When the flow stress reaches a steady state, the size of β grains almost remains constant with increasing the deformation strain. The continuous dynamic recrystallization plays a dominant role in the deformation. In order to characterize the evolution of dynamic recrystallization volume fraction, the dynamic recrystallization kinetics was studied by Avrami-type equation. Besides, the role of β phase and the softening mechanism during the hot deformation was also discussed in details. - Highlights: • The size of DRXed β grains decreases with increasing the value of the Z. • The CDRX plays a dominant role in the deformation. • The broken TiB{sub 2} particles can promote the nucleation of DRX.« 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.

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.

Dynamic recrystallization behavior of a biomedical Ti-13Nb-13Zr alloy.

PubMed

Bobbili, Ravindranadh; Madhu, V

2016-06-01

The dynamic recrystallization (DRX) behavior of a biomedical titanium Ti-13Nb-13Zr alloy has been investigated using the high temperature compression tests under wide range of strain rates (0.001-1/s) and temperatures 900-1050°C. A constitutive equation represented as a function of temperature, strain rate and true strain is developed and the hot deformation apparent activation energy is calculated about 534kJ/mol. By considering the exponential relationship between work-hardening rate (θ) and stress, a new mathematical model was proposed for predicting flow stress up to the critical strain during hot deformation. The mathematical model for predicting flow stress up to the critical strain exhibits better consistency and accuracy. The DRX kinetic equation of Ti-13Nb-13Zr alloy is described as XDRX=1-exp[-0.32(Ɛ-ƐcƐ(*))(2.3)] . The DRX kinetic model was validated by microstructure observation. It was also found that the process of DRX was promoted by decreasing strain rate and increasing deformation temperature. Eventually, the continuous dynamic recrystallization (CDRX) was identified to be the DRX mechanism using transmission electron microscope (TEM). Copyright © 2015 Elsevier Ltd. All rights reserved.

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

Dynamic Recrystallization of the Constituent γ Phase and Mechanical Properties of Ti-43Al-9V-0.2Y Alloy Sheet.

PubMed

Zhang, Yu; Wang, Xiaopeng; Kong, Fantao; Chen, Yuyong

2017-09-15

A crack-free Ti-43Al-9V-0.2Y alloy sheet was successfully fabricated via hot-pack rolling at 1200 °C. After hot-rolling, the β/γ lamellar microstructure of the as-forged TiAl alloy was completely converted into a homogeneous duplex microstructure with an average γ grain size of 10.5 μm. The dynamic recrystallization (DRX) of the γ phase was systematically investigated. A recrystallization fraction of 62.5% was obtained for the γ phase in the TiAl alloy sheet, when a threshold value of 0.8° was applied to the distribution of grain orientation spread (GOS) values. The high strain rate and high stress associated with hot-rolling are conducive for discontinuous dynamic recrystallization (DDRX) and continuous dynamic recrystallization (CDRX), respectively. A certain high-angle boundary (HAGB: θ = 89° ± 3°<100>), which is associated with DDRX, occurs in both the recrystallized and deformed γ grains. The twin boundaries play an important role in the DDRX of the γ phase. Additionally, the sub-structures and sub-boundaries originating from low-angle boundaries in the deformed grains also indicate that CDRX occurs. The mechanical properties of the alloy sheet were determined at both room and elevated temperatures. At 750 °C, the alloy sheet exhibited excellent elongation (53%), corresponding to a failure strength of 467 MPa.

Deformation Characteristics and Recrystallization Response of a 9310 Steel Alloy

NASA Astrophysics Data System (ADS)

Snyder, David; Chen, Edward Y.; Chen, Charlie C.; Tin, Sammy

2013-01-01

The flow behavior and recrystallization response of a 9310 steel alloy deformed in the ferrite temperature range were studied in this work. Samples were compressed under various conditions of strain (0.6, 0.8 and multi-axial), strain rate (10-4 seconds-1 to 10-1 seconds-1) and temperature [811 K to 1033 K (538 °C to 760 °C)] using a Gleeble thermo-mechanical simulator. Deformation was characterized by both qualitative and quantitative means, using standard microscopy, electron backscatter diffraction (EBSD) analysis and flow stress modeling. The results indicate that deformation is primarily accommodated through dynamic recovery in sub-grain formation. EBSD analysis shows a continuous increase in sub-grain boundary misorientation with increasing strain, ultimately producing recrystallized grains from the sub-grains at high strains. This suggests that a sub-grain rotation recrystallization mechanism predominates in this temperature range. Analyses of the results reveal a decreasing mean dynamically recrystallized grain size with increasing Zener-Hollomon parameter, and an increasing recrystallized fraction with increasing strain.

Microstructural Evolution and Dynamic Softening Mechanisms of Al-Zn-Mg-Cu Alloy during Hot Compressive Deformation

PubMed Central

Shi, Cangji; Lai, Jing; Chen, X.-Grant

2014-01-01

The hot deformation behavior and microstructural evolution of an Al-Zn-Mg-Cu (7150) alloy was studied during hot compression at various temperatures (300 to 450 °C) and strain rates (0.001 to 10 s−1). A decline ratio map of flow stresses was proposed and divided into five deformation domains, in which the flow stress behavior was correlated with different microstructures and dynamic softening mechanisms. The results reveal that the dynamic recovery is the sole softening mechanism at temperatures of 300 to 400 °C with various strain rates and at temperatures of 400 to 450 °C with strain rates between 1 and 10 s−1. The level of dynamic recovery increases with increasing temperature and with decreasing strain rate. At the high deformation temperature of 450 °C with strain rates of 0.001 to 0.1 s−1, a partially recrystallized microstructure was observed, and the dynamic recrystallization (DRX) provided an alternative softening mechanism. Two kinds of DRX might operate at the high temperature, in which discontinuous dynamic recrystallization was involved at higher strain rates and continuous dynamic recrystallization was implied at lower strain rates. PMID:28788454

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).

Dynamic Recrystallization of the Constituent γ Phase and Mechanical Properties of Ti-43Al-9V-0.2Y Alloy Sheet

PubMed Central

Zhang, Yu; Wang, Xiaopeng; Kong, Fantao

2017-01-01

A crack-free Ti-43Al-9V-0.2Y alloy sheet was successfully fabricated via hot-pack rolling at 1200 °C. After hot-rolling, the β/γ lamellar microstructure of the as-forged TiAl alloy was completely converted into a homogeneous duplex microstructure with an average γ grain size of 10.5 μm. The dynamic recrystallization (DRX) of the γ phase was systematically investigated. A recrystallization fraction of 62.5% was obtained for the γ phase in the TiAl alloy sheet, when a threshold value of 0.8° was applied to the distribution of grain orientation spread (GOS) values. The high strain rate and high stress associated with hot-rolling are conducive for discontinuous dynamic recrystallization (DDRX) and continuous dynamic recrystallization (CDRX), respectively. A certain high-angle boundary (HAGB: θ = 89° ± 3°<100>), which is associated with DDRX, occurs in both the recrystallized and deformed γ grains. The twin boundaries play an important role in the DDRX of the γ phase. Additionally, the sub-structures and sub-boundaries originating from low-angle boundaries in the deformed grains also indicate that CDRX occurs. The mechanical properties of the alloy sheet were determined at both room and elevated temperatures. At 750 °C, the alloy sheet exhibited excellent elongation (53%), corresponding to a failure strength of 467 MPa. PMID:28914797

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.

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.

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).

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.

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.

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.

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

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.

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.

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

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

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.

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.

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%.

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.

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.

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.

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).

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.

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

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.

Constitutive modeling and dynamic softening mechanism during hot deformation of an ultra-pure 17%Cr ferritic stainless steel stabilized with Nb

NASA Astrophysics Data System (ADS)

Gao, Fei; Liu, Zhenyu; Misra, R. D. K.; Liu, Haitao; Yu, Fuxiao

2014-09-01

The hot deformation behavior of an ultra-pure 17%Cr ferritic stainless steel was studied in the temperature range of 750-1000 °C and strain rates of 0.5 to 10 s-1 using isothermal hot compression tests in a thermomechanical simulator. The microstructural evolution was investigated using electron backscattered diffraction and transmission electron microscopy. A modified constitutive equation considering the effect of strain on material constant was developed, which predicted the flow stress for the deformation conditions studied, except at 950 °C in 1 s-1 and 900 °C in 10 s-1. Decreasing deformation temperature and increasing strain was beneficial in refining the microstructure. Decreasing deformation temperature, the in-grain shear bands appeared in the microstructure. It is suggested that the dynamic softening mechanism is closely related to deformation temperature. At low deformation temperature, dynamic recovery was major softening mechanism and no dynamic recrystallization occurred. At high deformation temperature, dynamic softening was explained in terms of efficient dynamic recovery and limited continuous dynamic recrystallization. A drop in the flow stress was not found due to very small fraction of new grains nucleated during dynamic recrystallization.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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%.

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.

Ferrite grain refinement in low carbon Cu–P–Cr–Ni–Mo weathering steel at various temperatures in the (α + γ) region

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

Zhang, Chunling, E-mail: zhangchl@ysu.edu.cn; School of Materials Science and Engineering, Hebei University of Technology, Tianjin 300401; Zhang, Mengmeng

2016-03-15

Self-designed Cu–P–Cr–Ni–Mo weathering steel was subjected to compression test to determine the mechanism of ferrite grain refinement from 750 °C to 925 °C. Optical microscopic images showed that ferrite grain size declined, whereas the ferrite volume fraction increased with increasing compression temperature. Electron backscatter diffraction patterns revealed that several low-angle boundaries shifted to high-angle boundaries, thereby generating fine ferrite grains surrounded by high-angle boundaries. Numerous low-angle boundaries were observed within ferrite grains at 750 °C, which indicated the existence of pre-eutectoid ferrite. Results showed that ferrite grain refinement could be due to continuous dynamic recrystallization at 750 °C and 775more » °C, and deformation-induced ferrite transformation could be the main mechanism at 800 °C and 850 °C. Fine equiaxed ferrite grains with size ranging from 1.77 μm to 2.69 μm were produced in the (α + γ) dual-phase region. - Graphical abstract: There is a close relationship between the microstructure evolution and flow curves during deformation. Fine equiaxed ferrite grains with size ranging from 1.77 μm to 2.69 μm were achieved in the (α + γ) dual-phase region. Ferrite grain refinement could be due to continuous dynamic recrystallization at 750 °C and 775 °C, and deformation-induced ferrite transformation at 800 °C and 850 °C. The occurrence of deformation-induced ferrite transformation and continuous dynamic recrystallization can be monitored by analysis of flow curves and microstructures. Deformation-induced ferrite transformation leads to the dynamic softening in flow curve when temperature just below A{sub r3}, while the dynamic softening in flow curve is ferrite continuous dynamic recrystallization (Special Fig. 5b). - Highlights: • Compression deformation was operated at temperatures from 750 °C to 925 °C at a strain rate of 0.1 s–1, and a strain of 1.2. • Fine equiaxed ferrite grains of ~1.77–2.19 μm were obtained at 750 °C and 775 °C via continuous dynamic recrystallization. • Ferrite grain size of ~2.31–2.69 μm at 800 °C and 850 °C can be obtained by deformation-induced ferrite transformation. • With decreasing deformation temperature the average grain size of ferrite decreased while volume fraction increased. • Ferrite refinement was from deformation-induced ferrite to continuous dynamic recrystallization as temperature reduced.« less

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.

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.

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).

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

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.

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.

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

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.

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

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 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.

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

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.

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

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

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.

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.

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.

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.

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.

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.

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.

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

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.

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.

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.

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.

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.

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

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.

[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.

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

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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

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.

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

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.

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

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

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.

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.

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.

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.

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.

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

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.

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

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.

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.

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.

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.

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

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.

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.

Research and development of low cost processes for integrated solar arrays. Final report, April 15, 1974--January 14, 1976

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

Graham, C.D.; Kulkarni, S.; Louis, E.

1976-05-01

Results of a program to study process routes leading to a low cost large area integrated silicon solar array manufacture for terrestrial applications are reported. Potential processes for the production of solar-grade silicon are evaluated from thermodynamic, economic, and technical feasibility points of view. Upgrading of the present arc-furnace process is found most favorable. Experimental studies of the Si/SiF/sub 4/ transport and purification process show considerable impurity removal and reasonable transport rates. Silicon deformation experiments indicate production of silicon sheet by rolling at 1350/sup 0/C is feasible. Significant recrystallization by strain-anneal technique has been observed. Experimental recrystallization studies using anmore » electron beam line source are discussed. A maximum recrystallization velocity of approximately 9 m/hr is calculated for silicon sheet. A comparative process rating technique based on detailed cost analysis is presented.« less

Hurst exponent used as a tool to differentiate between magmatic and fluid-induced processes as reflected in crystal geochemistry

NASA Astrophysics Data System (ADS)

Domonik, A.; Słaby, E.; Śmigielski, M.

2012-04-01

A self-similarity parameter, the Hurst exponent (H) (called also roughness exponent) has been used to show the long-range dependence of element behaviour during the processes. The H value ranges between 0 and 1; a value of 0.5 indicates a random distribution indistinguishable from noise. For values greater or less than 0.5, the system shows non-linear dynamics. H < 0.5 represents anti-persistent (more chaotic) behaviour, whereas H > 0.5 corresponds to increasing persistence (less chaotic). Such persistence is characterized as an effect of a long-term memory, and thus by a large degree of positive correlation. In theory, the preceding data constantly affect the next in the whole temporal series. Applied to chaotic dynamics, the system shows a subtle sensitivity to initial conditions. The process can show some degree of chaos, due to local variations, but generally, the trend preserves its persistent character through time. If the exponent value is low, the process shows frequent and sudden reversals e.g. the trends of such a process show mutual negative correlation of the succeding values in the data series. Thus, the system can be described as having a high degree of deterministic chaos. Alkali feldspar megacrysts grown from mixed magmas and recrystallized due to interaction with fluids have been selected for the study (Słaby et al., 2011). Hurst exponent variability has been calculated within some primary-magmatic and secondary-recrystallized crystal domains for some elements redistributed by crystal fluid interaction. Based on the Hurst exponent value two different processes can easily be recognized. In the core of the megacrysts the element distribution can be ascribed to magmatic growth. By contrast, the marginal zones can relate to inferred late crystal-fluid interactions. Both processes are deterministic, not random. The spatial distribution of elements in the crystal margins is irregular, with high-H values identifying the process as persistent. The trace element distributions in feldspar cores are almost homogeneous and only relatively small and irregular variations in trace element contents makes their growth morphology slightly patchy. Despite homogenization the fractal statistics reveal that trace elements were incorporated chaotically into the growing crystal. The anti-persistent chaotic behaviour of elements during magmatic growth of the feldspars progressively changes into persistent behaviour within domains, where re-crystallization reaction took place. Elements demonstrate variable dynamics of this exchange corresponding to increasing persistency. This dynamics is different for individual elements compared to analogical, observed for crystallization process proceeding from mixed magmas. Consequently, it appears that fractal statistics clearly discriminate between two different processes, with contrasted element behaviour during these processes. One process is magma crystallization and it is recorded in the core of the megacrysts; the second is recorded in the crystal rims and along cleavages and cracks, such that it can be related to a post-crystallization process linked to fluid percolation. Słaby, E., Martin, H., Hamada, M., Śmigielski, M., Domonik, A., Götze, J., Hoefs, J., Hałas, S., Simon, K., Devidal, J-L., Moyen, J-F., Jayananda, M. (2011) Evidence in Archaean alkali-feldspar megacrysts for high-temperature interaction with mantle fluids. Journal of Petrology (on line). doi:10.1093/petrology/egr056

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.

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.

[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.

Development of Ti microalloyed high strength steel plate by controlling thermo-mechanical control process schedule

NASA Astrophysics Data System (ADS)

Xia, Jinian; Huo, Xiangdong; Li, Liejun; Peng, Zhengwu; Chen, Songjun

2017-12-01

In this study, the TMCP parameters including non-recrystallization temperature (Tnr) and optimal isothermal temperature were determined by thermal simulation experiments, and a new Ti microalloyed high strength steel plate was developed by controlling thermo-mechanical control process (TMCP) schedule. The effects of TMCP process on microstructural features, precipitation behavior and mechanical properties of Ti microalloyed high strength steel plate were investigated. The results revealed that the double-stage rolling process consist of rolling in the γ recrystallization region and the γ non-recrystallization region was benefical to promoting the mechanical properties of Ti microalloyed steel by achieving grain refinement. It was also found that large amounts of fine TiC (<10 nm) particles were precipitated during the isothermal treatment at 600 °C, which generated a 215 MPa precipitation strengthening effect.

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.

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.

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

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.

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.

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

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

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.

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.

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.

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.

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

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.

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.

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

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.

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.

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].

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.

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.

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.

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 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.

Characterization of Hot Deformation Behavior of a Fe-Cr-Ni-Mo-N Superaustenitic Stainless Steel Using Dynamic Materials Modeling

NASA Astrophysics Data System (ADS)

Pu, Enxiang; Zheng, Wenjie; Song, Zhigang; Feng, Han; Zhu, Yuliang

2017-03-01

Hot deformation behavior of a Fe-24Cr-22Ni-7Mo-0.5N superaustenitic stainless steel was investigated by hot compression tests in a wide temperature range of 950-1250 °C and strain rate range of 0.001-10 s-1. The flow curves show that the flow stress decreases as the deformation temperature increases or the strain rate decreases. The processing maps developed on the basis of the dynamic materials model and flow stress data were adopted to optimize the parameters of hot working. It was found that the strain higher than 0.2 has no significant effect on the processing maps. The optimum processing conditions were in the temperature range of 1125-1220 °C and strain rate range of 0.1-3 s-1. Comparing to other stable domains, microstructural observations in this domain revealed the complete dynamic recrystallization (DRX) with finer and more uniform grain size. Flow instability occurred in the domain of temperature lower than 1100 °C and strain rate higher than 0.1 s-1.

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.

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

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.

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.

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.

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.

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.

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.

Hybrid C-nanotubes/Si 3D nanostructures by one-step growth in a dual-plasma reactor

NASA Astrophysics Data System (ADS)

Toschi, Francesco; Orlanducci, Silvia; Guglielmotti, Valeria; Cianchetta, Ilaria; Magni, Corrado; Terranova, Maria Letizia; Pasquali, Matteo; Tamburri, Emanuela; Matassa, Roberto; Rossi, Marco

2012-06-01

Hybrid nanostructures consisting of Si polycrystalline nanocones, with an anemone-like termination coated with C-nanotubes bundles, have been generated on a (1 0 0) Si substrate in a dual mode microwave/radio-frequency plasma reactor. The substrate is both heated and bombarded by energetic H ions during the synthesis process. The nanocones growth is explained considering pull of the growing Si nanocrystalline phase along the lines of the electrical field, likely via a molten/recrystallization mechanism. The one-step building of the achieved complex 3D architectures is described in terms of dynamic competition between Si and C nanotubes growth under the peculiar conditions of kinetically driven processes.

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

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.

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.

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.

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.

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.

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.

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.

Role of Y-Al Oxides During Extended Recovery Process of a Ferritic ODS Alloy

NASA Astrophysics Data System (ADS)

Capdevila, C.; Pimentel, G.; Aranda, M. M.; Rementeria, R.; Dawson, K.; Urones-Garrote, E.; Tatlock, G. J.; Miller, M. K.

2015-08-01

The microstructural stability of Y-Al oxides during the recrystallization of Fe-Cr-Al oxide dispersion strengthened alloy is studied in this work. The goal is to determine the specific distribution pattern of oxides depending where they are located: in the matrix or at the grain boundaries. It was concluded that those located at the grain boundaries yielded a faster coarsening than the ones in the matrix, although no significant differences in composition and/or crystal structure were observed. However, the recrystallization heat treatment leads to the dissolution of the Y2O3 and its combination with Al to form the YAlO3 perovskite oxide particles process, mainly located at the grain boundaries. Finally, atom probe tomography analysis revealed a significant Ti build-up at the grain boundaries that might affect subsequent migration during recrystallization.

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

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.

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

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.

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.

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.

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.

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.

Analysis of soft magnetic materials by electron backscatter diffraction as a powerful tool

NASA Astrophysics Data System (ADS)

Schuller, David; Hohs, Dominic; Loeffler, Ralf; Bernthaler, Timo; Goll, Dagmar; Schneider, Gerhard

2018-04-01

The current work demonstrates that electron backscatter diffraction (EBSD) is a powerful and versatile characterization technique for investigating soft magnetic materials. The properties of soft magnets, e.g., magnetic losses strongly depend on the materials chemical composition and microstructure, including grain size and shape, texture, degree of plastic deformation and elastic strain. In electrical sheet stacks for e-motor applications, the quality of the machined edges/surfaces of each individual sheet is of special interest. Using EBSD, the influence of the punching process on the microstructure at the cutting edge is quantitatively assessed by evaluating the crystallographic misorientation distribution of the deformed grains. Using an industrial punching process, the maximum affected deformation depth is determined to be 200 - 300 μm. In the case of laser cutting, the affected deformation depth is determined to be approximately zero. Reliability and detection limits of the developed EBSD approach are evaluated on non-affected sample regions and model samples containing different indentation test bodies. A second application case is the investigation of the recrystallization process during the annealing step of soft magnetic composites (SMC) toroids produced by powder metallurgy as a function of compaction pressure, annealing parameters and powder particle size. With increasing pressure and temperature, the recrystallized area fraction (e.g., grains with crystallographic misorientations < 3°) increases from 71 % (200 MPa, 800°C) to 90% (800 MPa, 800°C). Recrystallization of the compacted powder material starts at the particle boundaries or areas with existing plastic deformation. The progress of recrystallization is visualized as a function of time and of different particle to grain size distributions. Here, large particles with coarse internal grain structures show a favorable recrystallization behavior which results in large bulk permeability of up to 600 - 700 and lower amount of residual misorientations (>3°).

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

Effects of asymmetric rolling process on ridging resistance of ultra-purified 17%Cr ferritic stainless steel

NASA Astrophysics Data System (ADS)

Lu, Cheng-zhuang; Li, Jing-yuan; Fang, Zhi

2018-02-01

In ferritic stainless steels, a significant non-uniform recrystallization orientation and a substantial texture gradient usually occur, which can degrade the ridging resistance of the final sheets. To improve the homogeneity of the recrystallization orientation and reduce the texture gradient in ultra-purified 17%Cr ferritic stainless steel, in this work, we performed conventional and asymmetric rolling processes and conducted macro and micro-texture analyses to investigate texture evolution under different cold-rolling conditions. In the conventional rolling specimens, we observed that the deformation was not uniform in the thickness direction, whereas there was homogeneous shear deformation in the asymmetric rolling specimens as well as the formation of uniform recrystallized grains and random orientation grains in the final annealing sheets. As such, the ridging resistance of the final sheets was significantly improved by employing the asymmetric rolling process. This result indicates with certainty that the texture gradient and orientation inhomogeneity can be attributed to non-uniform deformation, whereas the uniform orientation gradient in the thickness direction is explained by the increased number of shear bands obtained in the asymmetric rolling process.

Low-temperature volume radiation annealing of cold-worked bands of Al-Li-Cu-Mg alloy by 20-40 keV Ar+ ion

NASA Astrophysics Data System (ADS)

Ovchinnikov, V. V.; Gushchina, N. V.; Mozharovsky, S. M.; Kaigorodova, L. I.

2017-01-01

The processes of radiation-dynamic nature (in contrast to the thermally-activated processes) in the course of short-term irradiation of 1 mm thick bands of cold-worked aluminum alloy 1441 (of system Al-Li-Cu-Mg) with Ar+ 20-40 keV were studied. An effect of in-the-bulk (throughout the whole of metal bands thickness) low-temperature radiation annealing of the named alloy, multiply accelerated as compared with common thermal annealing processes was registered (with projected ranges of ions of considered energies definitely not exceeding 0.1 μm). The processes of recrystallization and intermetallic structure changes (occurring within a few seconds of Ar+ irradiation) have the common features as well as the differences in comparison with the results of two hour standard thermal annealing.

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.

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.

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.

Role of Y-Al oxides during extended recovery process of a ferritic ODS alloy

DOE PAGES

Capdevila, C.; Pimentel, G.; Aranda, M. M.; ...

2015-08-04

The microstructural stability of Y-Al oxides during the recrystallization of Fe-Cr-Al oxide dispersion strengthened alloy is studied in this work. The goal is to determine the specific distribution pattern of oxides depending where they are located: in the matrix or at the grain boundaries. It was concluded that those located at the grain boundaries yielded a faster coarsening than the ones in the matrix, although no significant differences in composition and/or crystal structure were observed. However, the recrystallization heat treatment leads to the dissolution of the Y 2O 3 and its combination with Al to form the YAlO 3 perovskitemore » oxide particles process, mainly located at the grain boundaries. Lastly, atom probe tomography analysis revealed a significant Ti build-up at the grain boundaries that might affect subsequent migration during recrystallization.« less

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.

Synthesis and electrochemical properties of NiO nanospindles

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

Zhou, Hai; University of Chinese Academy of Sciences, Beijing 100049; Lv, Baoliang, E-mail: lbl604@sxicc.ac.cn

2014-02-01

Graphical abstract: NiO nanospindles with a different electrochemical activity as compared to those previous reports were synthesized via an agglomeration–dissolution–recrystallization growth process without the addition of any surfactant. - Highlights: • NiO nanospindles were synthesized without the addition of any surfactant. • The agglomeration–dissolution–recrystallization growth process was used to explain the precursors’ formation process of the spindle-like NiO. • As-obtained spindle-like NiO showed a different electrochemical activity as compared to those previous reports. - Abstract: NiO nanospindles were successfully synthesized via a hydrothermal and post-treatment method. The as-synthesized nanospindles were about several hundred nanometers in width and about one micrometermore » in length. X-ray diffraction (XRD) analysis revealed that the spindle-like structure was cubic NiO phase crystalline. Scanning electron microscopy (SEM) and high-resolution transmission electron microscopy (HRTEM) analysis indicated that these NiO nanospindles were of single crystal nature. On the basis of time-dependent experiments, a possible agglomeration–dissolution–recrystallization growth process was proposed to explain the formation process of the spindle-like precursors. The cyclic voltammetry (CV) measurement showed that the as-prepared spindle-like NiO exhibited a pseudo-capacitance behavior.« less

Materials processing apparatus development for fluoride glass

NASA Technical Reports Server (NTRS)

Smith, Guy A.; Kosten, Sue; Workman, Gary L.

1994-01-01

Fluoride glasses have great potential for optical fiber communications due to the high transmittance when no microcrystallites occur during drawing operations. This work has developed apparatus to test the occurrence of microcrystallites during recrystallization in reduced gravity on the KC-135. The apparatus allows fluoride glass fiber, such as ZBLAN, to be melted and recrystallized during both the low and high g portions the parabolic flight.

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.

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.

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.

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.

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

Complete grain boundaries from incomplete EBSD maps: the influence of segmentation on grain size determinations

NASA Astrophysics Data System (ADS)

Heilbronner, Renée; Kilian, Ruediger

2017-04-01

Grain size analyses are carried out for a number of reasons, for example, the dynamically recrystallized grain size of quartz is used to assess the flow stresses during deformation. Typically a thin section or polished surface is used. If the expected grain size is large enough (10 µm or larger), the images can be obtained on a light microscope, if the grain size is smaller, the SEM is used. The grain boundaries are traced (the process is called segmentation and can be done manually or via image processing) and the size of the cross sectional areas (segments) is determined. From the resulting size distributions, 'the grain size' or 'average grain size', usually a mean diameter or similar, is derived. When carrying out such grain size analyses, a number of aspects are critical for the reproducibility of the result: the resolution of the imaging equipment (light microscope or SEM), the type of images that are used for segmentation (cross polarized, partial or full orientation images, CIP versus EBSD), the segmentation procedure (algorithm) itself, the quality of the segmentation and the mathematical definition and calculation of 'the average grain size'. The quality of the segmentation depends very strongly on the criteria that are used for identifying grain boundaries (for example, angles of misorientation versus shape considerations), on pre- and post-processing (filtering) and on the quality of the recorded images (most notably on the indexing ratio). In this contribution, we consider experimentally deformed Black Hills quartzite with dynamically re-crystallized grain sizes in the range of 2 - 15 µm. We compare two basic methods of segmentations of EBSD maps (orientation based versus shape based) and explore how the choice of methods influences the result of the grain size analysis. We also compare different measures for grain size (mean versus mode versus RMS, and 2D versus 3D) in order to determine which of the definitions of 'average grain size yields the most stable results.

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.

Texture evolution during thermomechanical processing in rare earth free magnesium alloys

NASA Astrophysics Data System (ADS)

Miller, Victoria Mayne

The use of wrought magnesium alloys is highly desirable for a wide range of applications where low component weight is desirable due to the high specific strength and stiffness the alloys can achieve. However, the implementation of wrought magnesium has been hindered by the limited room temperature formability which typically results from deformation processing. This work identifies opportunities for texture modification during thermomechanical processing of conventional (rare earth free) magnesium alloys via a combination of experimental investigation and polycrystal plasticity simulations. During deformation, it is observed that a homogeneous distribution of coarse intermetallic particles efficiently weakens deformation texture at all strain levels, while a highly inhomogeneous particle distribution is only effective at high strains. The particle deformation effects are complemented by the addition of alkaline earth solute, which modifies the relative deformation mode activity. During recrystallization, grains with basal orientations recrystallize more readily than off-basal grains, despite similar levels of internal misorientation. Dislocation substructure investigations revealed that this is a result of enhanced nucleation in the basal grains due to the dominance of prismatic slip. This dissertation identifies avenues to enhance the potential formability of magnesium alloys during thermomechanical processing by minimizing the evolved texture strength. The following are the identified key aspects of microstructural control: -Maintaining a fine grain size, likely via Zener pinning, to favorably modify deformation mode activity and homogenize deformation. -Developing a coarse, homogeneously distributed population of coarse intermetallic particles to promote a diffuse deformation texture. -Minimizing the activity of prismatic slip to retard the recrystallization of grains with basal orientations, allowing the development of a more diffuse recrystallization texture.

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.

Modeling of AA5083 Material-Microstructure Evolution During Butt Friction-Stir Welding

NASA Astrophysics Data System (ADS)

Grujicic, M.; Arakere, G.; Yalavarthy, H. V.; He, T.; Yen, C.-F.; Cheeseman, B. A.

2010-07-01

A concise yet a fairly comprehensive overview of the friction stir welding (FSW) process is provided. This is followed by a computational investigation in which FSW behavior of a prototypical solution-strengthened and strain-hardened aluminum alloy, AA5083-H131, is modeled using a fully coupled thermo-mechanical finite-element procedure developed in our prior study. Particular attention is given to proper modeling of the welding work-piece material behavior during the FSW process. Specifically, competition and interactions between plastic-deformation and dynamic-recrystallization processes are considered to properly account for the material-microstructure evolution in the weld nugget zone. 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.

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.

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

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.

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 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

Microstructure, Texture and Mechanical Properties of Titanium Grade 2 Processed by ECAP (Route C)

NASA Astrophysics Data System (ADS)

Wroński, M.; Wierzbanowski, K.; Wojtas, D.; Szyfner, E.; Valiev, R. Z.; Kawałko, J.; Berent, K.; Sztwiertnia, K.

2018-03-01

In the present work the properties of titanium grade 2 after ECAP processing with original route and regimes (route C, channel angle Φ= 120°, deformation temperature 300 °C, number of passes up to 8) were examined. Texture development and microstructure parameters after ECAP processing and after recrystallization were determined using electron back scatter diffraction and analysed. A significant increase of the mechanical strength accompanied by some increase of ductility was observed in the deformed samples. The kernel average misorientation and average grain orientation spread were strongly increased after deformation, which confirms the material refinement and fragmentation. The proportion of low angle boundaries increased after four ECAP passes, but after four consecutive passes high angle grain boundaries became predominant. No deformation twins were observed after four and eight ECAP passes. The material recrystallized after deformation retained a fine grain microstructure. The textures of deformed and recrystallized samples were determined. It was found that texture after 8 passes is more homogeneous that that after 4 passes, which partly explains higher ductility of this first sample.

Mechanical Behavior of Additively Manufactured Uranium-6 wt. pct. Niobium

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

Wu, A. S.; Wraith, M. W.; Burke, S. C.

This report describes an effort to process uranium-6 weight% niobium using laser powder bed fusion. The chemistry, crystallography, microstructure and mechanical response resulting from this process are discussed with particular emphasis on the effect of the laser powder bed fusion process on impurities. In an effort to achieve homogenization and uniform mechanical behavior from different builds, as well as to induce a more conventional loading response, we explore post-processing heat treatments on this complex alloy. Elevated temperature heat treatment for recrystallization is evaluated and the effect of recrystallization on mechanical behavior in laser powder bed fusion processed U-6Nb is discussed.more » Wrought-like mechanical behavior and grain sizes are achieved through post-processing and are reported herein.« less

Monolith electroplating process

DOEpatents

Agarrwal, Rajev R.

2001-01-01

An electroplating process for preparing a monolith metal layer over a polycrystalline base metal and the plated monolith product. A monolith layer has a variable thickness of one crystal. The process is typically carried in molten salts electrolytes, such as the halide salts under an inert atmosphere at an elevated temperature, and over deposition time periods and film thickness sufficient to sinter and recrystallize completely the nucleating metal particles into one single crystal or crystals having very large grains. In the process, a close-packed film of submicron particle (20) is formed on a suitable substrate at an elevated temperature. The temperature has the significance of annealing particles as they are formed, and substrates on which the particles can populate are desirable. As the packed bed thickens, the submicron particles develop necks (21) and as they merge into each other shrinkage (22) occurs. Then as micropores also close (23) by surface tension, metal density is reached and the film consists of unstable metal grain (24) that at high enough temperature recrystallize (25) and recrystallized grains grow into an annealed single crystal over the electroplating time span. While cadmium was used in the experimental work, other soft metals may be used.

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.

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).

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.

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

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.

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.

A model to describe the surface gradient-nanograin formation and property of friction stir processed laser Co-Cr-Ni-Mo alloy

NASA Astrophysics Data System (ADS)

Li, Ruidi; Yuan, Tiechui; Qiu, Zili

2014-07-01

A gradient-nanograin surface layer of Co-base alloy was prepared by friction stir processing (FSP) of laser-clad coating in this work. However, it is lack of a quantitatively function relationship between grain refinement and FSP conditions. Based on this, an analytic model is derived for the correlations between carbide size, hardness and rotary speed, layer depth during in-situ FSP of laser-clad Co-Cr-Ni-Mo alloy. The model is based on the principle of typical plastic flow in friction welding and dynamic recrystallization. The FSP experiment for modification of laser-clad Co-based alloy was conducted and its gradient nanograin and hardness were characterized. It shows that the model is consistent with experimental results.

The effect of aluminum nanoparticles on the structure, mechanical properties and failure of aluminum processed by accumulative roll bonding

NASA Astrophysics Data System (ADS)

Ivanov, K. V.; Fortuna, S. V.; Kalashnikova, T. A.; Rodkevich, N. G.

2017-12-01

The microstructure, mechanical properties, and fracture type of aluminum with and without aluminum nanoparticles processed by accumulative roll bonding (ARB) have been studied using transmission and scanning electron microscopy, microhardness measurements, and tensile tests. It is shown that the injection of aluminum nanoparticles increases the structure refinement rate during ARB due to the increasing tendency for dynamic recrystallization. It has a different effect on different mechanical characteristics. The different effect of nanoparticles on different structural features is the reason for the different effect on different mechanical properties related with these features. The fracture mechanism is shown to change from ductile in aluminum to mixed ductile-brittle in the composite with a 1.5-fold decrease in ductility as a result of nanoparticle injection.

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.

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.

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.

Microstructural Evolutions During Reversion Annealing of Cold-Rolled AISI 316 Austenitic Stainless Steel

NASA Astrophysics Data System (ADS)

Naghizadeh, Meysam; Mirzadeh, Hamed

2018-03-01

Microstructural evolutions during reversion annealing of a plastically deformed AISI 316 stainless steel were investigated and three distinct stages were identified: the reversion of strain-induced martensite to austenite, the primary recrystallization of the retained austenite, and the grain growth process. It was found that the slow kinetics of recrystallization at lower annealing temperatures inhibit the formation of an equiaxed microstructure and might effectively impair the usefulness of this thermomechanical treatment for the objective of grain refinement. By comparing the behavior of AISI 316 and 304 alloys, it was found that the mentioned slow kinetics is related to the retardation effect of solute Mo in the former alloy. At high reversion annealing temperature, however, an equiaxed austenitic microstructure was achieved quickly in AISI 316 stainless steel due to the temperature dependency of retardation effect of molybdenum, which allowed the process of recrystallization to happen easily. Conclusively, this work can shed some light on the issues of this efficient grain refining approach for microstructural control of austenitic stainless steels.

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

Liu, Tingguang; Xia, Shuang, E-mail: xs@shu.edu.cn; Li, Hui

Grain boundary engineering was carried out on an aging-treated nickel based Alloy 690, which has precipitated carbides at grain boundaries. Electron backscatter diffraction technique was used to investigate the grain boundary networks. Results show that, compared with the solution-annealed samples, the aging-treated samples with pre-existing carbides at grain boundaries need longer duration or higher temperature during annealing after low-strain tensile deformation for forming high proportion of low-Σ coincidence site lattice grain boundaries (more than 75%). The reason is that the primary recrystallization is inhibited or retarded owing to that the pre-existing carbides are barriers to grain boundaries migration. - Highlights:more » • Study of GBE as function of pre-existing GB carbides, tensile strain and annealing • Recrystallization of GBE is inhibited or retarded by the pre-existing carbides. • Retained carbides after annealing show the original GB positions. • More than 80% of special GBs were formed after the modification of GBE processing. • Multiple twinning during recrystallization is the key process of GBE.« less

Microstructural Evolutions During Reversion Annealing of Cold-Rolled AISI 316 Austenitic Stainless Steel

NASA Astrophysics Data System (ADS)

Naghizadeh, Meysam; Mirzadeh, Hamed

2018-06-01

Microstructural evolutions during reversion annealing of a plastically deformed AISI 316 stainless steel were investigated and three distinct stages were identified: the reversion of strain-induced martensite to austenite, the primary recrystallization of the retained austenite, and the grain growth process. It was found that the slow kinetics of recrystallization at lower annealing temperatures inhibit the formation of an equiaxed microstructure and might effectively impair the usefulness of this thermomechanical treatment for the objective of grain refinement. By comparing the behavior of AISI 316 and 304 alloys, it was found that the mentioned slow kinetics is related to the retardation effect of solute Mo in the former alloy. At high reversion annealing temperature, however, an equiaxed austenitic microstructure was achieved quickly in AISI 316 stainless steel due to the temperature dependency of retardation effect of molybdenum, which allowed the process of recrystallization to happen easily. Conclusively, this work can shed some light on the issues of this efficient grain refining approach for microstructural control of austenitic stainless steels.

Small Molecule Ice Recrystallization Inhibitors Enable Freezing of Human Red Blood Cells with Reduced Glycerol Concentrations

PubMed Central

Capicciotti, Chantelle J.; Kurach, Jayme D. R.; Turner, Tracey R.; Mancini, Ross S.; Acker, Jason P.; Ben, Robert N.

2015-01-01

In North America, red blood cells (RBCs) are cryopreserved in a clinical setting using high glycerol concentrations (40% w/v) with slow cooling rates (~1°C/min) prior to storage at −80°C, while European protocols use reduced glycerol concentrations with rapid freezing rates. After thawing and prior to transfusion, glycerol must be removed to avoid intravascular hemolysis. This is a time consuming process requiring specialized equipment. Small molecule ice recrystallization inhibitors (IRIs) such as β-PMP-Glc and β-pBrPh-Glc have the ability to prevent ice recrystallization, a process that contributes to cellular injury and decreased cell viability after cryopreservation. Herein, we report that addition of 110 mM β-PMP-Glc or 30 mM β-pBrPh-Glc to a 15% glycerol solution increases post-thaw RBC integrity by 30-50% using slow cooling rates and emphasize the potential of small molecule IRIs for the preservation of cells. PMID:25851700

Small molecule ice recrystallization inhibitors enable freezing of human red blood cells with reduced glycerol concentrations.

PubMed

Capicciotti, Chantelle J; Kurach, Jayme D R; Turner, Tracey R; Mancini, Ross S; Acker, Jason P; Ben, Robert N

2015-04-08

In North America, red blood cells (RBCs) are cryopreserved in a clinical setting using high glycerol concentrations (40% w/v) with slow cooling rates (~1°C/min) prior to storage at -80°C, while European protocols use reduced glycerol concentrations with rapid freezing rates. After thawing and prior to transfusion, glycerol must be removed to avoid intravascular hemolysis. This is a time consuming process requiring specialized equipment. Small molecule ice recrystallization inhibitors (IRIs) such as β-PMP-Glc and β-pBrPh-Glc have the ability to prevent ice recrystallization, a process that contributes to cellular injury and decreased cell viability after cryopreservation. Herein, we report that addition of 110 mM β-PMP-Glc or 30 mM β-pBrPh-Glc to a 15% glycerol solution increases post-thaw RBC integrity by 30-50% using slow cooling rates and emphasize the potential of small molecule IRIs for the preservation of cells.

AP reclamation and reuse in RSRM propellant

NASA Technical Reports Server (NTRS)

Miks, Kathryn F.; Harris, Stacey A.

1995-01-01

A solid propellant ingredient reclamation pilot plant has been evaluated at the Strategic Operations of Thiokol Corporation, located in Brigham City, Utah. The plant produces AP wet cake (95 percent AP, 5 percent water) for recycling at AP vendors. AP has been obtained from two standard propellant binder systems (PBAN and HTPB). Analytical work conducted at Thiokol indicates that the vendor-recrystallized AP meets Space Shuttle propellant specification requirements. Thiokol has processed 1-, 5-, and 600-gallon propellant mixes with the recrystallized AP. Processing, cast, cure, ballistic, mechanical, and safety properties have been evaluated. Phillips Laboratory static-test-fired 70-pound and 800-pound BATES motors. The data indicate that propellant processed with reclaimed AP has nominal properties.

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.

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.

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.

Thermal stability of Cu-Cr-Zr alloy processed by equal-channel angular pressing

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

Abib, Khadidja

Thermal stability of a Cu-Cr-Zr alloy processed by equal-channel angular pressing up to16 passes was investigated using isochronal annealing ranging from 250 to 850 °C for 1 h. The microstructure, crystallographic texture and micro hardness of samples were characterized through electron back scatter diffraction and Vickers micro hardness measurements. The recrystallized grain size was stable between 250 °C and 500 °C then increased quickly. The achieved mean grain size, after 1, 4 and 16 ECAP passes, was around 5.5 μm. A discontinuous mode of recrystallization was found to occur and a Particle Simulated Nucleation mechanism was evidenced. The evolution ofmore » the high angle grain boundary fraction increased notably after annealing above 550 °C. The crystallographic texture after isochronal annealing was similar to that of ECAP simple shear, no change of the texture during annealing was observed but only slight intensity variations. Micro hardness of all Cu–Cr–Zr samples showed a hardening with two peaks at 400 and 500 °C associated with precipitation of Cu cluster and Cu{sub 5}Zr phase respectively, followed by a subsequent softening upon increasing the annealing temperature due to recrystallization. - Highlight: •The Cu-1Cr-0.1Zr alloy shows a very good thermal stability up to 550 °C after ECAP. •A discontinuous recrystallization was found to occur and PSN mechanism was evidenced. •The annealing texture was found weak and some new components appear. •Hardening is attributed to the Cr clustering followed by the Cu{sub 51}Zr{sub 14} precipitation. •Softening is a result of recrystallization and grain growth progressing.« less

Through-process characterization of local anisotropy of Non-oriented electrical steel using magnetic Barkhausen noise

NASA Astrophysics Data System (ADS)

He, Youliang; Mehdi, Mehdi; Hilinski, Erik J.; Edrisy, Afsaneh

2018-05-01

Magnetic Barkhausen noise (MBN) signals were measured on a non-oriented electrical steel through all the thermomechanical processing stages, i.e. hot rolling, hot band annealing, cold rolling and final annealing. The temperature of the final annealing was varied from 600 °C to 750 °C so that the steel consisted of partially or completely recrystallized microstructures and different levels of residual stresses. The angular MBNrms (root mean square) values were compared to the texture factors in the same directions, the latter being calculated from the crystallographic texture measured by electron backscatter diffraction (EBSD). It was found that, in the cold-rolled, hot-rolled and completely recrystallized steels, the angular MBNrms followed a cosine function with respect to the angle of magnetization, while in partially recrystallized state such a relation does not exist. After cold rolling, the maximum MBNrms was observed in the rolling direction (RD) and the minimum MBNrms was in the transverse direction (TD), which was inconsistent with the magnetocrystalline anisotropy as indicated by the texture factor. After hot rolling, the maximum and minimum MBNrms values were observed in the TD and RD, respectively, exactly opposite to the cold-rolled state. If the steel was completely recrystallized, the maximum MBNrms was normally observed at a direction that was 15-30° from the minimum texture factor. If the steel was partially recrystallized, both the magnetocrystalline anisotropy of the material and the residual stress contributed to the angular MBNrms, which resulted in the deviation of the relationship from a cosine function. The relative strength of the two factors determined which factor would dominate the overall magnetic anisotropy.

Didanosine polymorphism in a supercritical antisolvent process.

PubMed

Bettini, R; Menabeni, R; Tozzi, R; Pranzo, M B; Pasquali, I; Chierotti, M R; Gobetto, R; Pellegrino, L

2010-04-01

Solid-state properties of active ingredients are crucial in pharmaceutical development owing to their significant clinical and economical implications. In the present work we investigated the solid-state properties and the solubility in water of didanosine, DDI, re-crystallized from a dimethylsulfoxide solution using supercritical CO(2) as an antisolvent (SAS process) for comparison with the commercially available drug product. We also applied modern solid-state NMR (SS NMR) techniques, namely 2D (1)H DQ CRAMPS (Combined Rotation And Multiple Pulse Spectroscopy) and (1)H-(13)C on- and off-resonance CP (cross polarization) FSLG-HETCOR experiments, known for providing reliable information about (1)H-(1)H and (1)H-(13)C intra- and intermolecular proximities, in order to address polymorphism issues arising from the crystallization of a new form in the supercritical process. A new polymorph of didanosine was obtained from the supercritical antisolvent process and characterized by means of 1D and 2D multinuclear ((1)H, (13)C, (15)N) SS NMR. The particle size of the new crystal phase was reduced by varying the antisolvent density through a pressure increase. The structural differences between the commercial product and the SAS re-crystallized DDI are highlighted by X-ray diffractometry and well described by solid-state NMR. The carbon C6 (13)C chemical shift suggests that both commercial and re-crystallized didanosine samples are in the enol form. The analysis of homo- and heteronuclear proximities obtained by means of 2D NMR experiments shows that commercial and SAS re-crystallized DDI possess very similar molecular conformation and hydrogen bond network, but different packing. The new polymorph proved to be a metastable form at ambient conditions, showing higher solubility in water and lower stability to mechanical stress. 2009 Wiley-Liss, Inc. and the American Pharmacists Association

Hot deformation behavior of uniform fine-grained GH4720Li alloy based on its processing map

NASA Astrophysics Data System (ADS)

Yu, Qiu-ying; Yao, Zhi-hao; Dong, Jian-xin

2016-01-01

The hot deformation behavior of uniform fine-grained GH4720Li alloy was studied in the temperature range from 1040 to 1130°C and the strain-rate range from 0.005 to 0.5 s-1 using hot compression testing. Processing maps were constructed on the basis of compression data and a dynamic materials model. Considerable flow softening associated with superplasticity was observed at strain rates of 0.01 s-1 or lower. According to the processing map and observations of the microstructure, the uniform fine-grained microstructure remains intact at 1100°C or lower because of easily activated dynamic recrystallization (DRX), whereas obvious grain growth is observed at 1130°C. Metallurgical instabilities in the form of non-uniform microstructures under higher and lower Zener-Hollomon parameters are induced by local plastic flow and primary γ' local faster dissolution, respectively. The optimum processing conditions at all of the investigated strains are proposed as 1090-1130°C with 0.08-0.5 s-1 and 0.005-0.008 s-1 and 1040-1085°C with 0.005-0.06 s-1.

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

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.

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

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

Ultrafast amorphization in Ge(10)Sb(2)Te(13) thin film induced by single femtosecond laser pulse.

PubMed

Konishi, Mitsutaka; Santo, Hisashi; Hongo, Yuki; Tajima, Kazuyuki; Hosoi, Masaharu; Saiki, Toshiharu

2010-06-20

We demonstrate amorphization in a Ge(10)Sb(2)Te(13) (GST) thin film through a nonthermal process by femtosecond electronic excitation. Amorphous recording marks were formed by irradiation with a single femtosecond pulse, and were confirmed to be recrystallized by laser thermal annealing. Scanning electron microscope observations revealed that amorphization occurred below the melting temperature. We performed femtosecond pump-probe measurements to investigate the amorphization dynamics of a GST thin film. We found that the reflectivity dropped abruptly within 500fs after excitation by a single pulse and that a small change in the reflectivity occurred within 5ps of this drop.

Preliminary 3D In-situ measurements of the texture evolution of strained H2O ice during annealing using neutron Laue diffractometry

NASA Astrophysics Data System (ADS)

Journaux, Baptiste; Montagnat, Maurine; Chauve, Thomas; Ouladdiaf, Bachir; Allibon, John

2015-04-01

Dynamic recrystallization (DRX) strongly affects the evolution of microstructure (grain size and shape) and texture (crystal preferred orientation) in materials during deformation at high temperature. Since texturing leads to anisotropic physical properties, predicting the effect of DRX is essential for industrial applications, for interpreting geophysical data and modeling geodynamic flows, and predicting ice sheet flow and climate evolution. A large amount of literature is available related to metallurgy, geology or glaciology, but there remains overall fundamental questions about the relationship between nucleation, grain boundary migration and texture development at the microscopic scale. Previous measurements of DRX in ice were either conducted using 2D ex-situ techniques such as AITA [1,2] or Electron Backscattering Diffraction (EBSD) [3], or using 3D statistical ex-situ [4] or in-situ [5] techniques. Nevertheless, all these techniques failed to observe at the scale of nucleation processes during DRX in full 3D. Here we present a new approach using neutron Laue diffraction, which enable to perform 3D measurements of in-situ texture evolution of strained polycrystalline H2O ice (>2% at 266 K) during annealing at the microscopic scale. Thanks the CYCLOPS instrument [6] (Institut Laue Langevin Grenoble, France) and the intrinsic low background of this setup, preliminary observations enabled us to follow, in H2O ice, the evolution of serrated grain boundaries, and kink-band during annealing. Our observations show a significant evolution of the texture and internal misorientation over the course of few hours at an annealing temperature of 268.5 K. In the contrary, ice kink-band structures seem to be very stable over time at near melting temperatures. The same samples have been analyzed ex-situ using EBSD for comparison. These results represent a first step toward in-situ microscopic measurements of dynamic recrystallization processes in ice during strain. This experiment has been conducted in the frame of the ANR-funded DREAM project that focuses on the recrystallization processes in anisotropic materials. References [1] D. S. Russell-Head and C.J.L. Wilson., 2001, Journal of Glaciology, 24, 117-130. [2] Wilson, C.J.L., Peternell, M., Piazolo, S., Luzin, V., 2014, Journal of Structural Geology, Microdynamics of Ice, 61, 50-77. [3] M. Montagnat, T. Chauve, F. Barou, A. Tommasi, B. Beausir, C. Fressengeas., in prep. [4] T. H. Jacka and J. Li., 2000, In T. Hondoh, editor, Physics of Ice Core Records, pages 83-102. Hokkaido University Press, Sapporo. [5] S. Piazolo, C. J. L. Wilson, V. Luzin, C. Brouzet, and M. Peternell., 2013, Geochemistry, Geophysics, Geosystems, 14, 4185-4194. [6] B. Ouladdiaf et al., 2011, Journal of Applied Crystallography, 44, 392-397.

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.

Effects of Strain Path on the Microstructure of Aluminum Alloys During Equal Channel Angular Pressing (ECAP)

DTIC Science & Technology

2007-12-01

processing route at this level. A recent study by Garcia-Infanta, et al., of a hypo- eutectic Al-7%Si alloy with spheroidal primary aluminum grains is a...compared with the model proposed by Garcia-Infanta, et al. [10]. Further, annealing studies will be performed to determine the recrystallization ...study conducted at 450°C as a function of time to assess recrystallization and grain growth. Two data points per sample were taken from different

Heat-Affected Zone Liquation Cracking Resistance of Friction Stir Processed Aluminum-Copper Alloy AA 2219

NASA Astrophysics Data System (ADS)

Karthik, G. M.; Janaki Ram, G. D.; Kottada, Ravi Sankar

2017-04-01

In the current work, the effect of friction stir processing on heat-affected zone (HAZ) liquation cracking resistance of aluminum-copper alloy AA 2219 was evaluated. In Gleeble hot-ductility tests and longitudinal Varestraint tests, the FSPed material, despite its very fine dynamically recrystallized equiaxed grain structure, showed considerably higher susceptibility to HAZ liquation cracking when compared to the base material. Detailed microstructural studies showed that the increased cracking susceptibility of the FSPed material is due to (i) increase in the amount of liquating θ phase (equilibrium Al2Cu) and (ii) increase in the population of grain boundary θ particles. An important learning from the current work is that, in certain materials like alloy 2219, the use of FSP as a pretreatment to fusion welding can be counterproductive.

Time-resolved structural dynamics of thin metal films heated with femtosecond optical pulses.

PubMed

Chen, Jie; Chen, Wei-Kan; Tang, Jau; Rentzepis, Peter M

2011-11-22

We utilize 100 fs optical pulses to induce ultrafast disorder of 35- to 150-nm thick single Au(111) crystals and observe the subsequent structural evolution using 0.6-ps, 8.04-keV X-ray pulses. Monitoring the picosecond time-dependent modulation of the X-ray diffraction intensity, width, and shift, we have measured directly electron/phonon coupling, phonon/lattice interaction, and a histogram of the lattice disorder evolution, such as lattice breath due to a pressure wave propagating at sonic velocity, lattice melting, and recrystallization, including mosaic formation. Results of theoretical simulations agree and support the experimental data of the lattice/liquid phase transition process. These time-resolved X-ray diffraction data provide a detailed description of all the significant processes induced by ultrafast laser pulses impinging on thin metallic single crystals.

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/).

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.

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

Solar cells with low cost substrates and process of making same

DOEpatents

Mitchell, Kim W.

1984-01-01

A solar cell having a substrate and an intermediate recrystallized film and a semiconductor material capable of absorbing light with the substrate being selected from one of a synthetic organic resin, graphite, glass and a crystalline material having a grain size less than about 1 micron.sup.2. The intermediate recrystallized film has a grain size in the range of from about 10 microns.sup.2 to about 10,000 microns.sup.2 and a lattice mismatch with the semiconductor material not greater than about 4%. The semiconductor material has a grain size not less than about 10 microns.sup.2. An anti-reflective layer and electrical contact means are provided. Also disclosed is a subcombination of substrate, intermediate recrystallized film and semiconductor material. Also, methods of formulating the solar cell and subcombination are disclosed.

Solar cells with low cost substrates, process of making same and article of manufacture

DOEpatents

Mitchell, K.W.

A solar cell is disclosed having a substrate and an intermediate recrystallized film and a semiconductor material capable of absorbing light with the substrate being selected from one of a synthetic organic resin, graphite, glass and a crystalline material having a grain size less than about 1 micron/sup 2/. The intermediate recrystallized film has a grain size in the range of from about 10 microns/sup 2/ to about 10,000 microns/sup 2/ and a lattice mismatch with the semiconductor material not greater than about 4%. The semiconductor material has a grain size not less than about 10 microns/sup 2/. An anti-reflective layer and electrical contact means are provided. Also disclosed is a subcombination of substrate, intermediate recrystallized film and semiconductor material. Also, methods of formulating the solar cell and subcombination are disclosed.

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.

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.

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.

Recrystallization-Induced Surface Cracks of Carbon Ions Irradiated 6H-SiC after Annealing.

PubMed

Ye, Chao; Ran, Guang; Zhou, Wei; Shen, Qiang; Feng, Qijie; Lin, Jianxin

2017-10-25

Single crystal 6H-SiC wafers with 4° off-axis [0001] orientation were irradiated with carbon ions and then annealed at 900 °C for different time periods. The microstructure and surface morphology of these samples were investigated by grazing incidence X-ray diffraction (GIXRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). Ion irradiation induced SiC amorphization, but the surface was smooth and did not have special structures. During the annealing process, the amorphous SiC was recrystallized to form columnar crystals that had a large amount of twin structures. The longer the annealing time was, the greater the amount of recrystallized SiC would be. The recrystallization volume fraction was accorded with the law of the Johnson-Mehl-Avrami equation. The surface morphology consisted of tiny pieces with an average width of approximately 30 nm in the annealed SiC. The volume shrinkage of irradiated SiC layer and the anisotropy of newly born crystals during annealing process produced internal stress and then induced not only a large number of dislocation walls in the non-irradiated layer but also the initiation and propagation of the cracks. The direction of dislocation walls was perpendicular to the growth direction of the columnar crystal. The longer the annealing time was, the larger the length and width of the formed crack would be. A quantitative model of the crack growth was provided to calculate the length and width of the cracks at a given annealing time.

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.

Development and comparison of processing maps of Mg-3Sn-1Ca alloy from data obtained in tension versus compression

NASA Astrophysics Data System (ADS)

Rao, K. P.; Suresh, K.; Prasad, Y. V. R. K.; Hort, N.

2018-01-01

The hot workability of extruded Mg-3Sn-1Ca alloy has been evaluated by developing processing maps with flow stress data from compression and tensile tests with a view to find the effect of the applied state-of-stress. The processing maps developed at a strain of 0.2 are essentially similar irrespective of the mode of deformation - compression or tension, and exhibit three domains in the temperature ranges: (1) 350 - 425 °C, and (2) 450 - 550 °C and (3) 400 - 500 °C, the first two occurring at lower strain rates and the third occurring at higher strain rates. In all the three domains, dynamic recrystallization occurs and is caused by non-basal slip and controlled by lattice self-diffusion in the first and second domains and grain boundary self-diffusion in the third domain. The state-of-stress imposed on the specimen (compression or tension) does not have any significant effect on the processing maps.

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.

Optimized manufacture of nuclear fuel cladding tubes by FEA of hot extrusion and cold pilgering processes

NASA Astrophysics Data System (ADS)

Gaillac, Alexis; Ly, Céline

2018-05-01

Within the forming route of Zirconium alloy cladding tubes, hot extrusion is used to deform the forged billets into tube hollows, which are then cold rolled to produce the final tubes with the suitable properties for in-reactor use. The hot extrusion goals are to give the appropriate geometry for cold pilgering, without creating surface defects and microstructural heterogeneities which are detrimental for subsequent rolling. In order to ensure a good quality of the tube hollows, hot extrusion parameters have to be carefully chosen. For this purpose, finite element models are used in addition to experimental tests. These models can take into account the thermo-mechanical coupling conditions obtained in the tube and the tools during extrusion, and provide a good prediction of the extrusion load and the thermo-mechanical history of the extruded product. This last result can be used to calculate the fragmentation of the microstructure in the die and the meta-dynamic recrystallization after extrusion. To further optimize the manufacturing route, a numerical model of the cold pilgering process is also applied, taking into account the complex geometry of the tools and the pseudo-steady state rolling sequence of this incremental forming process. The strain and stress history of the tube during rolling can then be used to assess the damage risk thanks to the use of ductile damage models. Once validated vs. experimental data, both numerical models were used to optimize the manufacturing route and the quality of zirconium cladding tubes. This goal was achieved by selecting hot extrusion parameters giving better recrystallized microstructure that improves the subsequent formability. Cold pilgering parameters were also optimized in order to reduce the potential ductile damage in the cold rolled tubes.

Ethylcellulose film coating of guaifenesin-loaded pellets: A comprehensive evaluation of the manufacturing process to prevent drug migration.

PubMed

Melegari, Cecilia; Bertoni, Serena; Genovesi, Alberto; Hughes, Kevin; Rajabi-Siahboomi, Ali R; Passerini, Nadia; Albertini, Beatrice

2016-03-01

The aim of the research was to investigate the complete process of pellet production in a Wurster fluidized bed coater in order to determine the main factors affecting the migration phenomenon of a soluble API through the ethycellulose film coating (Surelease®) and hence the long-term stability of the controlled release pellets. Guaifenesin (GFN), as BCS class I model drug, was layered on sugar spheres using a binder-polymer solution containing the dissolved GFN. The drug loaded pellets were then coated with Surelease®. The influence of drug loading (4.5-20.0% w/w), curing conditions (40-60°C and dynamic-static equipment), coating level (12-20% theoretical weight gain) and composition of the binder-layering solution (hypromellose versus Na alginate) on process efficiency (RSDW%), GFN content uniformity (RSDC%), GFN solid state (DSC and XRD) and pellet release profiles was evaluated. The effectiveness of the Surelease film was strongly affected by the ability of GFN to cross the coating layer and to recrystallize on the pellet surface. Results indicated that this behaviour was dependent on the polymer used in the binder-layering solution. Using hypromellose as polymer, GFN recrystallized on the coated pellet surface at both drug loadings. The curing step was necessary to stabilize the film effectiveness at the higher drug loading. Increasing the coating level delayed but did not prevent the GFN diffusion. Replacing hypromellose with Na alginate, reduced the migration of GFN through the film to a negligible amount even after six months of storage and the curing step was not necessary to achieve stable controlled release profiles over storage. Copyright © 2015 Elsevier B.V. All rights reserved.

Measurement and analysis of applied power, forces and material response in friction stir welding of aluminum alloy 6061

NASA Astrophysics Data System (ADS)

Avila, Ricardo E.

The process of Friction Stir Welding (FSW) 6061 aluminum alloy is investigated, with focus on the forces and power being applied in the process and the material response. The main objective is to relate measurements of the forces and power applied in the process with mechanical properties of the material during the dynamic process, based on mathematical modeling and aided by computer simulations, using the LS-DYNA software for finite element modeling. Results of measurements of applied forces and power are presented. The result obtained for applied power is used in the construction of a mechanical variational model of FSW, in which minimization of a functional for the applied torque is sought, leading to an expression for shear stress in the material. The computer simulations are performed by application of the Smoothed Particle Hydrodynamics (SPH) method, in which no structured finite element mesh is used to construct a spatial discretization of the model. The current implementation of SPH in LS-DYNA allows a structural solution using a plastic kinematic material model. This work produces information useful to improve understanding of the material flow in the process, and thus adds to current knowledge about the behavior of materials under processes of severe plastic deformation, particularly those processes in which deformation occurs mainly by application of shear stress, aided by thermoplastic strain localization and dynamic recrystallization.

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.

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.

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

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.

Hot deformation characterization of duplex low-density steel through 3D processing map development

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

Mohamadizadeh, A.; Zarei-Hanzaki, A., E-mail: zareih@ut.ac.ir; Abedi, H.R.

The high temperature deformation behavior of duplex low-density Fe–18Mn–8Al–0.8C steel was investigated at temperatures in the range of 600–1000 °C. The primary constitutive analysis indicated that the Zener–Hollomon parameter, which represents the coupled effects of temperature and strain rate, significantly varies with the amount of deformation. Accordingly, the 3D processing maps were developed considering the effect of strain and were used to determine the safe and unsafe deformation conditions in association with the microstructural evolution. The deformation at efficiency domain I (900–1100 °C\\10{sup −} {sup 2}–10{sup −} {sup 3} s{sup −} {sup 1}) was found to be safe at differentmore » strains due to the occurrence of dynamic recrystallization in austenite. The safe efficiency domain II (700–900 °C\\1–10{sup −} {sup 1} s{sup −} {sup 1}), which appeared at logarithmic strain of 0.4, was characterized by deformation induced ferrite formation. Scanning electron microscopy revealed that the microband formation and crack initiation at ferrite\\austenite interphases were the main causes of deformation instability at 600–800 °C\\10{sup −} {sup 2}–10{sup −} {sup 3} s{sup −} {sup 1}. The degree of instability was found to decrease by increasing the strain due to the uniformity of microbanded structure obtained at higher strains. The shear band formation at 900–1100 °C\\1–10{sup −} {sup 1} s{sup −} {sup 1} was verified by electron backscattered diffraction. The local dynamic recrystallization of austenite and the deformation induced ferrite formation were observed within shear-banded regions as the results of flow localization. - Graphical abstract: Display Omitted - Highlights: • The 3D processing map is developed for duplex low-density Fe–Mn–Al–C steel. • The efficiency domains shrink, expand or appear with increasing strain. • The occurrence of DRX and DIFF increases the power efficiency. • Crack initiation at α/γ interphase and shear banding lead to failure.« less

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.

Reversible switching between pressure-induced amorphization and thermal-driven recrystallization in VO2(B) nanosheets

PubMed Central

Wang, Yonggang; Zhu, Jinlong; Yang, Wenge; Wen, Ting; Pravica, Michael; Liu, Zhenxian; Hou, Mingqiang; Fei, Yingwei; Kang, Lei; Lin, Zheshuai; Jin, Changqing; Zhao, Yusheng

2016-01-01

Pressure-induced amorphization (PIA) and thermal-driven recrystallization have been observed in many crystalline materials. However, controllable switching between PIA and a metastable phase has not been described yet, due to the challenge to establish feasible switching methods to control the pressure and temperature precisely. Here, we demonstrate a reversible switching between PIA and thermally-driven recrystallization of VO2(B) nanosheets. Comprehensive in situ experiments are performed to establish the precise conditions of the reversible phase transformations, which are normally hindered but occur with stimuli beyond the energy barrier. Spectral evidence and theoretical calculations reveal the pressure–structure relationship and the role of flexible VOx polyhedra in the structural switching process. Anomalous resistivity evolution and the participation of spin in the reversible phase transition are observed for the first time. Our findings have significant implications for the design of phase switching devices and the exploration of hidden amorphous materials. PMID:27426219

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.

Matrix Sublimation/Recrystallization for Imaging Proteins by Mass Spectrometry at High Spatial Resolution

PubMed Central

Yang, Junhai; Caprioli, Richard M.

2011-01-01

We have employed matrix deposition by sublimation for protein image analysis on tissue sections using a hydration/recrystallization process that produces high quality MALDI mass spectra and high spatial resolution ion images. We systematically investigated different washing protocols, the effect of tissue section thickness, the amount of sublimated matrix per unit area and different recrystallization conditions. The results show that an organic solvent rinse followed by ethanol/water rinses substantially increased sensitivity for the detection of proteins. Both the thickness of tissue section and amount of sinapinic acid sublimated per unit area have optimal ranges for maximal protein signal intensity. Ion images of mouse and rat brain sections at 50, 20 and 10 µm spatial resolution are presented and are correlated with H&E stained optical images. For targeted analysis, histology directed imaging can be performed using this protocol where MS analysis and H&E staining are performed on the same section. PMID:21639088

Reversible switching between pressure-induced amorphization and thermal-driven recrystallization in VO2(B) nanosheets.

PubMed

Wang, Yonggang; Zhu, Jinlong; Yang, Wenge; Wen, Ting; Pravica, Michael; Liu, Zhenxian; Hou, Mingqiang; Fei, Yingwei; Kang, Lei; Lin, Zheshuai; Jin, Changqing; Zhao, Yusheng

2016-07-18

Pressure-induced amorphization (PIA) and thermal-driven recrystallization have been observed in many crystalline materials. However, controllable switching between PIA and a metastable phase has not been described yet, due to the challenge to establish feasible switching methods to control the pressure and temperature precisely. Here, we demonstrate a reversible switching between PIA and thermally-driven recrystallization of VO2(B) nanosheets. Comprehensive in situ experiments are performed to establish the precise conditions of the reversible phase transformations, which are normally hindered but occur with stimuli beyond the energy barrier. Spectral evidence and theoretical calculations reveal the pressure-structure relationship and the role of flexible VOx polyhedra in the structural switching process. Anomalous resistivity evolution and the participation of spin in the reversible phase transition are observed for the first time. Our findings have significant implications for the design of phase switching devices and the exploration of hidden amorphous materials.

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

The improved dissolution performance of a post processing treated spray-dried crystalline solid dispersion of poorly soluble drugs.

PubMed

Chan, Siok-Yee; Toh, Seok-Ming; Khan, Nasir Hayat; Chung, Yin-Ying; Cheah, Xin-Zi

2016-11-01

Solution-mediated transformation has been cited as one of the main problems that deteriorate dissolution performances of solid dispersion (SD). This is mainly attributed by the recrystallization tendency of poorly soluble drug. Eventually, it will lead to extensive agglomeration which is a key process in reducing the dissolution performance of SD and offsets the true benefit of SD system. Here, a post-processing treatment is suggested in order to reduce the recrystallization tendency and hence bring forth the dissolution advantage of SD system. The current study investigates the effect of a post processing treatment on dissolution performance of SD in comparison to their performances upon production. Two poorly soluble drugs were spray dried into SD using polyvinyl alcohol (PVA) as hydrophilic carrier. The obtained samples were post processing treated by exposure to high humidity, i.e. 75% RH at room temperature. The physical properties and release rate of the SD system were characterized upon production and after the post-processing treatment. XRPD, Infrared and DSC results showed partial crystallinity of the fresh SD systems. Crystallinity of these products was further increased after the post-processing treatment at 75% RH. This may be attributed to the high moisture absorption of the SD system that promotes recrystallization process of the drug. However, dissolution efficiencies of the post-treated systems were higher and more consistent than the fresh SD. The unexpected dissolution trend was further supported by the results intrinsic dissolution and solubility studies. An increase of crystallinity in a post humidity treated SD did not exert detrimental effect to their dissolution profiles. A more stabilized system with a preferable enhanced dissolution rate was obtained by exposing the SD to a post processing humidity treatment.

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.

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.

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.

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.

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.

The effectiveness of sodium hydroxide (NaOH) and sodium carbonate (Na2CO3) on the impurities removal of saturated salt solution

NASA Astrophysics Data System (ADS)

Pujiastuti, C.; Ngatilah, Y.; Sumada, K.; Muljani, S.

2018-01-01

Increasing the quality of salt can be done through various methods such as washing (hydro-extraction), re-crystallization, ion exchange methods and others. In the process of salt quality improvement by re-crystallization method where salt product diluted with water to form saturated solution and re-crystallized through heating process. The quality of the salt produced is influenced by the quality of the dissolved salt and the crystallization mechanism applied. In this research is proposed a concept that before the saturated salt solution is recrystallized added a chemical for removal of the impurities such as magnesium ion (Mg), calcium (Ca), potassium (K) and sulfate (SO4) is contained in a saturated salt solution. The chemical reagents that used are sodium hydroxide (NaOH) 2 N and sodium carbonate (Na2CO3) 2 N. This research aims to study effectiveness of sodium hydroxide and sodium carbonate on the impurities removal of magnesium (Mg), calcium (Ca), potassium (K) and sulfate (SO4). The results showed that the addition of sodium hydroxide solution can be decreased the impurity ions of magnesium (Mg) 95.2%, calcium ion (Ca) 45%, while the addition of sodium carbonate solution can decreased magnesium ion (Mg) 66.67% and calcium ion (Ca) 77.5%, but both types of materials are not degradable sulfate ions (SO4). The sodium hydroxide solution more effective to decrease magnesium ion than sodium carbonate solution, and the sodium carbonate solution more effective to decrease calcium ion than sodium hydroxide solution.

Recrystallization-Induced Surface Cracks of Carbon Ions Irradiated 6H-SiC after Annealing

PubMed Central

Ye, Chao; Ran, Guang; Zhou, Wei; Shen, Qiang; Feng, Qijie; Lin, Jianxin

2017-01-01

Single crystal 6H-SiC wafers with 4° off-axis [0001] orientation were irradiated with carbon ions and then annealed at 900 °C for different time periods. The microstructure and surface morphology of these samples were investigated by grazing incidence X-ray diffraction (GIXRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). Ion irradiation induced SiC amorphization, but the surface was smooth and did not have special structures. During the annealing process, the amorphous SiC was recrystallized to form columnar crystals that had a large amount of twin structures. The longer the annealing time was, the greater the amount of recrystallized SiC would be. The recrystallization volume fraction was accorded with the law of the Johnson–Mehl–Avrami equation. The surface morphology consisted of tiny pieces with an average width of approximately 30 nm in the annealed SiC. The volume shrinkage of irradiated SiC layer and the anisotropy of newly born crystals during annealing process produced internal stress and then induced not only a large number of dislocation walls in the non-irradiated layer but also the initiation and propagation of the cracks. The direction of dislocation walls was perpendicular to the growth direction of the columnar crystal. The longer the annealing time was, the larger the length and width of the formed crack would be. A quantitative model of the crack growth was provided to calculate the length and width of the cracks at a given annealing time. PMID:29068408

Recovery and recrystalization kinetics of cold-worked Zircaloy-4 plate and tubing (LWBR Development Program)

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

Katz, O.M.

1968-02-01

Empirical kinetic equations were derived to describe the recovery region between 550 and 1020/sup 0/F for times to 4000 hours for 15 to 78% cold-worked Zircaloy-4 plate and tubing. The properties studied were electrical resistivity and X-ray line sharpening. Recrystallization kinetics were described with sigmoidal curves derived from X-ray intensity and microhardness data. Light, replica, and transmission electron microscopy and selected-area electron diffraction were used to postulate recovery and recrystallization mechanisms. From a structural aspect, the annealing process in cold-worked Zircaloy-4 is visualized as a dislocation climb and annihilation process to the limit allowed by the size of the deformationmore » subcells, a reorientation of the subgrain material into a recrystallization texture, a growth of reoriented cells located in the most highly worked bands, and a consumption of less favorably strained and/or oriented cells by the high-angle boundaries of the reoriented cells. Comparison of 15 and 73% cold-worked tubing showed the activation energy to be less (21 versus 60 kcal/mol) and the subcell size greater (8000A versus 1000A) for the 15% cold-worked material. (NSA 22: 21698)« less

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

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.

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.

Investigation on temporal evolution of the grain refinement in copper under high strain rate loading via in-situ synchrotron measurement and predictive modeling

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

Shah, Pooja Nitin; Shin, Yung C.; Sun, Tao

Synchrotron X-rays are integrated with a modified Kolsky tension bar to conduct in situ tracking of the grain refinement mechanism operating during the dynamic deformation of metals. Copper with an initial average grain size of 36 μm is refined to 6.3 μm when loaded at a constant high strain rate of 1200 s -1. The synchrotron measurements revealed the temporal evolution of the grain refinement mechanism in terms of the initiation and rate of refinement throughout the loading test. A multiscale coupled probabilistic cellular automata based recrystallization model has been developed to predict the microstructural evolution occurring during dynamic deformationmore » processes. The model accurately predicts the initiation of the grain refinement mechanism with a predicted final average grain size of 2.4 μm. As a result, the model also accurately predicts the temporal evolution in terms of the initiation and extent of refinement when compared with the experimental results.« less

Investigation on temporal evolution of the grain refinement in copper under high strain rate loading via in-situ synchrotron measurement and predictive modeling

DOE PAGES

Shah, Pooja Nitin; Shin, Yung C.; Sun, Tao

2017-10-03

Synchrotron X-rays are integrated with a modified Kolsky tension bar to conduct in situ tracking of the grain refinement mechanism operating during the dynamic deformation of metals. Copper with an initial average grain size of 36 μm is refined to 6.3 μm when loaded at a constant high strain rate of 1200 s -1. The synchrotron measurements revealed the temporal evolution of the grain refinement mechanism in terms of the initiation and rate of refinement throughout the loading test. A multiscale coupled probabilistic cellular automata based recrystallization model has been developed to predict the microstructural evolution occurring during dynamic deformationmore » processes. The model accurately predicts the initiation of the grain refinement mechanism with a predicted final average grain size of 2.4 μm. As a result, the model also accurately predicts the temporal evolution in terms of the initiation and extent of refinement when compared with the experimental results.« less

Hot deformation constitutive equation and processing map of Alloy 690

NASA Astrophysics Data System (ADS)

Feng, Han; Zhang, Songchuang; Ma, Mingjuan; Song, Zhigang

The hot deformation behavior of alloy 690 was studied in the temperature range of 800-1300 C and strain rate range of 0.1-10 s-1 by hot compression tests in a Gleeble 1500+ thermal mechanical simulator. The results indicated that flow stress of alloy 690 is sensitive to deformation temperature and strain rate and peak stress increases with decreasing of temperature and increasing of strain rate. In addition, the hot deformation parameters of deformation activation were calculated and the apparent activation energy of this alloy is about 300 kJ/mol. The constitutive equation which can be used to relate peak stress to the absolute temperature and strain rate was obtained. It's further found that the processing maps exhibited two domains which are considered as the optimum windows for hot working. The microstructure observations of the specimens deformed in this domain showed the full dynamic recrystallization (DRX) structure. There was a flow instability domain in the processing map where hot working should be avoided.

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.

Metamorphism, metasomatism, retrogression: the common control on isotope transport

NASA Astrophysics Data System (ADS)

Villa, I. M.; Williams, M. L.

2011-12-01

Compositional or isotopic modification of a mineral can be viewed as a single process with many names. Depending on the large-scale context, different names are used: aqueous alteration, retrogression, metasomatism, metamorphism, but it should be clear that the underlying atomic-scale mechanism is the same. Changes in stoichiometry and in crystallographic structure require recrystallization. Following [1], all recrystallization processes can be viewed as nano-scale dissolution/reprecipitation, mediated by an aqueous fluid. In fact, aqueous fluids are the main control on the formation of all metamorphic parageneses [2], and also isotope exchange in minerals [3]. The reason is that the rate constants for fluid-mediated isotope transport are orders of magnitude larger, and activation energies much smaller, than those for diffusion. Recrystallisation is energetically less costly at almost any temperature than diffusive reequilibration [3]. However, recrystallization is not the only cause of isotope loss/exchange. Temperature can also play a role in reducing the retentivity of a geochronometer by increasing diffusivity. In cases where diffusion was the factor limiting isotopic closure (or chemical closure), a bell-shaped isotope (or element) concentration profile is observed. The criterion to decide whether in a particular sample diffusion or recrystallization was the principal control on chemical/isotope transport lies in the spatial variation of elemental or isotopic composition. Patchy spatial patterns are certain evidence of fluid-mediated local recrystallization. Bell-shaped gradients are compatible with (but not unambiguous proof of) volume diffusion. In-situ dating over three decades has never described bell-shaped isotope gradients in patchily zoned minerals. On the contrary, age mapping usually coincides with microchemical mapping [4]. This is best explained by a common cause for the recrystallization and the isotope transport. The cause, fluid-mediated dissolution/reprecipitation, depends mainly on water activity and only very loosely on temperature, i.e. provides a geohygrometric but not a geothermometric datum. We conclude that only in rare cases diffusion is the sole promoter of isotope resetting. The observations require a major shift in perspective on the significance of mineral ages. Just as the "diffusionist" view that zircon discordance is due to thermal disturbances (e.g. [5]) was superseded by the petrological understanding that it is due to recrystallization (e.g. [6]), a blanket interpretation of intra-mineral age variations in terms of a purely thermal history neglecting the petrogenetic context is no longer tenable. [1] Putnis A (2009) Rev Mineral Geochem 70, 87-124 [2] Lasaga A (1986) Mineral Mag 50, 359-373 [3] Cole DR et al (1983) Geochim Cosmochim Acta 47, 1681-1693 [4] Williams ML et al (2007) Ann Rev Earth Planet Sci 35, 137-175 [5] Steiger RH, Wasserburg GJ (1969) Geochim Cosmochim Acta 33, 1213-1232 [6] Mezger K, Krogstadt EJ (1997) J Metam Geol 15, 127-140

Hot Deformation and Processing Window Optimization of a 70MnSiCrMo Carbide-Free Bainitic Steel.

PubMed

Han, Ying; Sun, Yu; Zhang, Wei; Chen, Hua

2017-03-21

The hot deformation behavior of a high carbon carbide-free bainitic steel was studied through isothermal compression tests that were performed on a Gleeble-1500D thermal mechanical simulator at temperatures of 1223-1423 K and strain rates of 0.01-5 s -1 . The flow behavior, constitutive equations, dynamic recrystallization (DRX) characteristics, and processing map were respectively analyzed in detail. It is found that the flow stress increases with increasing the strain rate and decreases with increasing the temperature, and the single-peak DRX can be easily observed at high temperatures and/or low strain rates. The internal relationship between the flow stress and processing parameters was built by the constitutive equations embracing a parameter of Z/A, where the activation energy for hot deformation is 351.539 kJ/mol and the stress exponent is 4.233. In addition, the DRX evolution and the critical conditions for starting DRX were discussed. Then the model of the DRX volume fraction was developed with satisfied predictability. Finally, the processing maps at different strains were constructed according to the dynamic material model. The safety domains and flow instability regions were identified. The best processing parameters of this steel are within the temperature range of 1323-1423 K and strain rate range of 0.06-1 s -1 .

Hot Deformation and Processing Window Optimization of a 70MnSiCrMo Carbide-Free Bainitic Steel

PubMed Central

Han, Ying; Sun, Yu; Zhang, Wei; Chen, Hua

2017-01-01

The hot deformation behavior of a high carbon carbide-free bainitic steel was studied through isothermal compression tests that were performed on a Gleeble-1500D thermal mechanical simulator at temperatures of 1223–1423 K and strain rates of 0.01–5 s−1. The flow behavior, constitutive equations, dynamic recrystallization (DRX) characteristics, and processing map were respectively analyzed in detail. It is found that the flow stress increases with increasing the strain rate and decreases with increasing the temperature, and the single-peak DRX can be easily observed at high temperatures and/or low strain rates. The internal relationship between the flow stress and processing parameters was built by the constitutive equations embracing a parameter of Z/A, where the activation energy for hot deformation is 351.539 kJ/mol and the stress exponent is 4.233. In addition, the DRX evolution and the critical conditions for starting DRX were discussed. Then the model of the DRX volume fraction was developed with satisfied predictability. Finally, the processing maps at different strains were constructed according to the dynamic material model. The safety domains and flow instability regions were identified. The best processing parameters of this steel are within the temperature range of 1323–1423 K and strain rate range of 0.06–1 s−1. PMID:28772678

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.

Steam-assisted crystallization of TPA{sup +}-exchanged MCM-41 type mesoporous materials with thick pore walls

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

Chen, Hong Li; Zhang, Kun; Wang, Yi Meng, E-mail: ymwang@chem.ecnu.edu.cn

2012-07-15

Highlights: ► Mesoporous Ti-containing silica with thicker pore walls was synthesized. ► Ion-exchange and steam-assisted crystallization led to MCM-41/MFI composite. ► The introduction of Ti inhibited the formation of separated MFI particles. ► Lower temperature favored retaining mesoporous characteristics and morphology. -- Abstract: Hierarchical MCM-41/MFI composites were synthesized through ion-exchange of as-made MCM-41 type mesoporous materials with tetrapropylammonium bromide and subsequent steam-assisted recrystallization. The obtained samples were characterized by powder X-ray diffraction (XRD), UV–vis diffuse reflectance spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), thermogravimetric analysis, FT-IR, {sup 1}H–{sup 13}C CP/MAS and nitrogen adsorption–desorption. The XRD patterns show thatmore » the MCM-41/MFI composite possesses both ordered MCM-41 phase and zeolite MFI phase. SEM and TEM images indicate that the recrystallized materials retained the mesoporous characteristics and the morphology of as-made mesoporous materials without the formation of bulky zeolite, quite different from the mechanical mixture of MCM-41 and MFI structured zeolite. Among others, lower recrystallization temperature and the introduction of the titanium to the parent materials are beneficial to preserve the mesoporous structure during the recrystallization process.« less

Influence of Oxalate on Ni Fate during Fe(II)-Catalyzed Recrystallization of Hematite and Goethite.

PubMed

Flynn, Elaine D; Catalano, Jeffrey G

2018-06-05

During biogeochemical iron cycling at redox interfaces, dissolved Fe(II) induces the recrystallization of Fe(III) oxides. Oxalate and other organic acids promote dissolution of these minerals and may also induce recrystallization. These processes may redistribute trace metals among the mineral bulk, mineral surface, and aqueous solution. However, the impact of interactions among organic acids, dissolved Fe(II), and iron oxide minerals on trace metal fate in such systems is unclear. The present study thus explores the effect of oxalate on Ni release from and incorporation into hematite and goethite in the absence and presence of Fe(II). When Ni is initially structurally incorporated into the iron oxides, both oxalate and dissolved Fe(II) promote the release of Ni to aqueous solution. When both species are present, their effects on Ni release are synergistic at pH 7 but inhibitory at pH 4, indicating that cooperative and competitive interactions vary with pH. In contrast, oxalate suppresses Ni incorporation into goethite and hematite during Fe(II)-induced recrystallization, decreasing the proportion of Ni substituting in a mineral structure by up to 36%. These observations suggest that at redox interfaces oxalate largely enhances trace metal mobility. In such settings, oxalate, and likely other organic acids, may thus enhance micronutrient availability and inhibit contaminant sequestration.

Recrystallization of fluconazole using the supercritical antisolvent (SAS) process.

PubMed

Park, Hee Jun; Kim, Min-Soo; Lee, Sibeum; Kim, Jeong-Soo; Woo, Jong-Soo; Park, Jeong-Sook; Hwang, Sung-Joo

2007-01-10

The supercritical antisolvent (SAS) process was used to modify solid state characteristics of fluconazole. Fluconazole was recrystallized at various temperatures (60-80 degrees C) and pressures (8-16MPa) using dichloromethane (DCM) as a solvent. Acetone and ethanol were also employed as solvents. The fluconazole polymorphs prepared by the SAS process were characterized by differential scanning calorimetry (DSC), thermogravimetry analysis (TGA), powder X-ray diffraction (PXRD), Fourier transform infrared spectroscopy (FT-IR) and scanning electron microscopy (SEM). Furthermore, the equilibrium solubility of the samples in aqueous solution was determined. Fluconazole anhydrate form I was obtained at low temperature (40 degrees C) and anhydrate form II was obtained at high temperature (80 degrees C). The variation of pressure during the SAS process may influence the preferred orientation. Anhydrate forms I and II were also obtained using various solvents. Therefore, it was shown that solid state characteristics of fluconazole, including the polymorphic form and preferred orientation, can be controlled by changing operating conditions of the SAS process such as temperature, pressure, and solvent.

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.

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.

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

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.

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.

Quantification of diagenetic overprint processes deduced from fossil carbonate shells and laboratory-based hydrothermal alteration experiments

NASA Astrophysics Data System (ADS)

Griesshaber, Erika; Casella, Laura; Mavromatis, Vasileios; Dietzel, Martin; Immenhauser, Adrian; Schmahl, Wolfgang

2016-04-01

Benthic and nektonic marine biogenic carbonate archives represent the foundation of numerous studies aiming at reconstructions of past climate dynamics and environmental change. However, living organisms are not in thermodynamic equilibrium and create local chemical environments where physiologic processes such as biomineralization takes place. After the death of the organism the former physiologic disequilibrium conditions are not sustained any more and all biological tissues are altered by equilibration according to the surrounding environment: diagenesis. With increasing diagenetic alteration, the biogenic structure and fingerprint fades away and is replaced by inorganic features. Thus, recrystallization of organism-specific microstructure is a clear indicator for diagenetic overprint. Microstructural data, which mirror recrystallization, are of great value for interpreting geochemical proxies for paleo-environment reconstruction. Despite more than a century of research dealing with carbonate diagenesis, many of the controlling processes and factors are only understood in a qualitative manner. One of the main issues is that diagenetically altered carbonates are usually present as the product of a complex preceding diagenetic pathway with an unknown number of intermediate steps. In this contribution we present and discuss laboratory based alteration experiments with the aim to investigate time-series data sets in a controlled manner. We conducted hydrothermal alteration experiments with modern Arctica islandica (bivalvia) and Notosaria nigricans (brachiopoda) in order to mimic diagenetic overprint. We explore first the potential of electron backscattered diffraction (EBSD) measurements together with statistical data evaluation as a tool to quantify diagenetic alteration of carbonate skeletons. Subsequently, we compare microstructural patterns obtained from experimentally altered shell material with those of fossil specimens that have undergone variable degrees of diagenetic overprint. We intend to come up with a process-oriented understanding of alteration parameters and products as the change in microstructure, texture and mineral phase needs a careful action when it comes to the interpretation of paleoclimate reconstruction data.

Constitutive Model for Hot Deformation of the Cu-Zr-Ce Alloy

NASA Astrophysics Data System (ADS)

Zhang, Yi; Sun, Huili; Volinsky, Alex A.; Wang, Bingjie; Tian, Baohong; Liu, Yong; Song, Kexing

2018-02-01

Hot compressive deformation behavior of the Cu-Zr-Ce alloy has been investigated according to the hot deformation tests in the 550-900 °C temperature range and 0.001-10 s-1 strain rate range. Based on the true stress-true strain curves, the flow stress behavior of the Cu-Zr-Ce alloy was investigated. Microstructure evolution was observed by optical microscopy. Based on the experimental results, a constitutive equation, which reflects the relationships between the stress, strain, strain rate and temperature, has been established. Material constants n, α, Q and ln A were calculated as functions of strain. The equation predicting the flow stress combined with these materials constants has been proposed. The predicted stress is consistent with experimental stress, indicating that developed constitutive equation can adequately predict the flow stress of the Cu-Zr-Ce alloy. Dynamic recrystallization critical strain was determined using the work hardening rate method. According to the dynamic material model, the processing maps for the Cu-Zr and Cu-Zr-Ce alloy were obtained at 0.4 and 0.5 strain. Based on the processing maps and microstructure observations, the optimal processing parameters for the two alloys were determined, and it was found that the addition of Ce can promote the hot workability of the Cu-Zr alloy.

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.

Reversible switching between pressure-induced amorphization and thermal-driven recrystallization in VO2(B) nanosheets

DOE PAGES

Wang, Yonggang; Zhu, Jinlong; Yang, Wenge; ...

2016-07-18

Pressure-induced amorphization (PIA) and thermal-driven recrystallization have been observed in many crystalline materials. However, controllable switching between PIA and a metastable phase has not been described yet, due to the challenge to establish feasible switching methods to control the pressure and temperature precisely. Here, we demonstrate a reversible switching between PIA and thermally-driven recrystallization of VO 2(B) nanosheets. Comprehensive in situ experiments are performed to establish the precise conditions of the reversible phase transformations, which are normally hindered but occur with stimuli beyond the energy barrier. Spectral evidence and theoretical calculations reveal the pressure–structure relationship and the role of flexiblemore » VO x polyhedra in the structural switching process. Anomalous resistivity evolution and the participation of spin in the reversible phase transition are observed for the first time. Our findings have significant implications for the design of phase switching devices and the exploration of hidden amorphous materials.« less

Oxide Dissolution and Oxygen Diffusion in Solid-State Recycled Ti-6Al-4V: Numerical Modeling, Verification by Nanoindentation, and Effects on Grain Growth and Recrystallization

NASA Astrophysics Data System (ADS)

Lui, E. W.; Palanisamy, S.; Dargusch, M. S.; Xia, K.

2017-12-01

The oxide dissolution and oxygen diffusion during annealing of Ti-6Al-4V solid-state recycled from machining chips by equal-channel angular pressing (ECAP) have been investigated using nanoindentation and numerical modeling. The hardness profile from nanoindentation was converted into the oxygen concentration distribution using the Fleisher and Friedel model. An iterative fitting method was then employed to revise the ideal model proposed previously, leading to correct predictions of the oxide dissolution times and oxygen concentration profiles and verifying nanoindentation as an effective method to measure local oxygen concentrations. Recrystallization started at the prior oxide boundaries where local strains were high from the severe plastic deformation incurred in the ECAP recycling process, forming a band of ultrafine grains whose growth was retarded by solute dragging thanks to high oxygen concentrations. The recrystallized fine-grained region would advance with time to eventually replace the lamellar structure formed during ECAP.

Early Stages of Microstructure and Texture Evolution during Beta Annealing of Ti-6Al-4V

NASA Astrophysics Data System (ADS)

Pilchak, A. L.; Sargent, G. A.; Semiatin, S. L.

2018-03-01

The early stages of microstructure evolution during annealing of Ti-6Al-4V in the beta phase field were established. For this purpose, a series of short-time heat treatments was performed using sheet samples that had a noticeable degree of alpha-phase microtexture in the as-received condition. Reconstruction of the beta-grain structure from electron-backscatter-diffraction measurements of the room-temperature alpha-phase texture revealed that microstructure evolution at short times was controlled not by general grain growth, but rather by nucleation-and-growth events analogous to discontinuous recrystallization. The nuclei comprised a small subset of beta grains that were highly misoriented relative to those comprising the principal texture component of the beta matrix. From a quantitative standpoint, the transformation kinetics were characterized by an Avrami exponent of approximately unity, thus suggestive of metadynamic recrystallization. The recrystallization process led to the weakening and eventual elimination of the initial beta texture through the growth of a population of highly misoriented grains.

Surface recrystallization theory of the wear of copper in liquid methane

NASA Technical Reports Server (NTRS)

Bill, R. C.; Wisander, D. W.

1974-01-01

Copper was subjected to sliding against 440C in liquid methane. The normal load range was from 1/4 to 2 kilograms, and the sliding velocity range was from 3.1 to 25 meters per second. Over this range of experimental parameters, the wear rate of the copper rider was found to be proportional to the sliding velocity squared and to the normal load. Transmission electron microscopy was used to study the dislocation structure in the copper very near the wear scar surface. It was found that near the wear scar surface, the microstructure was characterized by a fine-cell recrystallized zone in which individual dislocations could be distinguished in the cell walls. The interiors of the cells, about 0.5 micrometer in diameter, were nearly dislocation free. Below the recrystallized layer was a zone that was intensely cold worked by the friction process. With increasing depth, this intensely cold worked zone gradually became indistinguishable from the partially cold worked bulk of the copper, representative of the initial condition of the material.

Preparation of highly pure zeaxanthin particles from sea water-cultivated microalgae using supercritical anti-solvent recrystallization.

PubMed

Chen, Chao-Rui; Hong, Siang-En; Wang, Yuan-Chuen; Hsu, Shih-Lan; Hsiang, Daina; Chang, Chieh-Ming J

2012-01-01

Xanthophylls, including zeaxanthin, are considered dietary supplements with a potentially positive impact on age-related macular degeneration. Using pilot-scale column fractionation coupled with supercritical anti-solvent (SAS) recrystallization, highly pure zeaxanthin particulates were prepared from ultrasonic extracts of the microalgae, Nannochloropsis oculata, grown in sea water. Column partition chromatography increased the concentration of zeaxanthin from 36.2 mg/g of the ultrasonic extracts to 425.6 mg/g of the collected column fractions. A response surface methodology was systematically designed for the SAS process by changing feed concentration, CO(2) flow rate and anti-solvent pressure. Zeaxanthin-rich particles with a purity of 84.2% and a recovery of 85.3% were produced using supercritical anti-solvent recrystallization from the column eluate at a feed concentration of 1.5 mg/mL, CO(2) flow rate of 48.6 g/min and pressure of 135 bar. Copyright © 2011 Elsevier Ltd. All rights reserved.

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.

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)

Prediction of the Grain-Microstructure Evolution Within a Friction Stir Welding (FSW) Joint via the Use of the Monte Carlo Simulation Method

NASA Astrophysics Data System (ADS)

Grujicic, M.; Ramaswami, S.; Snipes, J. S.; Avuthu, V.; Galgalikar, R.; Zhang, Z.

2015-09-01

A thermo-mechanical finite element analysis of the friction stir welding (FSW) process is carried out and the evolution of the material state (e.g., temperature, the extent of plastic deformation, etc.) monitored. Subsequently, the finite-element results are used as input to a Monte-Carlo simulation algorithm in order to predict the evolution of the grain microstructure within different weld zones, during the FSW process and the subsequent cooling of the material within the weld to room temperature. To help delineate different weld zones, (a) temperature and deformation fields during the welding process, and during the subsequent cooling, are monitored; and (b) competition between the grain growth (driven by the reduction in the total grain-boundary surface area) and dynamic-recrystallization grain refinement (driven by the replacement of highly deformed material with an effectively "dislocation-free" material) is simulated. The results obtained clearly revealed that different weld zones form as a result of different outcomes of the competition between the grain growth and grain refinement processes.

Investigation of recrystallization of amorphous trehalose through hot-humidity stage X-ray powder diffraction.

PubMed

Jójárt-Laczkovich, Orsolya; Katona, Gábor; Aigner, Zoltán; Szabó-Révész, Piroska

2016-12-01

The aim of this work was an investigation of the physical changes of the amorphous model material spray-dried trehalose through the use of various analytical techniques and to identify a suitable, rapid method able to quantify the changes. The crystallinity changes and recrystallization process of amorphous samples were investigated by hot-humidity stage X-ray powder diffractometry (HH-XRPD) with fresh samples, conventional X-ray powder diffractometry (XRPD) used stored samples and by differential scanning calorimetry (DSC). The data from the three methods were compared and the various forms of trehalose were analysed. HH-XRPD demonstrated that the recrystallization began at 40 and 60°C up to 45% RH and at 70°C up to 30% RH into dihydrate form. At 70°C up to 60% RH the anhydrous form of trehalose appeared too. Conventional XRPD results showed, that in the 28days stored samples the dihydrate form was detected at 40°C, 50% RH. Storage at 60°C, 40% RH resulted in the appearance of the anhydrous form and at 60°C, 50% RH both polymorphic forms were detected. By carrying out the DSC measurements at different temperatures the fraction of recrystallized trehalose dihydrate was detected. The recrystallization investigated by HH-XRPD and DSC followed Avrami kinetics, the calculated rate constants of isothermal crystallization (K) were same. Both HH-XRPD and conventional XRPD was suitable for the detection of the physical changes of the amorphous model material. DSC measurements showed similar results as HH-XRPD. Primarily HH-XRPD could be suggested for prediction, because the method is fast and every changes could be studied on one sample. Copyright © 2016 Elsevier B.V. All rights reserved.

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.

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.

Petrologic and chemical changes in ductile shear zones as a function of depth in the continental crust

NASA Astrophysics Data System (ADS)

Yang, Xin-Yue

Petrologic and geochemical changes in ductile shear zones are important for understanding deformational and geochemical processes of the continental crust. This study examines three shear zones that formed under conditions varying from lower greenschist facies to upper amphibolite facies in order to document the petrologic and geochemical changes of deformed rocks at various metamorphic grades. The studied shear zones include two greenschist facies shear zones in the southern Appalachians and an upper amphibolite facies shear zone in southern Ontario. The mylonitic gneisses and mylonites in the Roses Mill shear zone of central Virginia are derived from a ferrodiorite protolith and characterized by a lower greenschist facies mineral assemblage. Both pressure solution and recrystallization were operative deformation mechanisms during mylonitization in this shear zone. Strain-driven dissolution and solution transfer played an important role in the mobilization of felsic components (Si, Al, K, Na, and Ca). During mylonitization, 17% to 32% bulk rock volume losses of mylonites are mainly attributed to removal of these mobile felsic components by a fluid phase. Mafic components (Fe, Mg, Ti, Mn and P) and trace elements, REE, Y, V and Sc, were immobile. At Rosman, North Carolina, the Brevard shear zone (BSZ) shows a deformational transition from the coarse-grained Henderson augen gneiss (HAG) to proto-mylonite, mylonite and ultra-mylonite. The mylonites contain a retrograde mineral assemblage as a product of fluid-assisted chemical breakdown of K-feldspar and biotite at higher greenschist facies conditions. Recrystallization and intra-crystalline plastic deformation are major deformation mechanisms in the BSZ. Fluid-assisted mylonitization in the BSZ led to 6% to 23% bulk volume losses in mylonites. During mylonitization, both major felsic and mafic elements and trace elements, Rb, Sr, Zr, V, Sc, and LREE were mobile; however, the HREEs were likely immobile. A shear zone in the Parry Sound domain, Ontario, formed at upper amphibolite facies conditions. The deformation process of the shear zone involves fully plastic deformation and high-temperature dynamic recrystallization and annealing recovery of both quartz and plagioclase. Geochemical evidence indicates that the chemical changes in the deformed rocks resulted from mixing of mafic and felsic layers together with fluid-assisted mass transfer within the shear zone. A geochemical model that incorporates closed-system two-component mixing with open-system mass transfer can well explain the observed major and trace element data.

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

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.

High-temperature deformation processing of Ti-24Al-20Nb

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

Sagar, P.K.; Banerjee, D.; Muraleedharan, K.

1996-09-01

Power dissipation maps have been generated in the temperature range of 900 C to 1,150 C and strain rate range of 10{sup {minus}3} to 10 s{sup {minus}1} for a cast aluminide alloy Ti-24Al-20Nb using dynamic material model. The results define two distinct regimes of temperature and strain rate in which efficiency of power dissipation is maximum. The first region, centered around 975 C/0.1 s{sup {minus}1}, is shown to correspond to dynamic recrystallization of the {alpha}{sub 2} phase and the second, centered around 1,150 C/0.001 s{sup {minus}1}, corresponds to dynamic recovery and superplastic deformation of the {beta} phase. Thermal activation analysismore » using the power law creep equation yielded apparent activation energies of 854 and 627 kJ/mol for the first and second regimes, respectively. Reanalyzing the data by alternate methods yielded activation energies in the range of 170 to 220 kJ/mol and 220 to 270 kJ/mol for the first and second regimes, respectively. Cross slip was shown to constitute the activation barrier in both cases. Two distinct regimes of processing instability--one at high strain rates and the other at the low strain rates in the lower temperature regions--have been identified, within which shear bands are formed.« less

Highly efficient chiral resolution of DL-arginine by cocrystal formation followed by recrystallization under preferential-enrichment conditions.

PubMed

Iwama, Sekai; Kuyama, Kazunori; Mori, Yuko; Manoj, Kochunnoonny; Gonnade, Rajesh G; Suzuki, Katsuaki; Hughes, Colan E; Williams, P Andrew; Harris, Kenneth D M; Veesler, Stéphane; Takahashi, Hiroki; Tsue, Hirohito; Tamura, Rui

2014-08-11

An excellent chiral symmetry-breaking spontaneous enantiomeric resolution phenomenon, denoted preferential enrichment, was observed on recrystallization of the 1:1 cocrystal of dl-arginine and fumaric acid, which is classified as a racemic compound crystal with a high eutectic ee value (>95 %), under non-equilibrium crystallization conditions. On the basis of temperature-controlled video microscopy and in situ time-resolved solid-state (13) C NMR spectroscopic studies on the crystallization process, a new mechanism of phase transition that can induce preferential enrichment is proposed. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Direct observation of growth front movement in electron beam recrystallization of silicon layer on insulator

NASA Astrophysics Data System (ADS)

Inoue, Tomoyasu; Hamasaki, Toshihiko

1987-04-01

A high-speed movie technique was used to investigate the growth front movement during electron beam recrystallization of thin silicon layers on insulating material. In a laterally epitaxial growth process, it was clearly observed that the molten zone shape dramatically changes across a seed opening, which is due to nonuniformity in heat dissipation toward the substrate in the vicinity of the seed opening. The molten zone width and velocities of the melt front and growth front were quantitatively analyzed using digital film motion analysis. The growth front velocity was found to drastically change by ˜30% across the seed opening.

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.

Modeling of thermomechanical and metallurgical phenomena in steel strip during hot direct rolling and runout table cooling of thin-cast slabs

NASA Astrophysics Data System (ADS)

Muojekwu, Cornelius Anaedu

The present research was directed at adequate prediction of the temperature, deformation behavior (roll force, flow stress, strain and strain rate) and microstructural evolution (recovery, recrystallization, grain growth, austenite and ferrite grain sizes) during rolling in the Compact Strip Production (CSP) process, as well as the final mechanical properties of the hot rolled strips. This was accomplished with the aid of integrated process modeling, involving mathematical simulation, laboratory experiments and industrial campaigns. The study covered two conventional plain carbon steel grades, the A36 (AISI 1018, 0.17C-0.74Mn) and DQSK (AISI 1005, 0.038C-0.3Mn), and a range of plain carbon steel grades (0.06-0.09 C, 0.16-0.9 Mn) produced at HYLSA's CSP mill at Monterrey, Mexico. In the laboratory, compression tests (both single and double-hits) were carried out on the Gleeble 1500 thermomechanical simulator in order to elucidate the effect of coarse austenite grain size on the flow stress and recrystallization behavior of the plain carbon steels. It was found that coarse grain size not only decreased the flow stress at a given strain but also substantially reduced the tendency toward dynamic recrystallization. An increase in grain size from 244 to 1110 mum which is typical of the first stands of a conventional finishing mill and CSP hot-strip mill respectively, resulted in up to a 30 MPa decrease in the flow stress of both A36 and DQSK steel grades at similar operating conditions of temperature, strain and strain rate. In order to validate the model and laboratory results with mill measurements from an operating CSP plant, an industrial trial was carried out at HYLSA's CSP mill in Monterrey, Mexico. During the industrial campaign, intermediate temperature measurements were made, CSP slab and coil samples were acquired, and all measured and recorded mill data and practices were obtained. Comprehensive mathematical modeling of the rolling process was carried out employing finite difference and finite element analysis. The CSP mill measurements were utilized to validate model predictions of temperature, roll force, grain size and mechanical properties. Good agreement was obtained between prediction and measurement in most of the cases. An estimate of the heat extraction from the various mill sub-units was conducted from the validated calculations. It was found that heat loss by radiation accounted for 48-51 percent of the total heat loss, the work rolls accounted for 41-44 percent, the descaling unit accounted for 4-6 percent and the interstand sprays accounted for the remaining 3-4 percent. It was found that the uniform strain model consistently predicts lower temperatures than the target exit temperature for thin gauges due to a low estimate of deformation heat. Model results captured the details of heat transfer, deformation, recrystallization and austenite decomposition in the CSP mill. The effect of various mill parameters were elucidated, and the similarities and differences between conventional cold-charge rolling and CSP rolling were highlighted. (Abstract shortened by UMI.)

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

Refining the structural framework of the Khimti Khola region, east-central Nepal Himalaya, using quartz textures and c-axis fabrics

NASA Astrophysics Data System (ADS)

Larson, Kyle P.

2018-02-01

New quartz texture and c-axis fabric data from across the Paleoproterozoic Ulleri-Phaplu-Melung orthogneiss in the Khimti Khola region of east central Nepal provide new constraints on the internal structural framework of the Himalaya that help shed light on the convergence accommodation processes active in the upper portion of the crust during orogenesis. These data outline a strain history that varies across the unit. Deformation near the base of the unit occurred at ∼605 (±50) °C with evidence of significant static recrystallization and recovery preserved in quartz, whereas deformation near the top of the unit occurred at ∼540 (±50) ˚C with quartz characterized by dynamic recrystallization mechanisms. The strength of the quartz c-axis fabrics follows a similar spatial pattern, with those from near the top of the unit recording stronger fabrics than those measured from lower in the unit. Together, these data are interpreted to indicate strain localization, possibly at progressively lower temperature, near the top of the Ulleri-Phaplu-Melung orthogneiss. This interpretation is consistent with cooling ages that indicate the upper boundary of the unit coincides with an out-of-sequence shear zone. This study not only provides a structural characterization of the shear zone, helping to refine the kinematic framework of this portion of the Himalaya, but also confirms the utility of fabric strength analysis in deciphering strain localization within pervasively deformed rocks.

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.

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.

Constraining the Texture and Composition of Pore-Filling Cements at Gale Crater, Mars

NASA Technical Reports Server (NTRS)

Siebach, K. L.; Grotzinger, J. P.; McLennan, S. M.; Hurowitz, J. A.; Ming, D. W.; Vaniman, D. T.; Rampe, E. B.; Blaney, D. L.; Kah, L. C.

2015-01-01

The Mars Science Laboratory (MSL) rover Curiosity has encountered a wide variety of sedimentary rocks deposited in fluvio-lacuestrine sequences at the base of Gale Crater. The presence of sedimentary rocks requires that initial sediments underwent diagenesis and were lithified. Lithification involves sediment compaction, cementation, and re-crystallization (or authigenic) processes. Analysis of the texture and composition of the cement can reveal the environmental conditions when the cements were deposited, enabling better understanding of early environments present within Gale Crater. The first step in lithification is sediment compaction. The Gale crater sediments do not show evidence for extensive compaction prior to cementation; the Sheepbed mudstone in Yellowknife Bay (YKB) has preserved void spaces ("hollow nodules"), indicating that sediments were cemented around the hollow prior to compaction, and conglomerates show imbrication, indicating minimal grain reorganization prior to lithification. Furthermore, assuming the maximum burial depth of these sediments is equivalent to the depth of Gale Crater, the sediments were never under more than 1 kb of pressure, and assuming a 15 C/km thermal gradient in the late Noachian, the maximum temperature of diagenesis would have been approximately 75 C. This is comparable to shallow burial diagenetic conditions on Earth. The cementation and recrystallization components of lithification are closely intertwined. Cementation describes the precipitation of minerals between grains from pore fluids, and recrystallization (or authigenesis) is when the original sedimentary mineral grains are altered into secondary minerals. The presence of authigenic smectites and magnetite in the YKB formation suggests that some recrystallization has taken place. The relatively high percentage of XRD-amorphous material (25-40%) detected by CheMin suggests that this recrystallization may be limited in scope, and therefore may not contribute significantly to the cementing material. However, relatively persistent amorphous components could exist in the Martian environment (e.g. amorphous MgSO4), so recrystallization, including loss of crystallinity, cannot yet be excluded as a method of cementation. In order to describe the rock cementation, both the rock textures and their composition must be considered. Here, we attempt to summarize the current understanding of the textural and compositional aspects of the cement across the rocks analyzed by Curiosity to this point.

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

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

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.

Modified laser-annealing process for improving the quality of electrical P-N junctions and devices

DOEpatents

Wood, Richard F.; Young, Rosa T.

1984-01-01

The invention is a process for producing improved electrical-junction devices. The invention is applicable, for example, to a process in which a light-sensitive electrical-junction device is produced by (1) providing a body of crystalline semiconductor material having a doped surface layer, (2) irradiating the layer with at least one laser pulse to effect melting of the layer, (3) permitting recrystallization of the melted layer, and (4) providing the resulting body with electrical contacts. In accordance with the invention, the fill-factor and open-circuit-voltage parameters of the device are increased by conducting the irradiation with the substrate as a whole at a selected elevated temperature, the temperature being selected to effect a reduction in the rate of the recrystallization but insufficient to effect substantial migration of impurities within the body. In the case of doped silicon substrates, the substrate may be heated to a temperature in the range of from about 200.degree. C. to 500.degree. C.

Effect of processing parameters on the earing and mechanical properties of strip cast type 3004 Al alloy

NASA Astrophysics Data System (ADS)

Es-Said, O. S.; Zeihen, A.; Ruprich, M.; Quattrocchi, J.; Thomas, M.; H. Shin, K.; O'Brien, M.; Johansen, D.; Tijoe, W. H.; Ruhl, D.

1995-06-01

Electrical resistivity, superficial hardness, tensile testing, and quantitative metallography techniques were used in this study. The strip cast type 3004 aluminum alloy received sixteen different thermomechanical treatments before cups were drawn. The top edges of the drawn cups were not flat. Rather there were high points or ears with valleys between them. The homogenization temperature varied form 510 to 621 °C at 24 h. Some samples received an additional 426 °C/24 h homogenization anneal. Most specimens were rolled along the longitudinal direction of the as-cast material, and some were rolled in the transverse direction. Most samples were recrystallized at 454 °C for 24 h in addition to the homogenization treatment. Some were recrystallized for 168 h. All samples were subsequently rolled to 0.33 mm for cup drawing and percent earing determination. The percent earing results of some samples were less than 1.5%, but the mechanical strength was also lowered. The high-temperature recrystallization anneal of 454 °C was the controlling factor in determining the earing and mechanical strength of the final rolled sheet.

Effect of processing parameters on the earing and mechanical properties of strip cast type 3004 Al alloy

NASA Astrophysics Data System (ADS)

Es-Said, O. S.; Zeihen, A.; Ruprich, M.; Quattrocchi, J.; Thomas, M.; Shin, K. H.; O'Brien, M.; Johansen, D.; Tijoe, W. H.; Ruhl, D.

1994-02-01

Electrical resistivity, superficial hardness, tensile testing, and quantitative metallography techniques were used in this study. The strip cast type 3004 aluminum alloy received sixteen different thermomechanical treatments before cups were drawn. The top edges of the drawn cups were not flat. Rather, there were high points or ears with valleys between them. The homogenization temperature varied from 510 to 621 °C at 24 h. Some samples received an additional 426 °C/24 h homogenization anneal. Most specimens were rolled along the longitudinal direction of the as-cast material, and some were rolled in the transverse direction. Most samples were recrystallized at 454 °C for 24 h in addition to the homogenization treatment. Some were recrystallized for 168 h. All samples were subsequently rolled to 0.33 mm for cup drawing and percent earing determination. The percent earing results of some samples were less than 1.5%, but the mechanical strength was also lowered. The high-temperature recrystallization anneal of 454 °C was the controlling factor in determining the earing and mechanical strength of the final rolled sheet.

Grain Cluster Microstructure and Grain Boundary Character Distribution in Alloy 690

NASA Astrophysics Data System (ADS)

Xia, Shuang; Zhou, Bangxin; Chen, Wenjue

2009-12-01

The effects of thermal-mechanical processing (TMP) on microstructure evolution during recrystallization and grain boundary character distribution (GBCD) in aged Alloy 690 were investigated by the electron backscatter diffraction (EBSD) technique and optical microscopy. The original grain boundaries of the deformed microstructure did not play an important role in the manipulation of the proportion of the Σ3 n ( n = 1, 2, 3…) type boundaries. Instead, the grain cluster formed by multiple twinning starting from a single nucleus during recrystallization was the key microstructural feature affecting the GBCD. All of the grains in this kind of cluster had Σ3 n mutual misorientations regardless of whether they were adjacent. A large grain cluster containing 91 grains was found in the sample after a small-strain (5 pct) and a high-temperature (1100 °C) recrystallization anneal, and twin relationships up to the ninth generation (Σ39) were found in this cluster. The ratio of cluster size over grain size (including all types of boundaries as defining individual grains) dictated the proportion of Σ3 n boundaries.

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.

3D microstructural evolution of primary recrystallization and grain growth in cold rolled single-phase aluminum alloys

NASA Astrophysics Data System (ADS)

Adam, Khaled; Zöllner, Dana; Field, David P.

2018-04-01

Modeling the microstructural evolution during recrystallization is a powerful tool for the profound understanding of alloy behavior and for use in optimizing engineering properties through annealing. In particular, the mechanical properties of metallic alloys are highly dependent upon evolved microstructure and texture from the softening process. In the present work, a Monte Carlo (MC) Potts model was used to model the primary recrystallization and grain growth in cold rolled single-phase Al alloy. The microstructural representation of two kinds of dislocation densities, statistically stored dislocations and geometrically necessary dislocations were quantified based on the ViscoPlastic Fast Fourier transform method. This representation was then introduced into the MC Potts model to identify the favorable sites for nucleation where orientation gradients and entanglements of dislocations are high. Additionally, in situ observations of non-isothermal microstructure evolution for single-phase aluminum alloy 1100 were made to validate the simulation. The influence of the texture inhomogeneity is analyzed from a theoretical point of view using an orientation distribution function for deformed and evolved texture.

Kinetics of Sub-Micron Grain Size Refinement in 9310 Steel

NASA Astrophysics Data System (ADS)

Kozmel, Thomas; Chen, Edward Y.; Chen, Charlie C.; Tin, Sammy

2014-05-01

Recent efforts have focused on the development of novel manufacturing processes capable of producing microstructures dominated by sub-micron grains. For structural applications, grain refinement has been shown to enhance mechanical properties such as strength, fatigue resistance, and fracture toughness. Through control of the thermo-mechanical processing parameters, dynamic recrystallization mechanisms were used to produce microstructures consisting of sub-micron grains in 9310 steel. Starting with initial bainitic grain sizes of 40 to 50 μm, various levels of grain refinement were observed following hot deformation of 9310 steel samples at temperatures and strain rates ranging from 755 K to 922 K (482 °C and 649 °C) and 1 to 0.001/s, respectively. The resulting deformation microstructures were characterized using scanning electron microscopy and electron backscatter diffraction techniques to quantify the extent of carbide coarsening and grain refinement occurring during deformation. Microstructural models based on the Zener-Holloman parameter were developed and modified to include the effect of the ferrite/carbide interactions within the system. These models were shown to effectively correlate microstructural attributes to the thermal mechanical processing parameters.

Improving hydro-formability of stainless steel tubes by tube channel pressing

NASA Astrophysics Data System (ADS)

Kitano, Y.; Yuasa, M.; Miyamoto, H.; Farshidi, M. H.; Bagherpour, E.

2017-05-01

Tube channel pressing (TCP), which is one of the severe plastic deformation (SPD) technologies to refine grain size into submicron size for tubular materials, have been applied to ferritic stainless steel tubes for one pass, in order to alleviate ridging and enhance the hydro-formability. It was found that grain-scale shear bands were introduced by one-pass TCP, and texture and microstructure was successfully modified by promoting recrystallization of deformation microstructure, which is otherwise hard-to-recrystallize, in the post-TCP annealing. Elongation to failure, strain-hardening exponent (n-value) and Lankford values of both longitudinal and circumferential directions increased in comparison to with the tube fabricated by conventional process.

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.

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.

Synthesis of hexagonal wurtzite Cu{sub 2}ZnSnS{sub 4} prisms by an ultrasound-assisted microwave solvothermal method

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

Long, Fei, E-mail: long.drf@gmail.com; Chi, Shangsen; Institute of Advanced Materials and Technology, University of Science and Technology Beijing, Beijing 100083

Wurtzite Cu{sub 2}ZnSnS{sub 4} (CZTS) hexagonal prisms were synthesized by a simple ultrasound-microwave solvothermal method. The product was characterized by XRD, FESEM, EDS, TEM, Raman and UV–vis spectrometer. The hexagonal prisms were 0.5–2 μm wide and 5–12 μm long. The PVP played an important role in the formation of the CZTS hexagonal prisms. In addition, the ultrasound-assisted microwave process was helpful for synthesis of wurtzite rather than kesterite phase CZTS. A nucleation–dissolution–recrystallization mechanism was also proposed to explain the growth of the CZTS hexagonal prisms. - Graphical abstract: Wurtzite Cu{sub 2}ZnSnS{sub 4} hexagonal prisms were synthesized by ultrasound-microwave solvothermal method.more » The ultrasound-assisted microwave process and PVP were useful to the growth of CZTS. A nucleation–dissolution–recrystallization growth mechanism was also proposed. - Highlights: • Wurtzite Cu{sub 2}ZnSnS{sub 4} was prepared by ultrasound-assisted microwave solvothermal method. • The wurtzite CZTS hexagonal prisms are demonstrated a band gap of 1.49 eV. • Synergistic effect of ultrasound and microwave is helpful to prepare Wurtzite CZTS. • PVP plays an important role in the formation of the CZTS hexagonal prisms. • Nucleation–dissolution–recrystallization growth mechanism of the CZTS was proposed.« less

Melt extrusion vs. spray drying: The effect of processing methods on crystalline content of naproxen-povidone formulations.

PubMed

Haser, Abbe; Cao, Tu; Lubach, Joe; Listro, Tony; Acquarulo, Larry; Zhang, Feng

2017-05-01

Our hypothesis is that melt extrusion is a more suitable processing method than spray drying to prepare amorphous solid dispersions of drugs with a high crystallization tendency. Naproxen-povidone K25 was used as the model system in this study. Naproxen-povidone K25 solid dispersions at 30% and 60% drug loadings were characterized by modulated DSC, powder X-ray diffraction, FT-IR, and solid-state 13 C NMR to identify phase separation and drug recrystallization during processing and storage. At 30% drug loading, hydrogen bond (H-bond) sites of povidone K25 were not saturated and the glass transition (T g ) temperature of the formulation was higher. As a result, both melt-extruded and spray-dried materials were amorphous initially and remained so after storage at 40°C. At 60% drug loading, H-bond sites were saturated, and T g was low. We were not able to prepare amorphous materials. The initial crystallinity of the formulations was 0.4%±0.2% and 5.6%±0.6%, and increased to 2.7%±0.3% and 21.6%±1.0% for melt-extruded and spray-dried materials, respectively. Spray-dried material was more susceptible to re-crystallization during processing, due to the high diffusivity of naproxen molecules in the formulation matrix and lack of kinetic stabilization from polymer solution. A larger number of crystalline nucleation sites and high surface area made the spray-dried material more susceptible to recrystallization during storage. This study demonstrated the unique advantages of melt extrusion over spray drying for the preparation of amorphous solid dispersions of naproxen at high drug level. Copyright © 2017 Elsevier B.V. All rights reserved.

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.

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.

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

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.

Size Controllable, Transparent, and Flexible 2D Silver Meshes Using Recrystallized Ice Crystals as Templates.

PubMed

Wu, Shuwang; Li, Linhai; Xue, Han; Liu, Kai; Fan, Qingrui; Bai, Guoying; Wang, Jianjun

2017-10-24

Ice templates have been widely utilized for the preparation of porous materials due to the obvious advantages, such as environmentally benign and applicable to a wide range of materials. However, it remains a challenge to have controlled pore size as well as dimension of the prepared porous materials with the conventional ice template, since it often employs the kinetically not-stable growing ice crystals as the template. For example, there is no report so far for the preparation of 2D metal meshes with tunable pore size based on the ice template, although facile and eco-friendly prepared metal meshes are highly desirable for wearable electronics. Here, we report the preparation of 2D silver meshes with tunable mesh size employing recrystallized ice crystals as templates. Ice recrystallization is a kinetically stable process; therefore, the grain size of recrystallized ice crystals can be easily tuned, e.g., by adding different salts and changing the annealing temperature. Consequently, the size and line width of silver meshes obtained after freeze-drying can be easily adjusted, which in turn varied the conductivity of the obtained 2D silver film. Moreover, the silver meshes are transparent and display stable conductivity after the repeated stretching and bending. It can be envisioned that this approach for the preparation of 2D conducting films is of practical importance for wearable electronics. Moreover, this study provides a generic approach for the fabrication of 2D meshes with a controllable pore size.

Microfibrous Solid Dispersions of Poorly Water-Soluble Drugs Produced via Centrifugal Spinning: Unexpected Dissolution Behavior on Recrystallization.

PubMed

Marano, Stefania; Barker, Susan A; Raimi-Abraham, Bahijja T; Missaghi, Shahrzad; Rajabi-Siahboomi, Ali; Aliev, Abil E; Craig, Duncan Q M

2017-05-01

Temperature-controlled, solvent-free centrifugal spinning may be used as a means of rapid production of amorphous solid dispersions in the form of drug-loaded sucrose microfibers. However, due to the high content of amorphous sucrose in the formulations, such microfibers may be highly hygroscopic and unstable on storage. In this study, we explore both the effects of water uptake of the microfibers and the consequences of deliberate recrystallization for the associated dissolution profiles. The stability of sucrose microfibers loaded with three selected BCS class II model drugs (itraconazole (ITZ), olanzapine (OLZ), and piroxicam (PRX)) was investigated under four different relative humidity conditions (11, 33, 53, and 75% RH) at 25 °C for 8 months, particularly focusing on the effect of the highest level of moisture (75% RH) on the morphology, size, drug distribution, physical state, and dissolution performance of microfibers. While all samples were stable at 11% RH, at 33% RH the ITZ-sucrose system showed greater resistance against devitrification compared to the OLZ- and PRX-sucrose systems. For all three samples, the freshly prepared microfibers showed enhanced dissolution and supersaturation compared to the drug alone and physical mixes; surprisingly, the dissolution advantage was largely maintained or even enhanced (in the case of ITZ) following the moisture-induced recrystallization under 75% RH. Therefore, this study suggests that the moisture-induced recrystallization process may result in considerable dissolution enhancement compared to the drug alone, while overcoming the physical stability risks associated with the amorphous state.

Thermal Decomposition of Nd3(+), Sr2(+) and Pb2(+) Exchanged Beta’’ Aluminas,

DTIC Science & Technology

1987-07-01

reconstructive recrystallization process is responsible for the formation of the MP phase; this perhaps is a surprising result. The decomposition processes of Nd3... eutectics may be present. A general trend for all decompositions of metastable substituted " aluminas would therefore seem to be that when occurring

Synthesis of polycrystalline Co{sub 3}O{sub 4} nanowires with excellent ammonium perchlorate catalytic decomposition property

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

Zhou, Hai; University of Chinese Academy of Sciences, Beijing 100049; Lv, Baoliang, E-mail: lbl604@sxicc.ac.cn

2014-12-15

Graphical abstract: Co{sub 3}O{sub 4} nanowires with excellent ammonium perchlorate catalytic decomposition property were synthesized via a methanamide-assisted hydrolysis and subsequent dissolution–recrystallization process in the presence of methanamide. - Abstract: Co{sub 3}O{sub 4} nanowires, with the length of tens of micrometers and the width of several hundred nanometers, were produced by a hydrothermal treatment and a post-anneal process. X-ray diffraction (XRD) result showed that the Co{sub 3}O{sub 4} nanowires belong to cubic crystal system. Scanning electron microscopy (SEM) and high-resolution transmission electron microscopy (HRTEM) analysis indicated that the Co{sub 3}O{sub 4} nanowires, composed by single crystalline nanoparticles, were of polycrystallinemore » nature. On the basis of time-dependent experiments, methanamide-assisted hydrolysis and subsequent dissolution–recrystallization process were used to explain the precursors' formation process of the polycrystalline Co{sub 3}O{sub 4} nanowires. The TGA experiments showed that the as-obtained Co{sub 3}O{sub 4} nanowires can catalyze the thermal decomposition of ammonium perchlorate (AP) effectively.« less

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

Molecular dynamics and crystallization phenomenon of supercooled and glassy DNA and RNA nucleosides: β-adenosine, β-thymidine, and β-uridine

NASA Astrophysics Data System (ADS)

Adrjanowicz, K.; Wojnarowska, Z.; Grzybowska, K.; Hawelek, L.; Kaminski, K.; Paluch, M.; Kasprzycka, A.; Walczak, K.

2011-11-01

Nucleosides are chemical compounds that have an extremely important biological role; they can be found in all types of living organisms. They are crucial components from which DNA and RNA acids are built. In addition, nucleosides are key regulators of many physiological processes. In this paper, the molecular dynamics in the liquid and glassy state of three selected nucleosides, β-adenosine, β-thymidine, and β-uridine, was investigated by means of dielectric spectroscopy. Our results revealed multiple relaxation processes associated with different types of molecular motions. Besides the primary α relaxation, two secondary modes in the glassy states of examined compounds were identified. Crystallization progress monitored by dielectric spectroscopy and x-ray diffraction technique at isostructural relaxation conditions revealed that the examined nucleosides possess completely different tendencies to recrystallize from the liquid as well as the glassy state. We have also made an attempt to predict the time scale of molecular motion below the glass transition temperatures of the respective nucleosides to discuss their potential stability at room temperature over prolonged storage time. Finally, combination of molecular mobility studies with evaluation of thermodynamic parameters from calorimetric measurements allowed us to discuss the fundamental roles of both kinetic and thermodynamic factors in governing the physical stability of the glassy state.

Method of producing superplastic alloys and superplastic alloys produced by the method

NASA Technical Reports Server (NTRS)

Troeger, Lillianne P. (Inventor); Starke, Jr., Edgar A. (Inventor); Crooks, Roy (Inventor)

2002-01-01

A method for producing new superplastic alloys by inducing in an alloy the formation of precipitates having a sufficient size and homogeneous distribution that a sufficiently refined grain structure to produce superplasticity is obtained after subsequent PSN processing. An age-hardenable alloy having at least one dispersoid phase is selected for processing. The alloy is solution heat-treated and cooled to form a supersaturated solid solution. The alloy is plastically deformed sufficiently to form a high-energy defect structure useful for the subsequent heterogeneous nucleation of precipitates. The alloy is then aged, preferably by a multi-stage low and high temperature process, and precipitates are formed at the defect sites. The alloy then is subjected to a PSN process comprising plastically deforming the alloy to provide sufficient strain energy in the alloy to ensure recrystallization, and statically recrystallizing the alloy. A grain structure exhibiting new, fine, equiaxed and uniform grains is produced in the alloy. An exemplary 6xxx alloy of the type capable of being produced by the present invention, and which is useful for aerospace, automotive and other applications, is disclosed and claimed. The process is also suitable for processing any age-hardenable aluminum or other alloy.

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.

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.

Ultra-thin grain-oriented silicon steel sheet fabricated by a novel way: Twin-roll strip casting and two-stage cold rolling

NASA Astrophysics Data System (ADS)

Wang, Yin-Ping; Liu, Hai-Tao; Song, Hong-Yu; Liu, Jia-Xin; Shen, Hui-Ying; Jin, Yang; Wang, Guo-Dong

2018-04-01

0.05-0.15 mm-thick ultra-thin grain-oriented silicon steel sheets were successfully produced by a novel processing route including strip casting, hot rolling, normalizing, two-stage cold rolling with intermediate annealing, primary recrystallization annealing and secondary recrystallization annealing. The evolutions of microstructure, texture and inhibitor along the processing were briefly investigated. The results showed that the initial Goss orientation originated due to the heterogenous nucleation of δ-ferrite grains during solidification. Because of the lack of shear deformation, only a few Goss grains were observed in the hot rolled sheet. After the first cold rolling and intermediate annealing, Goss texture was enhanced and distributed in the whole thickness. A small number of Goss grains having a high fraction of high energy boundaries exhibited in the primary recrystallization annealed sheet. A large number of fine and dispersed MnS and AlN and a few co-precipitates MnS and AlN with the size range of 10-70 nm were also observed. Interestingly, a well-developed secondary recrystallization microstructure characterized by 10-60 mm grains and a sharp Goss texture were finally produced in the 0.05-0.15 mm-thick ultra-thin sheets. A magnetic induction B8 of 1.72-1.84 T was obtained. Another new finding was that a few {2 3 0}〈0 0 1〉 and {2 1 0}〈1 2 7〉 grains also can grow up abnormally because of the high fraction of high energy boundaries and the size and number advantage, respectively. These non-Goss grains finally deteriorated the magnetic properties of the ultra-thin sheets. In addition, low surface energies of {hk0} planes may also contribute to the abnormal growth of Goss, {2 3 0}〈0 0 1〉 and {2 1 0}〈1 2 7〉 grains.

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

Is Myanmar jadeitite of Jurassic age? A result from incompletely recrystallized inherited zircon

NASA Astrophysics Data System (ADS)

Yui, Tzen-Fu; Fukoyama, Mayuko; Iizuka, Yoshiyuki; Wu, Chao-Ming; Wu, Tsai-Way; Liou, J. G.; Grove, Marty

2013-02-01

Zircons from two Myanmar jadeitite samples were separated for texture, mineral inclusion, U-Pb dating and trace element composition analyses. Three types of zircons, with respect to U-Pb isotope system, were recognized. Type I zircons are inherited ones, yielding an igneous protolith age of 160 ± 1 Ma; Type II zircons are metasomatic/hydrothermal ones, giving a (minimum) jadeitite formation age of 77 ± 3 Ma; and Type III zircons are incompletely recrystallized ones, with non-coherent and geologically meaningless ages from 153 to 105 Ma. These Myanmar jadeitites would therefore have formed through whole-sale metasomatic replacement processes. Compared with Type I zircons, Type II zircons show typical metasomatic/hydrothermal geochemical signatures, with low Th/U ratio (< 0.1), small Ce anomaly (Ce/Ce* = < 5) and low ΣREE content (40-115 ppm). Type III zircons, however, commonly have the above geochemical signatures straddle in between Type I and Type II zircons. It is shown that the resetting rates of various trace element compositions and U-Pb isotope system of inherited zircons are not coupled "in phase" in response to zircon recrystallization during jadeitite formation. The observed abnormally low Th/U ratio and small Ce anomaly of some Type I zircons, as well as the lack of negative Eu anomaly of all Type I zircons, should be suspected to be of secondary origin. In extreme cases, incompletely recrystallized zircons may show typical metasomatic/hydrothermal geochemical signatures, but leave U-Pb isotope system partially reset or even largely unchanged. Such zircons easily lead to incorrect age interpretation, and hence erroneous geological implication. The Myanmar jadeitites, based on the present study, might have formed during the Late Cretaceous subduction before the beginning of India-Asia continental collision at Paleocene. Previously proposed Late Jurassic ages for Myanmar jadeitites are suggested as results rooted on data retrieved from incompletely recrystallized inherited zircons.

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

Characterization of the Hot Deformation Behavior of a Newly Developed Nickel-Based Superalloy

NASA Astrophysics Data System (ADS)

Shi, Zhaoxia; Yan, Xiaofeng; Duan, Chunhua; Tang, Cunjiang; Pu, Enxiang

2018-03-01

To clarify the microstructural evolution and hot workability of GH4282 during hot forming processes, the hot deformation behavior of this superalloy was investigated by isothermal compression tests in the temperature interval of 950-1210 °C and the strain rate range of 0.01-10 s-1 with a true strain of 0.7. The results show that the flow stresses decrease with an increase in the deformation temperature and a decrease in the strain rate. The characteristic of dynamic recrystallization is revealed by the flow curves. The variation rule of the flow stress can be well described by the hyperbolic sine type equation, and the thermal deformation activation energy is determined to be 498.118 kJ/mol. The optimum hot working parameters are 1100-1180 °C and 0.01-0.1 s-1, under which the fine and uniform microstructure can be obtained.

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

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.

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.

Heterogeneous brittle-ductile deformation at shallow crustal levels under high thermal conditions: The case of a synkinematic contact aureole in the inner northern Apennines, southeastern Elba Island, Italy

NASA Astrophysics Data System (ADS)

Papeschi, Samuele; Musumeci, Giovanni; Mazzarini, Francesco

2017-10-01

We present an example of interaction between magmatism and tectonics at shallow crustal levels. In the Late Miocene the metamorphic units of the eastern Elba Island (northern Apennines) were intruded at very shallow crustal levels by a large pluton (> 60 km2) with the development of an hectometre-sized contact aureole defined by growth of low-pressure/high-temperature mineral assemblages (Pmax < 0.2 GPa, Tmax 650 °C). Structural data show that the contact aureole is associated with a km-sized antiform of the foliation and by several metre- to decametre-thick high-strain domains consisting of strongly foliated rocks containing synkinematic HT/LP mineral assemblages and ductile shear zones of variable thickness. These shear zones are characterized by a mylonitic foliation variably overprinted by cataclasis. Quartz microfabrics indicate that the dynamic crystallization processes progressively changed from grain boundary migration, associated with the thermal peak of contact metamorphism, to subgrain rotation and bulging recrystallization, the latter mostly associated with the cataclastic overprint. These transitions of recrystallization mechanisms in quartz are related to a progressive decrease of temperature during deformation. Deformation accompanied the development and cooling of the contact aureole, which recorded the switch from high temperature ductile to low temperature brittle conditions. The geometry of the studied deformation structures is consistent with the constraints of the regional tectonic evolution and its local interaction with the localized and transient thermal anomaly related to the coeval emplacement of igneous rocks.

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.

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.

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

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.

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).

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.

Semantic modeling of the structural and process entities during plastic deformation of crystals and rocks

NASA Astrophysics Data System (ADS)

Babaie, Hassan; Davarpanah, Armita

2016-04-01

We are semantically modeling the structural and dynamic process components of the plastic deformation of minerals and rocks in the Plastic Deformation Ontology (PDO). Applying the Ontology of Physics in Biology, the PDO classifies the spatial entities that participate in the diverse processes of plastic deformation into the Physical_Plastic_Deformation_Entity and Nonphysical_Plastic_Deformation_Entity classes. The Material_Physical_Plastic_Deformation_Entity class includes things such as microstructures, lattice defects, atoms, liquid, and grain boundaries, and the Immaterial_Physical_Plastic_Deformation_Entity class includes vacancies in crystals and voids along mineral grain boundaries. The objects under the many subclasses of these classes (e.g., crystal, lattice defect, layering) have spatial parts that are related to each other through taxonomic (e.g., Line_Defect isA Lattice_Defect), structural (mereological, e.g., Twin_Plane partOf Twin), spatial-topological (e.g., Vacancy adjacentTo Atom, Fluid locatedAlong Grain_Boundary), and domain specific (e.g., displaces, Fluid crystallizes Dissolved_Ion, Void existsAlong Grain_Boundary) relationships. The dynamic aspect of the plastic deformation is modeled under the dynamical Process_Entity class that subsumes classes such as Recrystallization and Pressure_Solution that define the flow of energy amongst the physical entities. The values of the dynamical state properties of the physical entities (e.g., Chemical_Potential, Temperature, Particle_Velocity) change while they take part in the deformational processes such as Diffusion and Dislocation_Glide. The process entities have temporal parts (phases) that are related to each other through temporal relations such as precedes, isSubprocessOf, and overlaps. The properties of the physical entities, defined under the Physical_Property class, change as they participate in the plastic deformational processes. The properties are categorized into dynamical, constitutive, spatial, temporal, statistical, and thermodynamical. The dynamical properties, categorized under the Dynamical_Rate_Property and Dynamical_State_Property classes, subsume different classes of properties (e.g., Fluid_Flow_Rate, Temperature, Chemical_Potential, Displacement, Electrical_Charge) based on the physical domain (e.g., fluid, heat, chemical, solid, electrical). The properties are related to the objects under the Physical_Entity class through diverse object type (e.g., physicalPropertyOf) and data type (e.g., Fluid_Pressure unit 'MPa') properties. The changes of the dynamical properties of the physical entities, described by the empirical laws (equations) modeled by experimental structural geologists, are modeled through the Physical_Property_Dependency class that subsumes the more specialized constitutive, kinetic, and thermodynamic expressions of the relationships among the dynamic properties. Annotation based on the PDO will make it possible to integrate and reuse experimental plastic deformation data, knowledge, and simulation models, and conduct semantic-based search of the source data originating from different rock testing laboratories.

Electron backscatter and X-ray diffraction studies on the deformation and annealing textures of austenitic stainless steel 310S

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

Nezakat, Majid, E-mail: majid.nezakat@usask.ca

We studied the texture evolution of thermo-mechanically processed austenitic stainless steel 310S. This alloy was cold rolled up to 90% reduction in thickness and subsequently annealed at 1050 °C. At the early stages of deformation, strain-induced martensite was formed from deformed austenite. By increasing the deformation level, slip mechanism was found to be insufficient to accommodate higher deformation strains. Our results demonstrated that twinning is the dominant deformation mechanism at higher deformation levels. Results also showed that cold rolling in unidirectional and cross rolling modes results in Goss/Brass and Brass dominant textures in deformed samples, respectively. Similar texture components aremore » observed after annealing. Thus, the annealing texture was greatly affected by texture of the deformed parent phase and martensite did not contribute as it showed an athermal reversion during annealing. Results also showed that when the fraction of martensite exceeds a critical point, its grain boundaries impeded the movement of austenite grain boundaries during annealing. As a result, recrystallization incubation time would increase. This caused an incomplete recrystallization of highly deformed samples, which led to a rational drop in the intensity of the texture components. - Highlights: •Thermo-mechanical processing through different cold rolling modes can induce different textures. •Martensite reversion is athermal during annealing. •Higher fraction of deformation-induced martensite can increase the annealing time required for complete recrystallization. •Annealing texture is mainly influenced by the deformation texture of austenite.« less

Three Microstructural Exercises for Students.

ERIC Educational Resources Information Center

Means, Winthrop D.

1986-01-01

Describes laboratory exercises which demonstrate a new simplified technique for deforming thin samples of crystalline materials on the stage of a petrographic microscope. Discusses how this process allows students to see the development of microstructures resulting from cracking, slipping, thinning, and recrystallization. References and sources of…

Characterization of Microstructure and Mechanical Properties of Mg-8Li-3Al-1Y Alloy Subjected to Different Rolling Processes

NASA Astrophysics Data System (ADS)

Zhou, Xiao; Liu, Qiang; Liu, Ruirui; Zhou, Haitao

2018-06-01

The mechanical properties and microstructure evolution of Mg-8Li-3Al-1Y alloy undergoing different rolling processes were systematically investigated. X-ray diffraction, optical microscope, scanning electron microscopy, transmission electron microscopy as well as electron backscattered diffraction were used for tracking the microstructure evolution. Tensile testing was employed to characterize the mechanical properties. After hot rolling, the MgLi2Al precipitated in β-Li matrix due to the transformation reaction: β-Li → β-Li + MgLi2Al + α-Mg. As for the alloy subjected to annealed hot rolling, β-Li phase was clearly recrystallized while recrystallization rarely occurred in α-Mg phase. With regard to the microstructure undergoing cold rolling, plenty of dislocations and dislocation walls were easily observed. In addition, the microstructure of alloys subjected to annealed cold rolling revealed the formation of new fresh α-Mg grains in β-Li phase due to the precipitation reaction. The mechanical properties and fracture modes of Mg-8Li-3Al-1Y alloys can be effectively tuned by different rolling processes.

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.

Evolution of Residual Stress and Distortion of Cold-Rolled Bearing Ring from Annealing to Quenched-Tempered Heat Treatment

NASA Astrophysics Data System (ADS)

Lu, Bohan; Lu, Xiaohui

2018-02-01

This study investigates the correlation between the residual stress and distortion behavior of a cold-rolled ring from the annealing to quenching-tempering (QT) process. Due to the cold-rolled process, the external periphery of the bearing ring experiences a compressive residual stress. To relieve the residual stress, cold-rolled rings are annealed at 700 °C which is higher than the starting temperature of recrystallization. When cold-rolled rings are annealed at 700 °C for 15 min, the compressive residual stress is reduced to zero and the outer diameter of the annealed ring becomes larger than that of a non-annealed sample, which is unrelated to annealing time. Simultaneously, the roundness and taper deviation do not obviously change compared with those of non-annealed sample. The stress relaxation during the annealing process was attributed to the recovery and recrystallization of ferrite. Annealing has a genetic influence on the following QT heat treatment, wherein the lowest residual stress is in the non-annealed cold-rolled ring. From the annealing to QT process, the deviation of the outer diameter, roundness, and taper increased with annealing time, a large extend than that of non-annealed samples.

Olivine tablets in peridotite xenoliths: Evidence for a static, foliation-producing recrystallization mechanism operative in the strained, fluid-bearing mantle

NASA Astrophysics Data System (ADS)

Špaček, Petr; Habler, Gerlinde; Krmíček, Lukáš; Libowitzky, Eugen

2014-05-01

The term "olivine tablet" is used for elongated, (sub-)idiomorphic, strain-free crystals of olivine with well developed parallel crystal faces, usually found in peridotite xenoliths. While only rarely occurring in basalt-hosted xenolith suites, such peculiar grains are relatively common in specific kimberlite-hosted peridotite xenoliths and often explained as a result of fluid-assisted recrystallization in xenoliths after their entrainment in host magma. Extremely well developed olivine tablets are common in some peridotite xenoliths from Pliocene Lutynia basanite (South Poland). These were studied in detail focusing on their crystallographic orientation and chemical composition in relation to their host grains, in order to learn more about their origin. The tablets are restricted to grain boundary regions of olivine(I) and enstatite or occur pervasively, in some cases constituting more than half of the rock volume. Together with strain-free mosaic grains they form a second generation of olivine growing at the expense of older and larger, strained olivine(I) grains. The tablets are typically 0.1-1 mm (up to 3 mm) long having typical aspect ratios of 2-3 (up to >10) and exhibit a strong shape preferred orientation at local scale or in the whole sample, in the latter case forming a distinct foliation in peridotite xenoliths. Tablet grains usually exhibit a lattice preferred orientation (LPOs) similar to the host olivine(I), suggesting that their orientation is inherited, likely by selective exaggerated growth of small grains at the margins of host grains (dynamically recrystallized grains were not observed directly). In some cases oriented growth of tablets along microcrackss, or planar sliding surfaces, is suggested by the microstructures. Traces of prominent tablet faces mostly correspond to (010) planes of tablet grains, while correlation to crystallographic orientations of host grains is poor. Compositional profiles across tablet/host grain boundaries (EMPA, long counting times) show Ca-enrichment (from 0.02-0.03 to 0.06-0.09 wt% CaO) in ≤50 μm wide rims both in tablets and host grains, and, in some cases a non-identified Al-rich phase at the grain boundary itself. However, the Ca-profiles are symmetric with respect to grain boundaries and therefore this enrichment is assumed to post-date the tablet growth, probably being linked to infiltration of components from the xenolith host magma (which is observed independently as pockets with alkali feldspar, a second generation of clinopyroxene and a third, high-Ca generation of olivine). Compositions in the cores of tablets and olivine(I) are virtually identical within the resolution of conventional EMPA. Trace element composition, analyzed by LA-ICP-MS in several tablet/host grain pairs, shows systematically and significantly higher P and Li contents in tablets relative to host grains: (P: 30-40 ppm in olivine(I) vs. 76-87 ppm in tablets; Li: 4.6-5.7 ppm in olivine(I) vs. 7.6-10.0 ppm in tablets). Preliminary polarized micro-FTIR spectra show generally low water contents in olivine, mostly below 10 ppm of H2O. The observed microstructural and compositional features suggest formation of tablets by fluid-assisted static recrystallization which took place in-situ in the upper mantle interacting with P- and Li-rich, Ca- and Fe-poor agents. This recrystallization resulted in the formation of a foliation in peridotite by parallelization of grain boundaries in recrystallized domains with the (010) plane of the original LPO pattern. Although such observations are relatively uncommon, they might document a poorly sampled but widespread process potentially important for shear localization and the acceleration of fluid migration in the mantle.

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

Improved electrochemical property of nanoparticle polyoxovanadate K7NiV13O38 as cathode material for lithium battery

NASA Astrophysics Data System (ADS)

Ni, Erfu; Uematsu, Shinya; Quan, Zhen; Sonoyama, Noriyuki

2013-06-01

Molecular cluster ion compound K7NiV13O38 (KNiV) has been studied as a novel cathode material for lithium ion battery. The nanoparticles are prepared by a simple re-crystallization method adding different volumes of acetone to the water solution containing the dissolved KNiV. The KNiV re-crystallized from water/acetone ratio of 1:5 shows the most uniform particle size distribution and the smallest particles with thickness of 100 nm and width of 150 nm. The nanoparticle KNiV shows significant improvement in initial discharge capacity and capacity retention after 50 cycles compared to the as-prepared micro-sized particles at various current densities. Ex situ XRD patterns demonstrate that the discharge-charge process proceeds with amorphous KNiV, which is independent from the crystal structure. Ex situ FT-IR spectra indicate that [NiV13O38]7- cluster ion is stable and reacts reversibly with lithium ion in the discharge-charge process.

Microstructures and mechanical behavior of magnesium processed by ECAP at ice-water temperature

NASA Astrophysics Data System (ADS)

Zuo, Dai; Li, Taotao; Liang, Wei; Wen, Xiyu; Yang, Fuqian

2018-05-01

Magnesium of high purity is processed by equal channel angular pressing (ECAP) up to eight passes at the ice-water temperature, in which a core–shell-like structure is used. The core–shell-like structure consists of pure iron (Fe) of 1.5 mm in thickness as the shell and magnesium (Mg) as the core. The microstructure, texture and mechanical behavior of the ECAP-processed Mg are studied. The ECAP processing leads to the formation of fine and equiaxed grains of ~1.1 µm. The basal planes initially parallel to the extrusion direction evolve to slanted basal planes with the tilting angle in a range of 25°–45° to the extrusion direction. Increasing the number of the extrusion passes leads to the decreasing of twins and dislocation density in grains, while individual grains after eight passes still have high dislocation density. The large decreases of twins and the dislocation density make dynamic recrystallization (DRX) difficult, resulting in the decrease of the degree of DRX. Tension test reveals that the mechanical behavior of the ECAP-processed Mg is dependent on grain refinement and textures. The yield strength of the ECAP-extruded Mg first increases with the decrease of the grain size, and then decreases with further decrease of the grain size.

The Effect of Hot Working on Structure and Strength of a Precipitation Strengthened Austenitic Stainless Steel

NASA Astrophysics Data System (ADS)

Mataya, M. C.; Carr, M. J.; Krauss, G.

1984-02-01

The development of microstructure and strength during forging in a γ' strengthened austenitic stainless steel, JBK-75, was investigated by means of forward extrusion of cylindrical specimens. The specimens were deformed in a strain range of 0.16 to 1.0, from 800°C to 1080°C, and at approximate strain rates of 2 (press forging) and 2 × 103 s-1 (high energy rate forging), and structures examined by light and transmission microscopy. Mechanical properties were determined by tensile testing as-forged and forged and aged specimens. The alloy exhibited an extremely wide variety of structures and properties within the range of forging pzrameters studied. Deformation at the higher strain rate via high energy rate forging resulted in unrecovered substructures and high strengths at low forging temperatures, and static recrystallization and low strengths at high temperatures. In contrast, however, deformation at the lower strain rate via press forging resulted in retention of the well developed subgrain structure and associated high strength produced at high forging temperatures and strains. At lower temperatures and strains during press forging a subgrain structure formed preferentially at high angle grain boundaries, apparently by a creep-type deformation mechanism. Dynamic recrystallization was not an important restoration mechanism for any of the forging conditions. The results are interpreted on the basis of stacking fault energy and the accumulation of strain energy during hot working. The significance of observed microstructural differences for equivalent deformation conditions (iso-Z, where Z is the Zener-Holloman parameter) is discussed in relation to the utilization of Z for predicting hot work structures and strengths. Aging showed that the γ' precipitation process is not affected by substructure and that the strengthening contributions, from substructure and precipitation, were independent and additive. Applications for these findings are discussed in terms of process design criteria.

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.

Optimization of consolidation parameters of 18Cr-ODS ferritic steel through microstructural and microtexture characterization

NASA Astrophysics Data System (ADS)

Dash, Manmath Kumar; Mythili, R.; Dasgupta, Arup; Saroja, S.

2018-04-01

This paper reports the optimization of consolidation process based on the evolution of microstructure, microtexture and densification in 18%-Cr Oxide Dispersion Strengthened steel. The steel powder of composition Fe-18Cr-0.01C-2W-0.25Ti-0.35Y2O3 has been consolidated by cold isostatic pressing (CIP) for green compaction after mechanical milling. Sintering (1000-1250 °C) and hot isostatic pressing (HIP) at 1150 °C has been employed to achieve good densification on compacted CIP specimen. The effect of sintering temperatures on densification behavior was evaluated and sintering at 1150°C was identified to be optimum for achieving good compaction (92% density) and homogeneous polygonal microstructure with a uniform distribution of fine pores. In addition, HIP of CIP product at 1150°C was found to yield a more homogeneous microstructure as compared to sintered product with 97% density. A static/dynamic recrystallization associated with (1 1 1) texture is observed during consolidation process. A statistical comparison has been made based on frequency of grain boundary distribution and associated texture with its theoretical attributes.

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.

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 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.

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.

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.

Thermal behavior of copper processed by ECAP at elevated temperatures

NASA Astrophysics Data System (ADS)

Gonda, Viktor

2018-05-01

Large amount of strengthening can be achieved by equal channel angular pressing (ECAP), by the applied severe plastic deformation during the processing. For pure metals, this high strength is accompanied with low thermal stability due to the large activation energy for recrystallization. In the present paper, the chosen technological route was elevated temperature single pass ECAP processing of copper, and its effect on the thermal behavior during the restoration processes of the deformed samples was studied.

Exploratory Development on a New Process to Produce Improved RDX crystals: Supercritical Fluid Anti-Solvent Recrystallization

DTIC Science & Technology

1988-05-02

G. and J. Chiovini. Decaffeination Process . U.S. Patent 4,251.559; 17 February 1981. 43. Friedrich, J.P.. G.R. List, and A.J. Leakin. Petroleum...0 CONTRACT REPORT BRL-CR-606 EXPLORATORY DEVELOPMENT ON A NEW PROCESS TO PRODUCE IMPROVED RDX CRYSTALS: SUPERCRITICAL FLUID ANTI-SOLVENT...CCESSION NO. 11. TITLE (icnude Sun• y Uasuihcanon) I . • EXPLORATORY DEVELOPMENT ON A NEW PROCESS TO PRODUCE IMPROVED RDX CRYSTALS: SUPERCRITICAL

Universal scaling of grain size distributions during dislocation creep

NASA Astrophysics Data System (ADS)

Aupart, Claire; Dunkel, Kristina G.; Angheluta, Luiza; Austrheim, Håkon; Ildefonse, Benoît; Malthe-Sørenssen, Anders; Jamtveit, Bjørn

2017-04-01

Grain size distributions are major sources of information about the mechanisms involved in ductile deformation processes and are often used as paleopiezometers (stress gauges). Several factors have been claimed to influence the stress vs grain size relation, including the water content (Jung & Karato 2001), the temperature (De Bresser et al., 2001), the crystal orientation (Linckens et al., 2016), the presence of second phase particles (Doherty et al. 1997; Cross et al., 2015), and heterogeneous stress distributions (Platt & Behr 2011). However, most of the studies of paleopiezometers have been done in the laboratory under conditions different from those in natural systems. It is therefore essential to complement these studies with observations of naturally deformed rocks. We have measured olivine grain sizes in ultramafic rocks from the Leka ophiolite in Norway and from Alpine Corsica using electron backscatter diffraction (EBSD) data, and calculated the corresponding probability density functions. We compared our results with samples from other studies and localities that have formed under a wide range of stress and strain rate conditions. All distributions collapse onto one universal curve in a log-log diagram where grain sizes are normalized by the mean grain size of each sample. The curve is composed of two straight segments with distinct slopes for grains above and below the mean grain size. These observations indicate that a surprisingly simple and universal power-law scaling describes the grain size distribution in ultramafic rocks during dislocation creep irrespective of stress levels and strain rates. Cross, Andrew J., Susan Ellis, and David J. Prior. 2015. « A Phenomenological Numerical Approach for Investigating Grain Size Evolution in Ductiley Deforming Rocks ». Journal of Structural Geology 76 (juillet): 22-34. doi:10.1016/j.jsg.2015.04.001. De Bresser, J. H. P., J. H. Ter Heege, and C. J. Spiers. 2001. « Grain Size Reduction by Dynamic Recrystallization: Can It Result in Major Theological Weakening? » International Journal of Earth Sciences 90 (1): 28-45. Doherty, R. D., D. A. Hughes, F. J. Humphreys, J. J. Jonas, D. J. Jensen, M. E. Kassner, W. E. King, T. R. McNelley, H. J. McQueen, and A. D. Rollett. 1997. « Current Issues in Recrystallization: A Review ». Materials Science and Engineering a-Structural Materials Properties Microstructure and Processing 238 (2): 219-74. doi:10.1016/S0921-5093(97)00424-3. Jung, H., and S. I. Karato. 2001. « Effects of Water on Dynamically Recrystallized Grain-Size of Olivine ». Journal of Structural Geology 23 (9): 1337-44. doi:10.1016/S0191-8141(01)00005-0. Linckens, J., G. Zulauf, and J. Hammer. 2016. « Experimental Deformation of Coarse-Grained Rock Salt to High Strain ». Journal of Geophysical Research-Solid Earth 121 (8): 6150-71. doi:10.1002/2016JB012890. Platt, J.P., and W.M. Behr. 2011. « Grainsize Evolution in Ductile Shear Zones: Implications for Strain Localization and the Strength of the Lithosphere ». Journal of Structural Geology 33 (4): 537-50. doi:10.1016/j.jsg.2011.01.018.

Physical and mechanical metallurgy of high purity Nb accelerator cavities.

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

Wright, N. T.; Bieler, T. R.; Pourgoghart , F.

2010-01-01

In the past decade, high Q values have been achieved in high purity Nb superconducting radio frequency (SRF) cavities. Fundamental understanding of the physical metallurgy of Nb that enables these achievements is beginning to reveal what challenges remain to establish reproducible and cost-effective production of high performance SRF cavities. Recent studies of dislocation substructure development and effects of recrystallization arising from welding and heat treatments and their correlations with cavity performance are considered. With better fundamental understanding of the effects of dislocation substructure evolution and recrystallization on electron and phonon conduction, as well as the interior and surface states, itmore » will be possible to design optimal processing paths for cost-effective performance using approaches such as hydroforming, which minimizes or eliminates welds in a cavity.« less

Physical and mechanical metallurgy of high purity Nb for accelerator cavities

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

Bieler, T. R.; Wright, N. T.; Pourboghrat, F.

2010-01-01

In the past decade, high Q values have been achieved in high purity Nb superconducting radio frequency (SRF) cavities. Fundamental understanding of the physical metallurgy of Nb that enables these achievements is beginning to reveal what challenges remain to establish reproducible and cost-effective production of high performance SRF cavities. Recent studies of dislocation substructure development and effects of recrystallization arising from welding and heat treatments and their correlations with cavity performance are considered. With better fundamental understanding of the effects of dislocation substructure evolution and recrystallization on electron and phonon conduction, as well as the interior and surface states, itmore » will be possible to design optimal processing paths for cost-effective performance using approaches such as hydroforming, which minimizes or eliminates welds in a cavity.« less

[Extraction, isolation and purification for ginkgolide B].

PubMed

Zhang, Chenfeng; Li, Minghui; Tang, Yun; Zhang, Yanhai; Shi, Min; Sheng, Longsheng

2010-08-01

To establish a simple extraction, isolation and purification method for ginkgolide B from ginkgo leaf. The optimum conditions of extraction, isolation and purification were studied by taking the transfer rate of ginkgolide B as index. Ginkgo leaf was extracted with 70% ethanol for three times, the extracts were concentrated to remove ethanol and diluted by water till the crude drug density reached 0.1 g x mL(-1). The dilution was adsorbed with HPD-450 macroporous resin. The impurities were eluted with 20% ethanol and ginkgolide B was eluted with 80% ethanol. Then the 80% ethanol eluant was concentrated and crystallized. Finally the crude crystals were recrystallized with isopropanol. The purity of the ginkgolide B recrystallization was 95%. The process was stable and easy to operate, which was suited to industrialized production.

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.

Modification of the crystal habit of celecoxib for improved processability.

PubMed

Banga, Sheere; Chawla, Garima; Varandani, Deepak; Mehta, B R; Bansal, Arvind K

2007-01-01

Crystallization is often used in the pharmaceutical industry for purification and isolation of drugs, and also as a means of generating polymorphs or isomorphs. The aim of this study was to investigate the role of extrinsic crystallization parameters on the crystallized product, with special emphasis on improving the mechanical properties of acicular celecoxib. Celecoxib isomorphs were prepared using different techniques (solvent crystallization and vapour diffusion) and crystallization conditions (solvents, stirring, degree of supersaturation, crystallization temperature and seeding). Powder X-ray diffractometry, spectroscopic and thermal methods were used to investigate physical characteristics of crystals. Growth kinetics and aggregation dynamics of crystallization in polar and non-polar solvents were simulated using a dynamic light scattering method. The quick appearance of broad peaks over the range of 10-8000 nm in chloroform during crystallization simulation studies indicated faster aggregation in non-polar solvents. Aspect ratio, flow, compressibility and surface area of recrystallized products were also determined. Surface topography was determined by atomic force microscopy and the lath-shaped crystals (aspect ratio of 2-4) exhibited a roughness index of 1.79 in comparison with 2.92 for needles. Overall, the lath-shaped isomorphs exhibited improved flow and better compressibility.

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.

Foveated Wide Field-of-View Imaging for Missile Warning/Tracking using Adaptive Optics

DTIC Science & Technology

2007-11-30

their melting temperatures are relatively high because of their long molecular conjugation. To lower the melting points, we have formulated eutectic ...compounds during recrystallization processes. 3. Polar, partially dissociated like organic acids, phenols or bases. Their dissociation level depends on the

Workshop on Repetitive Spark Gap Operation Held at Tamarron, Colorado on January 17-19, 1983.

DTIC Science & Technology

1983-05-20

microstructure . In addition, it is possible that because of temperature gradients, diffusion, and other related processes , recrystallization and grain growth are...characterized for explosive and laser shock events in many metals and alloys , (11,12). CHEMICAL AND PHYSICAL PROCESSES IN SPARK GAPS The chemical and... deposition and other reaction product formation). There are several examples of process characterization which support some of the reaction features

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

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.

The effect of water on recrystallization behavior and grain boundary morphology in calcite observations of natural marble mylonites

NASA Astrophysics Data System (ADS)

Schenk, Oliver; Urai, Janos L.; Evans, Brian

2005-10-01

Fluids are inferred to play a major role in the deformation and recrystallization of many minerals (e.g. quartz, olivine, halite, feldspar). In this study, we sought to identify the effect of fluids on grain boundary morphology and recrystallization processes in marble mylonites during shear zone evolution. We compared the chemistry, microstructure and mesostructure of calcite marble mylonites from the Schneeberg Complex, Southern Tyrole, Italy, to that from the Naxos Metamorphic Core Complex, Greece. These two areas were selected for comparison because they have similar lithology and resemble each other in chemical composition. In addition, calcite-dolomite geothermometry indicates similar temperatures for shear zone formation: 279±25 °C (Schneeberg Complex) and 271±15 °C (Naxos high-grade core). However, the two settings are different in the nature of the fluids present during the shear zone evolution. In the Schneeberg mylonites, both the alteration of minerals during retrograde metamorphism in the neighboring micaschists and the existence of veins suggest that aqueous fluids were present during mylonitization. The absence of these features in the Naxos samples indicates that aqueous fluids were not as prevalent during deformation. This conclusion is also supported by the stable isotope signature. Observations of broken and planar surfaces using optical and scanning electron microscopes did not indicate major differences between the two mylonites: grain boundaries in both settings display pores with shapes controlled by crystallography, and have pore morphologies that are similar to observations from crack and grain-boundary healing experiments. Grain size reduction was predominantly the result of subgrain rotation recrystallization. However, the coarse grains inside the wet protomylonites (Schneeberg) are characterized by intracrystalline shear zones.

Inhibition of ice recrystallization and cryoprotective activity of wheat proteins in liver and pancreatic cells

PubMed Central

Chow‐Shi‐Yée, Mélanie; Briard, Jennie G.; Grondin, Mélanie; Averill‐Bates, Diana A.

2016-01-01

Abstract Efficient cryopreservation of cells at ultralow temperatures requires the use of substances that help maintain viability and metabolic functions post‐thaw. We are developing new technology where plant proteins are used to substitute the commonly‐used, but relatively toxic chemical dimethyl sulfoxide. Recombinant forms of four structurally diverse wheat proteins, TaIRI‐2 (ice recrystallization inhibition), TaBAS1 (2‐Cys peroxiredoxin), WCS120 (dehydrin), and TaENO (enolase) can efficiently cryopreserve hepatocytes and insulin‐secreting INS832/13 cells. This study shows that TaIRI‐2 and TaENO are internalized during the freeze–thaw process, while TaBAS1 and WCS120 remain at the extracellular level. Possible antifreeze activity of the four proteins was assessed. The “splat cooling” method for quantifying ice recrystallization inhibition activity (a property that characterizes antifreeze proteins) revealed that TaIRI‐2 and TaENO are more potent than TaBAS1 and WCS120. Because of their ability to inhibit ice recrystallization, the wheat recombinant proteins TaIRI‐2 and TaENO are promising candidates and could prove useful to improve cryopreservation protocols for hepatocytes and insulin‐secreting cells, and possibly other cell types. TaENO does not have typical ice‐binding domains, and the TargetFreeze tool did not predict an antifreeze capacity, suggesting the existence of nontypical antifreeze domains. The fact that TaBAS1 is an efficient cryoprotectant but does not show antifreeze activity indicates a different mechanism of action. The cryoprotective properties conferred by WCS120 depend on biochemical properties that remain to be determined. Overall, our results show that the proteins' efficiencies vary between cell types, and confirm that a combination of different protection mechanisms is needed to successfully cryopreserve mammalian cells. PMID:26889747

Recrystallization method to selenization of thin-film Cu(In,Ga)Se.sub.2 for semiconductor device applications

DOEpatents

Albin, David S.; Carapella, Jeffrey J.; Tuttle, John R.; Contreras, Miguel A.; Gabor, Andrew M.; Noufi, Rommel; Tennant, Andrew L.

1995-07-25

A process for fabricating slightly Cu-poor thin-films of Cu(In,Ga)Se.sub.2 on a substrate for semiconductor device applications includes the steps of forming initially a slightly Cu-rich, phase separated, mixture of Cu(In,Ga)Se.sub.2 :Cu.sub.x Se on the substrate in solid form followed by exposure of the Cu(In,Ga)Se.sub.2 :Cu.sub.x Se solid mixture to an overpressure of Se vapor and (In,Ga) vapor for deposition on the Cu(In,Ga)Se.sub.2 :Cu.sub.x Se solid mixture while simultaneously increasing the temperature of the solid mixture toward a recrystallization temperature (about 550.degree. C.) at which Cu(In,Ga)Se.sub.2 is solid and Cu.sub.x Se is liquid. The (In,Ga) flux is terminated while the Se overpressure flux and the recrystallization temperature are maintained to recrystallize the Cu.sub.x Se with the (In, Ga) that was deposited during the temperature transition and with the Se vapor to form the thin-film of slightly Cu-poor Cu.sub.x (In,Ga).sub.y Se.sub.z. The initial Cu-rich, phase separated large grain mixture of Cu(In,Ga)Se.sub.2 :Cu.sub.x Se can be made by sequentially depositing or co-depositing the metal precursors, Cu and (In, Ga), on the substrate at room temperature, ramping up the thin-film temperature in the presence of Se overpressure to a moderate anneal temperature (about 450.degree. C.) and holding that temperature and the Se overpressure for an annealing period. A nonselenizing, low temperature anneal at about 100.degree. C. can also be used to homogenize the precursors on the substrates before the selenizing, moderate temperature anneal.

Inhibition of ice recrystallization and cryoprotective activity of wheat proteins in liver and pancreatic cells.

PubMed

Chow-Shi-Yée, Mélanie; Briard, Jennie G; Grondin, Mélanie; Averill-Bates, Diana A; Ben, Robert N; Ouellet, François

2016-05-01

Efficient cryopreservation of cells at ultralow temperatures requires the use of substances that help maintain viability and metabolic functions post-thaw. We are developing new technology where plant proteins are used to substitute the commonly-used, but relatively toxic chemical dimethyl sulfoxide. Recombinant forms of four structurally diverse wheat proteins, TaIRI-2 (ice recrystallization inhibition), TaBAS1 (2-Cys peroxiredoxin), WCS120 (dehydrin), and TaENO (enolase) can efficiently cryopreserve hepatocytes and insulin-secreting INS832/13 cells. This study shows that TaIRI-2 and TaENO are internalized during the freeze-thaw process, while TaBAS1 and WCS120 remain at the extracellular level. Possible antifreeze activity of the four proteins was assessed. The "splat cooling" method for quantifying ice recrystallization inhibition activity (a property that characterizes antifreeze proteins) revealed that TaIRI-2 and TaENO are more potent than TaBAS1 and WCS120. Because of their ability to inhibit ice recrystallization, the wheat recombinant proteins TaIRI-2 and TaENO are promising candidates and could prove useful to improve cryopreservation protocols for hepatocytes and insulin-secreting cells, and possibly other cell types. TaENO does not have typical ice-binding domains, and the TargetFreeze tool did not predict an antifreeze capacity, suggesting the existence of nontypical antifreeze domains. The fact that TaBAS1 is an efficient cryoprotectant but does not show antifreeze activity indicates a different mechanism of action. The cryoprotective properties conferred by WCS120 depend on biochemical properties that remain to be determined. Overall, our results show that the proteins' efficiencies vary between cell types, and confirm that a combination of different protection mechanisms is needed to successfully cryopreserve mammalian cells. © 2016 The Protein Society.

Characterization of microstructure and texture across dissimilar super duplex/austenitic stainless steel weldment joint by austenitic filler metal

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

Eghlimi, Abbas, E-mail: a.eghlimi@ma.iut.ac.ir; Shamanian, Morteza; Eskandarian, Masoomeh

The evolution of microstructure and texture across an as-welded dissimilar UNS S32750 super duplex/UNS S30403 austenitic stainless steel joint welded by UNS S30986 (AWS A5.9 ER309LMo) austenitic stainless steel filler metal using gas tungsten arc welding process was evaluated by optical micrography and EBSD techniques. Due to their fabrication through rolling process, both parent metals had texture components resulted from deformation and recrystallization. The weld metal showed the highest amount of residual strain and had large austenite grain colonies of similar orientations with little amounts of skeletal ferrite, both oriented preferentially in the < 001 > direction with cub-on-cube orientationmore » relationship. While the super duplex stainless steel's heat affected zone contained higher ferrite than its parent metal, an excessive grain growth was observed at the austenitic stainless steel's counterpart. At both heat affected zones, austenite underwent some recrystallization and formed twin boundaries which led to an increase in the fraction of high angle boundaries as compared with the respective base metals. These regions showed the least amount of residual strain and highest amount of recrystallized austenite grains. Due to the static recrystallization, the fraction of low degree of fit (Σ) coincident site lattice boundaries, especially Σ3 boundaries, was increased in the austenitic stainless steel heat affected zone, while the formation of subgrains in the ferrite phase increased the content of < 5° low angle boundaries at that of the super duplex stainless steel. - Graphical abstract: Display Omitted - Highlights: • Extensive grain growth in the HAZ of austenitic stainless steel was observed. • Intensification of < 100 > orientated grains was observed adjacent to both fusion lines. • Annealing twins with Σ3 CSL boundaries were formed in the austenite of both HAZ. • Cub-on-cube OR was observed between austenite and ferrite in the weld metal. • Weld metal had the lowest texture intensity and ratio of low angle and CSL boundaries.« less

Modeling of the static recrystallization for 7055 aluminum alloy by cellular automaton

NASA Astrophysics Data System (ADS)

Zhang, Tao; Lu, Shi-hong; Zhang, Jia-bin; Li, Zheng-fang; Chen, Peng; Gong, Hai; Wu, Yun-xin

2017-09-01

In order to simulate the flow behavior and microstructure evolution during the pass interval period of the multi-pass deformation process, models of static recovery (SR) and static recrystallization (SRX) by the cellular automaton (CA) method for the 7055 aluminum alloy were established. Double-pass hot compression tests were conducted to acquire flow stress and microstructure variation during the pass interval period. With the basis of the material constants obtained from the compression tests, models of the SR, incubation period, nucleation rate and grain growth were fitted by least square method. A model of the grain topology and a statistical computation of the CA results were also introduced. The effects of the pass interval time, temperature, strain, strain rate and initial grain size on the microstructure variation for the SRX of the 7055 aluminum alloy were studied. The results show that a long pass interval time, large strain, high temperature and large strain rate are beneficial for finer grains during the pass interval period. The stable size of the static recrystallized grain is not concerned with the initial grain size, but mainly depends on the strain rate and temperature. The SRX plays a vital role in grain refinement, while the SR has no effect on the variation of microstructure morphology. Using flow stress and microstructure comparisons of the simulated and experimental CA results, the established CA models can accurately predict the flow stress and microstructure evolution during the pass interval period, and provide guidance for the selection of optimized parameters for the multi-pass deformation process.

Development of spray-dried co-precipitate of amorphous celecoxib containing storage and compression stabilizers.

PubMed

Dhumal, Ravindra S; Shimpi, Shamkant L; Paradkar, Anant R

2007-09-01

The purpose of this study was to obtain an amorphous system with minimum unit operations that will prevent recrystallization of amorphous drugs since preparation, during processing (compression) and further storage. Amorphous celecoxib, solid dispersion (SD) of celecoxib with polyvinyl pyrrollidone (PVP) and co-precipitate with PVP and carrageenan (CAR) in different ratios were prepared by the spray drying technique and compressed into tablets. Saturation solubility and dissolution studies were performed to differentiate performance after processing. Differential scanning calorimetry and X-ray powder difraction revealed the amorphous form of celecoxib, whereas infrared spectroscopy revealed hydrogen bonding between celecoxib and PVP. The dissolution profile of the solid dispersion and co-precipitate improved compared to celecoxib and amorphous celecoxib. Amorphous celecoxib was not stable on storage whereas the solid dispersion and co-precipitate powders were stable for 3 months. Tablets of the solid dispersion of celecoxib with PVP and physical mixture with PVP and carrageenan showed better resistance to recrystallization than amorphous celecoxib during compression but recrystallized on storage. However, tablets of co-precipitate with PVP and carageenan showed no evidence of crystallinity during stability studies with comparable dissolution profiles. This extraordinary stability of spray-dried co-precipitate tablets may be attributed to the cushioning action provided by the viscoelastic polymer CAR and hydrogen bonding interaction between celecoxib and PVP. The present study demonstrates the synergistic effect of combining two types of stabilizers, PVP and CAR, on the stability of amorphous drug during compression and storage as compared to their effect when used alone.

Swift heavy ion-beam induced amorphization and recrystallization of yttrium iron garnet.

PubMed

Costantini, Jean-Marc; Miro, Sandrine; Beuneu, François; Toulemonde, Marcel

2015-12-16

Pure and (Ca and Si)-substituted yttrium iron garnet (Y3Fe5O12 or YIG) epitaxial layers and amorphous films on gadolinium gallium garnet (Gd3Ga5O12, or GGG) single crystal substrates were irradiated by 50 MeV (32)Si and 50 MeV (or 60 MeV) (63)Cu ions for electronic stopping powers larger than the threshold value (~4 MeV μm(-1)) for amorphous track formation in YIG crystals. Conductivity data of crystalline samples in a broad ion fluence range (10(11)-10(16) cm(-2)) are modeled with a set of rate equations corresponding to the amorphization and recrystallization induced in ion tracks by electronic excitations. The data for amorphous layers confirm that a recrystallization process takes place above ~10(14) cm(-2). Cross sections for both processes deduced from this analysis are discussed in comparison to previous determinations with reference to the inelastic thermal-spike model of track formation. Micro-Raman spectroscopy was also used to follow the related structural modifications. Raman spectra show the progressive vanishing and randomization of crystal phonon modes in relation to the ion-induced damage. For crystalline samples irradiated at high fluences (⩾10(14) cm(-2)), only two prominent broad bands remain like for amorphous films, thereby reflecting the phonon density of states of the disordered solid, regardless of samples and irradiation conditions. The main band peaked at ~660 cm(-1) is assigned to vibration modes of randomized bonds in tetrahedral (FeO4) units.

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.

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.

Solid State Recrystallization of Single Crystal Ce:LSO Scintillator Crystals for High Resolution Detectors

DTIC Science & Technology

2012-06-01

this report. The property measurements that have been focused on were the assessment of density ( Archimedes ). grain structure {optical and SEM...Scintillator", Materials Letters 60 1960-1963 (2006) [15] J.S. Reed, Forming Processes, Chapter 20 in Introduction to the Principles of Ceramic

Room Temperature Ion-Beam-Induced Recrystallization and Large Scale Nanopatterning.

PubMed

Satpati, Biswarup; Ghosh, Tanmay

2015-02-01

We have studied ion-induced effects in the near-surface region of two eutectic systems. Gold and Silver nanodots on Silicon (100) substrate were prepared by thermal evaporation under high vacuum condition at room temperature (RT) and irradiated with 1.5 MeV Au2+ ions at flux ~1.25 x 10(11) ions cm-2 s-1 also at RT. These samples were characterized using cross-sectional transmission electron microscopy (XTEM) and associated techniques. We have observed that gold act as catalysis in the recrystallization process of ion-beam-induced amorphous Si at room temperature and also large mass transport up to a distance of about 60 nm into the substrate. Mass transport is much beyond the size (~ 6-20 nm) of these Au nanodots. Ag nanoparticles with diameter 15-45 nm are half-way embedded into the Si substrate and does not stimulate in recrystallization. In case of Au nanoparticles upon ion irradiation, mixed phase formed only when the local composition and transient temperature during irradiation is sufficient to cause mixing in accordance with the Au-Si stable phase diagram. Spectroscopic imaging in the scanning TEM using spatially resolved electron energy loss spectroscopy provides one of the few ways to measure the real-space nanoscale mixing.

Development of re-crystallized W-1.1%TiC with enhanced room-temperature ductility and radiation performance

NASA Astrophysics Data System (ADS)

Kurishita, H.; Matsuo, S.; Arakawa, H.; Sakamoto, T.; Kobayashi, S.; Nakai, K.; Takida, T.; Kato, M.; Kawai, M.; Yoshida, N.

2010-03-01

Ultra-fine grained (UFG) W-TiC compacts fabricated by powder metallurgical methods utilizing mechanical alloying (MA) are very promising for use in irradiation environments. However, the assurance of room-temperature ductility and enhancement in surface resistances to low-energy hydrogen irradiation are unsettled issues. As an approach to solution to these, microstructural modification by hot plastic working has been applied to UFG W-TiC processed by MA in a purified Ar or H 2 atmosphere and hot isostatic pressing (HIP). Hot plastically worked compacts have been subjected to 3-point bend tests at room temperature and TEM microstructural examinations. It is found that the microstructural modification allows us to convert UFG W-1.1%TiC to compacts exhibiting a very high fracture strength and appreciable ductility at room temperature. The compacts of W-1.1%TiC/Ar (MA atmosphere: Ar) and W-1.1%TiC/H 2 (MA atmosphere: H 2) exhibit re-crystallized structures with approximately 0.5 and 1.5 μm in grain size, respectively. It is shown that the enhancement of fracture resistance by microstructural modifications is attributed to significant strengthening of weak grain boundaries in the re-crystallized state. As a result the modified compacts exhibit superior surface resistance to low-energy deuteron irradiation.

Deformation Mechanisms of Darreh Sary Metapelites, Sanandaj‒Sirjan Zone, Iran

NASA Astrophysics Data System (ADS)

Hemmati, O.; Tabatabaei Manesh, S. M.; Nadimi, A. R.

2018-03-01

The Darreh Sary metapelitic rocks are located in the northeast of Zagros orogenic belt and Sanandaj-Sirjan structural zone. The lithological composition of these rocks includes slate, phyllite, muscovitebiotite schist, garnet schist, staurolite-garnet schist and staurolite schist. The shale is the protolith of these metamorphic rocks, which was originated from the continental island arc tectonic setting and has been subjected to processes of Zagros orogeny. The deformation mechanisms in these rocks include bulging recrystallization (BLG), subgrain rotation recrystallization (SGR) and grain boundary migration recrystallization (GBM), which are considered as the key to estimate the deformation temperature of the rocks. The estimated ranges of deformation temperature and depth in these rocks show the temperatures of 275-375, 375-500, and >500°C and the depths of 10 to 17 km. The observed structures in these rocks such as faults, fractures and folds, often with the NW-SE direction coordinate with the structural trends of Zagros orogenic belt structures. The S-C mylonite fabrics is observed in these rocks with other microstructures such as mica fish, σ fabric and garnet deformation indicate the dextral shear deformation movements of study area. Based on the obtained results of this research, the stages of tectonic evolution of Darreh Sary area were developed.

A Convenient and Safer Synthesis of Diaminoglyoxime

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

Johnson, Eric C.; Sabatini, Jesse J.; Zuckerman, Nathaniel B.

A new procedure for the synthesis and isolation of diaminoglyoxime (DAG) is described. A previous procedure involved treating glyoxal with two equivalents each of hydroxylammonium chloride and sodium hydroxide to form glyoxime, followed by further treatment of this intermediate with two additional equivalents of hydroxylammonium chloride and sodium hydroxide at 95 °C to form DAG. Two recrystallizations were needed to obtain the desired product in pure form. Another previous procedure employed glyoxal in the presence of four equivalents each of hydroxylammonium chloride and sodium hydroxide at 95 °C to form DAG. Though this latter procedure gives product after a fewmore » hours, yields do not exceed 40%, and the reaction is prone to thermal runaway. Furthermore, the use of decolorizing carbon, and recrystallization of the crude solid is necessary to obtain a pure product. The new disclosed procedure involves treating a preheated aqueous hydroxylamine solution (50 wt. %, ten equivalents) with aqueous glyoxal (40 wt. %), followed by heating at 95 °C for 72-96 h. The reaction is cooled to room temperature, and then to 0-5 °C to obtain DAG in pure form, without recrystallization or decolorizing carbon in 77-80% yield. The exothermic nature of the reaction is also minimized by this updated process.« less