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.

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

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.

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

Deformation Behavior and Microstructure Evolution of As-Cast 42CrMo Alloy in Isothermal and Non-isothermal Compression

NASA Astrophysics Data System (ADS)

Qin, Fangcheng; Li, Yongtang; Qi, Huiping; Lv, Zhenhua

2016-11-01

The isothermal and non-isothermal multi-pass compression tests of centrifugal casting 42CrMo steel were conducted on a Gleeble-3500 thermal simulation machine. The effects of compression passes and finishing temperatures on deformation behavior and microstructure evolution were investigated. It is found that the microstructure is homogeneous with equiaxed grains, and the flow stress does not show significant change with the increase in passes, while the peak softening coefficient increases first and then decreases during inter-pass. Moreover, the dominant mechanisms of controlled temperature and accumulated static recrystallization for grain refinement and its homogeneous distribution are found after 5 passes deformation. As the finishing temperature increases, the flow stress decreases gradually, but the dynamic recrystallization accelerates and softening effect increases, resulting in the larger grain size and homogeneous microstructure. The microhardness decreases sharply because the sufficient softening occurs in microstructure. When the finishing temperature is 890 °C, the carbide particles are precipitated in the vicinity of the grain boundaries, thus inhibiting the dislocation motion. Thus, the higher finishing temperature (≥970 °C) for centrifugal casting 42CrMo alloy should be avoided in non-isothermal multi-pass deformation, which is beneficial to grain refinement and properties improvement.

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

Effects of the Strain Rate and Temperature on the Microstructural Evolution of Twin-Rolled Cast Wrought AZ31B Alloys Sheets

NASA Astrophysics Data System (ADS)

Rodriguez, A. K.; Kridli, G.; Ayoub, G.; Zbib, H.

2013-10-01

This article investigates the effects of the strain rate and temperature on the microstructural evolution of twin-rolled cast wrought AZ31B sheets. This was achieved through static heating and through tensile test performed at strain rates from 10-4 to 10-1 s-1 and temperatures between room temperature (RT) and 300 °C. While brittle fracture with high stresses and limited elongation was observed at the RT, ductile behavior was obtained at higher temperatures with low strain rates. The strain rate sensitivity and activation energy calculations indicate that grain boundary diffusion and lattice diffusion are the two rate-controlling mechanisms at warm and high temperatures, respectively. An analysis of the evolution of the microstructure provided some indications of the most probable deformation mechanisms in the material: twinning operates at lower temperatures, and dynamic recrystallization dominates at higher temperatures. The static evolution of the microstructure was also studied, proving a gradual static grain growth of the AZ31B with annealing temperature and time.

Compaction and sintering behaviors of a Nd-Fe-B permanent magnet alloy

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

Chin, T.; Hung, M.; Tsai, D.

1988-11-15

Extensive x-ray diffraction (XRD) and magnetic measurements were done on Nd/sub 15/ Fe/sub 77/ B/sub 8/ magnet alloy green compacts after cold isostatic pressing following a pulsed 2-T field (CIP) and die-pressing under a static 1.2-T perpendicular field (DP1) or parallel field (DP2), and on those after sintering. An alignment factor F, through the calculation of the integrated diffraction intensity ratio of the XRD patterns, was adopted as the effectiveness of magnetic alignment. At the green compact state, DP1 has the best alignment while CIP the worst. However, after sintering the alignment factor was such that CIP>DPI>DP2, the same ordermore » as the magnetic properties. Three mechanisms were proposed for the evolution of the alignment factor at different stages of sintering, i.e., that both the appearance of a liquid phase at low temperatures and preferred grain growth at high temperatures enhance F, while recrystallization at intermediate temperatures deteriorates F. CIP results in less-defect green compact, hence less recrystallization, leading to better resultant alignment« less

Hot Deformation and Dynamic Recrystallization Behavior of the Cu-Cr-Zr-Y Alloy

NASA Astrophysics Data System (ADS)

Zhang, Yi; Huili, Sun; Volinsky, Alex A.; Tian, Baohong; Chai, Zhe; Liu, Ping; Liu, Yong

2016-03-01

To study the workability and to optimize the hot deformation processing parameters of the Cu-Cr-Zr-Y alloy, the strain hardening effect and dynamic softening behavior of the Cu-Cr-Zr-Y alloy were investigated. The flow stress increases with the strain rate and stress decreases with deformation temperature. The critical conditions, including the critical strain and stress for the occurrence of dynamic recrystallization, were determined based on the alloy strain hardening rate. The critical stress related to the onset of dynamic recrystallization decreases with temperature. The evolution of DRX microstructure strongly depends on the deformation temperature and the strain rate. Dynamic recrystallization appears at high temperatures and low strain rates. The addition of Y can refine the grain and effectively accelerate dynamic recrystallization. Dislocation generation and multiplication are the main hot deformation mechanisms for the alloy. The deformation temperature increase and the strain rate decrease can promote dynamic recrystallization of the alloy.

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.

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

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.

Effect of alloying elements and coiling temperature on the recrystallization behavior and the bainitic transformation in TRIP steels

NASA Astrophysics Data System (ADS)

Han, Seongho; Seong, Hwangoo; Ahn, Yeonsang; Garcia, C. I.; DeArdo, A. J.; Kim, Inbae

2009-08-01

The effects of alloying elements and coiling temperature on recrystallization behavior and bainitic transformation were investigated based on 0.07C-Mn-Cr-Nb steel with a low carbon equivalent. Based on the ferrite recrystallization behavior, the proper intercritical annealing temperature of all studied steels was suggested to produce TRIP steel with good strength and elongation balance. All steels coiled at 550 °C showed much faster ferrite recrystallization behavior than steels coiled at 700 °C. In addition to the coiling temperature, the effect of increasing carbon content on the ferrite recrystallization was minor at a coiling temperature of 550 °C, but much more prominent at a coiling temperature of 700 °C. The highest Mo added steel showed the best strength and elongation balance, and the highest carbon and Mo added steel showed the highest tensile strength at a coiling temperature of 550 °C. The steel containing a higher amount of elemental Al (0.7 wt.% Al) exhibited much better elongation than the lower Al added steel (0.04 wt.% Al) in TS 780 MPa grade, about 24 % and 19 %, respectively.

Dynamic Recrystallization Behavior of Zr-1Sn-0.3Nb Alloy During Hot Rolling Process

NASA Astrophysics Data System (ADS)

Zhao, Siyu; Liu, Huiqun; Lin, Gaoyong; Jiang, Yilan; Xun, Jian

2017-11-01

Zirconium alloys are advanced materials with properties that are greatly affected by their crystalline structure. To investigate this, sheets of Zr-1Sn-0.3Nb alloy were hot rolled with different reductions (10%, 30%, 50%, and 60%) at 1023 K and 1073 K to investigate the alloy's dynamic recrystallization behavior. Recrystallization kinetics was observed via electron backscattering diffraction and transmission electron microscopy, and the results were compared with estimates based on the Johnson-Mehl-Avrami-Kolmogorov (JMAK) equation. The values of the JMAK exponent n and k increased with the rolling temperature. The estimates and microstructural observations of dynamic recrystallization (DRX) kinetics were in good agreement.

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.

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.

Prediction of recrystallization behavior of troglitazone/polyvinylpyrrolidone solid dispersion by solid-state NMR.

PubMed

Ito, Atsutoshi; Watanabe, Tomoyuki; Yada, Shuichi; Hamaura, Takeshi; Nakagami, Hiroaki; Higashi, Kenjirou; Moribe, Kunikazu; Yamamoto, Keiji

2010-01-04

The purpose of this study was to elaborate the relationship between the (13)C CP/MAS NMR spectra and the recrystallization behavior during the storage of troglitazone solid dispersions. The solid dispersions were prepared by either the solvent method or by co-grinding. The recrystallization behavior under storage conditions at 40 degrees C/94% RH was evaluated by the Kolmogorov-Johnson-Mehl-Avrami (KJMA) equation. Solid dispersions prepared by the solvent method or by prolonged grinding brought about inhibition of the nucleation and the nuclei growth at the same time. No differences in the PXRD profiles were found in the samples prepared by the co-grinding and solvent methods, however, (13)C CP/MAS NMR showed significant differences in the spectra. The correlation coefficients using partial least square regression analysis between the PXRD profiles and the apparent nuclei-growth constant or induction period to nucleation were 0.1305 or 0.6350, respectively. In contrast, those between the (13)C CP/MAS NMR spectra and the constant or the period were 0.9916 or 0.9838, respectively. The (13)C CP/MAS NMR spectra had good correlation with the recrystallization kinetic parameters evaluated by the KJMA equation. Consequently, solid-state NMR was judged to be a useful tool for the prediction of the recrystallization behavior of solid dispersions.

Recrystallization Behavior in Mixed Solder Joints of BGA Components during Thermal Shock

NASA Astrophysics Data System (ADS)

Tan, Shihai; Han, Jing; Guo, Fu

2018-03-01

Sn-37Pb and Sn-3.0Ag-0.5Cu solder pastes printed onto a board were attached to ball grid array (BGA) samples using Sn-3.0Ag-0.5Cu solder balls. Before thermal shock, the initial grain orientations on the cross-section were obtained by scanning electron microscopy equipped with an electron backscattered diffraction system. Three mixed solder joints (two from the corner and another from the middle of the BGA component) and three lead-free solder joints (at the same positions) were selected to investigate the recrystallization behavior under thermal shock (TS) cycling conditions. All of the mixed and lead-free solder joints were initially single crystal. The results showed that recrystallization occurred in both the mixed and lead-free solder joints after 200 TS. For the mixed solder joints, more recrystallization was observed and the location of samples had a significant influence on their recrystallization behavior, while location was not as important for the lead-free samples after 200 TS in this study. Both the mixed and lead-free solder joints at the corner of BGA components showed the poorest reliability. According to misorientation distribution maps and subgrain rotation behaviors, the reliability of mixed solder joints was much poorer than that of lead-free solder joints.

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)

Deformation, static recrystallization, and reactive melt transport in shallow subcontinental mantle xenoliths (Tok Cenozoic volcanic field, SE Siberia)

NASA Astrophysics Data System (ADS)

Tommasi, Andréa; Vauchez, Alain; Ionov, Dmitri A.

2008-07-01

Partial melting and reactive melt transport may change the composition, microstructures, and physical properties of mantle rocks. Here we explore the relations between deformation and reactive melt transport through detailed microstructural analysis and crystallographic orientation measurements in spinel peridotite xenoliths that sample the shallow lithospheric mantle beneath the southeastern rim of the Siberian craton. These xenoliths have coarse-grained, annealed microstructures and show petrographic and chemical evidence for variable degrees of reaction with silicate melts and fluids, notably Fe-enrichment and crystallization of metasomatic clinopyroxene (cpx). Olivine crystal preferred orientations (CPO) range from strong to weak. [010]-fiber patterns, characterized by a point concentration of [010] normal to the foliation and by dispersion of [100] in the foliation plane with a weak maximum parallel to the lineation, predominate relative to the [100]-fiber patterns usually observed in lithospheric mantle xenoliths and peridotite massifs. Variations in olivine CPO patterns or intensity are not correlated with modal and chemical compositions. This, together with the analysis of microstructures, suggests that reactive melt percolation postdated both deformation and static recrystallization. Preferential crystallization of metasomatic cpx along (010) olivine grain boundaries points to an influence of the preexisting deformation fabrics on melt transport, with higher permeability along the foliation. Similarity between orthopyroxene (opx) and cpx CPO suggests that cpx orientations may be inherited from those of opx during melt-rock reaction. As observed in previous studies, reactive melt transport does not weaken olivine CPO and seismic anisotropy in the upper mantle, except in melt accumulation domains. In contrast, recovery and selective grain growth during static recrystallization may lead to development of [010]-fiber olivine CPO and, if foliations are horizontal, result in apparent isotropy for vertically propagating SKS waves, but strong anisotropy for horizontally propagating surface waves.

Microstructural evolution during thermal annealing of ice-Ih

NASA Astrophysics Data System (ADS)

Hidas, Károly; Tommasi, Andréa; Mainprice, David; Chauve, Thomas; Barou, Fabrice; Montagnat, Maurine

2017-06-01

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 pre-deformed in uniaxial compression at temperature of -7 °C to macroscopic 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 initial evolution is similar for all studied samples irrespective of their initial strain or annealing temperature. After an incubation period ≥1.5 h, recovery is accompanied by recrystallization (nucleation and grain boundary migration). Grain growth proceeds at the expense of domains with high intragranular misorientations, consuming first the most misorientated parts of primary grains. Grain growth kinetics fits the parabolic growth law with grain growth exponents in the range of 2.4-4.0. Deformation-induced tilt boundaries and kink bands may slow down grain boundary migration. They are stable features during early stages of static recrystallization, only erased by normal growth, which starts after >24 h of annealing.

Enhancing the Damping Behavior of Dilute Zn-0.3Al Alloy by Equal Channel Angular Pressing

NASA Astrophysics Data System (ADS)

Demirtas, M.; Atli, K. C.; Yanar, H.; Purcek, G.

2017-06-01

The effect of grain size on the damping capacity of a dilute Zn-0.3Al alloy was investigated. It was found that there was a critical strain value (≈1 × 10-4) below and above which damping of Zn-0.3Al showed dynamic and static/dynamic hysteresis behavior, respectively. In the dynamic hysteresis region, damping resulted from viscous sliding of phase/grain boundaries, and decreasing grain size increased the damping capacity. While the quenched sample with 100 to 250 µm grain size showed very limited damping capacity with a loss factor tanδ of less than 0.007, decreasing grain size down to 2 µm by equal channel angular pressing (ECAP) increased tanδ to 0.100 in this region. Dynamic recrystallization due to microplasticity at the sample surface was proposed as the damping mechanism for the first time in the region where the alloy showed the combined aspects of dynamic and static hysteresis damping. In this region, tanδ increased with increasing strain amplitude, and ECAPed sample showed a tanδ value of 0.256 at a strain amplitude of 2 × 10-3, the highest recorded so far in the damping capacity-related studies on ZA alloys.

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.

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.

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

PubMed

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

2018-05-22

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

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.

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.

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

New insights on the rheological properties of a rocksalt

NASA Astrophysics Data System (ADS)

Speranza, G.; Vinciguerra, S.; Di Genova, D.; Romano, C.; Vona, A.; Mollo, S.; Iarocci, A.

2013-12-01

The importance and economic interest on rocksalt deposits and salt bodies are well known and extensively studied. The physical and mechanical properties of salt have a profound influence on the tectonics as well as they are considered to be vital for applicative purposes such as mining, petroleum and nuclear waste storage. However, previous scientific works have mainly focused on synthetic rocksalt or commercial salt, whereas natural salt facies have been scarcely investigated. In this view, we present new data on the role of natural heterogeneities (i.e., relative abundance of primary salt crystals and impurities) on the rheological parameters of a rocksalt. This rock belongs to the Saline di Volterra formation (Volterra basin, Tuscany, central Italy) that was deposited during the Messinian Salinity Crisis. The 49-metre-thick salt sequence (intersected by the S1113 borehole of the Solvay company) is characterized by a high salt facies variability. In particular, three end-members have been recognized: the first contains abundant primary salt crystals, with minor or no recrystallizazion; the second member is extensively recrystallized, with scarce primary crystal remnants; the third shows a great abundance of clay impurities. Rheological parameters, such as static and dynamic Young's Modulus and coefficient of linear expansion, were measured for the three rocksalt end-members throughout P and S seismic velocities, uniaxial compressive strength and thermal expansion measurements. Seismic velocity has been measured on cubic samples with a side ranging from 4 to 7 cm. A clear effect of the salt facies was found: the average velocity is faster in mostly recrystallized salt samples (4500 m/s), slower in primary salt-rich samples (4300 m/s), and intermediate (4350 m/s) in presence of clay impurities. Dynamic Young's Modulus calculated on velocities (average value ≈ 38 GPa) mirrors this behavior, with lowest values related to primary salt. The anisotropic effect induced by the deformation is evident considering the wave velocities measured for each axis of the cubes, with lower velocities along the Z (vertical) axis. Uniaxial compressive tests (carried out at ambient temperature) revealed the effect of the salt facies in the mechanical properties and, particularly, in the elastic properties and in the absolute peak stress value. Static Young's Moduli (average value ≈ 5,3 GPa) result much lower than the dynamic ones. In this case lowest values are related to recrystallized salt. Notably, the peak stress is inversely proportional to the static Young's Moduli. Moreover, data from thermal expansion curves (from 20 to 700 °C) show a greater amount of volume expansion of primary salt and allowed to identify an 'instability zone', between 300 and 500 °C, where fluid emission, samples cracking and a sudden increase in volume expansivity occur. Results from our experiments indicate that the different characteristics of salt facies determine the bulk rheological parameters and, consequently, the rocksalt deformation behavior. Although further analyses are necessary, we suggest that studies on salt bodies cannot be approached without detailed petrophysical and rheological analyses of rocksalt facies.

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

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

PubMed Central

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

2018-01-01

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

Deformation and recrystallization behavior of super high-purity niobium for SRF cavity

NASA Astrophysics Data System (ADS)

Yamaguchi, Y.; Doryo, H.; Yuasa, M.; Miyamoto, H.; Yamanaka, M.

2017-05-01

Deformation and recyrstallization behavior of pure niobium was investigated in order to clarify the origin of its low hydro-formability despite of its high ductility comparable with pure iron. It was found that pure niobium exhibits lower strain hardening in cold rolling compared with pure iron. Furthermore, in post-deformation annealing, the hardness of niobium decreased monotonously with an increase of temperature, and the typical sharp drop by recrystallization was not evident. This softening behavior was contrasted with the high-purity iron. It is suggested that niobium exhibit the so-called in-situ recrystallization possibly because of low elastic modulus and low accumulative plastic strain energy in spite of high melting temperature. The low hydro-formability of pure niobium sheets or tubes is caused by its low strain hardening and its unique plastic anisotropy which is associated with this recovered residual rolled texture.

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.

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

DTIC Science & Technology

2010-04-01

produced from eutectic melts. Nat. Mater. 2008, 7, 626-630. 9. Any attempt at recrystallizing the 1:1 mixture of cations in (12) is likely to afford... recrystallizations . So, rather than recrystallizing each individual adduct, we concentrated on performing a careful spectroscopic examination of the...suggested. [1] While it is well-known that an admixture of two neutral compounds often affords eutectic behavior, we wondered whether or not the same

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.

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.

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.

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

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

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

2014-06-01

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

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.

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

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

PubMed

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

2017-05-18

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

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.

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

NASA Astrophysics Data System (ADS)

Sakai, Tetsuo; Utsunomiya, Hiroshi; Takahashi, Yasuo

2014-08-01

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

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.

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

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.

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.

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.

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

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.

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

Modeling the Flow Behavior, Recrystallization, and Crystallographic Texture in Hot-Deformed Fe-30 Wt Pct Ni Austenite

NASA Astrophysics Data System (ADS)

Abbod, M. F.; Sellars, C. M.; Cizek, P.; Linkens, D. A.; Mahfouf, M.

2007-10-01

The present work describes a hybrid modeling approach developed for predicting the flow behavior, recrystallization characteristics, and crystallographic texture evolution in a Fe-30 wt pct Ni austenitic model alloy subjected to hot plane strain compression. A series of compression tests were performed at temperatures between 850 °C and 1050 °C and strain rates between 0.1 and 10 s-1. The evolution of grain structure, crystallographic texture, and dislocation substructure was characterized in detail for a deformation temperature of 950 °C and strain rates of 0.1 and 10 s-1, using electron backscatter diffraction and transmission electron microscopy. The hybrid modeling method utilizes a combination of empirical, physically-based, and neuro-fuzzy models. The flow stress is described as a function of the applied variables of strain rate and temperature using an empirical model. The recrystallization behavior is predicted from the measured microstructural state variables of internal dislocation density, subgrain size, and misorientation between subgrains using a physically-based model. The texture evolution is modeled using artificial neural networks.

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.

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

EBSD characterization of low temperature deformation mechanisms in modern alloys

NASA Astrophysics Data System (ADS)

Kozmel, Thomas S., II

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

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.

Recrystallization in Si upon ion irradiation at room temperature in Co/Si(111) thin film systems

NASA Astrophysics Data System (ADS)

Banu, Nasrin; Satpati, B.; Dev, B. N.

2018-04-01

After several decades of research it was concluded that for a constant flux recrystallization in Si upon ion irradiation is possible only at high temperature. At low temperature or at room temperature only amorphization can take place. However we have observed recrystallization in Si upon ion irradiation at room temperature in a Co/Si thin film system. The Co/Si sample was prepared by deposition of 25 nm Co on clean Si(111) substrate. An oxide layer (˜ 2nm) of cobalt at the top of the film due to air exposure. The ion irradiation was done at room temperature under high vacuum with 1MeV Si+ ion with low beam current < 400 nA. Earlier we have shown similar ion induced recrystallization in Si(100) substrate which had a sandwich Si/Ni/Si structure. This system had an epitaxial buffer Si layer on Si substrate. This study also shows that the phenomenon is independent of substrate orientation and buffer layer. We have used transmission electron microscopy (TEM) to study the recrystallization behavior.

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.

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.

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.

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).

Phase transformations in ion-irradiated silicides

NASA Technical Reports Server (NTRS)

Hewett, C. A.; Lau, S. S.; Suni, I.; Hung, L. S.

1985-01-01

The present investigation has three objectives. The first is concerned with the phase transformation of CoSi2 under ion implantation and the subsequent crystallization characteristics during annealing, taking into account epitaxial and nonepitaxial recrystallization behavior. The second objective is related to a study of the general trend of implantation-induced damage and crystallization behavior for a number of commonly used silicides. The last objective involves a comparison of the recrystallization behavior of cosputtered refractory silicides with that of the ion-implanted silicides. It was found that epitaxial regrowth of ion-irradiated CoSi2 occurred for samples with an epitaxial seed left at the Si/CoSi2 interface. A structural investigation of CoSi2 involving transmission electron microscopy (TEM) showed that after high-dose implantation CoSi2 is amorphous.

Effects of V addition on recrystallization resistance of 7150 aluminum alloy after simulative hot deformation

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

Lai, Jing; Shi, Cangji; Chen, X.-Grant, E-mail: xgrant_chen@uqac.ca

2014-10-15

The effects of different V contents (0.01 to 0.19 wt.%) on the recrystallization resistance of 7150 aluminum alloys during post-deformation heat treatment were investigated. The microstructural evolutions at as-cast, as-homogenized conditions and after post-deformation annealing were studied using optical, scanning electron and transmission electron microscopes and using the electron backscattered diffraction technique. The precipitation of Al{sub 21}V{sub 2} dispersoids was observed in alloys containing 0.11 to 0.19 wt.% V after homogenization. The dispersoids were mainly distributed in the dendrite cells, and the precipitate-free zones occurred in the interdendritic regions and near grain boundaries. V addition could significantly enhance the recrystallizationmore » resistance during post-deformation annealing, particularly in the presence of a great number of Al{sub 21}V{sub 2} dispersoids. Recrystallized grain growth was effectively restricted because of the dispersoid pinning effect. The alloy containing 0.15 wt.% V exhibited the highest recrystallization resistance amongst all V-containing alloys studied. - Highlights: • Investigated the effect of V level on microstructure and flow stress of 7150 alloys • Characterized microstructures using optical microscopy, SEM, TEM and EBSD • Described the precipitation behavior of V-dispersoids in the dendritic structure • Studied the V effect on recrystallization resistance during post heat treatment • V addition greatly enhanced the recrystallization resistance during annealing.« less

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

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.

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.

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.

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.

Effects of Laves phase particles on recovery and recrystallization behaviors of Nb-containing FeCrAl alloys

DOE PAGES

Sun, Zhiqian; Edmondson, Philip D.; Yamamoto, Yukinori

2017-11-15

The microstructures and mechanical properties of deformed and annealed Nb-containing FeCrAl alloys were investigated. Fine dispersion of Fe 2Nb-type Laves phase particles was observed in the bcc-Fe matrix after applying a thermomechanical treatment, especially along grain/subgrain boundaries, which effectively stabilized the recovered and recrystallized microstructures compared with the Nb-free FeCrAl alloy. The stability of recovered areas increased with Nb content up to 1 wt%. The recrystallized grain structure in Nb-containing FeCrAl alloys consisted of elongated grains along the rolling direction with a weak texture when annealed below 1100 °C. An abnormal relationship between recrystallized grain size and annealing temperature wasmore » found. Microstructural inhomogeneity in the deformed and annealed states was explained based on the Taylor factor. Annealed Nb-containing FeCrAl alloys showed a good combination of strength and ductility, which is desirable for their application as fuel cladding in light-water reactors.« less

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.

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.

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

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.

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.

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

Effect of cold deformation on the recrystallization behavior of FePd alloy at the ordering temperature using electron backscatter diffraction

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

Lin, Hung-Pin; Chen, Yen-Chun; Chen, Delphic

2014-08-15

In this study, the evolution of the recrystallization texture and microstructure was investigated after annealing of 50% and 90% cold-rolled FePd alloy at 530 °C. The FePd alloy was produced by vacuum arc melting in an atmosphere of 97% Ar and 3% H{sub 2}. The specimens were cold rolled to achieve 50% and 90% reduction in thickness. Electron backscatter diffraction measurements were performed on the rolling direction–normal direction section. With increased deformation from 50% to 90%, recrystallized texture transition occurs. For the 50% cold-rolled alloy, the preferred orientation is (0 1 0) [11 0 1], which is close to themore » cubic orientation after 400 h of annealing. For the 90% cold-rolled alloy, the orientation changes to (0 5 4) [22–4 5] after 16 h of annealing. - Highlights: • Texture and microstructure in cold-rolled FePd alloy was investigated during annealing using EBSD. • The recrystallized texture of 50% cold-rolled FePd is (0 1 0) [11 0 1] at 530 °C for 400 hours. • The recrystallized texture of 90% cold-rolled FePd is changed to (0 5 4) [22–4 5] at 530 °C after 16 hours.« less

Plasma deposited stability enhancement coating for amorphous ketoprofen.

PubMed

Bosselmann, Stephanie; Owens, Donald E; Kennedy, Rachel L; Herpin, Matthew J; Williams, Robert O

2011-05-01

A hydrophobic fluorocarbon coating deposited onto amorphous ketoprofen via pulsed plasma-enhanced chemical vapor deposition (PPECVD) significantly prolonged the onset of recrystallization compared to uncoated drug. Rapid freezing (RF) employed to produce amorphous ketoprofen was followed by PPECVD of perfluorohexane. The effect of coating thickness on the recrystallization and dissolution behavior of ketoprofen was investigated. Samples were stored in open containers at 40°C and 75% relative humidity, and the onset of recrystallization was monitored by DSC. An increase in coating thickness provided enhanced stability against recrystallization for up to 6 months at accelerated storage conditions (longest time of observation) when compared to three days for uncoated ketoprofen. Results from XPS analysis demonstrated that an increase in coating thickness was associated with improved surface coverage thus enabling superior protection. Dissolution testing showed that at least 80% of ketoprofen was released in buffer pH 6.8 from all coated samples. Overall, an increase in coating thickness resulted in a more complete drug release due to decreased adhesion of the coating to the substrate. Copyright © 2010 Elsevier B.V. All rights reserved.

Devitrification and recrystallization of nanoparticle-containing glycerol and PEG-600 solutions.

PubMed

Lv, Fukou; Liu, Baolin; Li, Weijie; Jaganathan, Ganesh K

2014-02-01

Nanoparticles in solution offer unique electrical, mechanical and thermal properties due to their physical presence and interaction with the state of dispersion. This work is aimed to study the effects of hydroxyapatite (HA) nanoparticles on the devitrification and recrystallization events of two important cryoprotective solutions used in cell and tissue preservation namely glycerol (60%w/w) and PEG-600 (50%w/w). HA nanoparticles (20, 40 or 60 nm) were incorporated into solutions at the content of 0.1% or 0.5%(w/w), and were studied by differential scanning calorimeter (DSC) and cryomicroscopy. The presence of nanoparticles does not change the glass transition temperatures and melting temperatures of quenched solutions, but significantly affects the behavior of devitrification and recrystallization upon warming. Cryomicroscopic investigation showed the complex interactions among solution type, nanoparticle size and nanoparticle content, which apparently influence ice crystal growth or recrystallization in the quenched dispersions. These findings have significant implications for biomaterial cryopreservation, cryosurgery, and food manufacturing. The complexity of ice crystal growth kinetics in nanoparticle-containing dispersions remains to be poorly understood at the moment. Copyright © 2013 Elsevier Inc. All rights reserved.

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.

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.

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.

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.

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.

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

Solid-state characterization of nevirapine.

PubMed

Sarkar, Mahua; Perumal, O P; Panchagnula, R

2008-09-01

The purpose of this investigation is to characterize nevirapine from commercial samples and samples crystallized from different solvents under various conditions. The solid-state behavior of nevirapine samples was investigated using a variety of complementary techniques such as microscopy (optical, polarized, hot stage microscopy), differential scanning calorimeter, thermogravimetric analysis, Fourier transform infrared spectroscopy and powder X-ray diffractometry. The commercial samples of nevirapine had the same polymorphic crystalline form with an anhedral crystal habit. Intrinsic dissolution of nevirapine was similar for both the commercial batches. Powder dissolution showed pH dependency, with maximum dissolution in acidic pH and there was no significant effect of particle size. The samples recrystallized from different solvent systems with varying polarity yielded different crystal habits. Stirring and degrees of supersaturation influenced the size and shape of the crystals. The recrystallized samples did not produce any new polymorphic form, but weak solvates with varying crystal habit were produced. Recrystallized samples showed differences in the x-ray diffractograms. However, all the samples had the same internal crystal lattice as revealed from their similar melting points and heat of fusion. The intrinsic dissolution rate of recrystallized samples was lower than the commercial sample. It was found that the compression pressure resulted in desolvation and partial conversion of the crystal form. After compression, the recrystallized samples showed similar x-ray diffractograms to the commercial sample. Amorphous form showed slightly higher aqueous solubility than the commercial crystalline form.

Recrystallization Behavior in SAC305 and SAC305 + 3.0POSS Solder Joints Under Thermal Shock

NASA Astrophysics Data System (ADS)

Han, Jing; Gu, Penghao; Ma, Limin; Guo, Fu; Liu, Jianping

2018-04-01

Sn-3.0Ag-0.5Cu (SAC305) and SAC305 + 3.0 polyhedral oligomeric silsesquioxanes (POSS) ball grid array (BGA) assemblies have been prepared, observed, and subjected to thermal shock. The microstructure and grain orientation evolution of the solder joints located at the same position of the package were characterized by scanning electron microscopy and electron backscattering diffraction, respectively. The results showed that the microstructure of the solder joints was refined by addition of POSS particles. In addition, compared with the single-grained or tricrystal joints normally observed in SAC305 BGA solder joints, the frequency of single-grained as-reflowed SAC305 + 3.0POSS BGA joints was greatly reduced, and the solder joints were typically composed of multicrystals with orientations separated by high-angle grain boundaries. These multicrystal joints appear to be obtained by dominant tricrystals or double tricrystals with deviation of the preferred [110] and [1\\bar{1}0] growth directions of Sn dendrites in Sn-Ag-based solder alloys during solidification from the melt. After 928 thermal shock cycles, the SAC305 solder joint had large-area recrystallization and cracks in contrast to the SAC305 + 3.0POSS solder joint located at the same position of the package, indicating that addition of POSS to SAC305 solder joints may contribute to postponement of recrystallization and subsequent crack initiation and propagation along recrystallized grain boundaries by pinning grain boundaries and movement of dislocations. This finding also confirms the double tricrystal solidification twinning nucleation behavior in Pb-free solder joints.

Microstructure and Mechanical Properties in Hot-Rolled Extra High-Yield-Strength Steel Plates for Offshore Structure and Shipbuilding

NASA Astrophysics Data System (ADS)

Liu, Dongsheng; Li, Qingliang; Emi, Toshihiko

2011-05-01

Key parameters for a thermomechanically controlled processing and accelerated cooling process (TMCP-AcC) were determined for integrated mass production to produce extra high-yield-strength microalloyed low carbon SiMnCrNiCu steel plates for offshore structure and bulk shipbuilding. Confocal scanning microscopy was used to make in-situ observations on the austenite grain growth during reheating. A Gleeble 3800 thermomechanical simulator was employed to investigate the flow stress behavior, static recrystallization (SRX) of austenite, and decomposition behavior of the TMCP conditioned austenite during continuous cooling. The Kocks-Mecking model was employed to describe the constitutive behavior, while the Johnson-Mehl-Avrami-Kolmogorov (JMAK) approach was used to predict the SRX kinetics. The effects of hot rolling schedule and AcC on microstructure and properties were investigated by test-scale rolling trials. The bridging between the laboratory observations and the process parameter determination to optimize the mass production was made by integrated industrial production trials on a set of a 5-m heavy plate mill equipped with an accelerated cooling system. Successful production of 60- and 50-mm-thick plates with yield strength in excess of 460 MPa and excellent toughness at low temperature (213 K (-60 °C)) in the parent metal and the simulated coarse-grained heat affected zone (CGHAZ) provides a useful integrated database for developing advanced high-strength steel plates via TMCP-AcC.

Impact of surface wettability on S-layer recrystallization: a real-time characterization by QCM-D.

PubMed

Iturri, Jagoba; Vianna, Ana C; Moreno-Cencerrado, Alberto; Pum, Dietmar; Sleytr, Uwe B; Toca-Herrera, José Luis

2017-01-01

Quartz crystal microbalance with dissipation monitoring (QCM-D) has been employed to study the assembly and recrystallization kinetics of isolated SbpA bacterial surface proteins onto silicon dioxide substrates of different surface wettability. Surface modification by UV/ozone oxidation or by vapor deposition of 1 H ,1 H ,2 H ,2 H -perfluorododecyltrichlorosilane yielded hydrophilic or hydrophobic samples, respectively. Time evolution of frequency and dissipation factors, either individually or combined as the so-called Df plots, showed a much faster formation of crystalline coatings for hydrophobic samples, characterized by a phase-transition peak at around the 70% of the total mass adsorbed. This behavior has been proven to mimic, both in terms of kinetics and film assembly steps, the recrystallization taking place on an underlying secondary cell-wall polymer (SCWP) as found in bacteria. Complementary atomic force microscopy (AFM) experiments corroborate these findings and reveal the impact on the final structure achieved.

The influence of gamma prime on the recrystallization of an oxide dispersion strengthened superalloy - MA 6000E

NASA Technical Reports Server (NTRS)

Hotzler, R. K.; Glasgow, T. K.

1982-01-01

The requirement of large, recrystallized, highly elongated grains is of primary importance to the development of suitable high temperature properties in oxide dispersion strengthened-superalloys. In the present study the recrystallization behavior of MA 6000E, a recently developed Y2O3 strengthened superalloy produced by mechanical alloying, was examined using transmission and replication microscopy. Gradient and isothermal annealing treatments were applied to extruded and hot rolled products. It was found that conversion from a very fine (0.2 micron) grain structure to a coarse (approximately 10 mm) grain structure is controlled by the dissolution of the gamma prime phase, while grain shape was controlled primarily by the thermal gradient. The fine uniform oxide dispersion appeared to have only a secondary influence in determining the grain shape as columnar grains could be grown transverse to the working direction by appropriate application of the thermal gradient.

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

Myers, M.A.; LaSalvia, J.C.; Hoke, D.

Combustion synthesis followed by densification was utilized in producing monolithic TiC and TiB2 materials, and TiC-Ni, TiB2-Ni, TiB2-Al2O3, and TiB2SiC ceramic composites. Static and dynamic densification equipments were developed with the loading applied immediately after the synthesis reaction was completed and the ceramic/composite was ductile. All the ceramics exhibited an equiaxed grain structure with alternating regions at high and low dislocation densities, indicating that recovery/recrystallization mechanisms are prevalent. The grain boundaries were, as far as could be established, devoid of impurities and second phases. Quasi-static and dynamic mechanical testing were performed and revealed that the materials exhibited strength levels comparablemore » to conventionally produced materials. Instrumented densification experiments were conducted and a temperature-dependent consitutive model was applied for plastic deformation of the porous combustion synthesis product.« less

Effects of Al3(Sc,Zr) and Shear Band Formation on the Tensile Properties and Fracture Behavior of Al-Mg-Sc-Zr Alloy

NASA Astrophysics Data System (ADS)

Huang, Hongfeng; Jiang, Feng; Zhou, Jiang; Wei, Lili; Qu, Jiping; Liu, Lele

2015-11-01

The mechanical properties and microstructures of Al-6Mg-0.25Sc-0.1Zr alloy (wt.%) during annealing were investigated by means of uniaxial tensile testing, optical microscope, scanning electron microscope, transmission electron microscope, and high-resolution transmission electron microscope. The results show that a large number of micro and grain-scale shear bands form in this alloy after cold rolling. As the tensile-loading force rises, strain softening would generate in shear bands, resulting in the occurrence of shear banding fracture in cold-rolled Al-Mg-Sc-Zr alloys. Recrystallization takes place preferentially in shear bands during annealing. Due to the formation of coarse-grain bands constructed by new subgrains, recrystallization softening tends to occur in these regions. During low-temperature annealing, recrystallization is inhibited by nano-scale Al3(Sc,Zr) precipitates which exert significant coherency strengthening and modulus hardening. However, the strengthening effect of Al3(Sc,Zr) decreases with the increasing of particle diameter at elevated annealing temperature. The mechanical properties of the recrystallized Al-Mg-Sc-Zr alloy decrease to a minimum level, and the fracture plane exhibits pure ductile fracture characteristics.

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.

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.

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

NASA Astrophysics Data System (ADS)

Fu, Xiaobin; Wang, Baoyu; Tang, Xuefeng

2017-10-01

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

The 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.

Microstructural study of the Mertz shear zone, East Antarctica. Implications for deformation processes and seismic anisotropy.

NASA Astrophysics Data System (ADS)

Lamarque, Gaëlle; Bascou, Jérôme; Maurice, Claire; Cottin, Jean-Yves; Ménot, René-Pierre

2015-04-01

The Mertz Shear Zone (MSZ; 146°E 67°S; East Antarctica) is one major lithospheric-scale structure which outcrops on the eastern edge of the Terre Adélie Craton (Ménot et al., 2007) and that could connected with shear zones of South Australia (e.g., Kalinjala or Coorong shear zone (Kleinschmidt and Talarico, 2000; Gibson et al., 2013)) before the Cretaceous opening of the Southern Ocean. Geochronological and metamorphic studies indicated an MSZ activity at 1.7 and 1.5 Ga respectively in amphibolite and greenschists facies conditions. The deformation affects both the intermediate and lower crust levels, without associated voluminous magma injection. Granulite crop out in the area of the MSZ. They were dated at 2.4 Ga (Ménot et al., 2005) and could represent some preserved Neoarchean tectonites. These rocks show various degrees of deformation including penetrative structures that may display comparable features with that observed in amphibolite and greenschists facies rocks, i.e. NS-striking and steeply dipping foliation with weekly plunging lineation. In the field, cinematic indicators for the MSZ argue for a dominant dextral shear sense. We proceed to optical analysis and crystallographic preferred orientation (CPO) measurements using EBSD technique in order to better constrain the deformation processes. Our results highlight (1) a microstructural gradient from highly deformed rocks (mylonites), forming plurimetric large shear bands and showing evidences of plastic deformation, to slightly deformed rocks in preserved cores with no evidences of plastic deformation or with a clear strong static recrystallization; (2) CPO of minerals related with variations on deformation conditions. Feldspar and quartz CPO argue for plastic deformation at high temperature in the most deformed domains and for the absence of deformation or an important stage of static recrystallization in preserved cores; (3) uncommon CPO in orthopyroxene which are characterized by [010]-axes perpendicular to the foliation and [001]-axes parallel to the lineation. These CPO seem to be related to static recrystallization processes. Seismic properties of amphibolite and granulite rocks from the MSZ were calculated in order to evaluate the impact of deformation observed in amphibolite and granulite tectonites to seismic anisotropy. Computations were performed from measured CPO, single crystal elastic stiffness matrix, modal composition and density of characteristic samples. P- and S-waves anisotropies of the cratonic crust affected by the MSZ are small and even tend to be isotropic in the case of S-waves propagating vertically in the crust. These results permit us to better discuss seismic studies and in particular SKS analysis which were recently carried out in this area (Lamarque et al., 2015).

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 effect of solute additions on the steady-state creep behavior of dispersion-strengthened aluminum.

NASA Technical Reports Server (NTRS)

Reynolds, G. H.; Lenel, F. V.; Ansell, G. S.

1971-01-01

The effect of solute additions on the steady-state creep behavior of coarse-grained dispersion-strengthened aluminum alloys was studied. Recrystallized dispersion-strengthened solid solutions were found to have stress and temperature sensitivities quite unlike those observed in single-phase solid solutions having the same composition and grain size. The addition of magnesium or copper to the matrix of a recrystallized dispersion-strengthened aluminum causes a decrease in the steady-state creep rate which is much smaller than that caused by similar amounts of solute in single-phase solid solutions. All alloys exhibited essentially a 4.0 power stress exponent in agreement with the model of Ansell and Weertman. The activation energy for steady-state creep in dispersion-strengthened Al-Mg alloys, as well as the stress dependence, was in agreement with the physical model of dislocation climb over the dispersed particles.

The DART dispersion analysis research tool: A mechanistic model for predicting fission-product-induced swelling of aluminum dispersion fuels. User`s guide for mainframe, workstation, and personal computer applications

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

Rest, J.

1995-08-01

This report describes the primary physical models that form the basis of the DART mechanistic computer model for calculating fission-product-induced swelling of aluminum dispersion fuels; the calculated results are compared with test data. In addition, DART calculates irradiation-induced changes in the thermal conductivity of the dispersion fuel, as well as fuel restructuring due to aluminum fuel reaction, amorphization, and recrystallization. Input instructions for execution on mainframe, workstation, and personal computers are provided, as is a description of DART output. The theory of fission gas behavior and its effect on fuel swelling is discussed. The behavior of these fission products inmore » both crystalline and amorphous fuel and in the presence of irradiation-induced recrystallization and crystalline-to-amorphous-phase change phenomena is presented, as are models for these irradiation-induced processes.« less

Static Recovery Modeling of Dislocation Density in a Cold Rolled Clad Aluminum Alloy

NASA Astrophysics Data System (ADS)

Penlington, Alex

Clad alloys feature one or more different alloys bonded to the outside of a core alloy, with non-equilibrium, interalloy interfaces. There is limited understanding of the recovery and recrystallization behaviour of cold rolled clad aluminum alloys. In order to optimize the properties of such alloys, new heat treatment processes may be required that differ from what is used for the monolithic alloys. This study examines the recovery behaviour of a cold rolled Novelis Fusion(TM) alloy containing an AA6XXX core with an AA3003 cladding on one side. The bond between alloys appears microscopically discrete and continuous, but has a 30 microm wide chemical gradient. The as-deformed structure at the interalloy region consists of pancaked sub-grains with dislocations at the misorientation boundaries and a lower density organized within the more open interiors. X-ray line broadening was used to extract the dislocation density from the interalloy region and an equivalently deformed AA6XXX following static annealing using a modified Williamson-Hall analysis. This analysis assumed that Gaussian broadening contributions in a pseudo-Voigt function corresponded only to strain from dislocations. The kinetics of the dislocation density evolution to recrystallization were studied isothermally at 2 minute intervals, and isochronally at 175 and 205°C. The data fit the Nes model, in which the interalloy region recovered faster than AA6XXX at 175°C, but was slower at 205°C. This was most likely caused by change in texture and chemistry within this region such as over-aging of AA6XXX . Simulation of a continuous annealing and self homogenization process both with and without pre-recovery indicates a detectable, though small change in the texture and grain size in the interalloy region.

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.

Recrystallization behavior and thermal shock resistance of the W-1.0 wt% TaC alloy

NASA Astrophysics Data System (ADS)

Xie, Z. M.; Miao, S.; Zhang, T.; Liu, R.; Wang, X. P.; Fang, Q. F.; Hao, T.; Zhuang, Z.; Liu, C. S.; Lian, Y. Y.; Liu, X.; Cai, L. H.

2018-04-01

The high-temperature stability and good mechanical strength of tungsten (W) alloys are highly desirable for a wide range of fusion applications, which can be achieved by dispersion strengthening. In this paper, TaC dispersion effects on the thermal stabilities, tensile properties and thermal shock resistances have been investigated. A hot-rolled W-1.0 wt% TaC plate has been fabricated which contains the high tensile strength and elongation. Nanosized particles in the W matrix improve the recrystallization temperature to about 1400 °C and the ultimate tensile strength to 571 MPa at 500 °C through hindering grain boundary migration, pinning dislocations and refining grains. The effects of edge-localized mode like transient heat events on the rolled and recrystallized W-1.0 wt% TaC alloys were investigated systematically. The cracking threshold (100 shots) at room temperature is in the range of 0.33-0.44 GW/m2 for the rolled W-1.0 wt% TaC. Recrystallization degrades mechanical strength and makes the material more prone to thermal shock damages. Coarse Ta2O5 and Ta-Cx-Oy particles are easy to fracture and introduce a preferential crack initiation in W matrix during cyclic heat loads.

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.

Impact of surface wettability on S-layer recrystallization: a real-time characterization by QCM-D

PubMed Central

Vianna, Ana C; Moreno-Cencerrado, Alberto; Pum, Dietmar; Sleytr, Uwe B

2017-01-01

Quartz crystal microbalance with dissipation monitoring (QCM-D) has been employed to study the assembly and recrystallization kinetics of isolated SbpA bacterial surface proteins onto silicon dioxide substrates of different surface wettability. Surface modification by UV/ozone oxidation or by vapor deposition of 1H,1H,2H,2H-perfluorododecyltrichlorosilane yielded hydrophilic or hydrophobic samples, respectively. Time evolution of frequency and dissipation factors, either individually or combined as the so-called Df plots, showed a much faster formation of crystalline coatings for hydrophobic samples, characterized by a phase-transition peak at around the 70% of the total mass adsorbed. This behavior has been proven to mimic, both in terms of kinetics and film assembly steps, the recrystallization taking place on an underlying secondary cell-wall polymer (SCWP) as found in bacteria. Complementary atomic force microscopy (AFM) experiments corroborate these findings and reveal the impact on the final structure achieved. PMID:28144568

Deformation, recrystallization, strength, and fracture of press-forged ceramic crystals.

NASA Technical Reports Server (NTRS)

Rice, R. W.

1972-01-01

Sapphire and ruby were very difficult to press-forge because they deformed without cracking only in a limited temperature range before they melted. Spinel crystals were somewhat easier and MgO, CaO, and TiC crystals much easier to forge. The degree of recrystallization that occurred during forging (which was related to the ease and type of slip intersections) varied from essentially zero in Al2O3 to complete (i.e., random polycrystalline bodies were produced) in CaO. Forging of bi- and polycrystalline bodies produced incoherent bodies as a result of grain-boundary sliding. Strengths of the forged crystals were comparable to those of dense polycrystalline bodies of similar grain size. However, forged and recrystallized CaO crystals were ductile at lower temperatures than dense hot-pressed CaO. This behavior is attributed to reduced grain-boundary impurities and porosity. Fracture origins could be located, indicating that fracture in the CaO occurs internally as a result of surface work hardening caused by machining.-

Creep-Rupture Behavior and Recrystallization in HR6W and Haynes Alloy 230 Cold-Bent Boiler Tubing for Ultrasupercritical (USC) Steam Boiler Applications

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

Shingledecker, John P

2007-01-01

Creep-rupture experiments were conducted on HR6W and Haynes 230, candidate Ultrasupercritical (USC) alloys, tubes to evaluate the effects of cold-work and recrystallization during high-temperature service. These creep tests were performed by internally pressurizing cold-bent boiler tubes at 775 C for times up to 8000 hours. The bends were fabricated with cold-work levels beyond the current ASME Boiler and Pressure Vessel (ASME B&PV) Code Section I limits for austenitic stainless steels. Destructive metallographic evaluation of the crept tube bends was used to determine the effects of cold-work and the degree of recrystallization. The metallographic analysis combined with an evaluation of themore » creep and rupture data suggest that solid-solution strengthened nickel-based alloys can be fabricated for high-temperature service at USC conditions utilizing levels of cold-work higher than the current allowed levels for austenitic stainless steels.« less

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

NASA Astrophysics Data System (ADS)

Liu, Fenjun; Fu, Li; Chen, Haiyan

2018-06-01

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

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.

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.

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.

Dynamic Recrystallization Model for Whisker and Hillock Growth

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

Vianco, Paul T.; Neilsen, Michael K.

2015-07-01

Tin (Sn) whiskers are not a recent development. Studies in the late 1930’s investigated thin filaments that grew spontaneously from Sn coatings used for the corrosion protection of electronic hardware. It was soon recognized that these Sn filaments,or whiskers, could create short circuits in the same electronic equipment. Figure 1a illustrates whisker growth in the hole of a printed circuit board having an immersion Sn surface finish. The engineering solution was to contaminate the Sn with > 3wt.% of lead (Pb). The result was that whisker growth was replaced with hillock formation (Fig. 1b) that posed a minimal reliability concerntomore » electrical circuits. Today, Pb-containing finishes are being replaced with pure Sn coatings to meet environmental restrictions on Pb use. The same short-circuit concerns have been raised, once again, with respect to Sn whiskers. The present authors have taken the approach that, in order to develop more widely applicable, first-principles strategies to mitigate Sn whisker formation, it is necessary to understand the fundamental mechanism(s) and rate kinetics underlying their development. Numerous mechanisms have been proposed by other authors to describe whisker growth, including static recrystallization by Boguslavsky and Bush.« less

Microscopic approach of the crystallization of tripalmitin and tristearin by microscopy.

PubMed

Silva, Roberta Claro da; Martini Soares, Fabiana Andrea Schafer De; Maruyama, Jéssica Mayumi; Dagostinho, Natália Roque; Silva, Ylana Adami; Ract, Juliana Neves Rodrigues; Gioielli, Luiz Antonio

2016-06-01

The crystallization behavior of lipids has important implications in industrial processing of food products, whose physical characteristics depend largely on crystallized fats. The study of the crystallization behavior and polymorphism of a pure lipid system is of great scientific importance as a means of gaining an understanding of the phenomena involved, serving as basic knowledge to help guide the addition or removal of these compounds in different raw materials. The crystallization behavior and polymorphism of pure tripalmitin (PPP) and tristearin (SSS) were investigated by Polarized Light Microscopy (PLM) and Differential Scanning Calorimetry (DSC) under different crystallization conditions. The polymorphic forms (β' and β) of PPP and SSS exhibited different morphologies depending on how they were obtained, either from α form recrystallization or from isotropic melt. Crystallization in the β form was faster in SSS than in PPP, indicating that the process occurs faster in TAGs composed of longer fatty acid chains. Both β' and β polymorphic forms were obtained from α form recrystallization, albeit with predominance of the β form. Copyright © 2016 Elsevier Ireland Ltd. All rights reserved.

Structure of aging Al-Li-Cu-Zr-Sc-Ag alloy after severe plastic deformation and long-term storage

NASA Astrophysics Data System (ADS)

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

2015-11-01

Structural and phase transformations in commercial aging aluminum-lithium Al-1.2 Li-3.2 Cu-0.09 Zr-0.11 Sc-0.4 Ag-0.3 Mg alloy have been studied after severe plastic deformation by high-pressure torsion (at a pressure of 4 GPa with 1, 5, and 10 revolutions of the anvil) and natural aging (roomtemperature storage) for 1 week and 2 years. It has been found that, in this case, the process of static recrystallization is achieved in the alloy, the degree of which increases with an increasing degree of deformation and time of storage.

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.

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°).

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

Thermogravimetric study of vapor pressure of TATP synthesized without recrystallization.

PubMed

Mbah, Jonathan; Knott, Debra; Steward, Scott

2014-11-01

This study aims at characterizing the vapor pressure signatures generated by triacetone triperoxide (TATP) that was synthesized without recrystallization by thermogravimmetric analysis (TGA) for exploitation by standoff detection technologies of explosive devices. The thermal behavior of the nonrecrystallized sample was compared with reported values. Any phase change, melting point and decomposition identification were studied by differential scanning calorimeter. Vapor pressures were estimated by the Langmuir method of evaporation from an open surface in a vacuum. Vapor pressures of TATP at different temperatures were calculated using the linear logarithmic relationship obtained from benzoic acid reference standard. Sublimation of TATP was found to follow apparent zero-order kinetics and sublimes at steady rates at 298 K and above. While the enthalpy of sublimation found, 71.7 kJ mol(-1), is in agreement with reported values the vapor pressures deviated significantly. The differences in the vapor pressures behavior are attributable to the synthesis pathway chosen in this study. Copyright © 2014 Elsevier B.V. All rights reserved.

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.

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.

Quartz grainsize evolution during dynamic recrystallization across a natural shear zone boundary

NASA Astrophysics Data System (ADS)

Xia, Haoran; Platt, John P.

2018-04-01

Although it is widely accepted that grainsize reduction by dynamic recrystallization can lead to strain localization, the details of the grainsize evolution during dynamic recrystallization remain unclear. We investigated the bulge size and grainsizes of quartz at approximately the initiation and the completion stages of bulging recrystallization across the upper boundary of a 500 m thick mylonite zone above the Vincent fault in the San Gabriel Mountains, southern California. Within uncertainty, the average bulge size of quartz, 4.7 ± 1.5 μm, is the same as the recrystallized grainsize, 4.5 ± 1.5 μm, at the incipient stage of dynamic recrystallization, and also the same within uncertainties as the recrystallized grainsize when dynamic recrystallization is largely complete, 4.7 ± 1.3 μm. These observations indicate that the recrystallized grainsize is controlled by the nucleation process and does not change afterwards. It is also consistent with the experimental finding that the quartz recrystallized grainsize paleopiezometer is independent of temperature.

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.

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.

Oxide formation and anodic polarization behavior of thin films of amorphous and crystalline FeCrP alloys prepared by ion beam mixing

NASA Astrophysics Data System (ADS)

Demaree, J. D.; Was, G. S.; Sorensen, N. R.

1991-07-01

An experimental program has been conducted to determine the effect of phosphorus on the corrosion and passivation behavior of FeCrP alloys. Chemically homogeneous 60 nm films of Fe10Cr xP ( x from 0 to 35 at.%) were prepared by multilayer evaporation followed by ion beam mixing with Kr + ions. Films with a phosphorus content of at least 25 at.% were found to be entirely amorphous, while films with 15 at.% P consisted of both amorphous and bcc phases. Recrystallization of the amorphous phase was accomplished by heating the samples to 450°C in a purified argon flow furnace. Electrochemical polarization tests in an acid solution have shown the Fe10Cr xP films to be more corrosion resistant than Fe10Cr, with the corrosion resistance increasing with the amount of P present. The corrosion resistance is not significantly affected when the amorphous films are recrystallized, indicating that the behavior is chemically controlled and not a result of the amorphous structure. When examined by XPS, the phosphorus appears to enhance passivation by encouraging Cr enrichment in the oxide and by incorporating in the oxide as phosphate.

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.

Hydride reorientation and its impact on ambient temperature mechanical properties of high burn-up irradiated and unirradiated recrystallized Zircaloy-2 nuclear fuel cladding with an inner liner

NASA Astrophysics Data System (ADS)

Auzoux, Q.; Bouffioux, P.; Machiels, A.; Yagnik, S.; Bourdiliau, B.; Mallet, C.; Mozzani, N.; Colas, K.

2017-10-01

Precipitation of radial hydrides in zirconium-based alloy cladding concomitant with the cooling of spent nuclear fuel during dry storage can potentially compromise cladding integrity during its subsequent handling and transportation. This paper investigates hydride reorientation and its impact on ductility in unirradiated and irradiated recrystallized Zircaloy-2 cladding with an inner liner (cladding for boiling water reactors) subjected to hydride reorientation treatments. Cooling from 400 °C, hydride reorientation occurs in recrystallized Zircaloy-2 with liner at a lower effective stress in irradiated samples (below 40 MPa) than in unirradiated specimens (between 40 and 80 MPa). Despite significant hydride reorientation, unirradiated recrystallized Zircaloy-2 with liner cladding containing ∼200 wppm hydrogen shows a high diametral strain at fracture (>15%) during burst tests at ambient temperature. This ductile behavior is due to (1) the lower yield stress of the recrystallized cladding materials in comparison to hydride fracture strength (corrected by the compression stress arising from the precipitation) and (2) the hydride or hydrogen-depleted zone as a result of segregation of hydrogen into the liner layer. In irradiated Zircaloy-2 with liner cladding containing ∼340 wppm hydrogen, the conservation of some ductility during ring tensile tests at ambient temperature after reorientation treatment at 400 °C with cooling rates of ∼60 °C/h is also attributed to the existence of a hydride-depleted zone. Treatments at lower cooling rates (∼6 °C/h and 0.6 °C/h) promote greater levels of hydrogen segregation into the liner and allow for increased irradiation defect annealing, both of which result in a significant increase in ductility. Based on this investigation, given the very low cooling rates typical of dry storage systems, it can be concluded that the thermal transients associated with dry storage should not degrade, and more likely should actually improve, ductility of recrystallized Zircaloy-2 cladding with inner liner with such hydrogen content.

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%.

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.

Nanoscale measurements of phosphorous-induced lattice expansion in nanosecond laser annealed germanium

NASA Astrophysics Data System (ADS)

Boninelli, S.; Milazzo, R.; Carles, R.; Houdellier, F.; Duffy, R.; Huet, K.; La Magna, A.; Napolitani, E.; Cristiano, F.

2018-05-01

Laser Thermal Annealing (LTA) at various energy densities was used to recrystallize and activate amorphized germanium doped with phosphorous by ion implantation. The structural modifications induced during the recrystallization and the related dopant diffusion were first investigated. After LTA at low energy densities, the P electrical activation was poor while the dopant distribution was mainly localized in the polycrystalline Ge resulting from the anneal. Conversely, full dopant activation (up to 1 × 1020 cm-3) in a perfectly recrystallized material was observed after annealing at higher energy densities. Measurements of lattice parameters performed on the fully activated structures show that P doping results in a lattice expansion, with a perpendicular lattice strain per atom βPs = +0.7 ± 0.1 Å3. This clearly indicates that, despite the small atomic radius of P compared to Ge, the "electronic contribution" to the lattice parameter modification (due to the increased hydrostatic deformation potential in the conduction band of P doped Ge) is larger than the "size mismatch contribution" associated with the atomic radii. Such behavior, predicted by theory, is observed experimentally for the first time, thanks to the high sensitivity of the measurement techniques used in this work.

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

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.

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.

Purification and thermal analysis of perfluoro-n-alkanoic acids.

PubMed

Tsuji, Minami; Inoue, Tohru; Shibata, Osamu

2008-01-15

Purification of perfluoro-n-alkanoic acids (C(n)F(2n+1)COOH, n=7, 9, 11, 13, 15 and 17) was made by repeated recrystallizations from n-hexane/acetone mixed solvent, and their purity was found to be more than 99.5% by GC-MS, NMR, and elemental analysis. The thermal behaviors such as melting point and enthalpy change of fusion were investigated using differential scanning calorimetry (DSC). The melting point monotonously increased with increasing carbon number (n) of the acids, while the enthalpy change showed irregularity at n=14. The crystal structure of these acids was found to be dependent upon solvent used for recrystallization; that is, the acids recrystallized from the above solvent becomes more stable energetically, indicating their higher enthalpy change of fusion than that of the solidified acids from fused ones. The solid state was also found to vary depending upon the thermal history, indicating that a few crystal structures of the solid state are quite similar energetically. The melting points (T(m)) of perfluoro-n-alkanoic acids are higher than those of corresponding n-alkanoic acids, and the difference in T(m) increases with increasing carbon number in the acids.

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.

Neural Correlates of Racial Ingroup Bias in Observing Computer-Animated Social Encounters.

PubMed

Katsumi, Yuta; Dolcos, Sanda

2017-01-01

Despite evidence for the role of group membership in the neural correlates of social cognition, the mechanisms associated with processing non-verbal behaviors displayed by racially ingroup vs. outgroup members remain unclear. Here, 20 Caucasian participants underwent fMRI recording while observing social encounters with ingroup and outgroup characters displaying dynamic and static non-verbal behaviors. Dynamic behaviors included approach and avoidance behaviors, preceded or not by a handshake; both dynamic and static behaviors were followed by participants' ratings. Behaviorally, participants showed bias toward their ingroup members, demonstrated by faster/slower reaction times for evaluating ingroup static/approach behaviors, respectively. At the neural level, despite overall similar responses in the action observation network to ingroup and outgroup encounters, the medial prefrontal cortex showed dissociable activation, possibly reflecting spontaneous processing of ingroup static behaviors and positive evaluations of ingroup approach behaviors. The anterior cingulate and superior frontal cortices also showed sensitivity to race, reflected in coordinated and reduced activation for observing ingroup static behaviors. Finally, the posterior superior temporal sulcus showed uniquely increased activity to observing ingroup handshakes. These findings shed light on the mechanisms of racial ingroup bias in observing social encounters, and have implications for understanding factors related to successful interactions with individuals from diverse backgrounds.

Neural Correlates of Racial Ingroup Bias in Observing Computer-Animated Social Encounters

PubMed Central

Katsumi, Yuta; Dolcos, Sanda

2018-01-01

Despite evidence for the role of group membership in the neural correlates of social cognition, the mechanisms associated with processing non-verbal behaviors displayed by racially ingroup vs. outgroup members remain unclear. Here, 20 Caucasian participants underwent fMRI recording while observing social encounters with ingroup and outgroup characters displaying dynamic and static non-verbal behaviors. Dynamic behaviors included approach and avoidance behaviors, preceded or not by a handshake; both dynamic and static behaviors were followed by participants’ ratings. Behaviorally, participants showed bias toward their ingroup members, demonstrated by faster/slower reaction times for evaluating ingroup static/approach behaviors, respectively. At the neural level, despite overall similar responses in the action observation network to ingroup and outgroup encounters, the medial prefrontal cortex showed dissociable activation, possibly reflecting spontaneous processing of ingroup static behaviors and positive evaluations of ingroup approach behaviors. The anterior cingulate and superior frontal cortices also showed sensitivity to race, reflected in coordinated and reduced activation for observing ingroup static behaviors. Finally, the posterior superior temporal sulcus showed uniquely increased activity to observing ingroup handshakes. These findings shed light on the mechanisms of racial ingroup bias in observing social encounters, and have implications for understanding factors related to successful interactions with individuals from diverse backgrounds. PMID:29354042

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

Why and How We Made a Problem Oriented AV Teaching Unit for Chemistry Students.

ERIC Educational Resources Information Center

Mulder, T. H. M.; Verdonk, A. H.

1984-01-01

Describes an audiovisual teaching unit on the chemical laboratory technique of recrystallization which was developed along problem-solving lines and based on observation of student laboratory behavior. Discussion includes usual procedures for developing such units, how this unit solves problems typically associated with teaching, and its general…

Behavior of Sn atoms in GeSn thin films during thermal annealing: Ex-situ and in-situ observations

NASA Astrophysics Data System (ADS)

Takase, Ryohei; Ishimaru, Manabu; Uchida, Noriyuki; Maeda, Tatsuro; Sato, Kazuhisa; Lieten, Ruben R.; Locquet, Jean-Pierre

2016-12-01

Thermally induced crystallization processes for amorphous GeSn thin films with Sn concentrations beyond the solubility limit of the bulk crystal Ge-Sn binary system have been examined by X-ray photoelectron spectroscopy, grazing incidence X-ray diffraction, and (scanning) transmission electron microscopy. We paid special attention to the behavior of Sn before and after recrystallization. In the as-deposited specimens, Sn atoms were homogeneously distributed in an amorphous matrix. Prior to crystallization, an amorphous-to-amorphous phase transformation associated with the rearrangement of Sn atoms was observed during heat treatment; this transformation is reversible with respect to temperature. Remarkable recrystallization occurred at temperatures above 400 °C, and Sn atoms were ejected from the crystallized GeSn matrix. The segregation of Sn became more pronounced with increasing annealing temperature, and the ejected Sn existed as a liquid phase. It was found that the molten Sn remains as a supercooled liquid below the eutectic temperature of the Ge-Sn binary system during the cooling process, and finally, β-Sn precipitates were formed at ambient temperature.

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.

Determination of grain boundary mobility during recrystallization by statistical evaluation of electron backscatter diffraction measurements

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

Basu, I., E-mail: basu@imm.rwth-aachen.de; Chen, M.; Loeck, M.

One of the key aspects influencing microstructural design pathways in metallic systems is grain boundary motion. The present work introduces a method by means of which direct measurement of grain boundary mobility vs. misorientation dependence is made possible. The technique utilizes datasets acquired by means of serial electron backscatter diffraction (EBSD) measurements. The experimental EBSD measurements are collectively analyzed, whereby datasets were used to obtain grain boundary mobility and grain aspect ratio with respect to grain boundary misorientation. The proposed method is further validated using cellular automata (CA) simulations. Single crystal aluminium was cold rolled and scratched in order tomore » nucleate random orientations. Subsequent annealing at 300 °C resulted in grains growing, in the direction normal to the scratch, into a single deformed orientation. Growth selection was observed, wherein the boundaries with misorientations close to Σ7 CSL orientation relationship (38° 〈111〉) migrated considerably faster. The obtained boundary mobility distribution exhibited a non-monotonic behavior with a maximum corresponding to misorientation of 38° ± 2° about 〈111〉 axes ± 4°, which was 10–100 times higher than the mobility values of random high angle boundaries. Correlation with the grain aspect ratio values indicated a strong growth anisotropy displayed by the fast growing grains. The observations have been discussed in terms of the influence of grain boundary character on grain boundary motion during recrystallization. - Highlights: • Statistical microstructure method to measure grain boundary mobility during recrystallization • Method implementation independent of material or crystal structure • Mobility of the Σ7 boundaries in 5N Al was calculated as 4.7 × 10{sup –8} m{sup 4}/J ⋅ s. • Pronounced growth selection in the recrystallizing nuclei in Al • Boundary mobility values during recrystallization 2–3 orders of magnitude larger vis-à-vis curvature driven motion.« less

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

DOE PAGES

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

2016-08-09

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

Microstructure and critical strain of dynamic recrystallization of 6082 aluminum alloy in thermal deformation

NASA Astrophysics Data System (ADS)

Ren, W. W.; Xu, C. G.; Chen, X. L.; Qin, S. X.

2018-05-01

Using high temperature compression experiments, true stress true strain curve of 6082 aluminium alloy were obtained at the temperature 460°C-560°C and the strain rate 0.01 s-1-10 s-1. The effects of deformation temperature and strain rate on the microstructure are investigated; (‑∂lnθ/∂ε) ‑ ε curves are plotted based on σ-ε curve. Critical strains of dynamic recrystallization of 6082 aluminium alloy model were obtained. The results showed lower strain rates were beneficial to increase the volume fraction of recrystallization, the average recrystallized grain size was coarse; High strain rates are beneficial to refine average grain size, the volume fraction of dynamic recrystallized grain is less than that by using low strain rates. High temperature reduced the dislocation density and provided less driving force for recrystallization so that coarse grains remained. Dynamic recrystallization critical strain model and thermal experiment results can effectively predict recrystallization critical point of 6082 aluminium alloy during thermal deformation.

Product Design and Production Practice of 700MPa High Strength Hot Rolled Strip for Auto Axle Tube

NASA Astrophysics Data System (ADS)

Hui, Pan; Zhao-dong, Wang; Ya-jun, Hui; Yang, Cui; Xiang-tao, Deng; Chun-lin, Bao

According to the technical specifications of 700MPa high strength automotive axle tube steel, a low cost of 0.07%C+1.5%Mn+0.05%Nb+0.10%Ti was designed. The high strength mainly relies on grain refinement strengthening and precipitation strengthening. The recrystallization, precipitation, and CCT curves of the 700MPa grade axle tube steel were studied in order to determine a reasonable TMCP process. By controlling the low level segregation band, low level of C and N content, 700MPa grade high strength automotive axle tube steel is successfully developed with excellent mechanical property, welding property, flattening and flaring property, torsion fatigue property, static torsional property and surface quality.

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.

BHQ revisited (1) - Looking at grain size

NASA Astrophysics Data System (ADS)

Heilbronner, Renée; Kilian, Rüdiger; Tullis, Jan

2016-04-01

Black Hills Quartzite (BHQ) has been used extensively in experimental rock deformation for numerous studies. Coaxial and general shear experiments have been carried out, for example, to define the dislocation creep regimes of quartz (Hirth & Tullis, 1992), to determine the effect of annealing (Heilbronner & Tullis, 2002) or to study the development of texture and microstructure with strain (Heilbronner & Tullis, 2006). BHQ was also used to determine the widely used quartz piezometer by Stipp & Tullis (2003). Among the microstructure analyses that were performed in those original papers, grain size was usually determined using CIP misorientation images. However, the CIP method (= computer-integrated polarization microscopy, details in Heilbronner and Barrett, 2014) is only capable of detecting the c-axis orientation of optically uniaxial materials and hence is only capable of detecting grain boundaries between grains that differ in c-axis orientation. One of the puzzling results we found (Heilbronner & Tullis, 2006) was that the recrystallized grain size seemed to depend on the crystallographic preferred orientation of the domain. In other words the grain size did not only depend on the flow stress but also on the orientation of the c-axis w/r to the shear direction. At the time, no EBSD analysis (electron back scatter diffraction) was carried out and hence the full crystallographic orientation was not known. In principle it is therefore possible that we missed some grain boundaries (between grains with parallel c-axes) and miscalculated our grain sizes. In the context of recent shear experiments on quartz gouge at the brittle-viscous transition (see Richter et al., this conference), where EBSD is used to measure the recrystallized grain size, we wanted to re-measure the CIP grain sizes of our 2006 samples (deformed in regime 1, 2 and 3 of dislocation) in exactly the same way. In two companion posters we use EBSD orientation imaging to repeat, refine and expand the microstructure and texture analysis of Heilbronner & Tullis (2006). Here, in poster (1), we focus on the recrystallized grain size with the aim of (a) comparing CIP- and EBSD derived grain size measurements, (b) of comparing the recrystallized grain size of coaxially deformed and sheared BHQ and (c) in order to confirm that the quartz piezometer indeed depends on texture, and (d) to test if it also depends on the type of deformation (irrotational versus rotational deformation). References cited: Heilbronner, R., and S.D. Barrett (2014) Image Analysis in Earth Sciences, Springer. Heilbronner, R., and J. Tullis (2002), The effect of static annealing on micro- structure and crystallographic preferred orientations of quartzites experimentally deformed in axial compression and shear, Geol. Soc. Spec. Publ., 200, 191 - 218. Heilbronner, R., and J. Tullis (2006), Evolution of c axis pole figures and grain size during dynamic recrystallization: Results from experimentally sheared quartzite. JGR, 111, B10202, doi:10.1029/2005JB004194, 2006 Hirth, G., and J. Tullis (1992), Dislocation creep regimes in quartz aggregates, JSG, 14, 145-159. Stipp, M., and J. Tullis (2003), The recrystallized grain size piezometer for quartz, Geophys. Res. Lett., 30(21), 2088, doi:10.1029/2003GL018444.

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.

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

PubMed

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

2012-12-01

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

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

PubMed Central

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

2017-01-01

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

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

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

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

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

PubMed

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

2013-12-01

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

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.

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.

Grain Growth and Precipitation Behavior of Iridium Alloy DOP-26 During Long Term Aging

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

Pierce, Dean T.; Muralidharan, Govindarajan; Fox, Ethan E.

The influence of long term aging on grain growth and precipitate sizes and spatial distribution in iridium alloy DOP-26 was studied. Samples of DOP-26 were fabricated using the new process, recrystallized for 1 hour (h) at 1375 C, then aged at either 1300, 1400, or 1500 C for times ranging from 50 to 10,000 h. Grain size measurements (vertical and horizontal mean linear intercept and horizontal and vertical projection) and analyses of iridium-thorium precipitates (size and spacing) were made on the longitudinal, transverse, and rolling surfaces of the as-recrystallized and aged specimens from which the two-dimensional spatial distribution and meanmore » sizes of the precipitates were obtained. The results obtained from this study are intended to provide input to grain growth models.« less

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.

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

PHYSICO-CHEMICAL CHARACTERISATION OF DIFFERENT CLINDAMYCIN PHOSPHATE SAMPLES

PubMed Central

Vranić, Edina; Planinšek, Odon; Tivadar, Andrijana; Hadžović, Sabira; Srčič, Stanko

2007-01-01

For the majority of the pharmaceutical dosage forms, the substances that are used maintain solid state under the standard storage conditions, i.e. powders. The interactions of pharmaceutical powders (active ingredient(s) and excipients) with liquids and vapors (particularly aqueous solutions and their vapors) occur almost always during the production process. From the physical point of view, the interactions among individual components may differ from the expected because chemically identical substances obtained from different producers vary very much. These differences influence either the production process and/or the pharmaceutical form properties. In order to overcome these problems it is necessary to establish a control over the physico-chemical properties of the used materials. The aim of this work was to determine physico-chemical properties of three powder clindamycin phosphate samples (labeled as sample S1, S2 and S3) acquired through different suppliers. All the analysis were made for the purpose of establishing possible differences among the tested samples that showed variable physical stability in the solution: recrystallization of the S3 sample in the aqueous solution has been established during storage under standard conditions. On the basis of the obtained data it was possible to recognize the differences among the tested clindamycin phosphate samples and to explain the anomalous behavior of one sample. The surface free energy components for the investigated clindamycin phosphate samples were determined using Wu and Goodvan Oss method. The investigated clindamycin phosphate samples exhibit certain differences in surface free energy values as well as in surface morphology and thermal behavior. Comparison of γ+ and γ- values leads to the conclusion that all three clindamycin phosphate samples perform as monopolar, more electron acceptors, i.e. Lewis acids. However, an important difference exists between samples S1 and S2 on one and S3 on the other side. Sample S3 exhibits stronger acidic behavior, what could be connected with its recrystallization during the storage. The samples S1, S2 and S3 have different melting points e.g. “onset” temperatures. When the melting points move towards 200oC, the width of the “onset” temperature peak is especially important. In the case of wider peak, the potential for recrystallization seems to be higher. According to the stated, the sample S1 would be the “sample of choice” for the formulation of the stable pharmaceutical dosage form and has not shown any recrystallization tendencies during the storage period.

High-Temperature Tensile Behaviors of Base Metal and Electron Beam-Welded Joints of Ni-20Cr-9Mo-4Nb Superalloy

NASA Astrophysics Data System (ADS)

Gupta, R. K.; Anil Kumar, V.; Sukumaran, Arjun; Kumar, Vinod

2018-05-01

Electron beam welding of Ni-20Cr-9Mo-4Nb alloy sheets was carried out, and high-temperature tensile behaviors of base metal and weldments were studied. Tensile properties were evaluated at ambient temperature, at elevated temperatures of 625 °C to 1025 °C, and at strain rates of 0.1 to 0.001 s-1. Microstructure of the weld consisted of columnar dendritic structure and revealed epitaxial mode of solidification. Weld efficiency of 90 pct in terms of strength (UTS) was observed at ambient temperature and up to an elevated temperature of 850 °C. Reduction in strength continued with further increase of test temperature (up to 1025 °C); however, a significant improvement in pct elongation is found up to 775 °C, which was sustained even at higher test temperatures. The tensile behaviors of base metal and weldments were similar at the elevated temperatures at the respective strain rates. Strain hardening exponent `n' of the base metal and weldment was 0.519. Activation energy `Q' of base metal and EB weldments were 420 to 535 kJ mol-1 determined through isothermal tensile tests and 625 to 662 kJ mol-1 through jump-temperature tensile tests. Strain rate sensitivity `m' was low (< 0.119) for the base metal and (< 0.164) for the weldment. The δ phase was revealed in specimens annealed at 700 °C, whereas, twins and fully recrystallized grains were observed in specimens annealed at 1025 °C. Low-angle misorientation and strain localization in the welds and the HAZ during tensile testing at higher temperature and strain rates indicates subgrain formation and recrystallization. Higher elongation in the weldment (at Test temperature > 775 °C) is attributed to the presence of recrystallized grains. Up to 700 °C, the deformation is through slip, where strain hardening is predominant and effect of strain rate is minimal. Between 775 °C to 850 °C, strain hardening is counterbalanced by flow softening, where cavitation limits the deformation (predominantly at lower strain rate). Above 925 °C, flow softening is predominant resulting in a significant reduction in strength. Presence of precipitates/accumulated strain at high strain rate results in high strength, but when the precipitates were coarsened at lower strain rates or precipitates were dissolved at a higher temperature, the result was a reduction in strength. Further, the accumulated strain assisted in recrystallization, which also resulted in a reduction in strength.

Physico-chemical characterisation of different clindamycin phosphate samples.

PubMed

Vranić, Edina; Planinsek, Odon; Tivadar, Andrijana; Hadzović, Sabira; Srcic, Stanko

2007-05-01

For the majority of the pharmaceutical dosage forms, the substances that are used maintain solid state under the standard storage conditions, i.e. powders. The interactions of pharmaceutical powders (active ingredient(s) and excipients) with liquids and vapors (particularly aqueous solutions and their vapors) occur almost always during the production process. From the physical point of view, the interactions among individual components may differ from the expected because chemically identical substances obtained from different producers vary very much. These differences influence either the production process and/or the pharmaceutical form properties. In order to overcome these problems it is necessary to establish a control over the physico-chemical properties of the used materials. The aim of this work was to determine physico-chemical properties of three powder clindamycin phosphate samples (labeled as sample S(1), S(2) and S(3)) acquired through different suppliers. All the analysis were made for the purpose of establishing possible differences among the tested samples that showed variable physical stability in the solution: recrystallization of the S(3) sample in the aqueous solution has been established during storage under standard conditions. On the basis of the obtained data it was possible to recognize the differences among the tested clindamycin phosphate samples and to explain the anomalous behavior of one sample. The surface free energy components for the investigated clindamycin phosphate samples were determined using Wu and Good- van Oss method. The investigated clindamycin phosphate samples exhibit certain differences in surface free energy values as well as in surface morphology and thermal behavior. Comparison of alpha + and alpha - values leads to the conclusion that all three clindamycin phosphate samples perform as monopolar, more electron acceptors, i.e. Lewis acids. However, an important difference exists between samples S(1) and S(2) on one and S(3) on the other side. Sample S(3) exhibits stronger acidic behavior, what could be connected with its recrystallization during the storage. The samples S(1), S(2) and S(3) have different melting points e.g. "onset" temperatures. When the melting points move towards 200 (o ) C, the width of the "onset" temperature peak is especially important. In the case of wider peak, the potential for recrystallization seems to be higher. According to the stated, the sample S1 would be the "sample of choice" for the formulation of the stable pharmaceutical dosage form and has not shown any recrystallization tendencies during the storage period.

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

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

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

Hot 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.

Solid state properties and drug release behavior of co-amorphous indomethacin-arginine tablets coated with Kollicoat® Protect.

PubMed

Petry, Ina; Löbmann, Korbinian; Grohganz, Holger; Rades, Thomas; Leopold, Claudia S

2017-10-01

A promising approach to improve the solubility of poorly water-soluble drugs and to overcome the stability issues related to the plain amorphous form of the drugs, is the formulation of drugs as co-amorphous systems. Although polymer coatings have been proven very useful with regard to tablet stability and modifying drug release, there is little known on coating co-amorphous formulations. Hence, the aim of the present study was to investigate whether polymer coating of co-amorphous formulations is possible without inducing recrystallization. Tablets containing either a physical mixture of crystalline indomethacin and arginine or co-amorphous indomethacin-arginine were coated with a water soluble polyvinyl alcohol-polyethylene glycol graft copolymer (Kollicoat® Protect) and stored at 23°C/0% RH and 23°C/75% RH. The solid state properties of the coated tablets were analyzed by XRPD and FTIR and the drug release behavior was tested for up to 4h in phosphate buffer pH 4.5. The results showed that the co-amorphous formulation did not recrystallize during the coating process or during storage at both storage conditions for up to three months, which confirmed the high physical stability of this co-amorphous system. Furthermore, the applied coating could partially inhibit recrystallization of indomethacin during drug release testing, as coated tablets reached a higher level of supersaturation compared to the respective uncoated formulations and showed a lower decrease of the dissolved indomethacin concentration upon precipitation. Thus, the applied coating enhanced the AUC of the dissolution curve of the co-amorphous tablets by about 30%. In conclusion, coatings might improve the bioavailability of co-amorphous formulations. Copyright © 2017 Elsevier B.V. All rights reserved.

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.

Static aeroelastic behavior of an adaptive laminated piezoelectric composite wing

NASA Technical Reports Server (NTRS)

Weisshaar, T. A.; Ehlers, S. M.

1990-01-01

The effect of using an adaptive material to modify the static aeroelastic behavior of a uniform wing is examined. The wing structure is idealized as a laminated sandwich structure with piezoelectric layers in the upper and lower skins. A feedback system that senses the wing root loads applies a constant electric field to the piezoelectric actuator. Modification of pure torsional deformaton behavior and pure bending deformation are investigated, as is the case of an anisotropic composite swept wing. The use of piezoelectric actuators to create an adaptive structure is found to alter static aeroelastic behavior in that the proper choice of the feedback gain can increase or decrease the aeroelastic divergence speed. This concept also may be used to actively change the lift effectiveness of a wing. The ability to modify static aeroelastic behavior is limited by physical limitations of the piezoelectric material and the manner in which it is integrated into the parent structure.

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…

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

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

NASA Astrophysics Data System (ADS)

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

2017-05-01

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

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

NASA Astrophysics Data System (ADS)

Rahl, Jeffrey M.; Skemer, Philip

2016-06-01

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

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

PubMed Central

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

2017-01-01

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

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

PubMed

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

2017-05-02

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

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

NASA Astrophysics Data System (ADS)

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

2018-07-01

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

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.

Equipment and Protocols for Quasi-Static and Dynamic Tests of Very-High-Strength Concrete (VHSC) and High-Strength High-Ductility Concrete (HSHDC)

DTIC Science & Technology

2016-08-01

quasi -static mechanical properties, deformation behavior, and damage mechanisms in HSHDC and compare the behavior with VHSC. 2. Develop experimental ...using the experimental setup described in Chapter 6. The quasi -static strain rate was approximately 10-4/s. All panels tested have nominal dimensions...ER D C TR -1 6- 13 Force Protection Basing; TeCD 1a Equipment and Protocols for Quasi -Static and Dynamic Tests of Very-High-Strength

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.

Hot Deformation Behavior and a Two-Stage Constitutive Model of 20Mn5 Solid Steel Ingot during Hot Compression

PubMed Central

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

2018-01-01

20Mn5 steel is widely used in the manufacture of heavy hydro-generator shaft forging due to its strength, toughness, and wear resistance. However, the hot deformation and recrystallization behaviors of 20Mn5 steel compressed under a high temperature were not studied. For this article, hot compression experiments under temperatures of 850–1200 °C and strain rates of 0.01 s−1–1 s−1 were conducted using a Gleeble-1500D thermo-mechanical simulator. Flow stress-strain curves and microstructure after hot compression were obtained. Effects of temperature and strain rate on microstructure are analyzed. Based on the classical stress-dislocation relationship and the kinetics of dynamic recrystallization, a two-stage constitutive model is developed to predict the flow stress of 20Mn5 steel. Comparisons between experimental flow stress and predicted flow stress show that the predicted flow stress values are in good agreement with the experimental flow stress values, which indicates that the proposed constitutive model is reliable and can be used for numerical simulation of hot forging of 20Mn5 solid steel ingot. PMID:29547570

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.

Development of advanced high strength tantalum base alloys. Phase 3: Influence of metallurgical condition on the mechanical properties of ASTAR-811C sheet

NASA Technical Reports Server (NTRS)

Ammon, R. L.; Buckman, R. W., Jr.; Harrod, D. L.

1972-01-01

Metallurgical condition was shown to have a significant effect on the creep properties of ASTAR-811C (Ta-8W-1Re-0.7Hf-0.025C) sheet. Cold worked material exhibited creep rates 30 times higher than solution annealed material and 10 times greater than for recrystallized material. Both grain size and the carbide morphology changes as the final annealing temperature was raised from 3000 F to 3600 F. However, the lowest creep rates were achieved for material which retained the high temperature form of the Ta2C precipitate. Samples with GTA weldments had essentially identical properties as recrystallized base metal. Cooling rates from 3600 F of 5, 50, and 800 F deg/min. had little effect on the 2000 and 2400 F creep behavior of ASTAR-811C.

1D Self-Assembly and Ice Recrystallization Inhibition Activity of Antifreeze Glycopeptide-Functionalized Perylene Bisimides.

PubMed

Adam, Madeleine K; Jarrett-Wilkins, Charles; Beards, Michael; Staykov, Emiliyan; MacFarlane, Liam R; Bell, Toby D M; Matthews, Jacqueline M; Manners, Ian; Faul, Charl F J; Moens, Pierre D J; Ben, Robert N; Wilkinson, Brendan L

2018-06-04

Antifreeze glycoproteins (AFGPs) are polymeric natural products that have drawn considerable interest in diverse research fields owing to their potent ice recrystallization inhibition (IRI) activity. Self-assembled materials have emerged as a promising class of biomimetic ice growth inhibitor, yet the development of AFGP-based supramolecular materials that emulate the aggregative behavior of AFGPs have not yet been reported. This work reports the first example of the 1D self-assembly and IRI activity of AFGP-functionalized perylene bisimides (AFGP-PBIs). Glycopeptide-functionalized PBIs underwent 1D self-assembly in water and showed modest IRI activity, which could be tuned through substitution of the PBI core. This work presents essential proof-of-principle for the development of novel IRIs as potential supramolecular cryoprotectants and glycoprotein mimics. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

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)

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

NASA Astrophysics Data System (ADS)

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

2014-05-01

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

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

NASA Astrophysics Data System (ADS)

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

2018-04-01

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

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

NASA Astrophysics Data System (ADS)

Hayakawa, Yasuyuki

2017-12-01

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

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

PubMed Central

Hayakawa, Yasuyuki

2017-01-01

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

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

PubMed Central

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

2017-01-01

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

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.

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

NASA Astrophysics Data System (ADS)

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

2017-09-01

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

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

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

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

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

Dynamic and static fatigue behavior of sintered silicon nitrides

NASA Technical Reports Server (NTRS)

Chang, J.; Khandelwal, P.; Heitman, P. W.

1987-01-01

The dynamic and static fatigue behavior of Kyocera SN220M sintered silicon nitride at 1000 C was studied. Fractographic analysis of the material failing in dynamic fatigue revealed the presence of slow crack growth (SCG) at stressing rates below 41 MPa/min. Under conditions of static fatigue this material also displayed SCG at stresses below 345 MPa. SCG appears to be controlled by microcracking of the grain boundaries. The crack velocity exponent (n) determined from both dynamic and static fatigue tests ranged from 11 to 16.

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.

Dynamic recrystallization in friction surfaced austenitic stainless steel coatings

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

Puli, Ramesh, E-mail: rameshpuli2000@gmail.com; Janaki Ram, G.D.

2012-12-15

Friction surfacing involves complex thermo-mechanical phenomena. In this study, the nature of dynamic recrystallization in friction surfaced austenitic stainless steel AISI 316L coatings was investigated using electron backscattered diffraction and transmission electron microscopy. The results show that the alloy 316L undergoes discontinuous dynamic recrystallization under conditions of moderate Zener-Hollomon parameter during friction surfacing. - Highlights: Black-Right-Pointing-Pointer Dynamic recrystallization in alloy 316L friction surfaced coatings is examined. Black-Right-Pointing-Pointer Friction surfacing leads to discontinuous dynamic recrystallization in alloy 316L. Black-Right-Pointing-Pointer Strain rates in friction surfacing exceed 400 s{sup -1}. Black-Right-Pointing-Pointer Estimated grain size matches well with experimental observations in 316L coatings.

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.

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.

Deformation behavior of welded steel sandwich panels under quasi-static loading

DOT National Transportation Integrated Search

2011-03-01

This report describes engineering studies that were conducted to examine the deformation behavior of flat, welded steel sandwich panels under two quasi-static loading conditions: (1) uniaxial compression; and (2) bending with an indenter. Testing and...

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.

Antifreeze (glyco)protein mimetic behavior of poly(vinyl alcohol): detailed structure ice recrystallization inhibition activity study.

PubMed

Congdon, Thomas; Notman, Rebecca; Gibson, Matthew I

2013-05-13

This manuscript reports a detailed study on the ability of poly(vinyl alcohol) to act as a biomimetic surrogate for antifreeze(glyco)proteins, with a focus on the specific property of ice-recrystallization inhibition (IRI). Despite over 40 years of study, the underlying mechanisms that govern the action of biological antifreezes are still poorly understood, which is in part due to their limited availability and challenging synthesis. Poly(vinyl alcohol) (PVA) has been shown to display remarkable ice recrystallization inhibition activity despite its major structural differences to native antifreeze proteins. Here, controlled radical polymerization is used to synthesize well-defined PVA, which has enabled us to obtain the first quantitative structure-activity relationships, to probe the role of molecular weight and comonomers on IRI activity. Crucially, it was found that IRI activity is "switched on" when the polymer chain length increases from 10 and 20 repeat units. Substitution of the polymer side chains with hydrophilic or hydrophobic units was found to diminish activity. Hydrophobic modifications to the backbone were slightly more tolerated than side chain modifications, which implies an unbroken sequence of hydroxyl units is necessary for activity. These results highlight that, although hydrophobic domains are key components of IRI activity, the random inclusion of addition hydrophobic units does not guarantee an increase in activity and that the actual polymer conformation is important.

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.

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

DTIC Science & Technology

2012-01-01

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

Ultrasonic determination of recrystallization

NASA Technical Reports Server (NTRS)

Generazio, E. R.

1986-01-01

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

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.

Static compression of Ca(OH)2 at room temperature - Observations of amorphization and equation of state measurements to 10.7 GPa

NASA Technical Reports Server (NTRS)

Meade, Charles; Jeanloz, Raymond

1990-01-01

X-ray diffraction measurements are reported for Ca(OH)2 portlandite as it is compressed to 37.6 GPa in the diamond cell at room temperature. Between 10.7 and 15.4 GPa crystalline Ca(OH)2 transforms to a glass, and on decompression the glass recrystallizes between 3.6 and 5.1 GPa. Below pressures of 10.7 GPa the elastic compression of crystalline Ca(OH)2 was measured. A finite strain analysis of these data shows that the isothermal bulk modulus and its pressure derivative are 37.8 + or - 1.8 GPa and 5.2 + or - 0.7 at zero pressure. The change in the unit cell dimensions indicates that the linear incompressibilities of Ca(OH)2 differ by a factor of three.

Deformation behavior of welded steel sandwich panels under quasi-static loading

DOT National Transportation Integrated Search

2011-03-16

This paper summarizes basic research (i.e., testing and analysis) : conducted to examine the deformation behavior of flat-welded : steel sandwich panels under two types of quasi-static loading: : (1) uniaxial compression; and (2) bending through an i...

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.

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.

CNEA/ANL collaboration program to develop an optimized version of DART validation and assessment by means of U{sub 3}Si{sub x} and U{sub 3}O{sub 8-}Al dispersed CNEA miniplate irradiation behavior.

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

Solis, D.

1998-10-16

The DART code is based upon a thermomechanical model that can predict swelling, recrystallization, fuel-meat interdiffusion and other issues related with MTR dispersed FE behavior under irradiation. As a part of a common effort to develop an optimized version of DART, a comparison between DART predictions and CNEA miniplates irradiation experimental data was made. The irradiation took place during 1981-82 for U3O8 miniplates and 1985-86 for U{sub 3}Si{sub x} at Oak Ridge Research Reactor (ORR). The microphotographs were studied by means of IMAWIN 3.0 Image Analysis Code and different fission gas bubbles distributions were obtained. Also it was possible tomore » find and identify different morphologic zones. In both kinds of fuels, different phases were recognized, like particle peripheral zones with evidence of Al-U reaction, internal recrystallized zones and bubbles. A very good agreement between code prediction and irradiation results was found. The few discrepancies are due to local, fabrication and irradiation uncertainties, as the presence of U{sub 3}Si phase in U{sub 3}Si{sub 2} particles and effective burnup.« less

Hot deformation behavior of microstructural constituents in a duplex stainless steel during high-temperature straining

NASA Astrophysics Data System (ADS)

Momeni, Amir; Kazemi, Shahab; Bahrani, Ali

2013-10-01

The hot deformation characteristics of 1.4462 duplex stainless steel (DSS) were analyzed by considering strain partitioning between austenite and ferrite constituents. The individual behavior of ferrite and austenite in microstructure was studied in an iso-stress condition. Hot compression tests were performed at temperatures of 800-1100°C and strain rates of 0.001-1 s-1. The flow stress was modeled by a hyperbolic sine constitutive equation, the corresponding constants and apparent activation energies were determined for the studied alloys. The constitutive equation and law of mixture were used to measure the contribution factor of each phase at any given strain. It is found that the contribution factor of ferrite exponentially declines as the Zener-Hollomon parameter ( Z) increases. On the contrary, the austenite contribution polynomially increases with the increase of Z. At low Z values below 2.6.×1015 (ln Z=35.5), a negative contribution factor is determined for austenite that is attributed to dynamic recrystallization. At high Z values, the contribution factor of austenite is about two orders of magnitude greater than that of ferrite, and therefore, austenite can accommodate more strain. Microstructural characterization via electron back-scattered diffraction (EBSD) confirms the mechanical results and shows that austenite recrystallization is possible only at high temperature and low strain rate.

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.

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

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

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

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

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

DOE PAGES

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

2016-06-27

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

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

NASA Astrophysics Data System (ADS)

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

2016-09-01

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

Correlation buildup during recrystallization in three-dimensional dusty plasma clusters

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

Schella, André; Mulsow, Matthias; Melzer, André

2014-05-15

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

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

PubMed

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

2016-09-01

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

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

NASA Technical Reports Server (NTRS)

Generazio, E. R.

1988-01-01

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

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

PubMed Central

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

2015-01-01

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

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

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

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

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).

The melt-recrystallization behavior of highly oriented α-iPP fibers embedded in a HIPS matrix.

PubMed

Ye, Liwei; Li, Huihui; Qiu, Zhaobin; Yan, Shouke

2015-03-21

The melt-recrystallization behavior of α-iPP fibers embedded in an amorphous HIPS matrix has been studied by means of optical microscopy. The amorphous HIPS serving as a supporter of iPP fibers does not become involved in the nucleation and crystallization process of the molten highly oriented iPP fibers. It also does not provide any birefringence under the optical microscope with crossed polarizers. This enables the study of orientation-induced β-iPP crystallization through a control of the melting status of the fibers. Through melting the fibers at different temperatures above 175 °C and subsequent recrystallization, some β-iPP crystals were always produced. The content of the β-iPP crystal depends strongly on the melting temperature and melting time of the iPP fibers. It was confirmed that melting the iPP fibers at relatively lower temperature, e.g. 176 °C, less amount of β-iPP crystals were observed. The content of β-iPP crystal enhances first with increasing melting temperature and then decreases with further increase of the fiber melting temperature. The β-iPP crystallization is found to be most favorable upon melting the fibers at 178 °C for 2 min. This demonstrates the requirement of a certain chain or chain segment orientation for generating β-iPP crystallization on the one hand, while higher orientation of the iPP chains or chain segments encourages the growth of iPP crystals in the α-form on the other hand. This has been further confirmed by varying the melting time of the fiber at different temperatures, since relaxation of the iPP molecular chains at a fixed temperature is time dependent. Moreover, the complete transformation of α-iPP fibers in some local places into β-iPP crystals implies that the αβ-transition may not be required for the orientation-induced β-iPP crystallization.

Linear Friction Welding of Dissimilar Materials 316L Stainless Steel to Zircaloy-4

NASA Astrophysics Data System (ADS)

Wanjara, P.; Naik, B. S.; Yang, Q.; Cao, X.; Gholipour, J.; Chen, D. L.

2018-02-01

In the nuclear industry, there are a number of applications where the transition of stainless steel to Zircaloy is of technological importance. However, due to the differences in their properties there are considerable challenges associated with developing a joining process that will sufficiently limit the heat input and welding time—so as to minimize the extent of interaction at the joint interface and the resulting formation of intermetallic compounds—but still render a functional metallurgical bond between these two alloys. As such, linear friction welding, a solid-state joining technology, was selected in the present study to assess the feasibility of welding 316L stainless steel to Zircaloy-4. The dissimilar alloy welds were examined to evaluate their microstructural characteristics, microhardness evolution across the joint interface, static tensile properties, and fatigue behavior. Microstructural observations revealed a central intermixed region and, on the Zircaloy-4 side, dynamically recrystallized and thermomechanically affected zones were present. By contrast, deformation on the 316L stainless steel side was limited. In the intermixed region a drastic change in the composition was observed along with a local increase in hardness, which was attributed to the presence of intermetallic compounds, such as FeZr3 and Cr2Zr. The average yield (316 MPa) and ultimate tensile (421 MPa) strengths met the minimum strength properties of Zircaloy-4, but the elongation was relatively low ( 2 pct). The tensile and fatigue fracture of the welds always occurred at the interface in the mode of partial cohesive failure.

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.

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

40Ar/ 39Ar dating of Late Permian evaporites, southeastern New Mexico, USA

NASA Astrophysics Data System (ADS)

Renne, Paul R.; Sharp, Warren D.; Montañez, Isabel P.; Becker, Tim A.; Zierenberg, Robert A.

2001-12-01

40Ar/ 39Ar dating of the potassium-magnesium sulfate mineral langbeinite from Permian evaporites of the Salado formation near Carlsbad, New Mexico, provides quantitative evidence that some salts in these deposits have not recrystallized for 251 Myr since deposition. Survival of Permian salts supports the possibility that Bacillus bacteria recovered from nearby halite was isolated in a closed system and represents a sample of uncontaminated Permian life. Local recrystallization of langbeinite and other nearby minerals is also indicated by the dating, suggesting both the need and the opportunity to document closed system behavior more rigorously. The shoaling and desiccation event recorded by the Salado formation began at least 1 Myr before the Permian-Triassic boundary. Temporal correlation of the Salado with the Zechstein evaporites of north-central Europe supports previously inferred regression models for the origin of these deposits. Significant paleoenvironmental change at the Permian-Triassic boundary thus occurred on a time scale more protracted than that implied by geologically instantaneous events such as bolide impacts.

EXAMINATION OF Zr AND Ti RECOMBINER LOOP SPECIMENS

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

Rittenhouse, P.L.

1958-12-19

Cold-worked specimens of iodide zirconium, Zircaloy-2, iodide titanium, and A-55 titanium were tested in a high-pressure recombiner loop in an attempt to duplicate anomalous results obtained in a prior recombiner loop. Hydrogen analyses and metallographic examinations were made on all specimens. The titanium materials and Zircaloy-2 picked up major amounts of hydrogen in the cell section. None of the materials tested showed appreciable hydrogen absorption in the recombiner section. Complete recrystallization occurred in all cell specimens while only Zircaloy-2, of the recombiner specimens, showed any degree of recrystallization. No explanation for this behavior can be given. A survnnary of themore » data obtained in previous recombiner loops is compared with the results of this loop. Conclusions were based on the results of three recombiner loops. Primarlly because of the hydrogen absorption data obtained in all three recombiner loops it is recommended that the zirconium and titunium materials tested not be used in environments similar to those encountered in high pressure recombiner loops. (auth)« less

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

NASA Astrophysics Data System (ADS)

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

2018-02-01

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

Effect of 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.

Anti-Le-Chatelet behavior driven by strong natural light

NASA Astrophysics Data System (ADS)

Antonyuk, B. P.

2007-01-01

We show that strong incoherent broad band light causes positive feedback in response to a static electric field in random media: electric current flows in opposite to a voltage drop direction; static polarization is induced in opposition to an applied electric field. This type of the electron motion amplifies the external action revealing anti-Le-Chatelet behavior. The applied static electric field is amplified up to the domain of optical damage of a silica glass ≈10 7 V/cm.

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

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

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

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

Investigating Dissolution and Precipitation Phenomena with a Smartphone Microscope

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

Lumetta, Gregg J.; Arcia, Edgar

A novel smartphone microscope can be used to observe the dissolution and crystallization of sodium chloride at a microscopic level. Observation of these seemingly simple phenomena through the microscope at 100× magnification can actually reveal some surprising behavior. These experiments offer the opportunity to discuss some basic concepts such as how the morphological features of the crystals dictates how the dissolution process proceeds, and how materials can be purified by re-crystallization techniques.

Abnormal grain growth in AISI 304L stainless steel

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

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

2014-11-15

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

On the influence of recrystallization on snow fabric and microstructure: study of a snow profile in Central East Antarctica

NASA Astrophysics Data System (ADS)

Calonne, Neige; Schneebeli, Martin; Montagnat, Maurine; Matzl, Margret

2016-04-01

Temperature gradient metamorphism affects the Antarctic snowpack up to 5 meters depth, which lead to a recrystallization of the ice grains by sublimation of ice and deposition of water vapor. By this way, it is well known that the snow microstructure evolves (geometrical changes). Also, a recent study shows an evolution of the snow fabric, based on a cold laboratory experiment. Both fabric and microstructure are required to better understand mechanical behavior and densification of snow, firn and ice, given polar climatology. The fabric of firn and ice has been extensively investigated, but the publications by Stephenson (1967, 1968) are to our knowledge the only ones describing the snow fabric in Antarctica. In this context, our work focuses on snow microstructure and fabric in the first meters depth of the Antarctic ice sheet, where temperature gradients driven recrystallization occurs. Accurate details of the snow microstructure are observed using micro-computed tomography. Snow fabrics were measured at various depths from thin sections of impregnated snow with an Automatic Ice Texture Analyzer (AITA). A definite relationship between microstructure and fabric is found and highlights the influence of metamorphism on both properties. Our results also show that the metamorphism enhances the differences between the snow layers properties. Our work stresses the significant and complex evolution of snow properties in the upper meters of the ice sheet and opens the question of how these layer properties will evolve at depth and may influence the densification.

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.

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

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

NASA Astrophysics Data System (ADS)

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

2018-05-01

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

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

NASA Astrophysics Data System (ADS)

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

2018-07-01

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

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

NASA Astrophysics Data System (ADS)

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

2014-12-01

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

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.

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.

Texture evolution and their effects on the mechanical properties of duplex Mg-Li alloy

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

Zou, Yun; Zhang, Lehao; Wang, Hongtao

Texture evolution is strongly dependent on the deformation mode during thermo-mechanical treatments. In this paper, we report the texture evolution in a duplex Mg-Li alloy. The results provide an evidence of deformation mode transition in the hexagonal-close-packed (hcp) alpha phase with various thickness reductions. The activation sequence of deformation modes is basal slip first, and then pyramidal slip during hot-rolling to a thickness reduction of 40%. The relative activity of slip decreases with further thickness reduction. After annealing, basal texture is strengthened and pyramidal component disappears due to static recrystallization and grain growth. The microstructure, specifically texture evolution in bothmore » hcp alpha and body-centered cubic (bcc) beta phase and their effects on mechanical properties are quantitatively analyzed and assessed. (C) 2016 Elsevier B.V. All rights reserved.« less

Texture evolution and their effects on the mechanical properties of duplex Mg-Li alloy

DOE PAGES

Zou, Yun; Zhang, Lehao; Wang, Hongtao; ...

2016-01-27

Texture evolution is strongly dependent on the deformation mode during thermo-mechanical treatments. In this paper, we report the texture evolution in a duplex Mg-Li alloy. The results provide an evidence of deformation mode transition in the hexagonal-close-packed (hcp) alpha phase with various thickness reductions. The activation sequence of deformation modes is basal slip first, and then pyramidal slip during hot-rolling to a thickness reduction of 40%. The relative activity of slip decreases with further thickness reduction. After annealing, basal texture is strengthened and pyramidal component disappears due to static recrystallization and grain growth. The microstructure, specifically texture evolution in bothmore » hcp alpha and body-centered cubic (bcc) beta phase and their effects on mechanical properties are quantitatively analyzed and assessed. (C) 2016 Elsevier B.V. All rights reserved.« 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.

High-quality Silicon Films Prepared by Zone-melting Recrystallization

NASA Technical Reports Server (NTRS)

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

1984-01-01

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

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

NASA Astrophysics Data System (ADS)

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

2014-04-01

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

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

PubMed

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

2016-09-13

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

Inhibiting ice recrystallization and optimization of cell viability after cryopreservation.

PubMed

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

2012-01-01

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

Incorporation of Eu(III) into Calcite under Recrystallization conditions

PubMed Central

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

2016-01-01

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

Static Strain Aging Behavior of a Manganese-Silicon Steel After Single and Multi-stage Straining

NASA Astrophysics Data System (ADS)

Seraj, P.; Serajzadeh, S.

2016-03-01

In this work, static strain aging behavior of an alloy steel containing high amounts of silicon and manganese was examined while the influences of initial microstructure and pre-strain on the aging kinetics were evaluated as well. The rate of strain aging in a low carbon steel was also determined and compared with that occurred in the alloy steel. The rates of static strain aging in the steels were defined at room temperature and at 95 °C by means of double-hit tensile testing and hardness measurements. In addition, three-stage aging experiments at 80 °C were carried out to estimate aging behavior under multi-pass deformation processing. The results showed that in-solution manganese and silicon atoms could significantly affect the aging behavior of the steel and reduce the kinetics of static strain aging as compared to the low carbon steel. The initial microstructure also played an important role on the aging behavior. The rapidly cooled steel having mean ferrite grain size of 9.7 μm showed the least aging susceptibility index during the aging experiments. Accordingly, the activation energies for static strain aging were calculated as 93.2 and 85.7 kJ/mole for the alloy steel having fine and coarse ferrite-pearlite structures, respectively while it was computed as 79.1 kJ/mole for the low carbon steel with ferrite mean grain size of about 16.2 μm.

Response of Gd 2 Ti 2 O 7 and La 2 Ti 2 O 7 to swift-heavy ion irradiation and annealing

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

Park, Sulgiye; Lang, Maik; Tracy, Cameron L.

2015-07-01

Swift heavy ion (2 GeV 181Ta) irradiation-induced amorphization and temperature-induced recrystallization of cubic pyrochlore Gd2Ti2O7 (Fd3¯m) are compared with the response of a compositionally-similar material with a monoclinic-layered perovskite-type structure, La2Ti2O7 (P21). The averaged electronic energy loss, dE/dx, was 37 keV/nm and 35 keV/nm in Gd2Ti2O7 and La2Ti2O7, respectively. Systematic analysis of the structural modifications was completed using transmission electron microscopy, synchrotron X-ray diffraction, Raman spectroscopy, and small-angle X-ray scattering. Increasing ion-induced amorphization with increasing ion fluence was evident in the X-ray diffraction patterns of both compositions by a reduction in the intensity of the diffraction maxima concurrent with themore » growth in intensity of a broad diffuse scattering halo. Transmission electron microscopy analysis showed complete amorphization within ion tracks (diameter: ~10 nm) for the perovskite-type material; whereas a concentric, core–shell morphology was evident in the ion tracks of the pyrochlore, with an outer shell of disordered yet still crystalline material with the fluorite structure surrounding an amorphous track core (diameter: ~9 nm). The radiation response of both titanate oxides with the same stoichiometry can be understood in terms of differences in their structures and compositions. While the radiation damage susceptibility of pyrochlore A2B2O7 materials decreases as a function of the cation radius ratio rA/rB, the current study correlates this behavior with the stability field of monoclinic structures, where rLa/rTi > rGd/rTi. Isochronal annealing experiments of the irradiated materials showed complete recrystallization of La2Ti2O7 at 775 °C and of Gd2Ti2O7 at 850 °C. The annealing behavior is discussed in terms of enhanced damage recovery in La2Ti2O7, compared to the pyrochlore compounds Gd2Ti2O7. The difference in the recrystallization behavior may be related to structural constraints, i.e., reconstructing a low symmetry versus a high symmetry phase.« less

Effect of upsetting deformation temperature on the formation of the fine-grained cast alloy structure of the Ni-Mn-Ga system

NASA Astrophysics Data System (ADS)

Musabirov, I. I.; Safarov, I. M.; Sharipov, I. Z.; Nagimov, M. I.; Koledov, V. V.; Khovailo, V. V.; Mulyukov, R. R.

2017-08-01

The plastic behavior during deformation by upsetting and its effect on the microstructure in the polycrystalline Ni2.19Fe0.04Mn0.77Ga alloy are studied. The temperatures of martensitic and magnetic phase transformations were determined by the method for analyzing the temperature dependence of the specific magnetization as M F = 320 K, A S = 360 K, and T C = 380 K. Using differential scanning calorimetry, it is shown that the phase transition from the ordered phase L21 to the disordered phase B2 is observed in the alloy during sample heating in the temperature range of 930-1070 K. The melting temperature is 1426 K. An analysis of the load curves constructed for sample deposition at temperatures of 773, 873, and 973 K shows that the behavior of the stress-strain curve at a temperature of 773 K is inherent to cold deformation. The behavior of the dependences for 873 and 973 K is typical of hot deformation. After deforming the alloy, its microstructure is studied using backscattered scanning electron microscopy. Plastic deformation of the alloy at study temperatures results in grain structure fragmentation in the localized deformation region. At all temperatures, a recrystallized grain structure is observed. It is found that the structure is heterogeneously recrystallized after upsetting at 973 K due to the process intensity at such a high temperature. The alloy microstructure after plastic deformation at a temperature of 873 K is most homogeneous in terms of the average grain size.

Structure-Property Relationships of Solid State Additive Manufactured Aluminum Alloy 2219 and Inconel 625

NASA Astrophysics Data System (ADS)

Rivera Almeyda, Oscar G.

In this investigation, the processing-structure-property relations are correlated for solid state additively manufactured (SSAM) Inconel 625 (IN 625) and a SSAM aluminum alloy 2219 (AA2219). This is the first research of these materials processed by a new SSAM method called additive friction stir (AFS). The AFS process results in a refined grain structure by extruding solid rod through a rotating tool generating heat and severe plastic deformation. In the case of the AFS IN625, the IN625 alloy is known for exhibiting oxidation resistance and temperature mechanical stability, including strength and ductility. This study is the first to investigate the beneficial grain refinement and densification produced by AFS in IN625 that results in advantageous mechanical properties (YS, UTS, epsilonf) at both quasi-static and high strain rate. Electron Backscatter Diffraction (EBSD) observed dynamic recrystallization and grain refinement during the layer deposition in the AFS specimens, where the results identified fine equiaxed grain structures formed by dynamic recrystallization (DRX) with even finer grain structures forming at the layer interfaces. The EBSD quantified grains as fine as 0.27 microns in these interface regions while the average grain size was approximately 1 micron. Additionally, this is the first study to report on the strain rate dependence of AFS IN625 through quasi-static (QS) (0.001/s) and high strain rate (HR) (1500/s) tensile experiments using a servo hydraulic frame and a direct tension-Kolsky bar, respectively, which captured both yield and ultimate tensile strengths increasing as strain rate increased. Fractography performed on specimens showed a ductile fracture surface on both QS, and HR. Alternatively, the other AFS material system investigated in this study, AA2219, is mostly used for aerospace applications, specifically for rocket fuel tanks. EBSD was performed in the cross-section of the AA2219, also exhibiting DRX with equiaxed microstructure in the three directions and an average grain size of 2.5 microns. EBSD PFs showed that the material has a strong torsional fiber A texture in the top of the build, and this texture gets weaker in the middle and bottom sections. TEM showed that there are no theta' precipitates in the as-deposited cross-section, therefore no precipitation strengthening should be expected. Strain rate and stress state dependence was study, and in both tension and compression, with an increase in strain rate, the YS increase and the UTS decreased. Ductile fracture surface was observed on specimens tested to failure in both QS and HR. The AFS AA2219 processing-structure-property relations are being studied in this investigation to address the stress-state and strain rate dependence of AFS AA2219 with an internal sate variable (ISV) plasticity-damage model to capture the different yield stress, work hardening and failure strain in the AFS AA2219 for high fidelity modeling of AFS components. The ISV plasticity model successfully captured the material behavior in tension, compression, tension-followed-by-compression and compression-followed-by-tension experiments. Furthermore, the damage parameters of the model were calibrated using the final void density measured from the fracture surfaces.

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.

Strength of Rocks Affected by Deformation Enhanced Grain Growth

NASA Astrophysics Data System (ADS)

Kellermann Slotemaker, A.; de Bresser, H.; Spiers, C.

2005-12-01

One way of looking into the possibility of long-term strength changes in the lithosphere is to study transient effects resulting from modifications of the microstructure of rocks. It is generally accepted that mechanical weakening may occur due to progressive grain size refinement resulting from dynamic recrystallization. A decrease in grain size may induce a switch from creep controlled by grain size insensitive dislocation mechanisms to creep governed by grain size sensitive (GSS) mechanisms involving diffusion and grain boundary sliding processes. This switch forms a well-known scenario to explain localization in the lithosphere. However, fine-grained rocks in localized deformation zones are prone to grain coarsening due to surface energy driven grain boundary migration (SED-GBM). This might harden the rock, affecting its role in localizing strain in the long term. The question has arisen if grain growth by SED-GBM in a rock deforming in the GSS creep field can be significantly affected by strain. The broad aim of this study is to shed more light onto this. We have experimentally investigated the microstructural and strength evolution of fine-grained (~0.6 μm) synthetic forsterite and Fe-bearing olivine aggregates that coarsen in grain size while deforming by GSS creep at elevated pressure (600 MPa) and temperature (850-1000 °C). The materials were prepared by `sol-gel' method and contained 0.3-0.5 wt% water and 5-10 vol% enstatite. We performed i) static heat treatment tests of various time durations involving hot isostatic pressing (HIP), and ii) heat treatment tests starting with HIP and continuing with deformation up to 45% axial strain at strain rates in the range 4x10-7 - 1x10-4 s-1. Microstructures were characterized by analyzing full grain size distributions and textures using SEM/EBSD. In addition to the experiments, we studied microstructural evolution in simple two-dimensional numerical models, combining deformation and SED-GBM by means of the modeling package ELLE. Synthetic olivine samples that were heat treated without straining showed only minor grain growth. Presumably, the second phase (enstatite) and/or porosity remaining in the starting material after densification slowed down or inhibited SED-GBM in the static situation. In contrast, samples heat treated and deformed for time durations similar to those of the static tests demonstrated, at identical temperature, an increase in grain size with increasing strain up to a value twice that of the static counterpart. This grain coarsening was associated with continuous hardening of the material, witnessed by the stress-strain curves. A random lattice preferred orientation combined with a low stress sensitivity (n~2) suggested dominant GSS creep controlled by grain boundary sliding. A dynamic grain growth model involving an increase in the fraction of non-hexagonal grains, related to grain neighbor switching, appears applicable to the observed grain growth that is held responsible for the hardening. The ELLE numerical modeling demonstrated that a combination of SED-GBM and geometrical deformation of a 2D grain aggregate can indeed result in enhanced grain growth compared to static grain growth tests. The fraction of non-hexagonal grains was found to remain more or less constant during static grain growth but increased during deformation. We suggest that the application of the dynamic grain growth model to the long-term microstructural evolution of fine-grained lithospheric shear zones can further improve our understanding of the transient or permanent character of strain localizations and related rheological behavior.

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

Investigation on Static Softening Behaviors of a Low Carbon Steel Under Ferritic Rolling Condition

NASA Astrophysics Data System (ADS)

Dong, Haifeng; Cai, Dayong; Zhao, Zhengzheng; Wang, Zhiyong; Wang, Yuhui; Yang, Qingxiang; Liao, Bo

2010-03-01

The study aims to postulate a theoretical hypothesis for the finishing period of ferritic rolling technique of the low carbon steel. The static softening behavior during multistage hot deformation of a low carbon steel has been studied by double hot compression tests at 700-800 °C and strain rate of 1 s-1 using a Gleeble-3500 simulator. Interrupted deformation is conducted with interpass times varying from 1 to 100 s after achieving a true strain of 0.5 in the first stage. The results indicate that the flow stress value at the second deformation is lower than that at the first one, and the flow stress drops substantially. The static softening effects increase with the increase of deformation temperature, holding temperature, and interpass time. The value of the ferritic static softening activation energy is obtained, and the static softening kinetics is modeled by the Avrami equation.

Experimental studies on the tripping behavior of narrow T-stiffened flat plates subjected to hydrostatic pressure and underwater shock

NASA Technical Reports Server (NTRS)

Budweg, H. L.; Shin, Y. S.

1987-01-01

An experimental investigation was conducted to determine the static and dynamic responses of a specific stiffened flat plate design. The air-backed rectangular flat plates of 6061-T6 aluminum with an externally machined longitudinal narrow-flanged T-stiffener and clamped boundary conditions were subjected to static loading by water hydropump pressure and shock loading from an eight pound TNT charge detonated underwater. The dynamic test plate was instrumented to measure transient strains and free field pressure. The static test plate was instrumented to measure transient strains, plate deflection, and pressure. Emphasis was placed upon forcing static and dynamic stiffener tripping, obtaining relevant strain and pressure data, and studying the associated plate-stiffener behavior.

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

NASA Astrophysics Data System (ADS)

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

2001-06-01

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

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

NASA Astrophysics Data System (ADS)

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

2017-12-01

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

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.

Photoacoustic Imaging.

DTIC Science & Technology

1983-12-01

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

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

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

Peng, Lixia

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

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

NASA Astrophysics Data System (ADS)

Miszczyk, M. M.; Paul, H.

2015-08-01

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

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

NASA Astrophysics Data System (ADS)

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

2018-01-01

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

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.

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.

Encapsulation of Capacitive Micromachined Ultrasonic Transducers Using Viscoelastic Polymer

PubMed Central

Lin, Der-Song; Zhuang, Xuefeng; Wong, Serena H.; Kupnik, Mario; Khuri-Yakub, Butrus Thomas

2010-01-01

The packaging of a medical imaging or therapeutic ultrasound transducer should provide protective insulation while maintaining high performance. For a capacitive micromachined ultrasonic transducer (CMUT), an ideal encapsulation coating would therefore require a limited and predictable change on the static operation point and the dynamic performance, while insulating the high dc and dc actuation voltages from the environment. To fulfill these requirements, viscoelastic materials, such as polydimethylsiloxane (PDMS), were investigated for an encapsulation material. In addition, PDMS, with a glass-transition temperature below room temperature, provides a low Young's modulus that preserves the static behavior; at higher frequencies for ultrasonic operation, this material becomes stiffer and acoustically matches to water. In this paper, we demonstrate the modeling and implementation of the viscoelastic polymer as the encapsulation material. We introduce a finite element model (FEM) that addresses viscoelasticity. This enables us to correctly calculate both the static operation point and the dynamic behavior of the CMUT. CMUTs designed for medical imaging and therapeutic ultrasound were fabricated and encapsulated. Static and dynamic measurements were used to verify the FEM and show excellent agreement. This paper will help in the design process for optimizing the static and the dynamic behavior of viscoelastic-polymer-coated CMUTs. PMID:21170294

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

Tectono-metamorphic evolution and magmatic processes in the thermo-metamorphic aureole of the Monte Capanne pluton (Elba Island, Northern Tyrrhenian Sea, Italy).

NASA Astrophysics Data System (ADS)

Morelli, M.; Pandeli, E.; Principi, G.

2003-04-01

Introduction In this work we present new structural and petrographic data collected in the thermo-metamorphic aureole of Monte Capanne (western Elba Island) and its metamorphic evolution. In the western Elba Island the Monte Capanne monzogranitic body (ca. 7 Ma) and its thermo-metamorphic aureole crop out. At least two different tectonic units can be distinguished: the Punta Le Tombe Unit, weak re-crystallized, and the Punta Nera Unit. In the latter one the re-crystallization is strong and a pre-intrusion tectono-metamorphic framework is evident (Morelli et al., 2002). The latter is mainly constituted by thermo-metamorphosed meta-ophiolites and meta-sedimentary successions previously correlated by Barberi et al. (1969) with the un-metamorphic ones (Complex IV and V of Trevisan, 1950) cropping out in the central-eastern Elba. According to Perrin (1975) and Reutter &Spohn (1982) a pre-intrusion tectono-metamorphic framework was recognized into such rocks. As suggested by Daniel &Jolivet (1995) complex relationships between metamorphic evolution and magmatic events are also recognizable. Geological Data The Punta Nera Unit crops out all around the Monte Capanne magmatic body and the primary contact with the underlying granitoid is somewhere preserved. This unit, strongly re-crystallized and locally crosscut by aplitic and porphyritic dikes, is represented by (Coli &Pandeli, 1997; Morelli, 2000) tectonized meta-serpentinites, meta-gabbros with rodingitic dikes, rare meta-basalts and meta-ophicalcites, meta-cherts, marbles, cherty meta-limestones, phyllites and meta-limestones with rare meta-arenites intercalations. A "pre-magmatic" tectono-metamorphic framework of this unit is well evident only in its meta-sedimentary portion. The meta-sediments are deformed by syn-metamorphic isoclinal folds caractherized by N-S trending axes, west dipping axial planes and easternward vergence. A later folding and flattening event clearly post-dated the above said folds and associated main foliation. Both at the meso- and micro-scale few generations of syn-/inter-kinematic and static thermo-metamorphic blasteses (e.g. biotite, wollastonite, garnet, epidote etc.) are evident. Finally weak local folding and faulting affected the Monte Capanne thermo-metamorphic aureole during the uplift of the cooled pluton. Along the coast of Spartaia (north-eastern side of Monte Capanne) the meta-sedimentary upper portion of the Punta Nera Unit crops out and it is represented by alternating marbles and phyllites with rare meta-arenites. Here, the relationships between tectono-metamorphic and thermo-metamorphic structures, and intrusive magmatic bodies are particularly evident. D_1M_1: is recognizable at the meso-scale only as rare relics of intrafolial isoclinal rootless hinges and locally as a transposed foliation (S1). At the microscope a relic fine-spaced foliation, locally preserved by the following re-crystallization and parallel to the original lithological partitions, is evident. The original mineral associations is often replaced by HT/LP mimetic and syn-kinematic or static blasteses. D_2M_2 is the most evident structural fabric pre-dating the thermo-metamorphic events. It is represented by tight to isoclinal folds with N-S trending axes and easternward vergence. At the microscope the S2 foliation deformed the previously S1 and at the fold hinges a variously penetrative discrete crenulation cleavage (S2) is recognizable. M_3 is the first thermo-metamorphic event. It is associated to the intrusions of the Capo Bianco, San Martino and Portoferraio laccoliths (between ca. 8 and 7.2 Ma, Rocchi et alii, 2002) along pre-existing tectonic and lithological discontinuity. The laccoliths clearly crosscut the tectono-metamorphic fabric of the Punta Nera Unit. At this first magmatic event is associated a HT/LP blastesis of static garnet, wollastonite and epidote. Close to the contact between the magmatic intrusive bodies the country rocks are strongly re-crystallized and the original structure is oblitered. D_3M_4: is linked to the intrusion of the Monte Capanne pluton (6.9 Ma). Because of the flattening of the country rocks a penetrative foliation, sub-parallel to the surface of the plutonic body, developed during its intrusion and the uplift. Fluidal structures and discharge folding also developed. This structures affected both the country rocks and the laccoliths intruded in. At the meso-scale are also evident fractures, filled by calcite, cutting the garnet/wollastonite aggregate and later flattened and-or partially transposed. Late felsic products associated with the Monte Capanne pluton partly are deformed by the flattening and partly cut the flattening structures. The contact between the pluton and the country rocks itself is locally deformed by flattening structures. At the microscope the growth of HT/LP minerals, mimetic on the previous associations, or syn-kinematic or static, is evident. M_5: finally, during the last intrusive event (Orano porphyries, 6.8 Ma) a static thermo-metamorphic blastesis locally occurs post-dating the structures previously described. Only gentle folding, veins and fractures formation, and faulting processes followed the tectono-metamorphic and thermo-metamorphic deformation events. Conclusions The Punta Nera Unit represents another important element to understand the relationships between Alps and Apennines. In fact, the evidences of a pre-granitoid polyphased tectono-metamorphic framework in this metamorphic oceanic unit allow to correlate it to the Schistes Lustrés of the Alpine Corsica (e.g. Inzecca Massif, Duran Delga, 1984) and of the Northern Tyrrhenian area (e.g. the outcrops of oceanic metamorphic units in the Gorgona Island, Giglio Island and eastern Elba Island: Bortolotti et al., 2001; Pandeli et alii, 2001; Rossetti et al., 2001; Orti et al., 2002). References Barberi et al. (1969). F.126. Isola d'Elba. Note Ill. Carta Geol. It., 1:100.000. Ser. Geol. d'It. Bortolotti V. et al. (2001), Ofioliti, 26, 2001. Coli &Pandeli, (2001), Ofioliti, 26, 2001. Daniel &Jolivet, (1995), Bull. Soc. Geol. France, 166(4), 341--354. Durand-Delga M. (1984), Mem. Soc. Geol. It., 28, 285--329. Morelli M. et alii, (2002), Proceedings of Eurogranites 2002, 15th--21th Sept. 2002. Orti et alii, (2002), Ofioliti, 27, 2002. Pandeli et alii, (2001), Ofioliti, 26, 2001. Perrin M. (1975), Boll. Soc. Geol. It., 94, pp.1929--1955. Reutter K.J. and Spohn A., (1982), Ofioliti, 7, 467--478. Rocchi et alii, (2002), in Eurogranites 2002 Field Meeting Guide. 15th--21th Sept. 2002 Rossetti et al., (2001), Ofioliti, 26, 2001. Trevisan L., (1950), Mem. Ist. Geol. Univ. Padova, 16, 2--39.

Effects of static tensile load on the thermal expansion of Gr/PI composite material

NASA Technical Reports Server (NTRS)

Farley, G. L.

1981-01-01

The effect of static tensile load on the thermal expansion of Gr/PI composite material was measured for seven different laminate configurations. A computer program was developed which implements laminate theory in a piecewise linear fashion to predict the coupled nonlinear thermomechanical behavior. Static tensile load significantly affected the thermal expansion characteristics of the laminates tested. This effect is attributed to a fiber instability micromechanical behavior of the constituent materials. Analytical results correlated reasonably well with free thermal expansion tests (no load applied to the specimen). However, correlation was poor for tests with an applied load.

Effect of Cold Rolling and Heat Treatment on Microstructure and Mechanical Properties of Ti-4Al-1Mn Titanium Alloy

NASA Astrophysics Data System (ADS)

Gaur, Rishi; Gupta, R. K.; AnilKumar, V.; Banwait, S. S.

2018-05-01

Mechanical behavior of Ti-4Al-1Mn titanium alloy has been studied in annealed, cold-rolled and heat-treated conditions. Room temperature tensile strength as well as % elongation has been found to be low with increasing amount of cold rolling. Lowering of strength in cold worked condition is attributed to premature failure. However, the same has been mitigated after heat treatment. Significant effect of cooling media (air and water) from heat treatment temperature on microstructure was not found except for the degree of fineness of α plates. Optimum properties (strength as well as ductility) were exhibited by samples subjected to 15% cold rolling and heat treatment below β transus temperature, which can be attributed to presence of recrystallized microstructure. In cold worked condition, the microstructure shows fine fragmented α plates/Widmanstätten morphology with high dislocation density along with a large amount of strain fields and twinning, which gets transformed to recrystallized equiaxed microstructure and with plate-like morphology after near β heat treatment. Prior cold work is found to have a significant effect on mechanical properties supported by evolution of microstructure. Twinning is found to be assisting in deformation as well as in recrystallization through the formation of deformation and annealing twins during cold working and heat treatment. Fracture analysis of the tested sample with prior cold work and heat-treated condition revealed quasi-ductile failure as compared to only ductile failure features seen for samples heat treated without prior cold work.

Solution behavior of PVP-VA and HPMC-AS-based amorphous solid dispersions and their bioavailability implications.

PubMed

Qian, Feng; Wang, Jennifer; Hartley, Ruiling; Tao, Jing; Haddadin, Raja; Mathias, Neil; Hussain, Munir

2012-10-01

To identify the mechanism behind the unexpected bio-performance of two amorphous solid dispersions: BMS-A/PVP-VA and BMS-A/HPMC-AS. Solubility of crystalline BMS-A in PVP-VA and HPMC-AS was measured by DSC. Drug-polymer interaction parameters were obtained by Flory-Huggins model fitting. Drug dissolution kinetics of spray-dried dispersions were studied under sink and non-sink conditions. BMS-A supersaturation was studied in the presence of pre-dissolved PVP-VA and HPMC-AS. Potency and crystallinity of undissolved solid dispersions were determined by HPLC and DSC. Polymer dissolution kinetics were obtained by mass balance calculation. Bioavailability of solid dispersions was assessed in dogs. In solid state, both polymers are miscible with BMS-A, while PVP-VA solublizes the drug better. BMS-A dissolves similarly from both solid dispersions in vitro regardless of dissolution method, while the HPMC-AS dispersion performed much better in vivo. At the same concentration, HPMC-AS is more effective in prolonging BMS-A supersaturation; this effect was negated by the slow dissolution rate of HPMC-AS. Further study revealed that fast PVP-VA dissolution resulted in elevated drug loading in undissolved dispersions and facilitated drug recrystallization before complete release. In contrast, the hydrophobicity and slower HPMC-AS dissolution prevented BMS-A recrystallization within the HPMC-AS matrix for >24 h. The lower bioavailability of PVP-VA dispersion was attributed to BMS-A recrystallization within the undissolved dispersion, due to hydrophilicity and fast PVP-VA dissolution rate. Polymer selection for solid dispersion development has significant impact on in vivo performance besides physical stability.

Influence of poly(L-lysine) on the structure of dipalmitoylphosphatidylglycerol/water dispersions studied by X-ray scattering.

PubMed

Förster, G; Schwieger, C; Faber, F; Weber, T; Blume, A

2007-04-01

The interaction between the negatively charged phospholipid DPPG and positively charged poly(L: -lysine) (PLL) of different lengths was studied by X-ray scattering in the SAXS and WAXS region. As a reference pure DPPG (Na salt) was investigated over a wide temperature range (-30 to 70 degrees C). The phase behavior of DPPG in aqueous and in buffer/salt dispersions showed a metastable subgel phase at low temperatures and a recrystallization upon heating before reaching the liquid-crystalline phase. The presence of additional salt stabilizes the bilayer structure and decreases the recrystallization temperature. Large changes in the SAXS region are not connected with changes in chain packing. In DPPG/PLL samples, the PLL is inserted between adjacent headgroup layers and liberates counterions which give rise to a freezing point depression. In the complex with DPPG PLL form an alpha-helical secondary structure at pH 7 and temperatures below the gel to liquid-crystalline phase transition. This prevents DPPG from recrystallization and strongly increases the stacking order. The lamellar repeat distance is decreased and fixed by the helix conformation of PLL in the gel phase. PLL with n = 14 is too short to form helices and is squeezed out reversibly from the interbilayer space upon cooling by freezing of trapped water. In dispersions with longer PLLs (n > 400) at -20 degrees C a 1D crystallization of PLL alpha-helices in the aqueous layer between the headgroups takes place. A structural model is presented for the lateral periodic complex, which is similar to the known cationic lipid/DNA complex.

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.

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.

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.

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.

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.

Deformation Enhanced Recrystallization of Titanite: Insight from the Western Gneiss Region Ultrahigh-Pressure Terrane

NASA Astrophysics Data System (ADS)

Gordon, S. M.; Reddy, S. M.; Blatchford, H.; Whitney, D. L.; Kirkland, C. L.; Teyssier, C.; Evans, N. J.; McDonald, B.

2017-12-01

Titanite readily recrystallizes due to metamorphism, deformation, and/or fluids making it an ideal chronometer for tracking the exhumation of high-grade rocks. The Western Gneiss Region (WGR), Norway, is a giant UHP terrane exhumed as a fairly coherent slab. Parts of the WGR underwent little deformation during exhumation; however, meters-scale shear zones, located across the WGR, deformed over a range of pressures, from (U)HP to amphibolite facies. Titanite from quartzofeldpathic gneiss within, directly adjacent to, and 300 m away from a mylonitic shear zone within the southern WGR have been analyzed to track exhumation and investigate effects of deformation on recrystallization and trace-element mobility. EBSD was used to characterize the microstructural evolution of the gneisses, and trace-element concentrations and timing of recrystallization were estimated by split-stream LA-ICPMS. Titanite grain size decreases from outside (>200) to inside (<75 µm) the shear zone. Gneiss in and directly adjacent to the shear zone contain partially to completely recrystallized grains, with 207-corrected 206Pb/238U ages of <405 Ma. Gneiss within the shear zone shows a greater percentage of recrystallized grains. EBSD data indicate that some titanite comprises multiple subgrains within an optically coherent single grain. Subgrains in titanite cores show evidence of inherited radiogenic Pb, whereas subgrains in rims and tails of deformed sigma grains were recrystallized. In a gneiss directly adjacent to the shear zone, optically coherent grains are zoned, with increasing Sr and decreasing Zr from core to rim; titanite subgrains within the shear-zone gneiss are too small to analyze. In comparison, titanite from the gneiss outside the shear zone does not show any internal microstructures or evidence for Scandian recrystallization and has low U and high 204Pb. These results show that most trace elements are unaffected by deformation of titanite; however, Pb is mobile. Deformation thus plays an important role in resetting U-Pb systematics and allows the timing of shear zone development to be linked to the early stages of eclogite exhumation at ca. 405 Ma. Atom-probe analyses of adjacent subgrains, one that has recrystallized and one with an inherited age, will provide insight into trace-element mobility on the nm-scale.

[Comporison Sduty of Microstructure by Metallographicalk on the Polarized Light and Texture by XRD of CC 5083 and CC 5182 Aluminium Alloy after Cold Rolling and Recrystallization].

PubMed

Chen, Ming-biao; Li, Yong-wei; Tan, Yuan-biao; Ma, Min; Wang, Xue-min; Liu, Wen-chang

2015-03-01

At present the study of relation between microstructure, texture and performance of CC 5083 aluminium alloy after cold tolling and recrystallization processes is still finitude. So that the use of the CC 5083 aluminium alloy be influenced. Be cased into electrical furnace, hot up with unlimited speed followed the furnace hot up to different temperature and annealed 2h respectively, and be cased into salt-beth furnace, hot up quickly to different temperature and annealed 30 min respectively for CC 5083 and CC 5182 aluminum alloy after cold roling with 91.5% reduction. The microstructure be watched use metallographic microscope, the texture be inspected by XRD. The start temperature of recrystallization and grain grow up temperature within annealing in the electric furnace of CC 5083 aluminum alloy board is 343 degrees C, and the shap of grain after grow up with long strip (the innovation point ); The start temperature of recrystallization within annealling in the salt bath furnace of CC 5083 is 343 degrees C. The start temperature and end temperature of recrystallization within annealling of CC 5083 and CC 5182 aluminum alloy is 371 degrees C. The grain grow up outstanding of cold rooled CC 5152 aluminum alloy after annealed with 454 degrees C in the electric furnace and salt bath furnace. The start temperature of grain grow up of CC 5083 alluminurn alloy annealed in the electric furnace and salt bath furnace respectively is higher than the start temperature of grain grow up of CC 5182 alluminum alloy annealed in the electric furnace and salt bath furnace respectively. The strat temperature of recrystallization grain grow up is higher than which annealled with other three manner annealing process. The recrystallization temperature of CC 5182 annealed in the salt bath furnace is higher than which annealed in the electric furnace. The recrystallization temperature of the surface layer of CC 5083 and CC 5182 aluminum alloy is higher than the inner layer (the innovation point). There is a difference each other of the structure and the texture of the four manner annealing aluminum alloy (the innovation point). There is a little difference at the recrystallization processes course reflectived by the observe results of structure transform and by the examination results of texture transmission.

Deformation Enhanced Recrystallization of Titanite: Insight from the Western Gneiss Region Ultrahigh-Pressure Terrane

NASA Astrophysics Data System (ADS)

Gordon, S. M.; Reddy, S. M.; Blatchford, H.; Whitney, D. L.; Kirkland, C. L.; Teyssier, C.; Evans, N. J.; McDonald, B.

2016-12-01

Titanite readily recrystallizes due to metamorphism, deformation, and/or fluids making it an ideal chronometer for tracking the exhumation of high-grade rocks. The Western Gneiss Region (WGR), Norway, is a giant UHP terrane exhumed as a fairly coherent slab. Parts of the WGR underwent little deformation during exhumation; however, meters-scale shear zones, located across the WGR, deformed over a range of pressures, from (U)HP to amphibolite facies. Titanite from quartzofeldpathic gneiss within, directly adjacent to, and 300 m away from a mylonitic shear zone within the southern WGR have been analyzed to track exhumation and investigate effects of deformation on recrystallization and trace-element mobility. EBSD was used to characterize the microstructural evolution of the gneisses, and trace-element concentrations and timing of recrystallization were estimated by split-stream LA-ICPMS. Titanite grain size decreases from outside (>200) to inside (<75 µm) the shear zone. Gneiss in and directly adjacent to the shear zone contain partially to completely recrystallized grains, with 207-corrected 206Pb/238U ages of <405 Ma. Gneiss within the shear zone shows a greater percentage of recrystallized grains. EBSD data indicate that some titanite comprises multiple subgrains within an optically coherent single grain. Subgrains in titanite cores show evidence of inherited radiogenic Pb, whereas subgrains in rims and tails of deformed sigma grains were recrystallized. In a gneiss directly adjacent to the shear zone, optically coherent grains are zoned, with increasing Sr and decreasing Zr from core to rim; titanite subgrains within the shear-zone gneiss are too small to analyze. In comparison, titanite from the gneiss outside the shear zone does not show any internal microstructures or evidence for Scandian recrystallization and has low U and high 204Pb. These results show that most trace elements are unaffected by deformation of titanite; however, Pb is mobile. Deformation thus plays an important role in resetting U-Pb systematics and allows the timing of shear zone development to be linked to the early stages of eclogite exhumation at ca. 405 Ma. Atom-probe analyses of adjacent subgrains, one that has recrystallized and one with an inherited age, will provide insight into trace-element mobility on the nm-scale.

Thermodynamics of radiation induced amorphization and thermal annealing of Dy 2Sn 2O 7 pyrochlore

DOE PAGES

Chung, Cheng-Kai; Lang, Maik; Xu, Hongwu; ...

2018-06-14

Thermodynamics and annealing behavior of swift heavy ion amorphized Dy 2Sn 2O 7 pyrochlore were studied. Its amorphization enthalpy, defined as the total energetic difference between the irradiation amorphized and undamaged Dy 2Sn 2O 7 states, was determined to be 283.6 ± 6.5 kJ/mol by high temperature oxide melt drop solution calorimetry. It has been an enigma that stannate and some other pyrochlores do not follow the general r A/r B-radiation resistance relation seen in most pyrochlore systems. In this paper, we use the amorphization enthalpy, which reflects all the complex chemical and structural characteristics, as a more effective parametermore » to correlate the radiation damage resistance of pyrochlores with their compositions. It successfully explains the superior radiation damage resistance of the stannate pyrochlores compared with titanate pyrochlores. Differential scanning calorimetry (DSC) reveals a strong exothermic event starting at 978 K, which is attributed to long-range recrystallization based on X-ray diffraction (XRD) analysis, similar to the effect previously observed in Dy 2Ti 2O 7. A second pronounced heat event beginning at ~1148 K, which results from local structural rearrangement, is clearly decoupled from the first event for irradiated Dy 2Sn 2O 7. Both the heat releases measured by DSC on heating to 1023 and 1473 K, and the excess enthalpies of the annealed samples indicate that the recovery to the original, ordered state was not fully achieved up to even 1473 K, despite XRD showing the apparent restoration of crystalline pyrochlore structure. The remaining metastability may be attributed to local disorder in the form of weberite-like short-range domains in the recrystallized material. Intriguingly, the second event for different pyrochlores generally starts at similar temperatures while the onset of the long range recrystallization is compositionally dependent. Finally, the amorphization and thermal annealing behavior observed in irradiated Dy 2Sn 2O 7 may provide insights into the general mechanisms of radiation damage and recovery of pyrochlores relevant to their nuclear applications.« less

The Influence of Grain Boundary Fluids on the Recrystallization Behavior in Calcite: A Comparison of "dry" and "wet" Marble Mylonites

NASA Astrophysics Data System (ADS)

Schenk, O.; Urai, J.; Evans, B.

2003-12-01

Carbonate rocks are able to accumulate large amounts of strain and deform crystal-plastically even at low p-T conditions and thus, marble sequences are often the site of strain localization in the upper crust during late-stage deformation in mountain building processes. 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, as fluids play a major role in the flow behavior of many rock materials during deformation (e.g. quartz, olivine, halite, feldspar). We compared calcite marble mylonites from two geological settings: (a) Schneeberg Complex, Southern Tyrole, Italy and (b) Naxos Metamorphic Core Complex, Greece. The shear zones of the selected areas are suitable for comparison, because they consist of similar lithology and the marble mylonites resemble each other in chemical composition. In addition, calcite-dolomite solvus geothermometry and TEM observations indicate similar p-T conditions for the shear zones formation. However, the two settings are different in the availability of fluids during the shear zone evolution: In the Schneeberg mylonites, both the alteration of minerals during retrograde metamorphism of neighboring micaschists and the existence of veins suggest that fluids were present during mylonitization. The absence of these features in the Naxos samples indicates that fluids were not present during deformation of these mylonites. This difference is also supported by the signature of stable isotopes. Microstructural investigations using optical and scanning electron microscopes on broken and planar surfaces did not indicate major differences between wet and dry mylonites: Grain boundaries of both types of samples display pores with shapes controlled by crystallography, and 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. With the exception of the intracrystalline shear zones, there were no obvious microstructural signatures that were obvious indicators of the presence of fluids, at least for these two field examples.

Recrystallization and grain growth phenomena in a particle-reinforced aluminum composite

NASA Astrophysics Data System (ADS)

van Aken, D. C.; Krajewski, P. E.; Vyletel, G. M.; Allison, J. E.; Jones, J. W.

1995-06-01

Recrystallization and grain growth in a 2219/TiC/15p composite were investigated as functions of the amount of deformation and deformation temperature. Both cold and hot deformed samples were annealed at the normal solution treatment temperature of 535 °C. It was shown that large recrystallized grain diameters, relative to the interparticle spacing, could be produced in a narrow range of deformation for samples cold-worked and those hot-worked below 450 °C. For cold-worked samples, between 4 to 6 pct deformation, the recrystallized grain diameters varied from 530 to 66 μm as the amount of deformation increased. Subsequent grain growth was not observed in these recrystallized materials and noncompact grain shapes were observed. For deformations greater than 15 pct, recrystallized grain diameters less than the interparticle spacing were observed and subsequent grain growth produced a pinned grain diameter of 27 μm. The pinned grain diameter agreed well with an empirical model based on three dimensional (3-D) Monte Carlo simulations of grain growth and particle pinning in a two-phase material. Tensile properties were determined as a function of grain size, and it was shown that grain size had a weak influence on yield strength. A maximum in the yield strength was observed at a grain size larger than the normal grain growth and particle-pinned diameter.

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.

[Investigation of the recrystallization of trehalose as a good glass-former excipient].

PubMed

Katona, Gábor; Orsolya, Jójártné Laczkovich; Szabóné, Révész Piroska

2014-01-01

An amorphous form of trehalose is easy to prepare by using a solvent method. The recrystallization kinetics can be followed well, which is important because of the occurrence of polymorphic forms of trehalose. This is especially significant in the case of dry powder inhalers. Spray-drying was used as a preparation method this being one of the most efficient technologies with which to obtain an amorphous form. This method can result in the required particle size and a monodisperse distribution with excellent flowability and with moreover considerable amorphization. In our work, trehalose was applied as a technological auxiliary agent, and literature data relating to the spray-drying technology of trehalose were collected. Studies were made of the influence of the spraying process on the amorphization of trehalose and on the recrystallization of amorphous trehalose during storage. Amorphous samples were investigated under 3 different conditions during 3 months. The recrystallization process was followed by differential scanning calorimetry and X-ray powder diffraction. The results demonstrated the perfect amorphization of trehalose during the spray-drying process. The glass transition temperature was well measurable in the samples and proved to be the same as the literature data. Recrystallization under normal conditions was very slow but at high relative humidity the process was accelerated greatly. Amorphous trehalose gave rise to dihydrate forms (gamma- and h-trehaloses) during recrystallization, and beta-trehalose was also identified as an anhydrous form.

Composite Magnetite and Protein Containing CaCO3 Crystals. External Manipulation and Vaterite → Calcite Recrystallization-Mediated Release Performance.

PubMed

Sergeeva, Alena; Sergeev, Roman; Lengert, Ekaterina; Zakharevich, Andrey; Parakhonskiy, Bogdan; Gorin, Dmitry; Sergeev, Sergey; Volodkin, Dmitry

2015-09-30

Biocompatibility and high loading capacity of mesoporous CaCO3 vaterite crystals give an option to utilize the polycrystals for a wide range of (bio)applications. Formation and transformations of calcium carbonate polymorphs have been studied for decades, aimed at both basic and applied research interests. Here, composite multilayer-coated calcium carbonate polycrystals containing Fe3O4 magnetite nanoparticles and model protein lysozyme are fabricated. The structure of the composite polycrystals and vaterite → calcite recrystallization kinetics are studied. The recrystallization results in release of both loaded protein and Fe3O4 nanoparticles (magnetic manipulation is thus lost). Fe3O4 nanoparticles enhance the recrystallization that can be induced by reduction of the local pH with citric acid and reduction of the polycrystal crystallinity. Oppositely, the layer-by-layer assembled poly(allylamine hydrochloride)/poly(sodium styrenesulfonate) polyelectrolyte coating significantly inhibits the vaterite → calcite recrystallization (from hours to days) most likely due to suppression of the ion exchange giving an option to easily tune the release kinetics for a wide time scale, for example, for prolonged release. Moreover, the recrystallization of the coated crystals results in formulation of multilayer capsules keeping the feature of external manipulation. This study can help to design multifunctional microstructures with tailor-made characteristics for loading and controlled release as well as for external manipulation.

Purification and crystal growth of NPB via imidazolium based ionic liquids

NASA Astrophysics Data System (ADS)

Oh, Yong-Taeg; Shin, Dong-Chan

2018-04-01

Here we report the production of high purity and crystallinity organic electronic material of NPB (N,N‧-Di-[(1-naphthyl)-N,N‧-diphenyl]-1,1‧-biphenyl-4,4‧-diamine (C44H32N2) through solution recrystallization within imidazolium based ionic liquids. When low purity NPB was recrystallized at 170 °C within C8MIM[TFSI], its purity was drastically improved from 82% to 99.92%. These recrystallized NPB crystals showed 0.040° FWHM (Full Width Half Maximum) of X-ray (1 1 1) diffraction peak. Such small FWHM angle indicates single-crystal like crystallinity. Initial NPB powder was dissolved at 100 °C and recrystallized at temperature above 110 °C. At higher temperature of 170 °C, a small number of bigger crystals were formed compared to those at 110 °C. This can be well explained by the classical nucleation and growth theory. Therefore, solution recrystallization process using ionic liquid might be promising for mass production of organic electronic materials by replacing the widely-used sublimation purification method.

Microstructural Evolution During Cold Rolling and Subsequent Annealing in Low-Carbon Steel with Different Initial Microstructures

NASA Astrophysics Data System (ADS)

Ogawa, Toshio; Dannoshita, Hiroyuki; Maruoka, Kuniaki; Ushioda, Kohsaku

2017-08-01

Microstructural evolution during cold rolling and subsequent annealing of low-carbon steel with different initial microstructures was investigated from the perspective of the competitive phenomenon between recrystallization of ferrite and reverse phase transformation from ferrite to austenite. Three kinds of hot-rolled sheet specimens were prepared. Specimen P consisted of ferrite and pearlite, specimen B consisted of bainite, and specimen M consisted of martensite. The progress of recovery and recrystallization of ferrite during annealing was more rapid in specimen M than that in specimens P and B. In particular, the recrystallized ferrite grains in specimen M were fine and equiaxed. The progress of ferrite-to-austenite phase transformation during intercritical annealing was more rapid in specimen M than in specimens P and B. In all specimens, the austenite nucleation sites were mainly at high-angle grain boundaries, such as those between recrystallized ferrite grains. The austenite distribution was the most uniform in specimen M. Thus, we concluded that fine equiaxed recrystallized ferrite grains were formed in specimen M, leading to a uniform distribution of austenite.

Cryogenic strength improvement by utilizing room-temperature deformation twinning in a partially recrystallized VCrMnFeCoNi high-entropy alloy

PubMed Central

Jo, Y. H.; Jung, S.; Choi, W. M.; Sohn, S. S.; Kim, H. S.; Lee, B. J.; Kim, N. J.; Lee, S.

2017-01-01

The excellent cryogenic tensile properties of the CrMnFeCoNi alloy are generally caused by deformation twinning, which is difficult to achieve at room temperature because of insufficient stress for twinning. Here, we induced twinning at room temperature to improve the cryogenic tensile properties of the CrMnFeCoNi alloy. Considering grain size effects on the critical stress for twinning, twins were readily formed in the coarse microstructure by cold rolling without grain refinement by hot rolling. These twins were retained by partial recrystallization and played an important role in improving strength, allowing yield strengths approaching 1 GPa. The persistent elongation up to 46% as well as the tensile strength of 1.3 GPa are attributed to additional twinning in both recrystallized and non-recrystallization regions. Our results demonstrate that non-recrystallized grains, which are generally avoided in conventional alloys because of their deleterious effect on ductility, can be useful in achieving high-strength high-entropy alloys. PMID:28604656

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.

Manipulating Cells with Static Magnetic Fields

NASA Astrophysics Data System (ADS)

Valles, J. M.; Guevorkian, K.

2005-07-01

We review our investigations of the use of static magnetic fields, B, for manipulating cells and cellular processes. We describe how B fields modify the cell division pattern of frog embryos and consequently can be used to probe the pattern determinants. We also observe that magnetic fields modify the swimming behavior of Paramecium Caudatum. We describe these modifications and their potential application to investigations of their swimming behavior.

Ice-Active Substances from the Infective Juveniles of the Freeze Tolerant Entomopathogenic Nematode, Steinernema feltiae

PubMed Central

Ali, Farman; Wharton, David A.

2016-01-01

Steinernema feltiae is a moderately freezing tolerant nematode, that can withstand intracellular ice formation. We investigated recrystallization inhibition, thermal hysteresis and ice nucleation activities in the infective juveniles of S. feltiae. Both the splat cooling assay and optical recrystallometry indicate the presence of ice active substances that inhibit recrystallization in the nematode extract. The substance is relatively heat stable and largely retains the recrystallization inhibition activity after heating. No thermal hysteresis activity was detected but the extract had a typical hexagonal crystal shape when grown from a single seed crystal and weak ice nucleation activity. An ice active substance is present in a low concentration, which may be involved in the freezing survival of this species by inhibiting ice recrystallization. PMID:27227961

Behavior of plywood and fiberglass steel composite tube structures subjected to impact loading

NASA Astrophysics Data System (ADS)

Armaghani, Seyamend Bilind

Paratransit buses are custom built as the major vehicle manufacturer produces the custom built passenger cage installed on the chassis for the Paratransit bus. In order for these Paratransit bus members to be sufficient, they have to be evaluated for crashworthiness and energy absorption. This has prompted Florida Department of Transportation (FDOT) to fund research for the safety evaluation of Paratransit busses consisting of crash and safety analysis. There has been a large body of research done on steel subjected to static loads, but more research is needed for steel applied under dynamic loading and high speeds in order to improve crashworthiness in events such as rollovers and side impacts. Bare steel Hollow Structural Section (HSS) tubing are used a lot as structural members of Paratransit buses because of their lightness and progressive buckling under loading. The research will be conducted on quantifying the tubing's behavior under bending by conducting static three point bending and impact loading tests. In addition to the bare tubing, plywood and fiberglass composites are investigated because they are both strong and lightweight and their behavior under dynamic loading hasn't been quantified. As a result, the main purpose of this research is to quantify the differences between the dynamic and static behavior of plywood steel composite and fiberglass steel composite tubing and compare these findings with those of bare steel tubing. The differences will be quantified using detailed and thorough experiments that will examine the composites behavior under both static and dynamic loading. These tests will determine if there are any advantages of using the composite materials and thus allow for recommendations to be made to the FDOT with the goal of improving the safety of Paratransit busses. Tensile tests were conducted to determine the material properties of the tested specimens. Before the static and dynamic experiments are run to investigate the differences between static and dynamic behavior, Preliminary three point bending testing was conducted to determine the parameters for the final experiments. Static bending testing was conducted on the bare, plywood composite, and fiberglass composite steel tubing. The point of these experiments was to produce a Moment vs. Rotation plot to determine the specimens' maximum moments and their associated rotation, as that is when the steel buckles and fails. The dynamic three point bending experiments were conducted using the impact loading apparatus and had the same purpose as the static experiments. For both static and dynamic experiments, the performances of the different types of specimens were compared based upon their Moment vs. Rotation plots. This will determine the effect that the composite has on the rotation and maximum moment at which the tubing fails. After conducting these experiments, amplification factors were established for each specimen by comparing the maximum moment and their associated rotation between static and dynamic testing. lambda was calculated to quantify the ratio between the static and dynamic maximum moments. beta was used to quantify the ratio between the rotation needed to produce the maximum moment between static and dynamic events. A small amplification factor denotes that material performs well under impact loading and the material doesn't experience dramatic change in behavior during dynamic events. Amplification factors were compared between the bare, plywood, and fiberglass composite steel tubing in order to evaluate the performance of the composites. After comparing the amplification factors of the different types of tubing, recommendations can be made. Fiberglass and plywood composite were shown to be valuable because it decreased the effect of dynamic forces as beta was reduced by a factor of 2 in comparison to bare tubing. Based upon the amplification factors, it was recommended to use 14 gauge fiberglass composite tubing as Paratransit bus structural members because it was affected the least by dynamic loading.

Ostwald ripening of clays and metamorphic minerals

USGS Publications Warehouse

Eberl, D.D.; Srodon, J.; Kralik, M.; Taylor, B.E.; Peterman, Z.E.

1990-01-01

Analyses of particle size distributions indicate that clay minerals and other diagenetic and metamorphic minerals commonly undergo recrystallization by Ostwald ripening. The shapes of their particle size distributions can yield the rate law for this process. One consequence of Ostwald ripening is that a record of the recrystallization process is preserved in the various particle sizes. Therefore, one can determine the detailed geologic history of clays and other recrystallized minerals by separating, from a single sample, the various particle sizes for independent chemical, structural, and isotopic analyses.

Orientation filtering for crystalline films

DOEpatents

Smith, Henry I.; Atwater, Harry A.; Thompson, Carl V.; Geis, Michael W.

1986-12-30

A substrate is coated with a film to be recrystallized. A pattern of crystallization barriers is created in the film, for example, by etching voids in the film. An encapsulation layer is generally applied to protect the film, fill the voids and otherwise enhance a recrystallization process. Recrystallization is carried out such that certain orientations pass preferentially through the barrier, generally as a result of growth-velocity anisotropy. The result is a film of a specific predetermined crystallographic orientation, a range of orientations or a set of discrete orientations.

Supercooled smectic nanoparticles: a potential novel carrier system for poorly water soluble drugs.

PubMed

Kuntsche, J; Westesen, K; Drechsler, M; Koch, M H J; Bunjes, H

2004-10-01

The possibility of preparing nanoparticles in the supercooled thermotropic liquid crystalline state from cholesterol esters with saturated acyl chains as well as the incorporation of model drugs into the dispersions was investigated using cholesteryl myristate (CM) as a model cholesterol ester. Nanoparticles were prepared by high-pressure melt homogenization or solvent evaporation using phospholipids, phospholipid/ bile salt, or polyvinyl alcohol as emulsifiers. The physicochemical state and phase behavior of the particles was characterized by particle size measurements (photon correlation spectroscopy, laser diffraction with polarization intensity differential scattering), differential scanning calorimetry, X-ray diffraction, and electron and polarizing light microscopy. The viscosity of the isotropic and liquid crystalline phases of CM in the bulk was investigated in dependence on temperature and shear rate by rotational viscometry. CM nanoparticies can be obtained in the smectic phase and retained in this state for at least 12 months when stored at 230C in optimized systems. The recrystallization tendency of CM in the dispersions strongly depends on the stabilizer system and the particle size. Stable drug-loaded smectic nanoparticles were obtained after incorporation of 10% (related to CM) ibuprofen, miconazole, etomidate, and 1% progesterone. Due to their liquid crystalline state, colloidal smectic nanoparticles offer interesting possibilities as carrier system for lipophilic drugs. CM nanoparticles are suitable model systems for studying the crystallization behavior and investigating the influence of various parameters for the development of smectic nanoparticles resistant against recrystallization upon storage.

The crystallization and crystalline properties of LARC-TPI

NASA Technical Reports Server (NTRS)

Theil, Michael H.; Gangal, Pravin D.

1992-01-01

LARC-TPI, a thermoplastic polyimide, has been studied in order to develop an understanding of its crystalline phase transition. Our experiments suggest that samples synthesized in different laboratories apparently had different degrees of imidization and their thermal behaviors differed accordingly. When the most crystalline of these polyimides was studied in some detail, we found that it melted irreversibly in that once a sample was completely melted it would not recrystallize. A polymer that did not recrystallize displayed a glass transition, which increased in temperature upon subsequent cooling and reheating. Solubility experiments indicated that heating above the crystalline melting temperature led to network formation in the polymer, a conclusion that is consistent with other behavior just mentioned. Differential calorimetric studies revealed that annealing at slow heating rates or under isothermal conditions resulted in dual melting transitions. These studies, supported by X-ray diffraction results, strongly indicate that the annealing process involves a solid-liquid-solid transformation. From an existing phenomenological model for the kinetics of phase transitions, kinetic parameters for these crystallizations have been evaluated. The Avrami exponents n increased with the annealing temperature in the protocol used in this study. Their values were about 2 or lower, thus indicating that crystallization may have followed a mechanism that included heterogeneous nucleation of a low dimensional order in which all the embryonic crystallites formed at the beginning of the process. A positive temperature coefficient for these crystallizations indicated that diffusion may have had a rate controlling influence and affected the values of n.

Behavioral compliance for dynamic versus static signs in an immersive virtual environment.

PubMed

Duarte, Emília; Rebelo, Francisco; Teles, Júlia; Wogalter, Michael S

2014-09-01

This study used an immersive virtual environment (IVE) to examine how dynamic features in signage affect behavioral compliance during a work-related task and an emergency egress. Ninety participants performed a work-related task followed by an emergency egress. Compliance with uncued and cued safety signs was assessed prior to an explosion/fire involving egress with exit signs. Although dynamic presentation produced the highest compliance, the difference between dynamic and static presentation was only statistically significant for uncued signs. Uncued signs, both static and dynamic, were effective in changing behavior compared to no/minimal signs. Findings are explained based on sign salience and on task differences. If signs must capture attention while individuals are attending to other tasks, salient (e.g., dynamic) signs are useful in benefiting compliance. This study demonstrates the potential for IVEs to serve as a useful tool in behavioral compliance research. Copyright © 2013 Elsevier Ltd and The Ergonomics Society. All rights reserved.

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.

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.

Static aeroelastic behavior of a subsonic plate wing

NASA Astrophysics Data System (ADS)

Berci, M.

2017-07-01

The static aeroelastic behavior of a subsonic plate wing is here described by semi-analytical means. Within a generalised modal formulation, any distribution of the plate's properties is allowed. Modified strip theory is employed for the aerodynamic modelling and a linear aeroelastic model is eventually derived. Numerical results are then shown for the plate's aeroelastic stability in terms of divergence speed, with respect to the most relevant aero-structural parameters.

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

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

Recrystallization plays an important role in swelling kinetics of irradiated metallic nuclear fuels. This talk will present a three-dimensional microstructure-dependent swelling model by integrating the evolution of intra-and inter- granular gas bubbles, dislocation loop density, and recrystallization.

Recrystallization characteristics and interfacial oxides on the compression bonding interface

NASA Astrophysics Data System (ADS)

Xie, Bijun; Sun, Mingyue; Xu, Bin; Li, Dianzhong

2018-05-01

Up to now, the mechanism of interface bonding is still not fully understood. This work presents interfacial characteristics of 316LN stainless steel bonding joint after cold compression bonding with subsequent annealing. EBSD analysis shows that fine recrystallization grains preferentially appear near the bonding interface and grow towards both sides of the interface. Transmission electron microscopy reveals that initial cold compression bonding disintegrates the native oxide scales and brings pristine metal from both sides of the interface come into intimate contact, while the broken oxide particles are remained at the original interface. The results indicate that partial bonding can be achieved by cold compression bonding with post-annealing treatment and recrystallization firstly occurs along the bonding interface. However, the interfacial oxides impede the recrystallization grains step over the interface and hinder the complete healing of the bonding interface.

Recrystallization characteristics of oxide dispersion strengthened nickel-base alloys

NASA Technical Reports Server (NTRS)

Hotzler, R. K.; Glasgow, T. K.

1980-01-01

Electron microscopy was employed to study the process of recrystallization in two oxide dispersion strengthened (ODS) mechanically alloyed nickel-base alloys, MA 754 and MA 6000E. MA 754 contained both fine, uniformly dispersed particles and coarser oxides aligned along the working direction. Hot rolled MA 754 had a grain size of 0.5 microns and high dislocation densities. After partial primary recrystallization, the fine grains transformed to large elongated grains via secondary (or abnormal) grain growth. Extruded and rolled MA 6000E contained equiaxed grains of 0.2 micron diameter. Primary recrystallization occurring during working eliminated virtually all dislocations. Conversion from fine to coarse grains was triggered by gamma prime dissolution; this was also a process of secondary or abnormal grain growth. Comparisons were made to conventional and oxide dispersion strengthened nickel-base alloys.

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

Behavior of sheets from Ti-alloys by rolling and heat treatment

NASA Astrophysics Data System (ADS)

Isaenkova, M.; Perlovich, Yu.; Fesenko, V.; Gritskevich, M.; Stolbov, S.; Zaripova, M.

2017-10-01

Sheets from single- and two-phase Ti-alloys (VT1-0, Ti-22Nb-9%Zr and VT-16) were rolled at the room temperature up to various deformation degrees and annealed at temperatures 500-900 °C. The regularities of texture formation in both phases were established. In the technically pure Ti (VT1-0) with the single α-Ti phase the final stable texture component is (0001)±30-40°ND-TD<101 ¯0>. In the two-phase alloy the reorientation of basal axes of α-Ti occurs by the same trajectories as in the single phase alloy. However, in the case of two-phase alloy texture development in α-Ti stops at the intermediate stage, when this texture consists of components with rolling planes (0001)±15-20°ND-RD and (0001)±30-40°ND-TD. The stability of the first components can be provided both by the mutually balanced operation of pyramidal and basal slip systems, activity of which remains at the high deformation degree of two-phase alloy, and by the dynamic α↔β phase transformations, taking place in the distorted structures of α- and β-phases in the course of its cold rolling. At recrystallization of technically pure Ti the basal component disappears in its texture. At the same time, prismatic axes turn by angles 20÷30° depending on the heating rate of the rolled sheet and annealing temperature. At recrystallization of the two-phase Ti-alloy prismatic axes of its α-grains doesn't turn relative to their positions in the rolling texture, as it occurs in the single-phase alloy. This fact indicates to some alternative mode of arising new recrystallized grains in two-phase alloys.

Recrystallization and grain growth induced by ELMs-like transient heat loads in deformed tungsten samples

NASA Astrophysics Data System (ADS)

Suslova, A.; El-Atwani, O.; Sagapuram, D.; Harilal, S. S.; Hassanein, A.

2014-11-01

Tungsten has been chosen as the main candidate for plasma facing components (PFCs) due to its superior properties under extreme operating conditions in future nuclear fusion reactors such as ITER. One of the serious issues for PFCs is the high heat load during transient events such as ELMs and disruption in the reactor. Recrystallization and grain size growth in PFC materials caused by transients are undesirable changes in the material, since the isotropic microstructure developed after recrystallization exhibits a higher ductile-to-brittle transition temperature which increases with the grain size, a lower thermal shock fatigue resistance, a lower mechanical strength, and an increased surface roughening. The current work was focused on careful determination of the threshold parameters for surface recrystallization, grain growth rate, and thermal shock fatigue resistance under ELM-like transient heat events. Transient heat loads were simulated using long pulse laser beams for two different grades of ultrafine-grained tungsten. It was observed that cold rolled tungsten demonstrated better power handling capabilities and higher thermal stress fatigue resistance compared to severely deformed tungsten. Higher recrystallization threshold, slower grain growth, and lower degree of surface roughening were observed in the cold rolled tungsten.

Solid dispersion of acetaminophen and poly(ethylene oxide) prepared by hot-melt mixing.

PubMed

Yang, Min; Wang, Peng; Huang, Chien-Yueh; Ku, M Sherry; Liu, Huiju; Gogos, Costas

2010-08-16

In this study, a model drug, acetaminophen (APAP), was melt mixed with poly(ethylene oxide) (PEO) using a Brabender mixer. APAP was found to recrystallize upon cooling to room temperature for all the drug loadings investigated. Higher drug loading leads to faster recrystallization rate. However, the morphology of the recrystallized drug crystals is identical in samples with different drug loadings and does not change with the storage time. To adjust the drug's dissolution rate, nanoclay Cloisite 15A and 30B were added into the binary mixture. The presence of either of the nanoclay dramatically accelerates the drug's recrystallization rate and slows down the drug's releasing rate. The drop of the releasing rate is mainly due to the decrease of wettability, as supported by the contact angle data. Data analysis of the dissolution results suggests that the addition of nanoclays changes the drug's release mechanism from erosion dominant to diffusion dominant. This study suggests that nanoclays may be utilized to tailor the drug's releasing rate and to improve the dosage form's stability by dramatically shortening the lengthy recrystallization process. Copyright (c) 2010 Elsevier B.V. All rights reserved.

Recrystallization and grain growth induced by ELMs-like transient heat loads in deformed tungsten samples

PubMed Central

Suslova, A.; El-Atwani, O.; Sagapuram, D.; Harilal, S. S.; Hassanein, A.

2014-01-01

Tungsten has been chosen as the main candidate for plasma facing components (PFCs) due to its superior properties under extreme operating conditions in future nuclear fusion reactors such as ITER. One of the serious issues for PFCs is the high heat load during transient events such as ELMs and disruption in the reactor. Recrystallization and grain size growth in PFC materials caused by transients are undesirable changes in the material, since the isotropic microstructure developed after recrystallization exhibits a higher ductile-to-brittle transition temperature which increases with the grain size, a lower thermal shock fatigue resistance, a lower mechanical strength, and an increased surface roughening. The current work was focused on careful determination of the threshold parameters for surface recrystallization, grain growth rate, and thermal shock fatigue resistance under ELM-like transient heat events. Transient heat loads were simulated using long pulse laser beams for two different grades of ultrafine-grained tungsten. It was observed that cold rolled tungsten demonstrated better power handling capabilities and higher thermal stress fatigue resistance compared to severely deformed tungsten. Higher recrystallization threshold, slower grain growth, and lower degree of surface roughening were observed in the cold rolled tungsten. PMID:25366885

Recrystallization of water in non-water-soluble (meth)acrylate polymers is not rare and is not devitrification.

PubMed

Gemmei-Ide, Makoto; Ohya, Atsushi; Kitano, Hiromi

2012-02-16

Change in the state of water sorbed into four kinds of non-water-soluble poly(meth)acrylates with low water content by temperature (T) perturbation was examined on the basis of T variable mid-infrared (MIR) spectroscopy. Many studies using differential scanning calorimetry suggested that there was no change in the state. T dependence of their MIR spectra, however, clearly demonstrated various changes in the state. Furthermore, recrystallization, which was crystallization during heating, was observed in all four polymers. The recrystallization observed in this study was not devitrification, which is the change in the state from glassy water to crystalline water, but vapor deposition during heating (vapor re-deposition). There were only two reports about recrystallization of water in a non-water-soluble polymer before this report; therefore, it might be considered to be a rare phenomenon. However, as demonstrated in this study, it is not a rare phenomenon. Recrystallization (vapor re-deposition) of water in the polymer matrices is related to a balance between flexibility and strength of the electrostatic interaction sites of polymer matrices but might not be related to the biocompatibility of polymers.

Recrystallization and grain growth induced by ELMs-like transient heat loads in deformed tungsten samples.

PubMed

Suslova, A; El-Atwani, O; Sagapuram, D; Harilal, S S; Hassanein, A

2014-11-04

Tungsten has been chosen as the main candidate for plasma facing components (PFCs) due to its superior properties under extreme operating conditions in future nuclear fusion reactors such as ITER. One of the serious issues for PFCs is the high heat load during transient events such as ELMs and disruption in the reactor. Recrystallization and grain size growth in PFC materials caused by transients are undesirable changes in the material, since the isotropic microstructure developed after recrystallization exhibits a higher ductile-to-brittle transition temperature which increases with the grain size, a lower thermal shock fatigue resistance, a lower mechanical strength, and an increased surface roughening. The current work was focused on careful determination of the threshold parameters for surface recrystallization, grain growth rate, and thermal shock fatigue resistance under ELM-like transient heat events. Transient heat loads were simulated using long pulse laser beams for two different grades of ultrafine-grained tungsten. It was observed that cold rolled tungsten demonstrated better power handling capabilities and higher thermal stress fatigue resistance compared to severely deformed tungsten. Higher recrystallization threshold, slower grain growth, and lower degree of surface roughening were observed in the cold rolled tungsten.

Unraveling the Effect of Thermomechanical Treatment on the Dissolution of Delta Ferrite in Austenitic Stainless Steels

NASA Astrophysics Data System (ADS)

Rezayat, Mohammad; Mirzadeh, Hamed; Namdar, Masih; Parsa, Mohammad Habibi

2016-02-01

Considering the detrimental effects of delta ferrite stringers in austenitic stainless steels and the industrial considerations regarding energy consumption, investigating, and optimizing the kinetics of delta ferrite removal is of vital importance. In the current study, a model alloy prone to the formation of austenite/delta ferrite dual phase microstructure was subjected to thermomechanical treatment using the wedge rolling test aiming to dissolve delta ferrite. The effect of introducing lattice defects and occurrence of dynamic recrystallization (DRX) were investigated. It was revealed that pipe diffusion is responsible for delta ferrite removal during thermomechanical process, whereas when the DRX is dominant, the kinetics of delta ferrite dissolution tends toward that of the static homogenization treatment for delta ferrite removal that is based on the lattice diffusion of Cr and Ni in austenite. It was concluded that the optimum condition for dissolution of delta ferrite can be defined by the highest rolling temperature and strain in which DRX is not pronounced.

Orientation filtering for crystalline films

DOEpatents

Smith, H.I.; Atwater, H.A.; Thompson, C.V.; Geis, M.W.

1986-12-30

A substrate is coated with a film to be recrystallized. A pattern of crystallization barriers is created in the film, for example, by etching voids in the film. An encapsulation layer is generally applied to protect the film, fill the voids and otherwise enhance a recrystallization process. Recrystallization is carried out such that certain orientations pass preferentially through the barrier, generally as a result of growth-velocity anisotropy. The result is a film of a specific predetermined crystallographic orientation, a range of orientations or a set of discrete orientations. 7 figs.

Strong Surface Diffusion Mediated Glancing-Angle Deposition: Growth, Recrystallization and Reorientation of Tin Nanorods

NASA Astrophysics Data System (ADS)

Wang, Huan-Hua; Shi, Yi-Jian; William, Chu; Yigal, Blum

2008-01-01

Different from usual glancing-angle deposition where low surface diffusion is necessary to form nanorods, strong surface diffusion mediated glancing-angle deposition is exemplified by growing tin nanorod films on both silicon and glass substrates simultaneously via thermal evaporation. During growth, the nanorods were simultaneously baked by the high-temperature evaporator, and therefore re-crystallized into single crystals in consequence of strong surface diffusion. The monocrystalline tin nanorods have a preferred orientation perpendicular to the substrate surface, which is quite different from the usual uniformly oblique nanorods without recrystallization.

Role of the Double-Layer Cation on the Potential-Dependent Stretching Frequencies and Binding Geometries of Carbon Monoxide at Platinum-Nonaqueous Interfaces

DTIC Science & Technology

1992-02-01

were recrystallized twice from water, or water, and then ethanol , and methanol/water, respectively, and dried at 100"C under vacuum for 24 hours. The...hexafluorophosphate, and recrystallized twice from absolute ethanol . The alkali perchlorates (LiCIO4, NaCl0 4, KCIO 4, from G.F. Smith) were recrystallized twice from...which a Ag/AgCl (3M KCI) reference electrode was used. All measurements were made at room 5 temperature , 23 ± VC. RESULTS In our earlier preliminary

Optically induced melting of colloidal crystals and their recrystallization.

PubMed

Harada, Masashi; Ishii, Masahiko; Nakamura, Hiroshi

2007-04-15

Colloidal crystals melt by applying focused light of optical tweezers and recrystallize after removing it. The disturbed zone by the light grows radially from the focus point and the ordering starts from the interface with the crystal. Although the larger disturbed zone is observed for the higher power optical tweezers, a master curve is extracted by normalization of the disturbed zone. The temporal changes of the normalized disturbed zone are well described with exponential functions, indicating that the melting and recrystallization process is governed by a simple relaxation mechanism.

Annealing effects in plated-wire memory elements. II - Recrystallization in Permalloy films.

NASA Technical Reports Server (NTRS)

Marquardt, S. J.; Kench, J. R.

1971-01-01

Results of grain-size measurements in Permalloy platings suggest that recrystallization is possible at temperatures as low as 200 C, but that it is an extremely heterogeneous process. No worthwhile correlation was found to exist between observed grain size and magnetic dispersion in samples aged in the temperature range from 180 to 230 C. It is suggested that the magnetic aging which occurs under these conditions may be due to some other diffusion-controlled process than recrystallization; a process such as chemical homogenization is tentatively preferred.

Cyclic tensile response of a pre-tensioned polyurethane

NASA Astrophysics Data System (ADS)

Nie, Yizhou; Liao, Hangjie; Chen, Weinong W.

2018-05-01

In the research reported in this paper, we subject a polyurethane to uniaxial tensile loading at a quasi-static strain rate, a high strain rate and a jumping strain rate where the specimen is under quasi-static pre-tension and is further subjected to a dynamic cyclic loading using a modified Kolsky tension bar. The results obtained at the quasi-static and high strain rate clearly show that the mechanical response of this material is significantly rate sensitive. The rate-jumping experimental results show that the response of the material behavior is consistent before jumping. After jumping the stress-strain response of the material does not jump to the corresponding high-rate curve. Rather it approaches the high-rate curve asymptotically. A non-linear hyper-viscoelastic (NLHV) model, after having been calibrated by monotonic quasi-static and high-rate experimental results, was found to be capable of describing the material tensile behavior under such rate jumping conditions.

Experimental data of the static behavior of reinforced concrete beams at room and low temperature.

PubMed

Mirzazadeh, M Mehdi; Noël, Martin; Green, Mark F

2016-06-01

This article provides data on the static behavior of reinforced concrete at room and low temperature including, strength, ductility, and crack widths of the reinforced concrete. The experimental data on the application of digital image correlation (DIC) or particle image velocimetry (PIV) in measuring crack widths and the accuracy and precision of DIC/PIV method with temperature variations when is used for measuring strains is provided as well.

Oxidation behavior of TD-NiCr in a dynamic high temperature environment

NASA Technical Reports Server (NTRS)

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

1974-01-01

The oxidation behavior of TD-NiCr has been studied in static and high-speed flowing air environments at 1100 and 1200 C. It has been found that the stable oxide morphologies formed on the specimens exposed to the static and dynamic environments were markedly different. The faceted crystal morphology characteristic of static oxidation was found to be unstable under high-temperature, high-speed flow conditions and was quickly replaced by a porous NiO 'mushroom' type structure. Also, it was found that the rate of formation of CrO3 from Cr2O3 was greatly enhanced by high gas velocity conditions. The stability of Cr2-O3 was found to be greatly improved by the presence of an outer NiO layer, even though the NiO layer was very porous. An oxidation model is proposed to explain the observed microstructures and overall oxidation behavior of TD-NiCr alloys.

MSC products for the simulation of tire behavior

NASA Technical Reports Server (NTRS)

Muskivitch, John C.

1995-01-01

The modeling of tires and the simulation of tire behavior are complex problems. The MacNeal-Schwendler Corporation (MSC) has a number of finite element analysis products that can be used to address the complexities of tire modeling and simulation. While there are many similarities between the products, each product has a number of capabilities that uniquely enable it to be used for a specific aspect of tire behavior. This paper discusses the following programs: (1) MSC/NASTRAN - general purpose finite element program for linear and nonlinear static and dynamic analysis; (2) MSC/ADAQUS - nonlinear statics and dynamics finite element program; (3) MSC/PATRAN AFEA (Advanced Finite Element Analysis) - general purpose finite element program with a subset of linear and nonlinear static and dynamic analysis capabilities with an integrated version of MSC/PATRAN for pre- and post-processing; and (4) MSC/DYTRAN - nonlinear explicit transient dynamics finite element program.

Cocrystallization out of the blue: DL-mandelic acid/ethyl-DL-mandelate cocrystal

NASA Astrophysics Data System (ADS)

Tumanova, Natalia; Payen, Ricky; Springuel, Géraldine; Norberg, Bernadette; Robeyns, Koen; Le Duff, Cécile; Wouters, Johan; Leyssens, Tom

2017-01-01

This work focuses on a peculiar behavior of racemic mandelic acid in ethanol solution. Dissolution of racemic mandelic acid in ethanol followed by evaporation to dryness results in a DL-mandelic acid/ethyl-DL-mandelate cocrystal. This behavior indicates that racemic mandelic acid tends not only to transform into an ester in ethanol, but also to cocrystallize with untransformed acid molecules. Cocrystal formation for mandelic acid in ethanol was found to be reproducible under various conditions. DL-tropic acid and DL-phenyllactic acid that contain similar functional groups and that were tested as well, on the other hand, showed no cocrystal formation: DL-phenyllactic acid partly converted into an ester, whereas DL-tropic acid mostly recrystallized.

Effect of Heat Index on Microstructure and Mechanical Behavior of Friction Stir Processed AZ31

NASA Astrophysics Data System (ADS)

Yuan, Wei; Mishra, Rajiv S.

Friction stir processing modifies the micro structure and properties of metals through intense plastic deformation. The frictional heat input affects the microstructure evolution and resulting mechanical properties. 2 mm thick commercial AZ31B-H24 Mg alloy was friction stir processed under various process parameter combinations to investigate the effect of heat index on micro structure and properties. Recrystallized grain structure in the nugget region was observed for all processing conditions with decrease in hardness. Results indicate a reduced tensile yield strength and ultimate tensile strength compared to the as-received material in H-temper, but with an improved hardening capacity. The strain hardening behavior of friction stir processed material is discussed.

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

Deibler, Lisa Anne; Brown, Arthur; Puskar, Joseph D.

Drawn 304L stainless steel tubing was subjected to 42 different annealing heat treatments with the goal of initializing a microstructural model to select a heat treatment to soften the tubing from a hardness of 305 Knoop to 225–275 Knoop. The amount of recrystallization and grain size caused by 18 heat treatments were analyzed via optical microscopy and image analysis, revealing the full range of recrystallization from 0 to 100%. The formation of carbides during the longer duration and higher-temperature heat treatments was monitored via transmission electron microscope evaluation. The experimental results informed a model which includes recovery, recrystallization, and grainmore » growth to predict microstructure and hardness. After initialization of the model, it was able to predict hardness with a R 2 value of 0.95 and recrystallization with an R 2 value of 0.99. As a result, the model was then utilized in the design and testing of a heat treatment to soften the tubing.« less

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

NASA Astrophysics Data System (ADS)

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

2015-03-01

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

Deformation-Induced Dynamic Precipitation and Resulting Microstructure in a Mg-Zn-Ca Alloy

NASA Astrophysics Data System (ADS)

Du, Yuzhou; Zheng, Mingyi; Jiang, Bailing; Zhou, Kesong

2018-05-01

The microstructure of an Mg-Zn-Ca extrusion was investigated by transmission electron microscopy, and the interaction between dynamic precipitation and dynamic recrystallization was analyzed. The results showed that dynamic precipitation significantly affected the microstructure of the as-extruded Mg-Zn-Ca alloy. The pinning effects of precipitates on dislocations effectively prohibited dynamic recrystallization processes, while the grain boundary precipitate Ca2Mg6Zn3, inhibited the growth of dynamically recrystallized grains. Consequently, a bimodal microstructure with fine dynamically recrystallized (DRXed) grains and elongated deformed regions was obtained for the Mg-Zn-Ca extrusion. High-resolution transmission electron microscopy indicated that the intragranular precipitate MgZn2 had a crystal orientation relationship with α-Mg in the form of (0002)Mg//(10-13)MgZn2 and [1-100]Mg//[1-210]MgZn2, which was beneficial for strength improvement.

A comparative study on the direct deposition of μc-Si:H and plasma-induced recrystallization of a-Si:H: Insight into Si crystallization in a high-density plasma

NASA Astrophysics Data System (ADS)

Zhou, H. P.; Xu, M.; Xu, S.; Feng, Y. Y.; Xu, L. X.; Wei, D. Y.; Xiao, S. Q.

2018-03-01

Deep insight into the crystallization mechanism of amorphous silicon is of theoretical and technological significance for the preparation of high-quality microcrystalline/polycrystalline silicon. In this work, we intensively compare the present two plasma-involved routes, i.e., the direct deposition and recrystallization of precursor amorphous silicon (a-Si) films, to fabricate microcrystalline silicon. Both the directly deposited and recrystallized samples show multi-layered structures as revealed by electronic microscopy. High-density hydrogen plasma involved recrystallization process, which is mediated by the hydrogen diffusion into the deep region of the precursor a-Si film, displays significantly different nucleation configuration, interface properties, and crystallite shape. The underlying mechanisms are analyzed in combination with the interplay of high-density plasma and growing or treated surface.

FEM study of recrystallized tungsten under ELM-like heat loads

NASA Astrophysics Data System (ADS)

Du, J.; Yuan, Y.; Wirtz, M.; Linke, J.; Liu, W.; Greuner, H.

2015-08-01

FEM thermal analysis has been performed on rolled tungsten plate loaded with heat load of 23 MW/m2 for 1.5 s. Gradient temperature field is generated due to the Gaussian shape beam profile. Recrystallization and grain growth of various scales were found at different areas of the sample depending on the localized thermal field. FEM thermal-mechanical analyses have been performed on the recrystallized tungsten exposed to ELMs-like heat loads. The analyzed load conditions were 0.38 and 1.14 GW/m2 with different base temperatures. Material deterioration due to recrystallization was implemented by adopting decreased yield stress, tangent modulus, strength coefficient and ductility coefficients. Life time predicted by adopting strain life criterion indicates grain growth from 5 μm to 100 μm causes the life decrease of 80%. This result is gained by pure mathematical calculation based on the empiric assumptions of material properties.

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.

Disclination mediated dynamic recrystallization in metals at low temperature.

PubMed

Aramfard, Mohammad; Deng, Chuang

2015-09-16

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

A study of the oxide dispersion and recrystallization in NiCrAl prepared from preoxidized powder

NASA Technical Reports Server (NTRS)

Glasgow, T. K.

1975-01-01

The SAP technique of dispersion strengthening (formation of an oxide dispersion by preoxidation of metal powders) was applied to atomized powder of the alloy Ni-17Cr-5Al-0.2 Y. SAP-NiCrAl was worked by extrusion and rod rolling at 1205 C and by swaging at 760 C. A variety of annealing treatments were applied after working to determine the recrystallization response. NiCrAlY, similarly prepared from atomized powder, but without a preoxidation treatment, was examined for comparison. The SAP-NiCrAl of this study exhibited oxide particle size and spacing much larger than that usually observed in oxide dispersion strengthened alloys; nonetheless, it was possible to achieve abnormal (secondary) recrystallization in the SAP-NiCrAl as has been reported for other oxide dispersion strengthened alloys. In contrast, unoxidized NiCrAlY exhibited only primary recrystallization.

Copper Refinement from Anode to Cathode and then to Wire Rod: Effects of Impurities on Recrystallization Kinetics and Wire Ductility.

PubMed

Helbert, Anne-Laure; Moya, Alice; Jil, Tomas; Andrieux, Michel; Ignat, Michel; Brisset, François; Baudin, Thierry

2015-10-01

In this paper, the traceability of copper from the anode to the cathode and then the wire rod has been studied in terms of impurity content, microstructure, texture, recrystallization kinetics, and ductility. These characterizations were obtained based on secondary ion mass spectrometry, differential scanning calorimetry (DSC), X-ray diffraction, HV hardness, and electron backscattered diffraction. It is shown that the recrystallization was delayed by the total amount of impurities. From tensile tests performed on cold drawn and subsequently annealed wires for a given time, a simplified model has been developed to link tensile elongation to the chemical composition. This model allowed quantification of the contribution of some additional elements, present in small quantity, on the recrystallization kinetics. The proposed model adjusted for the cold-drawn wires was also validated on both the cathode and wire rod used for the study of traceability.

Disclination mediated dynamic recrystallization in metals at low temperature

PubMed Central

Aramfard, Mohammad; Deng, Chuang

2015-01-01

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

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.

Pigeons and humans use action and pose information to categorize complex human behaviors.

PubMed

Qadri, Muhammad A J; Cook, Robert G

2017-02-01

The biological mechanisms used to categorize and recognize behaviors are poorly understood in both human and non-human animals. Using animated digital models, we have recently shown that pigeons can categorize different locomotive animal gaits and types of complex human behaviors. In the current experiments, pigeons (go/no-go task) and humans (choice task) both learned to conditionally categorize two categories of human behaviors that did not repeat and were comprised of the coordinated motions of multiple limbs. These "martial arts" and "Indian dance" action sequences were depicted by a digital human model. Depending upon whether the model was in motion or not, each species was required to engage in different and opposing responses to the two behavioral categories. Both species learned to conditionally and correctly act on this dynamic and static behavioral information, indicating that both species use a combination of static pose cues that are available from stimulus onset in addition to less rapidly available action information in order to successfully discriminate between the behaviors. Human participants additionally demonstrated a bias towards the dynamic information in the display when re-learning the task. Theories that rely on generalized, non-specific visual mechanisms involving channels for motion and static cues offer a parsimonious account of how humans and pigeons recognize and categorize behaviors within and across species. Copyright © 2016 Elsevier Ltd. All rights reserved.

Solvent Effects on the Kinetics of Simple Electrochemical Reactions. I. Comparison of the Behavior of Co(III)/(II) Trisethylenediamine and Ammine Couples with the Predictions of Dielectric Continuum Theory.

DTIC Science & Technology

1981-01-08

lithium perchlorate was dried at -180°C for several days. Tetraethylammonium perchlorate was recrystallized from water and dried in a vacuum oven at...cases the electrolyte composition p, was chosen to be 0.1 M lithium perchlorate or 0.1 M tetraethyl ammonium perchlorate (TEAP). These electrolytes...perchlorate specific adsorption is quite noticeable. Hexafluorophosphate adsorption is sufficiently weak so that small positive values of the potential across

Fundamental Studies on Ambient Temperature Creep Deformation Behavior of Alpha and Alpha-Beta Titanium Alloys

DTIC Science & Technology

1994-02-15

Solutions [49] A-Etch 25 (mL) Hydrofluoric Acid (HF 50%) 25 Nitric Acid Cone (HN03) 50 Glycerine R-Etch 18.5 gm (17 mL) Benzalkonium Chloride 35 (mL... Reduction Project (0704-0188) Washington, DC 20503. 1. AGENCY USE ONLY (Leave Blank) 2. REPORT DATE 1994 3. REPORT TYPE AND DATES COVERED Final 4...K and a 60% reduction in area was given for all of the alloys. This work was found to be sufficient to recrystallize all of the alloys within 12

A Comparison of the Quasi-static Mechanical and Nonlinear Viscoelastic Properties of the Human Semitendinosus and Gracilis Tendons

PubMed Central

Abramowitch, Steven D.; Zhang, Xiaoyan; Curran, Molly; Kilger, Robert

2010-01-01

Background Over fifty-percent of anterior cruciate ligament reconstructions are performed using semitendinosus and gracilis tendon autografts. Despite their increased use, there remains little quantitative data on their mechanical behavior. Therefore, the objective of this study was to investigate the quasi-static mechanical and nonlinear viscoelastic properties of human semitendinosus and gracilis tendons, as well as the variation of these properties along their length. Methods Specimens were subjected to a series of uniaxial tensile tests: one-hour static stress-relaxation test, 30-cycle cyclic stress-relaxation test and load to failure test. To describe the nonlinear viscoelastic behavior, the quasi-linear viscoelastic theory was utilized to model data from the static stress relaxation experiment. Findings The constants describing the viscoelastic behavior were similar between the proximal and distal halves of the gracilis tendon. The proximal half of the semitendinosus tendon, however, had a greater viscous response than its distal half, which was also significantly higher than the proximal gracilis tendon. In terms of the quasi-static mechanical properties, the properties were similar between the proximal and distal halves of the semitendinosus tendon. However, the distal gracilis tendon showed a significantly higher tangent modulus and ultimate stress compared to its proximal half, which was also significantly higher than the distal semitendinosus tendon. Interpretation The results of this study demonstrate differences between the semitendinosus and gracilis tendons in terms of their quasi-static mechanical and nonlinear viscoelastic properties. These results are important for establishing surgical preconditioning protocols and graft selection. PMID:20092917

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

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.

Can Facebook Reduce Perceived Anxiety Among College Students? Randomized Controlled Exercise Trial Using the Transtheoretical Model of Behavior Change

PubMed Central

Frith, Emily

2017-01-01

Background Recent studies suggest social media may be an attractive strategy to promote mental health and wellness. There remains a need to examine the utility for individually tailored wellness messages posted to social media sites such as Facebook to facilitate positive psychological outcomes. Objective Our aim was to extend the growing body of evidence supporting the potential for social media to enhance mental health. We evaluated the influence of an 8-week social media intervention on anxiety in college students and examined the impact of dynamic (active) versus static (passive) Facebook content on physical activity behaviors. Methods Participants in the static group (n=21) accessed a Facebook page featuring 96 statuses. Statuses were intended to engage cognitive processes followed by behavioral processes of change per the transtheoretical model of behavior change. Content posted on the static Facebook page was identical to the dynamic page; however, the static group viewed all 96 statuses on the first day of the study, while the dynamic group received only 1 to 2 of these status updates per day throughout the intervention. Anxiety was measured using the Overall Anxiety Severity and Impairment Scale (OASIS). Time spent engaging in physical activity was assessed using the International Physical Activity Questionnaire (IPAQ). Results The OASIS change score for the dynamic Facebook group was statistically significant (P=.003), whereas the change score for the static group was not (P=.48). A statistically significant group-by-time interaction was observed (P=.03). The total IPAQ group-by-time interaction was not statistically significant (P=.06). Conclusions We observed a decrease in anxiety and increase in total physical activity for the dynamic group only. Dynamic social networking sites, featuring regularly updated content, may be more advantageous than websites that retain static content over time. Trial Registration ClinicalTrials.gov NCT03363737; https://clinicaltrials.gov/ct2/show/NCT03363737 (Archived by WebCite at http://www.webcitation.org/6vXzNbOWJ) PMID:29222077

Oxidation of a Commercial Nickel-Based Superalloy under Static Loading

NASA Astrophysics Data System (ADS)

Foss, B. J.; Hardy, M. C.; Child, D. J.; McPhail, D. S.; Shollock, B. A.

2014-12-01

The current demands of the aviation industry for increased gas-turbine efficiency necessitate higher turbine entry temperatures, requiring that alloys exhibit superior oxidation resistance. The synergistic effects of oxidation and mechanical stresses pose a complex issue. The purpose of the current research was to examine the effects of stress on the oxidation and oxygen transport in a commercial nickel-based superalloy. Fine grain RR1000 in both polished and shot-peened conditions was studied for classic (zero load) and statically loaded conditions using integrated two-stage isotopic tracing combined with focused-ion-beam secondary ion mass spectrometry (FIB-SIMS). Cr2O3 external oxide formed with semicontinuous TiO2 above and below. Preferential grain boundary Al2O3 internal oxide formation, γ'-dissolution, and recrystallization occurred subsurface. Oxidation mechanisms were dominated by anionic/cationic growth in the external oxide with inward oxygen transport, initially through the partially unprotective external oxide, then along internal oxide/alloy interfaces. Loading did not influence the oxidation products formed but did bring about expedited oxidation kinetics and changes to the oxide morphology. The oxygen diffusivity D {O/ * } (×10-13 cm2s-1) ranged from 0.39 for the polished alloy to 3.7 for the shot-peened condition under compressive stress. Arguably, the most significant effects took place in the subsurface regions. Increased oxidation kinetics were attributed to the development of fast cation diffusion paths as the alloy deformed by creep.

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

PubMed Central

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

2018-01-01

20Mn5 steel is widely used in the manufacture of heavy hydro-generator shaft due to its good performance of strength, toughness and wear resistance. However, the hot deformation and recrystallization behaviors of 20Mn5 steel compressed under high temperature were not studied. In this study, the hot compression experiments under temperatures of 850–1200 °C and strain rates of 0.01/s–1/s are conducted using Gleeble thermal and mechanical simulation machine. And the flow stress curves and microstructure after hot compression are obtained. Effects of temperature and strain rate on microstructure are analyzed. Based on the classical stress-dislocation relation and the kinetics of dynamic recrystallization, a two-stage constitutive model is developed to predict the flow stress of 20Mn5 steel. Comparisons between experimental flow stress and predicted flow stress show that the predicted flow stress values are in good agreement with the experimental flow stress values, which indicates that the proposed constitutive model is reliable and can be used for numerical simulation of hot forging of 20Mn5 hollow steel ingot. PMID:29561826

A novel ultrafine-grained Fe−22Mn−0.6C TWIP steel with superior strength and ductility

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

Tian, Y.Z., E-mail: yztian@imr.ac.cn

A fully recrystallized ultrafine-grained (UFG) Fe−22wt.%Mn−0.6wt.%C twinning-induced plasticity (TWIP) steel with mean grain size of 576 nm was fabricated by cold rolling and annealing process. Tensile test showed that this UFG steel possessed high yield strength of 785 MPa, and unprecedented uniform elongation of 48%. The Hall-Petch relationship was verified from the coarse-grained (CG) regime to the ultrafine-grained (UFG) regime. The microstructures at specified tensile strains were characterized by electron backscattered diffraction (EBSD) and transmission electron microscopy (TEM). The microstructures and strain hardening behavior of the UFG TWIP steel were compared with the CG counterpart. The strong strain hardening capabilitymore » of the UFG steel is supposed to be responsible for the high strength and good ductility. - Highlights: • A fully recrystallized Fe−22Mn−0.6C TWIP steel with mean grain size of 576 nm was fabricated. • The ultrafine-grained (UFG) steel exhibits strong strain-hardening capability, excellent strength and ductility. • The Hall-Petch relationship is fitted well from the CG regime to the UFG regime.« 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

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.

Modification of solid-state property of sulfasalazine by using the supercritical antisolvent process

NASA Astrophysics Data System (ADS)

Wu, Wei-Yi; Su, Chie-Shaan

2017-02-01

In this study, the supercritical antisolvent (SAS) process was used to recrystallize an active pharmaceutical ingredient, sulfasalazine, to modify the solid-state properties including particle size, crystal habit and polymorphic form. Supercritical CO2 and tetrahydrofuran were used as the antisolvent and solvent, respectively. SAS results obtained from different operating temperatures (35, 45, 55 and 65 °C) were compared and discussed. The results indicate that at 55 °C, spherical sulfasalazine crystals were produced and that their mean particle size was micronized to approximately 1 μm. In addition, according to the analytical results of powder X-ray diffractometry (PXRD), a novel polymorphic form of sulfasalazine was obtained after SAS. Furthermore, the spectroscopic and thermal behavior of produced sulfasalazine crystals were also studied by Fourier transform infrared spectrometry (FTIR), differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). Finally, SAS results obtained from different operating temperature was discussed on the basis of the mixture critical point (MCP) of CO2 and tetrahydrofuran. Operation at slightly higher than the MCP is favorable for recrystallization of sulfasalazine through SAS. These results demonstrate that the SAS process is an efficient tool for controlling and modifying the solid-state property of sulfasalazine.

Dynamic XRD, Shock and Static Compression of CaF2

NASA Astrophysics Data System (ADS)

Kalita, Patricia; Specht, Paul; Root, Seth; Sinclair, Nicholas; Schuman, Adam; White, Melanie; Cornelius, Andrew; Smith, Jesse; Sinogeikin, Stanislav

2017-06-01

The high-pressure behavior of CaF2 is probed with x-ray diffraction (XRD) combined with both dynamic compression, using a two-stage light gas gun, and static compression, using diamond anvil cells. We use XRD to follow the unfolding of a shock-driven, fluorite to cotunnite phase transition, on the timescale of nanoseconds. The dynamic behavior of CaF2 under shock loading is contrasted with that under static compression. This work leverages experimental capabilities at the Advanced Photon Source: dynamic XRD and shock experiments at the Dynamic Compression Sector, as well as XRD and static compression in diamond anvil cell at the High-Pressure Collaborative Access Team. These experiments and cross-platform comparisons, open the door to an unprecedented understanding of equations of state and phase transitions at the microstructural level and at different time scales and will ultimately improve our capability to simulate the behavior of materials at extreme conditions. Sandia National Laboratories is a multi-mission laboratory managed and operated by Sandia Corporation, a wholly owned subsidiary of Lockheed Martin Corporation, for the U.S. Department of Energy's National Nuclear Security Administration under contract DE-AC04-94AL85000.

Experimental data of the static behavior of reinforced concrete beams at room and low temperature

PubMed Central

Mirzazadeh, M. Mehdi; Noël, Martin; Green, Mark F.

2016-01-01

This article provides data on the static behavior of reinforced concrete at room and low temperature including, strength, ductility, and crack widths of the reinforced concrete. The experimental data on the application of digital image correlation (DIC) or particle image velocimetry (PIV) in measuring crack widths and the accuracy and precision of DIC/PIV method with temperature variations when is used for measuring strains is provided as well. PMID:27158650

Dynamic mechanical characterization of aluminum: analysis of strain-rate-dependent behavior

NASA Astrophysics Data System (ADS)

Rahmat, Meysam

2018-05-01

A significant number of materials show different mechanical behavior under dynamic loads compared to quasi-static (Salvado et al. in Prog. Mater. Sci. 88:186-231, 2017). Therefore, a comprehensive study of material dynamic behavior is essential for applications in which dynamic loads are dominant (Li et al. in J. Mater. Process. Technol. 255:373-386, 2018). In this work, aluminum 6061-T6, as an example of ductile alloys with numerous applications including in the aerospace industry, has been studied under quasi-static and dynamic tensile tests with strain rates of up to 156 s^{-1}. Dogbone specimens were designed, instrumented and tested with a high speed servo-hydraulic load frame, and the results were validated with the literature. It was observed that at a strain rate of 156 s^{-1} the yield and ultimate strength increased by 31% and 33% from their quasi-static values, respectively. Moreover, the failure elongation and fracture energy per unit volume also increased by 18% and 52%, respectively. A Johnson-Cook model was used to capture the behavior of the material at different strain rates, and a modified version of this model was presented to enhance the capabilities of the original model, especially in predicting material properties close to the failure point. Finally, the fracture surfaces of specimens tested under quasi-static and dynamic loads were compared and conclusions about the differences were drawn.

Stress in recrystallized quartz by electron backscatter diffraction mapping

NASA Astrophysics Data System (ADS)

Llana-Fúnez, S.

2017-07-01

The long-term state of stress at middle and lower crustal depths can be estimated through the study of the microstructure of exhumed rocks from active and/or ancient shear zones. Constitutive equations for deformation mechanisms in experimentally deformed rocks relate differential stress to the size of recrystallized grains. Cross et al. (2017) take advantage of electron backscatter diffraction mapping to systematically separate new recrystallized grains from host grains on the basis of the measurable lattice distorsion within the grains. They produce the first calibrated piezometer for quartz with this technique, reproducing within error a previous calibration based on optical microscopy.

Application of two-level factorial design to investigate the effect of process parameters on the sonocrystallization of sulfathiazole

NASA Astrophysics Data System (ADS)

Kuo, Peng-Hsuan; Zhang, Bo-Cong; Su, Chie-Shaan; Liu, Jun-Jen; Sheu, Ming-Thau

2017-08-01

In this study, cooling sonocrystallization was used to recrystallize an active pharmaceutical ingredient, sulfathiazole, using methanol as the solvent. The effects of three operating parameters-sonication intensity, sonication duration, and solution concentration-on the recrystallization were investigated by using a 2k factorial design. The solid-state properties of sulfathiazole, including the mean particle size, crystal habit, and polymorphic form, were analyzed. Analysis of variance showed that the effect of the sonication intensity, cross-interaction effect of sonication intensity/sonication duration, and cross-interaction effect of sonication intensity/solution concentration on the recrystallization were significant. The results obtained using the 2k factorial design indicated that a combination of high sonication intensity and long sonication duration is not favorable for sonocrystallization, especially at a high solution concentration. A comparison of the solid-state properties of the original and the recrystallized sulfathiazole revealed that the crystal habit of the recrystallized sulfathiazole was more regular and that its mean particle size could be reduced to approximately 10 μm. Furthermore, the analytical results obtained using the PXRD, DSC, and FTIR spectroscopy indicated that the polymorphic purity of sulfathiazole improved from the original Form III/IV mixture to Form III after sonocrystallization.

Microstructure study of a severely plastically deformed Mg-Zn-Y alloy by application of low angle annular dark field diffraction contrast imaging.

PubMed

Basha, Dudekula Althaf; Rosalie, Julian M; Somekawa, Hidetoshi; Miyawaki, Takashi; Singh, Alok; Tsuchiya, Koichi

2016-01-01

Microstructural investigation of extremely strained samples, such as severely plastically deformed (SPD) materials, by using conventional transmission electron microscopy techniques is very challenging due to strong image contrast resulting from the high defect density. In this study, low angle annular dark field (LAADF) imaging mode of scanning transmission electron microscope (STEM) has been applied to study the microstructure of a Mg-3Zn-0.5Y (at%) alloy processed by high pressure torsion (HPT). LAADF imaging advantages for observation of twinning, grain fragmentation, nucleation of recrystallized grains and precipitation on second phase particles in the alloy processed by HPT are highlighted. By using STEM-LAADF imaging with a range of incident angles, various microstructural features have been imaged, such as nanoscale subgrain structure and recrystallization nucleation even from the thicker region of the highly strained matrix. It is shown that nucleation of recrystallized grains starts at a strain level of revolution [Formula: see text] (earlier than detected by conventional bright field imaging). Occurrence of recrystallization of grains by nucleating heterogeneously on quasicrystalline particles is also confirmed. Minimizing all strain effects by LAADF imaging facilitated grain size measurement of [Formula: see text] nm in fully recrystallized HPT specimen after [Formula: see text].

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

NASA Astrophysics Data System (ADS)

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

1998-06-01

In Part II of this article, the experimental work undertaken to measure the effect of deformation parameters (temperature, strain, and strain rate) on the texture formation during hot deformation and the evolution during subsequent recrystallization is described. In addition, the isothermal kinetics of development of individual texture components were also determined. A neutron diffractometer was used to measure the texture in the as-hot-deformed aluminum samples, and the samples were then heat treated in a 400 °C salt bath for various lengths of time, with the texture being remeasured at various stages in the recrystallization process. Using data from the experimental program, the texture evolution during recrystallization was modeled by applying a modified form of the Avrami equation. Results indicated that, of the deformation parameters studied, textural development was most sensitive to the deformation temperature for both alloys. In addition, modeling results revealed that the Cu component ({112} <111>) was the first to recrystallize, typically followed by the S ({123} <634>) and Bs ({110} <112>) components. This is in agreement with earlier work which indicated that the Bs component was the hardest to recrystallize, possibly because it is able to deform on very few slip systems and, hence, the dislocation interaction may be low.

Measurement of process-dependent material properties of pharmaceutical solids by nanoindentation.

PubMed

Liao, Xiangmin; Wiedmann, Timothy Scott

2005-01-01

The purpose of this work was to evaluate nanoindentation as a means to characterize the material properties of pharmaceutical solids. X-ray diffraction of potassium chloride and acetaminophen showed that samples prepared by cooling a melt to a crystalline sample as opposed to slow recrystallization had the same crystal structure. With analysis of the force-displacement curves, the KCl quenched samples had a hardness that was 10 times higher than the recrystallized KCl, while acetaminophen quenched samples were 25% harder than the recrystallized samples. The elastic moduli of the quenched samples were also much greater than that observed for the recrystallized samples. Although the elasticity was independent of load, the hardness increased with load for acetaminophen. With each sample, the flow at constant load increased with applied load. Etching patterns obtained by atomic force microscopy showed that the KCl quenched sample had a higher dislocation density than the recrystallized sample, although there was no evident difference in the acetaminophen samples. Overall, the differences in the observed sample properties may be related to the dislocation density. Thus, nanoindentation has been shown to be a sensitive method for determining a processed-induced change in the hardness, creep, and elasticity of KCl and acetaminophen. (c) 2004 Wiley-Liss, Inc.

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.

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

Attentional synchrony and the influence of viewing task on gaze behavior in static and dynamic scenes.

PubMed

Smith, Tim J; Mital, Parag K

2013-07-17

Does viewing task influence gaze during dynamic scene viewing? Research into the factors influencing gaze allocation during free viewing of dynamic scenes has reported that the gaze of multiple viewers clusters around points of high motion (attentional synchrony), suggesting that gaze may be primarily under exogenous control. However, the influence of viewing task on gaze behavior in static scenes and during real-world interaction has been widely demonstrated. To dissociate exogenous from endogenous factors during dynamic scene viewing we tracked participants' eye movements while they (a) freely watched unedited videos of real-world scenes (free viewing) or (b) quickly identified where the video was filmed (spot-the-location). Static scenes were also presented as controls for scene dynamics. Free viewing of dynamic scenes showed greater attentional synchrony, longer fixations, and more gaze to people and areas of high flicker compared with static scenes. These differences were minimized by the viewing task. In comparison with the free viewing of dynamic scenes, during the spot-the-location task fixation durations were shorter, saccade amplitudes were longer, and gaze exhibited less attentional synchrony and was biased away from areas of flicker and people. These results suggest that the viewing task can have a significant influence on gaze during a dynamic scene but that endogenous control is slow to kick in as initial saccades default toward the screen center, areas of high motion and people before shifting to task-relevant features. This default-like viewing behavior returns after the viewing task is completed, confirming that gaze behavior is more predictable during free viewing of dynamic than static scenes but that this may be due to natural correlation between regions of interest (e.g., people) and motion.

Compression Behavior and Energy Absorption of Aluminum Alloy AA6061 Tubes with Multiple Holes

NASA Astrophysics Data System (ADS)

Simhachalam, Bade; Lakshmana Rao, C.; Srinivas, Krishna

2014-05-01

In this article, compression behavior and energy absorption of aluminum alloy AA6061 tubes are investigated both experimentally and numerically. Static and dynamic simulations are done using LS-Dyna Software for AA6061 tubes. True stress-plastic strain curves from the tensile test are used in the static and dynamic simulations of AA6061 tubes. The energy absorption values between experimental compression results and numeral simulation are found to be in good agreement. Dynamic simulations are done with drop velocity of up to 10 m/s to understand the inertia effects on energy absorption. The deformed modes from the numerical simulation are compared between tubes with and without holes in static and dynamic conditions.

Prediction of Ductile Fracture Behaviors for 42CrMo Steel at Elevated Temperatures

NASA Astrophysics Data System (ADS)

Lin, Y. C.; Liu, Yan-Xing; Liu, Ge; Chen, Ming-Song; Huang, Yuan-Chun

2015-01-01

The ductile fracture behaviors of 42CrMo steel are studied by hot tensile tests with the deformation temperature range of 1123-1373 K and strain rate range of 0.0001-0.1 s-1. Effects of deformation temperature and strain rate on the flow stress and fracture strain of the studied steel are discussed in detail. Based on the experimental results, a ductile damage model is established to describe the combined effects of deformation temperature and strain rate on the ductile fracture behaviors of 42CrMo steel. It is found that the flow stress first increases to a peak value and then decreases, showing an obvious dynamic softening. This is mainly attributed to the dynamic recrystallization and material intrinsic damage during the hot tensile deformation. The established damage model is verified by hot forging experiments and finite element simulations. Comparisons between the predicted and experimental results indicate that the established ductile damage model is capable of predicting the fracture behaviors of 42CrMo steel during hot forging.

Biosignatures in the Recrystallized Shock Melt Pocket of ALH-77005 Shergottite — Clues to Martian Life

NASA Astrophysics Data System (ADS)

Gyollai, I.; Polgári, M.; Bérczi, Sz.; Gucsik, A.; Pál-Molnár, E.

2017-11-01

In the spinifex textured, recrystallized shock melt portion in ALH 77005 shergottite mineralized microbially produced texture (MMPT) - in form of pearl necklace-like, vermiform inner signatures - was measured, which we propose to have Martian origin.

Dynamic stiffness characteristics of high eccentricity ratio bearings and seals by perturbation testing

NASA Technical Reports Server (NTRS)

Bently, D. E.; Muszynska, A.

1984-01-01

The complex behavior of cylindrical bearings and seals that are statically loaded to eccentricities in excess of 0.7 are examined. The stiffness algorithms as a function of static load are developed from perturbation methodology by empirical modeling.

Fatigue and shear behavior of HPC bulb tee girders : LTRC technical summary report.

DOT National Transportation Integrated Search

2008-04-01

The objectives of the research were (1) to provide assurance that full size, deep prestressed concrete girders made with HPC would perform satisfactorily under flexural fatigue, static shear, and static flexural loading conditions; (2) to determine i...

Moisture-induced phase separation and recrystallization in amorphous solid dispersions.

PubMed

Luebbert, Christian; Sadowski, Gabriele

2017-10-30

Active Pharmaceutical Ingredients (APIs) are often dissolved in polymeric matrices to control the gastrointestinal dissolution and to stabilize the amorphous state of the API. During the pharmaceutical development of new formulations, stability studies via storage at certain temperature and relative humidity (RH) have to be carried out to verify the long-term thermodynamic stability of these formulations against unwanted recrystallization and moisture-induced amorphous-amorphous phase separation (MIAPS). This study focuses on predicting the MIAPS of API/polymer formulations at elevated RH. In a first step, the phase behavior of water-free formulations of ibuprofen (IBU) and felodipine (FEL) combined with the polymers poly(vinyl pyrrolidone) (PVP), poly(vinyl acetate) (PVAC) and poly (vinyl pyrrolidone-co-vinyl acetate) (PVPVA64) was determined experimentally by differential scanning calorimetry (DSC). The phase behavior of these water-free formulations was modeled using the Perturbed-Chain Statistical Associating Fluid Theory (PC-SAFT). Based on this, the API solubility and MIAPS in the above-mentioned formulations at humid conditions was predicted in perfect agreement with the results of two-year lasting stability studies at 25°C/0% RH and 40°C/75% RH. MIAPS was predicted and also experimentally found for the FEL/PVP, FEL/PVPVA64 and IBU/PVP formulations, whereas MIAPS was neither predicted nor measured for the IBU/PVPVA64 system and PVAC-containing formulations. It was thus shown that the results of time-consuming long-term stability tests can be correctly predicted via thermodynamic modeling with PC-SAFT. Copyright © 2017 Elsevier B.V. All rights reserved.

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.

Toward a mechanistic understanding of the damage evolution of SnAgCu solder joints in accelerated thermal cycling test

NASA Astrophysics Data System (ADS)

Mahin Shirazi, Sam

Accelerated thermal cycling (ATC) tests are the most commonly used tests for the thermo-mechanical performance assessment of microelectronics assemblies. Currently used reliability models have failed to incorporate the microstructural dependency of lead free solder joint behavior and its microstructure evolution during cycling. Thus, it is essential to have a mechanistic understanding of the effect of cycling parameters on damage evolution and failure of lead free solder joints in ATC. Recrystallization has been identified as the damage rate controlling mechanism in ATC. Usually it takes 1/3 of life for completion of recrystallization regardless of cycling parameters. Thus, the life of the solder joints can be predicted by estimating global recrystallization. The objective of the first part of the study was to examine whether the damage scenario applies in service is the same as the harsh thermal cycling tests (i.e. 0/100 °C and -40/125 °C) commonly used in industry. Microstructure analysis results on a variety of lead free solder SnAgCu assemblies subjected to the both harsh (0/100 °C) and mild (20/80 °C) ATC confirmed similar failure mechanism under the both testing conditions. Sn grain morphology (interlaced versus beach ball) has a significant effect on the thermo-mechanical performance (and thus the model) of the lead free solder joints. The longer thermal cycling lifetime observed in the interlaced solder joints subjected to the ATC compared to the beach ball structure was correlated to the different initial microstructure and the microstructure evolution during cycling. For the modeling proposes, the present study was focused on Sn-Ag-Cu solder joints with either a single Sn grain or beach ball structure. Microstructural analysis results of the simulated thermal cycling experiment revealed that, the life can be approximated as determined by the accumulation of a certain amount of work during the high temperature dwells. Finally the effect of precipitates spacing on acceleration factor was investigated. Results indicated that a smaller initial precipitate spacing would tend to result in a longer life in mild thermal cycling/service (where there is lower stresses). Accordingly, it is essential to incorporate the dependence of damage rate (i.e. recrystallization) on precipitate coarsening in any predictions.

Predicting the Kinetics of Ice Recrystallization in Aqueous Sugar Solutions

PubMed Central

2018-01-01

The quality of stored frozen products such as foods and biomaterials generally degrades in time due to the growth of large ice crystals by recrystallization. While there is ample experimental evidence that recrystallization within such products (or model systems thereof) is often dominated by diffusion-limited Ostwald ripening, the application of Ostwald-ripening theories to predict measured recrystallization rates has only met with limited success. For a model system of polycrystalline ice within an aqueous solution of sugars, we here show recrystallization rates can be predicted on the basis of Ostwald ripening theory, provided (1) the theory accounts for the fact the solution can be nonideal, nondilute and of different density than the crystals, (2) the effect of ice-phase volume fraction on the diffusional flux of water between crystals is accurately described, and (3) all relevant material properties (involving binary Fick diffusion coefficients, the thermodynamic factor of the solution, and the surface energy of ice) are carefully estimated. To enable calculation of material properties, we derive an alternative formulation of Ostwald ripening in terms of the Maxwell–Stefan instead of the Fick approach to diffusion. First, this leads to a cancellation of the thermodynamic factor (a measure for the nonideality of a solution), which is a notoriously difficult property to obtain. Second, we show that Maxwell–Stefan diffusion coefficients can to a reasonable approximation be related to self-diffusion coefficients, which are relatively easy to measure or predict in comparison to Fick diffusion coefficients. Our approach is validated for a binary system of water and sucrose, for which we show predicted recrystallization rates of ice compare well to experimental results, with relative deviations of at most a factor of 2. PMID:29651228

Predicting the Kinetics of Ice Recrystallization in Aqueous Sugar Solutions.

PubMed

van Westen, Thijs; Groot, Robert D

2018-04-04

The quality of stored frozen products such as foods and biomaterials generally degrades in time due to the growth of large ice crystals by recrystallization. While there is ample experimental evidence that recrystallization within such products (or model systems thereof) is often dominated by diffusion-limited Ostwald ripening, the application of Ostwald-ripening theories to predict measured recrystallization rates has only met with limited success. For a model system of polycrystalline ice within an aqueous solution of sugars, we here show recrystallization rates can be predicted on the basis of Ostwald ripening theory, provided (1) the theory accounts for the fact the solution can be nonideal, nondilute and of different density than the crystals, (2) the effect of ice-phase volume fraction on the diffusional flux of water between crystals is accurately described, and (3) all relevant material properties (involving binary Fick diffusion coefficients, the thermodynamic factor of the solution, and the surface energy of ice) are carefully estimated. To enable calculation of material properties, we derive an alternative formulation of Ostwald ripening in terms of the Maxwell-Stefan instead of the Fick approach to diffusion. First, this leads to a cancellation of the thermodynamic factor (a measure for the nonideality of a solution), which is a notoriously difficult property to obtain. Second, we show that Maxwell-Stefan diffusion coefficients can to a reasonable approximation be related to self-diffusion coefficients, which are relatively easy to measure or predict in comparison to Fick diffusion coefficients. Our approach is validated for a binary system of water and sucrose, for which we show predicted recrystallization rates of ice compare well to experimental results, with relative deviations of at most a factor of 2.

Indentation-flexure and low-velocity impact damage in graphite/epoxy laminates

NASA Technical Reports Server (NTRS)

Kwon, Young S.; Sankar, Bhavani V.

1992-01-01

Static indentation and low velocity impact tests were performed on quasi-isotropic and cross ply graphite/epoxy composite laminates. The load deflection relations in static tests and impact force history in the impact tests were recorded. The damage was assessed by using ultrasonic C-scanning and photomicrographic techniques. The static behavior of the laminates and damage progression during loading, unloading, and reloading were explained by a simple plate delamination model. A good correlation existed between the static and impact responses. It was found that results from a few static indentation-flexture tests can be used to predict the response and damage in composite laminates due to a class of low velocity impact events.

Fabric and texture at Siple Dome, Antarctica

USGS Publications Warehouse

Diprinzio, C.L.; Wilen, Lawrence A.; Alley, R.B.; Fitzpatrick, J.J.; Spencer, M.K.; Gow, A.J.

2005-01-01

Preferred c-axis orientations are present in the firn at Siple Dome, West Antarctica, and recrystallization begins as shallow as 200 m depth in ice below -20??C, based on digital analysis of c-axis fabrics, grain-sizes and other characteristics of 52 vertical thin sections prepared in the field from the kilometer-long Siple Dome ice core. The shallowest section analyzed, from 22 m, shows clustering of c axes toward the vertical. By 200 m depth, girdle fabric and other features of recrystallized ice are evident in layers (or regions), separated by layers (regions) of typically finer-grained ice lacking evidence of recrystallization. Ice from about 700-780 m depth, which was deposited during the last ice age, is especially fine-grained, with strongly vertical c axes, but deeper ice shows much larger crystals and strong evidence of recrystallization. Azimuthal asymmetry of some c-axis fabrics, trends in grain-size, and other indicators reveal additional information on processes and history of ice flow at Siple Dome.

Effect of Thermomechanical Processing on Texture and Superelasticity in Fe-Ni-Co-Al-Ti-B Alloy

NASA Astrophysics Data System (ADS)

Lee, Doyup; Omori, Toshihiro; Han, Kwangsik; Hayakawa, Yasuyuki; Kainuma, Ryosuke

2018-03-01

The texture and superelasticity were investigated in austenitic Fe-Ni-Co-Al-Ti-B alloy with various reduction ratios of cold rolling and heating ratios in annealing. The rolled sheets show the {110} <112> deformation texture at a reduction ratio higher than 80%, while the texture hardly changes in the primary recrystallization at 1000 °C. The β (B2) precipitates inhibit the grain growth at this temperature, but they dissolve during heating, and secondary recrystallization occurs due to decreased pinning force at temperatures higher than 1100 °C, resulting in texture change to {210} <001> . The recrystallization texture is more strongly developed when the reduction ratio and heating rate are high and slow, respectively. The 90% cold-rolled and slowly heated sheet shows the recrystallization texture and high fraction of low-angle boundaries. As a result, ductility and superelasticity can be drastically improved in the 90% cold-rolled sheet, although superelasticity was previously obtained only in thin sheets with 98.5% reduction.

A study of the oxide dispersion and recrystallization in NiCrAl prepared from preoxidized powder

NASA Technical Reports Server (NTRS)

Glasgow, T. K.

1975-01-01

The sintered aluminum powder (SAP) technique of dispersion strengthening (formation of an oxide dispersion by preoxidation of metal powders) was applied to atomized powder of a nickel alloy containing, by weight, 17% Cr, 5% Al, and 0.2% Y. The SAP-NiCrAl alloy (without the ytterbium removed by oxdation) was worked by extrusion and rod rolling at 1205 C and by swaging at 760 C. Annealing treatments were applied after working to determine the recrystallization response. The NiCrAlY alloy, similarly prepared from atomized powder, but without a preoxidation treatment, was examined for comparison. The SAP-NiCrAl alloy exhibited oxide particle size and spacing much larger than that usually observed in oxide dispersion strengthened alloys; nonetheless, it was possible to achieve abnormal (secondary) recrystallization in the SAP-NiCrAl alloy as has been reported for other oxide dispersion strengthened alloys. In contrast, the unoxidized NiCrAlY alloy exhibited only primary recrystallization.

Experiments and modeling to characterize microstructure and hardness in 304L

DOE PAGES

Deibler, Lisa Anne; Brown, Arthur; Puskar, Joseph D.

2017-01-12

Drawn 304L stainless steel tubing was subjected to 42 different annealing heat treatments with the goal of initializing a microstructural model to select a heat treatment to soften the tubing from a hardness of 305 Knoop to 225–275 Knoop. The amount of recrystallization and grain size caused by 18 heat treatments were analyzed via optical microscopy and image analysis, revealing the full range of recrystallization from 0 to 100%. The formation of carbides during the longer duration and higher-temperature heat treatments was monitored via transmission electron microscope evaluation. The experimental results informed a model which includes recovery, recrystallization, and grainmore » growth to predict microstructure and hardness. After initialization of the model, it was able to predict hardness with a R 2 value of 0.95 and recrystallization with an R 2 value of 0.99. As a result, the model was then utilized in the design and testing of a heat treatment to soften the tubing.« less

A method for the monitoring of metal recrystallization based on the in-situ measurement of the elastic energy release using neutron diffraction

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

Christien, F., E-mail: frederic.christien@univ-nantes.fr; Le Gall, R.; Telling, M. T. F.

2015-05-15

A method is proposed for the monitoring of metal recrystallization using neutron diffraction that is based on the measurement of stored energy. Experiments were performed using deformed metal specimens heated in-situ while mounted at the sample position of the High Resolution Powder Diffractometer, HRPD (ISIS Facility), UK. Monitoring the breadth of the resulting Bragg lines during heating not only allows the time-dependence (or temperature-dependence) of the stored energy to be determined but also the recrystallized fraction. The analysis method presented here was developed using pure nickel (Ni270) specimens with different deformation levels from 0.29 to 0.94. In situ temperature rampingmore » as well as isothermal annealing was undertaken. The method developed in this work allows accurate and quantitative monitoring of the recrystallization process. The results from neutron diffraction are satisfactorily compared to data obtained from calorimetry and hardness measurements.« less

Shock-induced fine-grained recrystallization of olivine - Evidence against subsolidus reduction of Fe/2+/

NASA Technical Reports Server (NTRS)

Ahrens, T. J.; Tsay, F.-D.; Live, D. H.

1976-01-01

Electron spin resonance (ESR) studies have been carried out on three single grains of terrestrial olivine (Fo90) shock loaded along the 010 line to peak pressures of 280, 330, and 440 kbar. The results indicate that neither metallic Fe similar to that observed in returned lunar soils nor paramagnetic Fe(3+) caused by oxidation of Fe(2+) has been produced in these shock experiments. Trace amounts of Mn (2+) have been detected in both shocked and unshocked olivine. The ESR signals of Mn(2+) show spectral features which are found to correlate with the degree of shock-induced recrystallization observed petrographically. The increasing mass fraction of recrystallized olivine correlates with increasing shock pressures. This phenomenon is modelled assuming it results from the progressive effect of the shock-induced transformation of the olivine to a yet unknown high-pressure phase and its subsequent reversion to the low-pressure olivine phase. The mass fraction of recrystallized material is predicted to be nearly linear with shock pressure.

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

PubMed

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

2018-05-23

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

Learning Enterprise Malware Triage from Automatic Dynamic Analysis

DTIC Science & Technology

2013-03-01

Kolter and Maloof n-gram method, Dube’s malware target recognition (MaTR) static method performs significantly more accurately at the 95% confidence...from the static method as in Kolter and Maloof. The MIST approach with behavior sequences 9 allows researchers to tailor the level of analysis to the...citations, none publish work that implements it. Only Kolter and Maloof use nearly as long gram structures, although that research uses static grams rather

Static Holdup of Liquid Slag in Simulated Packed Coke Bed Under Oxygen Blast Furnace Ironmaking Conditions

NASA Astrophysics Data System (ADS)

Wang, Guang; Liu, Yingli; Zhou, Zhenfeng; Wang, Jingsong; Xue, Qingguo

2018-01-01

The liquid-phase flow behavior of slag in the lower zone of a blast furnace affects the furnace permeability, performance, and productivity. The effects of pulverized coal injection (PCI) on the behavior of simulated primary slag flow were investigated by quantifying the effect of key variables including Al/Si ratio [Al2O3 (wt.%) to SiO2 (wt.%)] and the amount of unburnt pulverized coal (UPC) at 1500°C. Viscosity analysis demonstrated that the slag fluidity decreased as the Al/Si ratio was increased (from 0.35 to 0.50), resulting in gradual increase of the static holdup. Increasing the amount of UPC resulted in a significant increase of the static holdup. Flooding analysis was applied to determine the maximum static holdup, which was found to be 11.5%. It was inferred that the burnout rates of pulverized coal should exceed 78.6% and 83.9% in traditional and oxygen blast furnaces, respectively.

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.

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.

Avian behavior and mortality at power lines in coastal South Carolina

USGS Publications Warehouse

Savereno, A.J.; Savereno, L.A.; Boettcher, R.; Haig, S.M.

1996-01-01

We compared avian behavior and mortality associated with two 115-kV transmission lines on the central South Carolina coast during 3,392 hours of observation from May 1991 through May 1994. One line was marked with 30-cm-diameter yellow aviation markers. The second line was unmarked, but was similar in most other aspects. We conducted ground searches (n = 445) beneath each line year-round to document avian mortality due to power-line collisions. At marked lines, birds that approached at line height changed behavior more at unmarked lines (P< 0.001), and fewer crossed between static and conductor wires. Collision rate was 53% lower at marked than unmarked lines. Among collisions at both sites, 82% of birds collided with static wires. Based on observed collisions and carcass recoveries, wading birds particularly appeared to be at risk. We concluded that aviation markers were effective at increasing line visibility and reducing collisions and recommend marking static wires of power lines in potentially sensitive areas.

Coarsening Kinetics and Morphological Evolution in a Two-Phase Titanium Alloy During Heat Treatment

NASA Astrophysics Data System (ADS)

Xu, Jianwei; Zeng, Weidong; Jia, Zhiqiang; Sun, Xin; Zhao, Yawei

2016-03-01

The effects of alpha/beta heat treatment on microstructure evolution of Ti-17 alloy with a lamellar colony structure are established. Heat treatment experiments are conducted at 1103 or 1063 K for times ranging from 10 min to 8 h. The main features of microstructure evolution during heat treatment comprise static globularization and coarsening of primary alpha phase. Such behaviors can be accelerated by higher heat treatment temperature. Furthermore, globularization and coarsening behaviors show a faster rate at higher prestrain. In order to better understand the microstructure evolution of Ti-17 alloy during alpha/beta heat treatment, static globularization and coarsening behaviors are modeled in the theoretical frame of the Johnson-Mehl-Avarmi-Kolmogorov (JMAK) and Lifshitz-Slyozov-Wagner (LSW) theories, respectively. The JMAK and LSW kinetics parameters are derived under different experimental conditions. Agreements between measurements and predictions are found, indicating that the JMAK and LSW theories can be used to predict and trace static globularization and coarsening processes of Ti-17 alloy during alpha/beta heat treatment.

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.

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

PubMed

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

2016-01-01

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

Evolution of quartz microstructure and c-axis crystallographic preferred orientation within ductilely deformed granitoids (Arolla unit, Western Alps)

NASA Astrophysics Data System (ADS)

Menegon, Luca; Pennacchioni, Giorgio; Heilbronner, Renee; Pittarello, Lidia

2008-11-01

We have studied quartz microstructures and the c-axis crystallographic preferred orientations (CPOs) in four granitoid samples representative of increasing ductile shear deformation, from a weakly deformed granitoid (stage 1) to a mylonitic granitoid (stage 4). The quartz c-axis CPO measured in the mylonitic granitoid has been compared with the one observed in a fully recrystallized quartz mylonite from the same area. All the samples belong to the Austroalpine Arolla unit (Western Alps) and were deformed at greenschist facies conditions. The quartz c-axis CPO was analyzed using a U-stage and the optical orientation imaging technique. The magmatic plagioclase, forming more than 50% of the volume of the granitoid, is extensively replaced by a mica-rich aggregate even in weakly deformed samples of stage 1. These aggregates flow to form an interconnected weak matrix with increasing deformation, wrapping relatively less strained quartz grains that undergo dominantly coaxial strain. Recrystallization of quartz ranges from less than 1% in the weakly deformed granitoid to up to 85% in the mylonitic granitoid, with average grain strain of 41% and 64%, respectively. With increasing strain and recrystallization, quartz grains in the granitoids show a sequence of transient microstructures and CPOs. Crystal plastic deformation is initially accomplished by dislocation glide with limited recovery, and at 50% grain strain it results in a CPO consistent with dominantly basal < a> slip. At 60% grain strain, recrystallization is preferentially localized along shear bands, which appear to develop along former intragranular cracks, and the recrystallized grains develop a strong c-axis CPO with maxima orthogonal to the shear band boundaries and independent of the host grain orientation. Within the granitoid mylonite, at an average quartz grain strain of 64%, recrystallization is extensive and the c-axis CPO of new grains displays maxima overlapping the host c-axis orientation and, therefore, unrelated to the bulk sense of shear. The host-controlled CPO is inferred to reflect pervasive recrystallization by progressive subgrain rotation. The switch from 'shear band-control' to 'host-control' on c-axis CPO occurred between 40% and 70% of recrystallization. In the quartz mylonite, the quartz c-axis CPO develops an asymmetric single girdle consistent with the bulk sense of shear and the synkinematic greenschist facies conditions. This study indicates that the CPO evolution of quartz may significantly differ in cases of polymineralic vs. monomineralic rocks under the same deformation conditions, if quartz in the polymineralic rock behaves as a 'strong' phase.

Ca. 400 Ma Recrystallization of Norwegian Ultrahigh-pressure Eclogites: an ion Microprobe and Chemical Abrasion Study

NASA Astrophysics Data System (ADS)

Root, D. B.; Mattinson, J. M.; Hacker, B. R.; Wooden, J. L.

2002-12-01

Understanding the formation and exhumation of the ultrahigh-pressure (UHP) rocks of western Norway hinges on precise determination of the time of eclogite recrystallization. Our study consists of SHRIMP analysis, in conjunction with CL imagery, of zircon from four UHP and high-pressure (HP) eclogites; and detailed TIMS analysis of zircon from two samples subjected to combined thermal annealing and multi-step chemical abrasion (CA). SHRIMP analyses of the Otnheim and Langenes eclogites yield Caledonian spot ages of ca. 400 Ma from zircon rims. CL imagery and Th/U ratios from the Langenes eclogite indicate formation of rims by recrystallization of inherited zircon. SHRIMP analysis of the UHP Flatraket eclogite yielded a broad range of apparently concordant Caledonian ages. CA analyses of two fractions yielded moderate Pb loss from the first (lowest T) steps; possible minor Pb loss or minor growth at 400 Ma from the second steps; and a 407-404 Ma cluster of slightly discordant 206Pb/238U ages, most likely free from Pb loss, from the remaining steps. We interpret the latter to reflect recrystallization of inherited zircon, with possible new growth, at ca. 400-395 Ma. Alternatively, the high-temperature CA steps could represent growth at 407-404 Ma, with apparent discordance due to intermediate daughter product effects. HP/UHP zircon recrystallization in the Flatraket eclogite is inferred from three lines of evidence: i) zircon occurs as inclusions in garnet, omphacite, breunnerite, dolomite, and quartz, as well as in symplectites after phengite and omphacite; ii) association of zircon with rutile implies zircon formation during HP breakdown of Zr-ilmenite; and iii) chondrite-normalized ICP-MS analyses of the CA steps reveal small Eu anomalies and shallow HREE profiles, indicating zircon recrystallization in the presence of garnet. CA analysis of the Verpeneset eclogite yielded distinctly discordant step ages from two steps comprising <90% of the sample, with 206Pb/238U ages of 408 and 414 Ma. CL imagery indicates incomplete recrystallization of inherited igneous zircon, in keeping with steep HREE profiles determined from chondrite-normalized ICP-MS analyses. Our zircon age of ca. 400-395 Ma for the Flatraket eclogite is significantly younger than the 425 Ma age often cited for western Norway eclogite recrystallization, implying, in conjunction with 390-385 Ma 40Ar/39Ar white mica cooling ages, faster rates of exhumation (ca. 15 km/m.y.), and weakening the link between UHP metamorphism and ophiolite emplacement at 430-425 Ma.

Factors controlling in vitro recrystallization of the Caulobacter crescentus paracrystalline S-layer.

PubMed Central

Nomellini, J F; Kupcu, S; Sleytr, U B; Smit, J

1997-01-01

The S-layer of Caulobacter is a two-dimensional paracrystalline array on the cell surface composed of a single protein, RsaA. We have established conditions for preparation of stable, soluble protein and then efficient in vitro recrystallization of the purified protein. Efficient recrystallization and long range order could not be obtained with pure protein only, though it was apparent that calcium was required for crystallization. Recrystallization was obtained when lipid vesicles were provided, but only when the vesicles contained the specific species of Caulobacter smooth lipopolysaccharide (SLPS) that previous studies implicated as a requirement for attaching the S-layer to the cell surface. The specific type of phospholipids did not appear critical; phospholipids rather different from those present in Caulobacter membranes or archaebacterial tetraether lipids worked equally well. The source of LPS was critical; rough and smooth variants of Salmonella typhimurium LPS as well as the rough form of Caulobacter LPS were ineffective. The requirement for calcium ions for recrystallization was further evaluated; strontium ions could substitute for calcium, and to a lesser extent, cobalt, barium, manganese and magnesium ions also stimulated crystallization. On the other hand, nickel and cadmium provided only weak crystallization stimulation, and zinc, copper, iron, aluminum ions, and the monovalent potassium, sodium, and lithium ions were ineffective. The recrystallization could also be reproduced with Langmuir-Blodgett lipid monolayers at an air-water interface. As with the vesicle experiments, this was only successful when SLPS was incorporated into the lipid mix. The best method for RsaA preparation, leading to apparently monomeric protein that was stable for many months, was an extraction with a low pH aqueous solution. We also achieved recrystallization, albeit at lower efficiency, using RsaA protein solubilized by 8 M urea, a method which allows retrieval of protein from inclusions, when expressed as heterologous protein in Escherichia coli or when retrieved as shed, precipitated protein from certain mutant caulobacters. In summary, the clarification of recrystallization methods has confirmed the requirement of SLPS as a surface attachment component and suggests that its presence in a membrane-like structure greatly stimulates the extent and quality of S-layer formation. The in vitro approach allowed the demonstration that specific ions are capable of participating in crystallization and now provides an assay for the crystallization potential of modified S-layer proteins, whether they were produced in or can be secreted by caulobacters. PMID:9335282

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.

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.

Ice Recrystallization in a Solution of a Cryoprotector and Its Inhibition by a Protein: Synchrotron X-Ray Diffraction Study.

PubMed

Zakharov, Boris; Fisyuk, Alexander; Fitch, Andy; Watier, Yves; Kostyuchenko, Anastasia; Varshney, Dushyant; Sztucki, Michael; Boldyreva, Elena; Shalaev, Evgenyi

2016-07-01

Ice formation and recrystallization is a key phenomenon in freezing and freeze-drying of pharmaceuticals and biopharmaceuticals. In this investigation, high-resolution synchrotron X-ray diffraction is used to quantify the extent of disorder of ice crystals in binary aqueous solutions of a cryoprotectant (sorbitol) and a protein, bovine serum albumin. Ice crystals in more dilute (10 wt%) solutions have lower level of microstrain and larger crystal domain size than these in more concentrated (40 wt%) solutions. Warming the sorbitol-water mixtures from 100 to 228 K resulted in partial ice melting, with simultaneous reduction in the microstrain and increase in crystallite size, that is, recrystallization. In contrast to sorbitol solutions, ice crystals in the BSA solutions preserved both the microstrain and smaller crystallite size on partial melting, demonstrating that BSA inhibits ice recrystallization. The results are consistent with BSA partitioning into quasi-liquid layer on ice crystals but not with a direct protein-ice interaction and protein sorption on ice surface. The study shows for the first time that a common (i.e., not-antifreeze) protein can have a major impact on ice recrystallization and also presents synchrotron X-ray diffraction as a unique tool for quantification of crystallinity and disorder in frozen aqueous systems. Copyright © 2016 American Pharmacists Association®. Published by Elsevier Inc. All rights reserved.

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

PubMed

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

2018-05-01

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

A study of microstructure, quasi-static response, fatigue, deformation and fracture behavior of high strength alloy steels

NASA Astrophysics Data System (ADS)

Kannan, Manigandan

The history of steel dates back to the 17th century and has been instrumental in the betterment of every aspect of our lives ever since, from the pin that holds the paper together to the Automobile that takes us to our destination steel touches everyone every day. Path breaking improvements in manufacturing techniques, access to advanced machinery and understanding of factors like heat treatment, corrosion resistance have aided in the advancement in the properties of steel in the last few years. In this dissertation document, the results of a study aimed at the influence of alloy chemistry, processing and influence of the quasi static and fatigue behavior of seven alloy steels is discussed. The microstructure of the as-received steel was examined and characterized for the nature and morphology of the grains and the presence of other intrinsic features in the microstructure. The tensile, cyclic fatigue and bending fatigue tests were done on a fully automated closed-loop servo-hydraulic test machine at room temperature. The failed samples of high strength steels were examined in a scanning electron microscope for understanding the fracture behavior, especially the nature of loading be it quasi static, cyclic fatigue or bending fatigue . The quasi static and cyclic fatigue fracture behavior of the steels examined coupled with various factors contributing to failure are briefly discussed in light of the conjoint and mutually interactive influences of intrinsic microstructural effects, nature of loading, and stress (load)-deformation-microstructural interactions.

Analysis of the behavior of a wiper blade around the reversal in consideration of dynamic and static friction

NASA Astrophysics Data System (ADS)

Unno, M.; Shibata, A.; Yabuno, H.; Yanagisawa, D.; Nakano, T.

2017-04-01

Reducing noise generated by automobile windshield wipers during reversals is a desirable feature. For this purpose, details of the behavior of the wiper blade need to be ascertained. In this study, we present theoretical and experimental clarification of this behavior during reversals. Using simulation algorithms to consider exactly the effects of dynamic and static friction, we determined theoretical predictions for the vibrational response caused by friction and the response frequency and compared these results with experimental ones obtained from a mock-up incorporating an actual wiper blade. We introduce an analytical link model with two degrees of freedom and consider two types of states at the blade tip. In the stick and the slip states, static friction and dynamic friction, respectively, act on the blade tip. In the theoretical approach, the static friction is expressed by a set-valued function. The transition between the two states is repeated and an evaluation of an exact transition time leads to an accurate prediction of the behavior of the wiper system. In the analysis, the slack variable method is used to find the exact transition time. Assuming low blade speeds during reversal, a parameter study indicates that the blade tip transitions between slip and stick states and the frequency of the vibration caused by this transitions is close to the natural frequency of the neck of the wiper blade. The theoretical predictions are in good agreement with experimental observations.

Measurements of Some Properties on Non-Hookean Springs.

ERIC Educational Resources Information Center

Lancaster, G.

1983-01-01

Describes an experiment in which static/dynamic properties of a helical, steel spring are investigated. During the experiment students discover that the behavior of the springs is non-Hookean at small loads. Background information (including static deflection and period of oscillation) and typical results are provided. (JM)

Study of Plastic Deformation in Binary Aluminum Alloys by Internal-Friction Methods

NASA Technical Reports Server (NTRS)

Olson, E. C.; Maringer, R. E.; Marsh, L. L.; Manning, G. K.

1959-01-01

The damping capacity of several aluminum-copper alloys has been investigated during tensile elongation. This damping is shown to depend on strain rate, strain, temperature, alloy content, and heat treatment. A tentative hypothesis, based on the acceleration of solute atom diffusion by deformation-produced vacancies, is proposed to account for the observed behavior. Internal-friction maxima are observed in deformed aluminum and aluminum-copper alloys at -70 deg and -50 deg C. The peaks appear to be relatively insensitive to frequency and alloy content, but they disappear after annealing at temperatures nearing the recrystallization temperature.

Mechanical Behavior and Microcrack Development in Nominally Dry Synthetic Salt-rock During Cyclic Loading

NASA Astrophysics Data System (ADS)

Ding, J.; Chester, F. M.; Chester, J. S.; Zhu, C.; Shen, X.; Arson, C. F.

2016-12-01

Synthetic salt-rock is produced through uniaxial consolidation of sieved granular salt (0.3-0.355 mm grain diam.) at 75-107 MPa pressure and 100-200 0 C for 15 min duration, to produce low porosity (3%-6%) aggregates. Based on microstructural observations, consolidation mechanisms are grain rearrangement, intragranular plastic flow, and minor microfracture and recrystallization. Following consolidation, the salt-rock is deformed by cyclic, triaxial loading at room temperature and 4 MPa confining pressure to investigate microfracture development, closure and healing effects on elastic properties and flow strength. Load cycles are performed within the elastic regime, up to yielding, and during steady ductile flow. The mechanical properties are determined using an internal load cell and strain gages bonded to the samples. Elastic properties vary systematically during deformation reflecting cracking and pore and grain shape changes. Between triaxial load cycles, samples are held at isostatic loads for durations up to one day to determine healing rates and strength recovery; a change in mechanical behavior is observed when significant healing is induced. The microstructures of all samples are characterized before and after cyclic loading using optical microscopy. The consolidation and cyclic triaxial tests, and optical microscopy investigations, are conducted in a controlled low-humidity environment to ensure nominally dry conditions. The microstructures of samples from different stages of cyclic triaxial deformation indicate that intracrystalline plasticity, accompanied by minor recovery by recrystallization, is dominant; but, grain-boundary crack opening also becomes significant. Grain-boundary microcracks have preferred orientations that are sub-parallel to the load axis. The stress-strain behavior correlates with microcrack fabrics and densities during cyclic loading. These experiments are used to both inform and test continuum damage mechanics models of salt-rock deformation in the semibrittle domain, as well as to help design and optimize salt-rock storage facilities.

Water Touch-and-Bounce from a Soft Viscoelastic Substrate: Wetting, Dewetting, and Rebound on Bitumen.

PubMed

Lee, Jae Bong; Dos Santos, Salomé; Antonini, Carlo

2016-08-16

Understanding the interaction between liquids and deformable solid surfaces is a fascinating fundamental problem, in which interaction and coupling of capillary and viscoelastic effects, due to solid substrate deformation, give rise to complex wetting mechanisms. Here we investigated as a model case the behavior of water drops on two smooth bitumen substrates with different rheological properties, defined as hard and soft (with complex shear moduli in the order of 10(7) and 10(5) Pa, respectively, at 1 Hz), focusing both on wetting and on dewetting behavior. By means of classical quasi-static contact angle measurements and drop impact tests, we show that the water drop behavior can significantly change from the quasi-static to the dynamic regime on soft viscoelastic surfaces, with the transition being defined by the substrate rheological properties. As a result, we also show that on the hard substrate, where the elastic response is dominant under all investigated conditions, classical quasi-static contact angle measurements provide consistent results that can be used to predict the drop dynamic wetting behavior, such as drop deposition or rebound after impact, as typically observed for nondeformable substrates. Differently, on soft surfaces, the formation of wetting ridges did not allow to define uniquely the substrate intrinsic advancing and receding contact angles. In addition, despite showing a high adhesion to the soft surface in quasi-static measurements, the drop was surprisingly able to rebound and escape from the surface after impact, as it is typically observed for hydrophobic surfaces. These results highlight that measurements of wetting properties for viscoelastic substrates need to be critically used and that wetting behavior of a liquid on viscoelastic surfaces is a function of the characteristic time scales.

The factor structure of static actuarial items: its relation to prediction.

PubMed

Barbaree, Howard E; Langton, Calvin M; Peacock, Edward J

2006-04-01

Principal components analysis was conducted on items contained in actuarial instruments used with adult sex offenders, including: the Rapid Assessment of Sex Offender Risk for Recidivism (RASORR), the Static-99, the Violence Risk Appraisal Guide (VRAG), the Sex Offender Risk Appraisal Guide (SORAG), and the Minnesota Sex Offender Screening Tool-Revised (MnSOST-R). In a data set that included child molesters and rapists (N = 311), six interpretable components were identified: Antisocial Behavior, Child Sexual Abuse, Persistence, Detached Predatory Behavior, Young and Single, and Male Victim(s). The RRASOR was highly correlated with Persistence, and the VRAG and SORAG were highly correlated with Antisocial Behavior. Antisocial Behavior was a significant predictor of violent recidivism, while Persistence and Child Sexual Abuse were significant predictors of sexual recidivism.

Dynamic Investigation of Static Divergence: Analysis and Testing

NASA Technical Reports Server (NTRS)

Heeg, Jennifer

2000-01-01

The phenomenon known as aeroelastic divergence is the focus of this work. The analyses and experiment presented here show that divergence can occur without a structural dynamic mode losing its oscillatory nature. Aeroelastic divergence occurs when the structural restorative capability or stiffness of a structure is overwhelmed by the static aerodynamic moment. This static aeroelastic coupling does not require the structural dynamic system behavior to cease, however. Aeroelastic changes in the dynamic mode behavior are governed not only by the stiffness, but by damping and inertial properties. The work presented here supports these fundamental assertions by examining a simple system: a typical section airfoil with only a rotational structural degree of freedom. Analytical results identified configurations that exhibit different types of dynamic mode behavior as the system encounters divergence. A wind tunnel model was designed and tested to examine divergence experimentally. The experimental results validate the analytical calculations and explicitly examine the divergence phenomenon where the dynamic mode persists. Three configurations of the wind tunnel model were tested. The experimental results agree very well with the analytical predictions of subcritical characteristics, divergence velocity, and behavior of the noncritical dynamic mode at divergence.

Knowledge Acquisition with Static and Animated Pictures in Computer-Based Learning.

ERIC Educational Resources Information Center

Schnotz, Wolfgang; Grzondziel, Harriet

In educational settings, computers provide specific possibilities of visualizing information for instructional purposes. Besides the use of static pictures, computers can present animated pictures which allow exploratory manipulation by the learner and display the dynamic behavior of a system. This paper develops a theoretical framework for…

Can Facebook Reduce Perceived Anxiety Among College Students? Randomized Controlled Exercise Trial Using the Transtheoretical Model of Behavior Change.

PubMed

Frith, Emily; Loprinzi, Paul

2017-12-08

Recent studies suggest social media may be an attractive strategy to promote mental health and wellness. There remains a need to examine the utility for individually tailored wellness messages posted to social media sites such as Facebook to facilitate positive psychological outcomes. Our aim was to extend the growing body of evidence supporting the potential for social media to enhance mental health. We evaluated the influence of an 8-week social media intervention on anxiety in college students and examined the impact of dynamic (active) versus static (passive) Facebook content on physical activity behaviors. Participants in the static group (n=21) accessed a Facebook page featuring 96 statuses. Statuses were intended to engage cognitive processes followed by behavioral processes of change per the transtheoretical model of behavior change. Content posted on the static Facebook page was identical to the dynamic page; however, the static group viewed all 96 statuses on the first day of the study, while the dynamic group received only 1 to 2 of these status updates per day throughout the intervention. Anxiety was measured using the Overall Anxiety Severity and Impairment Scale (OASIS). Time spent engaging in physical activity was assessed using the International Physical Activity Questionnaire (IPAQ). The OASIS change score for the dynamic Facebook group was statistically significant (P=.003), whereas the change score for the static group was not (P=.48). A statistically significant group-by-time interaction was observed (P=.03). The total IPAQ group-by-time interaction was not statistically significant (P=.06). We observed a decrease in anxiety and increase in total physical activity for the dynamic group only. Dynamic social networking sites, featuring regularly updated content, may be more advantageous than websites that retain static content over time. ClinicalTrials.gov NCT03363737; https://clinicaltrials.gov/ct2/show/NCT03363737 (Archived by WebCite at http://www.webcitation.org/6vXzNbOWJ). ©Emily Frith, Paul Loprinzi. Originally published in JMIR Mental Health (http://mental.jmir.org), 08.12.2017.

Fatigue Behavior of Steel Fiber Reinforced High-Strength Concrete under Different Stress Levels

NASA Astrophysics Data System (ADS)

Zhang, Chong; Gao, Danying; Gu, Zhiqiang

2017-12-01

The investigation was conducted to study the fatigue behavior of steel fiber reinforced high-strength concrete (SFRHSC) beams. A series of 5 SFRHSC beams was conducted flexural fatigue tests at different stress level S of 0.5, 0.55, 0.6, 0.7 and 0.8 respectively. Static test was conducted to determine the ultimate static capacity prior to fatigue tests. Fatigue modes and S-N curves were analyzed. Besides, two fatige life prediction model were analyzed and compared. It was found that stress level S significantly influenced the fatigue life of SFRHSC beams and the fatigue behavior of SFRHSC beams was mainly determined by the tensile reinforcement.

Boundary conditioning of capacitive MEMS devices through fabrication methods and operating environments

NASA Astrophysics Data System (ADS)

Muthukumaran, Packirisamy; Stiharu, Ion G.; Bhat, Rama B.

2003-10-01

This paper presents and applies the concept of micro-boundary conditioning to the design synthesis of microsystems in order to quantify the influence of inherent limitations of the fabrication process and the operating conditions on both static and dynamic behavior of microsystems. The predicted results on the static and dynamic behavior of a capacitive MEMS device, fabricated through MUMPs process, under the influence of the fabrication limitation and operating environment are presented along with the test results. The comparison between the predicted and experimental results shows a good agreement.

Unusual Thermoelectric Behavior Indicating a Hopping to Bandlike Transport Transition in Pentacene

NASA Astrophysics Data System (ADS)

Germs, W. Chr.; Guo, K.; Janssen, R. A. J.; Kemerink, M.

2012-07-01

An unusual increase in the Seebeck coefficient with increasing charge carrier density is observed in pentacene thin film transistors. This behavior is interpreted as being due to a transition from hopping transport in static localized states to bandlike transport, occurring at temperatures below ˜250K. Such a transition can be expected for organic materials in which both static energetic disorder and dynamic positional disorder are important. While clearly visible in the temperature and density dependent Seebeck coefficient, the transition hardly shows up in the charge carrier mobility.

Holographic fabrication of gratings in metal substrates

NASA Technical Reports Server (NTRS)

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

1982-01-01

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

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.

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

PubMed Central

Raychaudhuri, Arup Kumar; Saha-Dasgupta, Tanusri

2016-01-01

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

Analysis of Semiconductor Structures by Nuclear and Electrical Techniques.

DTIC Science & Technology

temperatures well below the Si-Al eutectic (577C), fine grained polycrystalline Si in contact with Al films recrystallizes in the Al matrix. The... recrystallization can be deferred or suppressed by placing a buffer layer of V or Ti between the Al film and poly Si. (2) When annealing Pt films deposited on Si

Manufacturing process to reduce large grain growth in zirconium alloys

DOEpatents

Rosecrans, Peter M.

1987-01-01

A method of treating cold-worked zirconium alloys to reduce large grain gth during thermal treatment at temperatures above the recrystallization temperature of the alloy comprising heating the cold-worked alloy between about 1300.degree.-1350.degree. F. for 1 to 3 hours prior to treatment above its recrystallization temperature.

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.

Gold Nanoparticle Aggregation as a Probe of Antifreeze (Glyco) Protein-Inspired Ice Recrystallization Inhibition and Identification of New IRI Active Macromolecules

NASA Astrophysics Data System (ADS)

Mitchell, Daniel E.; Congdon, Thomas; Rodger, Alison; Gibson, Matthew I.

2015-10-01

Antifreeze (glyco)proteins are found in polar fish species and act to slow the rate of growth of ice crystals; a property known as ice recrystallization inhibition. The ability to slow ice growth is of huge technological importance especially in the cryopreservation of donor cells and tissue, but native antifreeze proteins are often not suitable, nor easily available. Therefore, the search for new materials that mimic this function is important, but currently limited by the low-throughout assays associated with the antifreeze properties. Here 30 nm gold nanoparticles are demonstrated to be useful colorimetric probes for ice recrystallization inhibition, giving a visible optical response and is compatible with 96 well plates for high-throughout studies. This method is faster, requires less infrastructure, and has easier interpretation than the currently used ‘splat’ methods. Using this method, a series of serum proteins were identified to have weak, but specific ice recrystallization inhibition activity, which was removed upon denaturation. It is hoped that high-throughput tools such as this will accelerate the discovery of new antifreeze mimics.

Gold Nanoparticle Aggregation as a Probe of Antifreeze (Glyco) Protein-Inspired Ice Recrystallization Inhibition and Identification of New IRI Active Macromolecules

PubMed Central

Mitchell, Daniel E.; Congdon, Thomas; Rodger, Alison; Gibson, Matthew I.

2015-01-01

Antifreeze (glyco)proteins are found in polar fish species and act to slow the rate of growth of ice crystals; a property known as ice recrystallization inhibition. The ability to slow ice growth is of huge technological importance especially in the cryopreservation of donor cells and tissue, but native antifreeze proteins are often not suitable, nor easily available. Therefore, the search for new materials that mimic this function is important, but currently limited by the low-throughout assays associated with the antifreeze properties. Here 30 nm gold nanoparticles are demonstrated to be useful colorimetric probes for ice recrystallization inhibition, giving a visible optical response and is compatible with 96 well plates for high-throughout studies. This method is faster, requires less infrastructure, and has easier interpretation than the currently used ‘splat’ methods. Using this method, a series of serum proteins were identified to have weak, but specific ice recrystallization inhibition activity, which was removed upon denaturation. It is hoped that high-throughput tools such as this will accelerate the discovery of new antifreeze mimics. PMID:26499135

Gold Nanoparticle Aggregation as a Probe of Antifreeze (Glyco) Protein-Inspired Ice Recrystallization Inhibition and Identification of New IRI Active Macromolecules.

PubMed

Mitchell, Daniel E; Congdon, Thomas; Rodger, Alison; Gibson, Matthew I

2015-10-26

Antifreeze (glyco)proteins are found in polar fish species and act to slow the rate of growth of ice crystals; a property known as ice recrystallization inhibition. The ability to slow ice growth is of huge technological importance especially in the cryopreservation of donor cells and tissue, but native antifreeze proteins are often not suitable, nor easily available. Therefore, the search for new materials that mimic this function is important, but currently limited by the low-throughout assays associated with the antifreeze properties. Here 30 nm gold nanoparticles are demonstrated to be useful colorimetric probes for ice recrystallization inhibition, giving a visible optical response and is compatible with 96 well plates for high-throughout studies. This method is faster, requires less infrastructure, and has easier interpretation than the currently used 'splat' methods. Using this method, a series of serum proteins were identified to have weak, but specific ice recrystallization inhibition activity, which was removed upon denaturation. It is hoped that high-throughput tools such as this will accelerate the discovery of new antifreeze mimics.

Tensile Properties of Molybdenum and Tungsten from 2500 to 3700 F

NASA Technical Reports Server (NTRS)

Hall, Robert W.; Sikora, Paul F.

1959-01-01

Specimens of commercially pure sintered tungsten, arc-cast unalloyed molybdenum, and two arc-cast molybdenum-base alloys (one with 0.5 percent titanium, the other with 0.46 percent titanium and 0.07 percent zirconium) were fabricated from 1/2-inch-diameter rolled or swaged bars. All specimens were evaluated in short-time tensile tests in the as-received condition, and all except the molybdenum-titanium-zirconium alloy were tested after a 30-minute recrystallization anneal at 3800 F in a vacuum of approximately 0.1 micron. Results showed that the tungsten was considerably stronger than either the arc-cast unalloyed molybdenum or the molybdenum-base alloys over the 2500 to 3700 F temperature range. Recrystallization of swaged tungsten at 3800 F considerably reduced its tensile strength at 2500 F. However, above 3100 F, the as-swaged tungsten specimens recrystallized during testing, and had about the same strength as when recrystallized at 3800 F before evaluation. The ductility of molybdenum-base materials was very high at all test temperatures; the ductility of tungsten decreased sharply above about 3120 F.

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.

Fluid-rock interactions related to metamorphic reducing fluid flow in meta-sediments: example of the Pic-de-Port-Vieux thrust (Pyrenees, Spain)

NASA Astrophysics Data System (ADS)

Trincal, Vincent; Buatier, Martine; Charpentier, Delphine; Lacroix, Brice; Lanari, Pierre; Labaume, Pierre; Lahfid, Abdeltif; Vennemann, Torsten

2017-09-01

In orogens, shortening is mainly accommodated by thrusts, which constitute preferential zones for fluid-rock interactions. Fluid flow, mass transfer, and mineralogical reactions taking place along thrusts have been intensely investigated, especially in sedimentary basins for petroleum and uranium research. This study combines petrological investigations, mineralogical quantifications, and geochemical characterizations with a wide range of analytical tools with the aim of defining the fluid properties (nature, origin, temperature, and redox) and fluid-host rock interactions (mass transfers, recrystallization mechanisms, and newly formed synkinematic mineralization) in the Pic-de-Port-Vieux thrust fault zone (Pyrenees, Spain). We demonstrate that two geochemically contrasted rocks have been transformed by fluid flow under low-grade metamorphism conditions during thrusting. The hanging-wall Triassic red pelite was locally bleached, while the footwall Cretaceous dolomitic limestone was mylonitized. The results suggest that thrusting was accompanied by a dynamic calcite recrystallization in the dolomitic limestone as well as by leaching of iron via destabilization of iron oxides and phyllosilicate crystallization in the pelite. Geochemical and physical changes highlighted in this study have strong implications on the understanding of the thrust behavior (tectonic and hydraulic), and improve our knowledge of fluid-rock interactions in open fluid systems in the crust.

Dry Sliding Wear Behavior and Subsurface Microstructure Evolution of Mg97Zn1Y2 Alloy in a Wide Sliding Speed Range

NASA Astrophysics Data System (ADS)

An, J.; Xuan, X. H.; Zhao, J.; Sun, W.; Liang, C.

2016-12-01

The wear properties of Mg97Zn1Y2 alloy were investigated using the pin-on-disk wear machine within a load range of 20-380 N and a sliding speed range of 0.2-4.0 m/s. Analysis of worn surfaces using scanning electron microscope and energy-dispersive x-ray spectrometer revealed that wear mechanisms including abrasion + oxidation, delamination accompanied by heavy surface oxidation and delamination operated in mild wear regime, while wear mechanisms such as severe plastic deformation, severe plastic deformation accompanied by spallation of oxidation layer and surface melting prevailed in severe wear regime. The microstructural evolution and hardness change in subsurfaces were examined by optical microscopy and hardness tester. The transformation of surface material from the deformed into dynamic recrystallization (DRX) microstructure was observed before and after mild-to-severe transition. The reason for mild-to-severe wear transition was identified as the transformation of strain hardening to DRX softening in subsurface. Mg97Zn1Y2 alloy has a superior mild-to-severe wear transition resistance to AZ alloys because of its higher recrystallization temperature. A novel model for evaluating the critical surface temperature of mild-to-severe wear transition was established using DRX kinetics.

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.

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.

The Corrosion Characteristics and Tensile Behavior of Reinforcement under Coupled Carbonation and Static Loading

PubMed Central

Xu, Yidong

2015-01-01

This paper describes the non-uniform corrosion characteristics and mechanical properties of reinforcement under coupled action of carbonation and static loading. The two parameters, namely area-box (AB) value and arithmetical mean deviation (Ra), are adopted to characterize the corrosion morphology and pitting distribution from experimental observations. The results show that the static loading affects the corrosion characteristics of reinforcement. Local stress concentration in corroded reinforcement caused by tensile stress drives the corrosion pit pattern to be more irregular. The orthogonal test results from finite element simulations show that pit shape and pit depth are the two significant factors affecting the tensile behavior of reinforcement. Under the condition of similar corrosion mass loss ratio, the maximum plastic strain of corroded reinforcement increases with the increase of Ra and load time-history significantly. PMID:28793729

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.

Quasicrystal-reinforced Mg alloys.

PubMed

Kyun Kim, Young; Tae Kim, Won; Hyang Kim, Do

2014-04-01

The formation of the icosahedral phase (I-phase) as a secondary solidification phase in Mg-Zn-Y and Mg-Zn-Al base systems provides useful advantages in designing high performance wrought magnesium alloys. The strengthening in two-phase composites (I-phase + α -Mg) can be explained by dispersion hardening due to the presence of I-phase particles and by the strong bonding property at the I-phase/matrix interface. The presence of an additional secondary solidification phase can further enhance formability and mechanical properties. In Mg-Zn-Y alloys, the co-presence of I and Ca 2 Mg 6 Zn 3 phases by addition of Ca can significantly enhance formability, while in Mg-Zn-Al alloys, the co-presence of the I-phase and Mg 2 Sn phase leads to the enhancement of mechanical properties. Dynamic and static recrystallization are significantly accelerated by addition of Ca in Mg-Zn-Y alloy, resulting in much smaller grain size and more random texture. The high strength of Mg-Zn-Al-Sn alloys is attributed to the presence of finely distributed Mg 2 Sn and I-phase particles embedded in the α -Mg matrix.

Quasicrystal-reinforced Mg alloys

PubMed Central

Kyun Kim, Young; Tae Kim, Won; Hyang Kim, Do

2014-01-01

The formation of the icosahedral phase (I-phase) as a secondary solidification phase in Mg–Zn–Y and Mg–Zn–Al base systems provides useful advantages in designing high performance wrought magnesium alloys. The strengthening in two-phase composites (I-phase + α-Mg) can be explained by dispersion hardening due to the presence of I-phase particles and by the strong bonding property at the I-phase/matrix interface. The presence of an additional secondary solidification phase can further enhance formability and mechanical properties. In Mg–Zn–Y alloys, the co-presence of I and Ca2Mg6Zn3 phases by addition of Ca can significantly enhance formability, while in Mg–Zn–Al alloys, the co-presence of the I-phase and Mg2Sn phase leads to the enhancement of mechanical properties. Dynamic and static recrystallization are significantly accelerated by addition of Ca in Mg–Zn–Y alloy, resulting in much smaller grain size and more random texture. The high strength of Mg–Zn–Al–Sn alloys is attributed to the presence of finely distributed Mg2Sn and I-phase particles embedded in the α-Mg matrix. PMID:27877660

Equal channel angular extrusion for bulk processing of Fe–Co–2V soft magnetic alloys, part II: Texture analysis and magnetic properties

DOE PAGES

Kustas, Andrew B.; Michael, Joseph R.; Susan, Don F.; ...

2018-06-04

In Part I, equal channel angular extrusion (ECAE) was demonstrated as a novel, simple-shear deformation process for producing bulk forms of the low ductility Fe–Co–2V (Hiperco 50A®) soft ferromagnetic alloy with refined grain sizes. Microstructures and mechanical properties were discussed. In this Part II contribution, the crystallographic textures and quasi-static magnetic properties of ECAE-processed Hiperco were characterized. The textures were of a simple-shear character defined by partial {110} and <111> fibers inclined relative to the extrusion direction, in agreement with the expectations for simple-shear deformation textures of BCC metals. These textures were observed throughout all processing conditions and only slightlymore » reduced in intensity by subsequent recrystallization heat treatments. Characterization of the magnetic properties revealed a lower coercivity and higher permeability for ECAE-processed Hiperco specimens relative to the conventionally processed and annealed Hiperco bar. In conclusion, the effects of the resultant microstructure and texture on the coercivity and permeability magnetic properties are discussed.« less

Equal channel angular extrusion for bulk processing of Fe–Co–2V soft magnetic alloys, part II: Texture analysis and magnetic properties

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

Kustas, Andrew B.; Michael, Joseph R.; Susan, Don F.

In Part I, equal channel angular extrusion (ECAE) was demonstrated as a novel, simple-shear deformation process for producing bulk forms of the low ductility Fe–Co–2V (Hiperco 50A®) soft ferromagnetic alloy with refined grain sizes. Microstructures and mechanical properties were discussed. In this Part II contribution, the crystallographic textures and quasi-static magnetic properties of ECAE-processed Hiperco were characterized. The textures were of a simple-shear character defined by partial {110} and <111> fibers inclined relative to the extrusion direction, in agreement with the expectations for simple-shear deformation textures of BCC metals. These textures were observed throughout all processing conditions and only slightlymore » reduced in intensity by subsequent recrystallization heat treatments. Characterization of the magnetic properties revealed a lower coercivity and higher permeability for ECAE-processed Hiperco specimens relative to the conventionally processed and annealed Hiperco bar. In conclusion, the effects of the resultant microstructure and texture on the coercivity and permeability magnetic properties are discussed.« less

Use of Hot Rolling for Generating Low Deviation Twins and a Disconnected Random Boundary Network in Inconel 600 Alloy

NASA Astrophysics Data System (ADS)

Sahu, Sandeep; Yadav, Prabhat Chand; Shekhar, Shashank

2018-02-01

In this investigation, Inconel 600 alloy was thermomechanically processed to different strains via hot rolling followed by a short-time annealing treatment to determine an appropriate thermomechanical process to achieve a high fraction of low-Σ CSL boundaries. Experimental results demonstrate that a certain level of deformation is necessary to obtain effective "grain boundary engineering"; i.e., the deformation must be sufficiently high to provide the required driving force for postdeformation static recrystallization, yet it should be low enough to retain a large fraction of original twin boundaries. Samples processed in such a fashion exhibited 77 pct length fraction of low-Σ CSL boundaries, a dominant fraction of which was from Σ3 ( 64 pct), the latter with very low deviation from its theoretical misorientation. The application of hot rolling also resulted in a very low fraction of Σ1 ( 1 pct) boundaries, as desired. The process also leads to so-called "triple junction engineering" with the generation of special triple junctions, which are very effective in disrupting the connectivity of the random grain boundary network.

Mimicking natural systems: Changes in behavior as a result of dynamic exposure to naproxen.

PubMed

Neal, Alexandra E; Moore, Paul A

2017-01-01

Animals living in aquatic habitats regularly encounter anthropogenic chemical pollution. Typically, the toxicity of a chemical toxicant is determined by the median lethal concentration (LC 50 ) through a static exposure test. However, LC 50 values and static tests do not provide an accurate representation of exposure to pollutants within natural stream systems. In their native habitats, animals experience exposure as a fluctuating concentration due to turbulent mixing, temporal variations of contamination (seasonal inputs), and contaminant input type (point vs. non-point). Research has shown that turbulent environments produce exposures with a high degree of fluctuation in frequency, duration, and intensity. In order to more effectively evaluate the effects of pollutants, we created a dynamic exposure paradigm, utilizing both flow and substrate within a small mesocosm. A commonly used pharmaceutical, naproxen, was used as the toxicant and female crayfish (Orconectes virilis) as the target organism to investigate changes in fighting behavior as a result of dynamic exposure. Crayfish underwent either a 23h long static or a dynamic exposure to naproxen. Following exposure, the target crayfish and an unexposed size matched opponent underwent a 15min fight trial. These fight trials were recorded and later analyzed using a standard ethogram. Results indicate that exposure to sublethal concentrations of naproxen, in both static and flowing conditions, negatively impact aggressive behavior. Results also indicate that a dynamic exposure paradigm has a greater negative impact on behavior than a static exposure. Turbulence and habitat structure play important roles in shaping chemical exposure. Future research should incorporate features of dynamic chemical exposure in order to form a more comprehensive image of chemical exposure and predict the resulting sublethal effects from exposure. Possible techniques for assessment include utilizing flow-through experimental set-ups in tandem with behavioral or physiological endpoints as opposed to acute toxicity. Other possibilities of assessment could involve utilizing fine-scale chemical measurements of pollutants to determine the actual concentrations animals encounter during an exposure event. Copyright © 2016 Elsevier Inc. All rights reserved.

Crystal doping aided by rapid expansion of supercritical solutions.

PubMed

Vemavarapu, Chandra; Mollan, Matthew J; Needham, Thomas E

2002-01-01

The purpose of this study was to test the utility of rapid expansion of supercritical solution (RESS) based cocrystallizations in inducing polymorph conversion and crystal disruption of chlorpropamide (CPD). CPD crystals were recrystallized by the RESS process utilizing supercritical carbon dioxide as the solvent. The supercritical region investigated for solute extraction ranged from 45 to 100 degrees C and 2000 to 8000 psi. While pure solute recrystallization formed stage I of these studies, stage II involved recrystallization of CPD in the presence of urea (model impurity). The composition, morphology, and crystallinity of the particles thus produced were characterized utilizing techniques such as microscopy, thermal analysis, x-ray powder diffractometry, and high-performance liquid chromatography. Also, comparative evaluation between RESS and evaporative crystallization from liquid solvents was performed. RESS recrystallizations of commercially available CPD (form A) resulted in polymorph conversion to metastable forms C and V, depending on the temperature and pressure of the recrystallizing solvent. Cocrystallization studies revealed the formation of eutectic mixtures and solid solutions of CPD + urea. Formation of the solid solutions resulted in the crystal disruption of CPD and subsequent amorphous conversion at urea levels higher than 40% wt/wt. Consistent with these results were the reductions in melting point (up to 9 degrees C) and in the DeltaH(f) values of CPD (up to 50%). Scanning electron microscopy revealed a particle size reduction of up to an order of magnitude upon RESS processing. Unlike RESS, recrystallizations from liquid organic solvents lacked the ability to affect polymorphic conversions. Also, the incorporation of urea into the lattice of CPD was found to be inadequate. In providing the ability to control both the particle and crystal morphologies of active pharmaceutical ingredients, RESS proved potentially advantageous to crystal engineering. Rapid crystallization kinetics were found vital in making RESS-based doping superior to conventional solvent-based cocrystallizations.

Evolution of microstructure, texture and inhibitor along the processing route for grain-oriented electrical steels using strip casting

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

Liu, Hai-Tao, E-mail: liuht@ral.neu.edu.cn; Institute of Research of Iron and Steel, Shasteel, Zhangjiagang 215625, Jiangsu; Yao, Sheng-Jie

2015-08-15

In the present work, a regular grade GO sheet was produced successively by strip casting, hot rolling, normalizing annealing, two-stage cold rolling with intermediate annealing, primary recrystallization annealing, secondary recrystallization annealing and purification. The aim of this paper was to characterize the evolution of microstructure, texture and inhibitor along the new processing route by comprehensive utilization of optical microscopy, X-ray diffraction and transmission electron microscopy. It was found that a fine microstructure with the ferrite grain size range of 7–12 μm could be obtained in the primary recrystallization annealed sheet though a very coarse microstructure was produced in the initialmore » as-cast strip. The main finding was that the “texture memory” effect on Goss texture started on the through-thickness intermediate annealed strip after first cold rolling, which was not similar to the “texture memory” effect on Goss texture starting on the surface layers of the hot rolled strip in the conventional production route. As a result, the origin of Goss nuclei capable of secondary recrystallization lied in the grains already presented in Goss orientation in the intermediate annealed strip after first cold rolling. Another finding was that fine and dispersive inhibitors (mainly AlN) were easy to be produced in the primary recrystallization microstructure due to the initial rapid solidification during strip casting and the subsequent rapid cooling, and the very high temperature reheating usually used before hot rolling in the conventional production route could be avoided. - Highlights: • A regular grade grain-oriented electrical steel was produced. • Evolution of microstructure, texture and inhibitor was characterized. • Origin of Goss nuclei lied in the intermediate annealed strip. • A fine primary recrystallization microstructure could be produced. • Effective inhibitors were easy to be obtained in the new processing route.« less

Content of toxic and essential metals in recrystallized and washed table salt in Shiraz, Iran

PubMed Central

2014-01-01

Background Table salt is the most commonly used food additive. Since most of the salt consumed in Iran comes from mines, contamination with heavy metals is a health concern. The commonest salt purification method in Iran is washing with water. But recently, some industries have turned to recrystallization method. The present study aimed to determine the level of essential and non-essential heavy metals in the table salt refined with recrystallization and washing methods. Methods Thirty eight pre-packed salt samples were directly collected from retail market in Shiraz (22 samples refined with recrystallization method and 16 with washing method). The level of lead, cadmium, copper, zinc, nickel and cobalt was determined using Voltammetric method. Daily intakes of lead and cadmium as well as their weekly intakes were calculated. Results The levels of lead, cadmium, copper, zinc, nickel and cobalt in recrystallized samples were 0. 30 ± 0.26, 0.02 ± 0.02, 0.11 ± 0.06, 0.34 ± 0.22, 0.15 ± 0.19 and 0.008 ± 0.007 μg/g, respectively, and also 0.37 ± 0.27, 0.017 ± 0.021, 0.19 ± 0.18, 0.37 ± 0.20, 0.13 ± 0.23 and 0.037 ± 0.06 μg/g in washed salt samples. The calculated weekly intake of lead and cadmium was 0.216 and 0.014 μg/kg, respectively for the recrystallized and 0.2653 and 0.0119 μg/kg for the washed salts. Conclusion All values for toxic metals were lower than the permitted maximum for human consumption as prescribed by Codex and Institute of Standards and Industrial Research of Iran. Only 0.8652-1.0612% of lead and 0.17-0.2% of cadmium PTWIs are received via salt consumption weekly. PMID:24398299

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.

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.

Transformation characteristics of TiNi/TiNi alloys synthesized by explosive welding

NASA Astrophysics Data System (ADS)

Li, Juntao; Zheng, Yanjun; Cui, Lishan

2007-10-01

Effects of severe deformation and heat treatment on the transformation behaviors of explosively welded duplex TiNi/TiNi shape memory alloys (SMAs) were investigated by the differential scanning calorimeter (DSC). The explosively welded duplex TiNi/TiNi plate of 0.7 mm in thickness was cold-rolled at room temperature to the extent of 60% reduction in thickness and then annealed at different temperatures (573-973 K) for different time (15 min-10 h). Low temperature (623-723 K) heat treatment led to amorphous crystallization. At higher temperature (873 K), the re-crystallization took place in the specimens. Analysis showed that the change of internal stresses is just the root cause of the change of transformation temperature. The relationships between the transformation behaviors and the heat treatment were discussed in the present report.

Full melting of a two-dimensional complex plasma crystal triggered by localized pulsed laser heating

NASA Astrophysics Data System (ADS)

Couëdel, L.; Nosenko, V.; Rubin-Zuzic, M.; Zhdanov, S.; Elskens, Y.; Hall, T.; Ivlev, A. V.

2018-04-01

The full melting of a two-dimensional plasma crystal was induced in a principally stable monolayer by localized laser stimulation. Two distinct behaviors of the crystal after laser stimulation were observed depending on the amount of injected energy: (i) below a well-defined threshold, the laser melted area recrystallized; (ii) above the threshold, it expanded outwards in a similar fashion to mode-coupling instability-induced melting, rapidly destroying the crystalline order of the whole complex plasma monolayer. The reported experimental observations are due to the fluid mode-coupling instability, which can pump energy into the particle monolayer at a rate surpassing the heat transport and damping rates in the energetic localized melted spot, resulting in its further growth. This behavior exhibits remarkable similarities with impulsive spot heating in ordinary reactive matter.

Effects of age and loading rate on equine cortical bone failure.

PubMed

Kulin, Robb M; Jiang, Fengchun; Vecchio, Kenneth S

2011-01-01

Although clinical bone fractures occur predominantly under impact loading (as occurs during sporting accidents, falls, high-speed impacts or other catastrophic events), experimentally validated studies on the dynamic fracture behavior of bone, at the loading rates associated with such events, remain limited. In this study, a series of tests were performed on femoral specimens obtained post-mortem from equine donors ranging in age from 6 months to 28 years. Fracture toughness and compressive tests were performed under both quasi-static and dynamic loading conditions in order to determine the effects of loading rate and age on the mechanical behavior of the cortical bone. Fracture toughness experiments were performed using a four-point bending geometry on single and double-notch specimens in order to measure fracture toughness, as well as observe differences in crack initiation between dynamic and quasi-static experiments. Compressive properties were measured on bone loaded parallel and transverse to the osteonal growth direction. Fracture propagation was then analyzed using scanning electron and scanning confocal microscopy to observe the effects of microstructural toughening mechanisms at different strain rates. Specimens from each horse were also analyzed for dry, wet and mineral densities, as well as weight percent mineral, in order to investigate possible influences of composition on mechanical behavior. Results indicate that bone has a higher compressive strength, but lower fracture toughness when tested dynamically as compared to quasi-static experiments. Fracture toughness also tends to decrease with age when measured quasi-statically, but shows little change with age under dynamic loading conditions, where brittle "cleavage-like" fracture behavior dominates. Copyright © 2010 Elsevier Ltd. All rights reserved.

Impaired recognition of body expressions in the behavioral variant of frontotemporal dementia.

PubMed

Van den Stock, Jan; De Winter, François-Laurent; de Gelder, Beatrice; Rangarajan, Janaki Raman; Cypers, Gert; Maes, Frederik; Sunaert, Stefan; Goffin, Karolien; Vandenberghe, Rik; Vandenbulcke, Mathieu

2015-08-01

Progressive deterioration of social cognition and emotion processing are core symptoms of the behavioral variant of frontotemporal dementia (bvFTD). Here we investigate whether bvFTD is also associated with impaired recognition of static (Experiment 1) and dynamic (Experiment 2) bodily expressions. In addition, we compared body expression processing with processing of static (Experiment 3) and dynamic (Experiment 4) facial expressions, as well as with face identity processing (Experiment 5). The results reveal that bvFTD is associated with impaired recognition of static and dynamic bodily and facial expressions, while identity processing was intact. No differential impairments were observed regarding motion (static vs. dynamic) or category (body vs. face). Within the bvFTD group, we observed a significant partial correlation between body and face expression recognition, when controlling for performance on the identity task. Voxel-Based Morphometry (VBM) analysis revealed that body emotion recognition was positively associated with gray matter volume in a region of the inferior frontal gyrus (pars orbitalis/triangularis). The results are in line with a supramodal emotion recognition deficit in bvFTD. Copyright © 2015 Elsevier Ltd. All rights reserved.

A Multiscale Model for the Quasi-Static Thermo-Plastic Behavior of Highly Cross-Linked Glassy Polymers

DOE PAGES

Vu-Bac, N.; Bessa, M. A.; Rabczuk, Timon; ...

2015-09-10

In this paper, we present experimentally validated molecular dynamics predictions of the quasi- static yield and post-yield behavior for a highly cross-linked epoxy polymer under gen- eral stress states and for different temperatures. In addition, a hierarchical multiscale model is presented where the nano-scale simulations obtained from molecular dynamics were homogenized to a continuum thermoplastic constitutive model for the epoxy that can be used to describe the macroscopic behavior of the material. Three major conclusions were achieved: (1) the yield surfaces generated from the nano-scale model for different temperatures agree well with the paraboloid yield crite- rion, supporting previous macroscopicmore » experimental observations; (2) rescaling of the entire yield surfaces to the quasi-static case is possible by considering Argon’s theoretical predictions for pure compression of the polymer at absolute zero temperature; (3) nano- scale simulations can be used for an experimentally-free calibration of macroscopic con- tinuum models, opening new avenues for the design of materials and structures through multi-scale simulations that provide structure-property-performance relationships.« less

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.)

Tensile behavior of tungsten and tungsten-alloy wires from 1300 to 1600 K

NASA Technical Reports Server (NTRS)

Hee, Man Yun

1988-01-01

The tensile behavior of a 200-micrometer-diameter tungsten lamp (218CS-W), tungsten + 1.0 atomic percent (a/o) thoria (ST300-W), and tungsten + 0.4 a/o hafnium carbide (WHfC) wires was determined over the temperature range 1300 t0 1600 K at strain rates of 3.3 X 10 to the -2 to 3.3 X 10 to the -5/sec. Although most tests were conducted on as-drawn materials, one series of tests was undertaken on ST300-W wires in four different conditions: as-drawn and vacuum-annealed at 1535 K for 1 hr, with and without electroplating. Whereas heat treatment had no effect on tensile properties, electropolishing significantly increased both the proportional limit and ductility, but not the ultimate tensile strength. Comparison of the behavior of the three alloys indicates that the HfC-dispersed material possesses superior tensile properties. Theoretical calculations indicate that the strength/ductility advantage of WHfC is due to the resistance to recrystallization imparted by the dispersoid.

Kinetics Study on the Effect of NaCl on the CaSO4 Dissolution Behavior

NASA Astrophysics Data System (ADS)

Song, Jingyao; Shi, Peiyang; Wang, Yeguang; Jiang, Maofa

2018-01-01

The study of the dissolution kinetics of CaSO4 is essential for the control of the dissolution and recrystallization behavior of CaSO4. In this work, the kinetic behavior of CaSO4 dissolved in NaCl solution was investigated by means of conductivity meter. The results show that with the increase of concentration of NaCl, the temperature rise and the time prolonged, the dissolution rate of dihydrate CaSO4 gradually increases, and the dissolved apparent activation energy is gradually decreased. When the NaCl concentration is 1.8%, the dissolution kinetic equation is 1-(1-α) 1/3=5.46*10-4exp (-9147/RT) t; When the NaCl concentration is 3.0%, the dissolution kinetic equation is 1-(1-α) 1/3=2.81×10-4 exp (-6753/RT)t; When the NaCl concentration is 3.6%, the dissolution kinetic equation is 1-(1-α) 1/3=3.07×l0-4exp(-6103/RT)t.

Comparison studies of rheological and thermal behaviors of ionic liquids and nanoparticle ionic liquids.

PubMed

Xu, Yiting; Zheng, Qiang; Song, Yihu

2015-08-14

Novel nanoparticle ionic liquids (NILs) are prepared by grafting modified nanoparticles with long-chain ionic liquids (ILs). The NIL behaves like a liquid at ambient temperature. We studied the rheological behavior of the IL and NIL over the range of 10-55 °C and found an extraordinary difference between the IL and NIL: a small content of nanosilica (7%) moderately improves the crystallinity by 7% of the poly(ethylene glycol) (PEG) segment in the IL, and it improves the dynamic moduli significantly (by 5 times at room temperature). It retards the decay temperature (by 10 °C) of the dynamic moduli during heating as well. The thermal rheological hysteresis observed during heating-cooling temperature sweeps is ascribed to the melting-recrystallization of the PEG segments. Meanwhile, the IL and NIL express accelerated crystallization behavior in comparison with the oligomeric anion. For the first time, we find that ILs and NILs are able to form nanoparticle-containing spherulites at room temperature after long time aging.

An electron microscopy examination of primary recrystallization in TD-nickel.

NASA Technical Reports Server (NTRS)

Petrovic, J. J.; Ebert, L. J.

1972-01-01

Primary recrystallization in TD-nickel 1 in. bar has previously been regarded as the process by which the initial fine grain structure is converted to a coarse grain size (increases in grain size by 500 times) under suitable deformation and annealing conditions. This process is dependent on deformation mode. While it occurs readily after rolling transverse to the bar axis and annealing (800 C), it is completely inhibited by longitudinal rolling and swaging deformations, even for very high (1320 C) annealing temperatures. A transmission electron microscopy examination of deformation and annealing substructures indicates that primary recrystallization in TD-nickel 1 in. bar actually occurs on the sub-light optical level, to produce a grain structure similar in size to the initial fine grained state.

Facially Amphipathic Glycopolymers Inhibit Ice Recrystallization.

PubMed

Graham, Ben; Fayter, Alice E R; Houston, Judith E; Evans, Rachel C; Gibson, Matthew I

2018-05-02

Antifreeze glycoproteins (AFGPs) from polar fish are the most potent ice recrystallization (growth) inhibitors known, and synthetic mimics are required for low-temperature applications such as cell cryopreservation. Here we introduce facially amphipathic glycopolymers that mimic the three-dimensional structure of AFGPs. Glycopolymers featuring segregated hydrophilic and hydrophobic faces were prepared by ring-opening metathesis polymerization, and their rigid conformation was confirmed by small-angle neutron scattering. Ice recrystallization inhibition (IRI) activity was reduced when a hydrophilic oxo-ether was installed on the glycan-opposing face, but significant activity was restored by incorporating a hydrophobic dimethylfulvene residue. This biomimetic strategy demonstrates that segregated domains of distinct hydrophilicity/hydrophobicity are a crucial motif to introduce IRI activity, which increases our understanding of the complex ice crystal inhibition processes.

Failure of a laminated composite under tension-compression fatigue loading

NASA Technical Reports Server (NTRS)

Rotem, A.; Nelson, H. G.

1989-01-01

The fatigue behavior of composite laminates under tension-compression loading is analyzed and compared with behavior under tension-tension and compression-compression loading. It is shown that for meaningful fatigue conditions, the tension-compression case is the dominant one. Both tension and compression failure modes can occur under the reversed loading, and failure is dependent on the specific lay-up of the laminate and the difference between the tensile static strength and the absolute value of the compressive static strength. The use of a fatigue failure envelope for determining the fatigue life and mode of failure is proposed and demonstrated.

Static heterogeneities in liquid water

NASA Astrophysics Data System (ADS)

Stanley, H. Eugene; Buldyrev, Sergey V.; Giovambattista, Nicolas

2004-10-01

The thermodynamic behavior of water seems to be closely related to static heterogeneities. These static heterogeneities are related to the local structure of water molecules, and when properly characterized, may offer an economical explanation of thermodynamic data. The key feature of liquid water is not so much that the existence of hydrogen bonds, first pointed out by Linus Pauling, but rather the local geometry of the liquid molecules is not spherical or oblong but tetrahedral. In the consideration of static heterogeneities, this local geometry is critical. Recent experiments suggested more than one phase of amorphous solid water, while simulations suggest that one of these phases is metastable with respect to another, so that in fact there are only two stable phases.

Transient electronic anisotropy in overdoped NaF e1 -xC oxAs superconductors

NASA Astrophysics Data System (ADS)

Liu, Shenghua; Zhang, Chunfeng; Deng, Qiang; Wen, Hai-hu; Li, Jian-xin; Chia, Elbert E. M.; Wang, Xiaoyong; Xiao, Min

2018-01-01

By combining polarized pump-probe spectroscopic and Laue x-ray diffraction measurements, we have observed nonequivalent transient optical responses with the probe beam polarized along the x and y axes in overdoped NaF e1 -xC oxAs superconductors. Such transient anisotropic behavior has been uncovered in the tetragonal phase with the doping level and temperature range far from the borders of static nematic phases. The measured transient anisotropy can be well explained as a result of nematic fluctuation driven by an orbital order with energy splitting of the dx z- and dy z-dominant bands. In addition, the doping level dependence and the pressure effect of the crossover temperature show significant differences between the transient nematic fluctuation and static nematic phase, implying spin and orbital orders may play different roles in static and transient nematic behaviors.

Recrystallization of Manganite (γ-MnOOH) and Implications for Trace Element Cycling.

PubMed

Hens, Tobias; Brugger, Joël; Cumberland, Susan A; Etschmann, Barbara; Frierdich, Andrew J

2018-02-06

The recrystallization of Mn(III,IV) oxides is catalyzed by aqueous Mn(II) (Mn(II) aq ) during (bio)geochemical Mn redox cycling. It is poorly understood how trace metals associated with Mn oxides (e.g., Ni) are cycled during such recrystallization. Here, we use X-ray absorption spectroscopy (XAS) to examine the speciation of Ni associated with Manganite (γ-Mn(III)OOH) suspensions in the presence or absence of Mn(II) aq under variable pH conditions (pH 5.5 and 7.5). In a second set of experiments, we used a 62 Ni isotope tracer to quantify the amount of dissolved Ni that exchanges with Ni incorporated in the Manganite crystal structure during reactions in 1 mM Mn(II) aq and in Mn(II)-free solutions. XAS spectra show that Ni is initially sorbed on the Manganite mineral surface and is progressively incorporated into the mineral structure over time (13% after 51 days) even in the absence of dissolved Mn(II). The amount of Ni incorporation significantly increases to about 40% over a period of 51 days when Mn(II) aq is present in solution. Similarly, Mn(II) aq promotes Ni exchange between Ni-substituted Manganite and dissolved Ni(II), with around 30% of Ni exchanged at pH 7.5 over the duration of the experiment. No new mineral phases are detected following recrystallization as determined by X-ray diffraction and XAS. Our results reveal that Mn(II)-catalyzed mineral recrystallization partitions Ni between Mn oxides and aqueous fluids and can therefore affect Ni speciation and mobility in the environment.

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

NASA Astrophysics Data System (ADS)

Wang, Zhenhua; Xue, Hongpeng; Fu, Wantang

2018-03-01

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

Internal Shear Forging Processes for Missile Primary Structures.

DTIC Science & Technology

1981-07-20

received condition. The as-received micro- structure displayed elongated recrystallized grains interspersed with particles of precipitate phases. SEM...re- crystallization regime for this alloy, and rolled specimens were reheated to 3160 C between passes, some recrystallization and grain size changes...experiment revealed that the actual solution treatment temperature was probably higher than 5000C. This resulted in melting of the eutectic and solid

Chemical Characterization of Dimethylsulfoxide (DMSO) Munitions Recrystallization Process Samples.

DTIC Science & Technology

1984-10-01

position unless so designated by other aulthorized documents. Disposition Destroy this report when it is no longer needed. Do riot return it to the... DESTRIBUTION LIST ....... ........... ... ................................. -12 rABLES 1. HPLC Analyses of Munitions from DMS0 Recrystallization Process...characterization and identification of any trace organics present in addition to the nitramines. Portions of the two samples, designated as evaporator

Ice recrystallization kinetics in the presence of synthetic antifreeze glycoprotein analogues using the framework of LSW theory.

PubMed

Budke, C; Heggemann, C; Koch, M; Sewald, N; Koop, T

2009-03-05

The Ostwald ripening of polycrystalline ice in aqueous sucrose solutions was investigated experimentally. The kinetics of this ice recrystallization process was studied at temperatures between -6 and -10 degrees C and varying ice volume fractions. Using the theory of Lifshitz, Slyozov, and Wagner (LSW), the diffusion-limited rate constant for ice recrystallization was determined. Also, the effects of synthetic analogues of natural antifreeze glycoproteins (AFGP) were studied. These analogues synAFGPmi (i = 3-5) contained monosaccharide side groups instead of disaccharide side groups that occur in natural AFGP. In order to account for the inhibition effect of the synAFGPmi, we have modified classical LSW theory, allowing for the derivation of inhibition rate constants. It was found that the investigated synAFGPmi inhibit ice recrystallization at concentrations down to approximately 3 microg mL(-1) or, equivalently, approximately 1 micromol L(-1) for the largest synAFGPmi investigated: synAFGPm5. Hence, our new method is capable of quantitatively assessing the efficiency of very similar AFGP with a sensitivity that is at least 2 orders of magnitude larger than that typical for quantitative thermal hysteresis measurements.

Influence of phosphate glass recrystallization on the stability of a waste matrix to leaching

NASA Astrophysics Data System (ADS)

Yudintsev, S. V.; Pervukhina, A. M.; Mokhov, A. V.; Malkovsky, V. I.; Stefanovsky, S. V.

2017-04-01

In Russia, highly radioactive liquid wastes from recycling of spent fuel of nuclear reactors are solidified into Na-Al-P glass for underground storage. The properties of the matrix including the radionuclide fixation will change with time due to crystallization. This is supported by the results of study of the interaction between glassy matrices, products of their crystallization, and water. The concentration of Cs in a solution at the contact of a recrystallized sample increased by three orders of magnitude in comparison with an experiment with glass. This difference is nearly one order of magnitude for Sr, Ce, and Nd (simulators of actinides) and U due to their incorporation into phases with low solubility in water. Based on data on the compositional change of solutions after passing through filters of various diameters, it is concluded that Cs occurs in the dissolved state in runs with a glass and recrystallized matrix. At the same time, Sr, lanthanides, and U occur in the dissolved state and in the composition of colloids in runs with glass, and mostly in colloid particles after contact with the recrystallized sample. These results should be regarded for substantiation of safety for geological waste storage.

Small molecule ice recrystallization inhibitors mitigate red blood cell lysis during freezing, transient warming and thawing

NASA Astrophysics Data System (ADS)

Briard, Jennie G.; Poisson, Jessica S.; Turner, Tracey R.; Capicciotti, Chantelle J.; Acker, Jason P.; Ben, Robert N.

2016-03-01

During cryopreservation, ice recrystallization is a major cause of cellular damage. Conventional cryoprotectants such as dimethyl sulfoxide (DMSO) and glycerol function by a number of different mechanisms but do not mitigate or control ice recrystallization at concentrations utilized in cryopreservation procedures. In North America, cryopreservation of human red blood cells (RBCs) utilizes high concentrations of glycerol. RBC units frozen under these conditions must be subjected to a time-consuming deglycerolization process after thawing in order to remove the glycerol to <1% prior to transfusion thus limiting the use of frozen RBC units in emergency situations. We have identified several low molecular mass ice recrystallization inhibitors (IRIs) that are effective cryoprotectants for human RBCs, resulting in 70-80% intact RBCs using only 15% glycerol and slow freezing rates. These compounds are capable of reducing the average ice crystal size of extracellular ice relative to a 15% glycerol control validating the positive correlation between a reduction in ice crystal size and increased post-thaw recovery of RBCs. The most potent IRI from this study is also capable of protecting frozen RBCs against the large temperature fluctuations associated with transient warming.

S-Isovaline Contained in Meteorites, Induces Enantiomeric Excess in D,L-glutamic Acid During Recrystallization

NASA Astrophysics Data System (ADS)

Kojo, Shosuke

2015-06-01

S-Isovaline (S-Iva: 6.7 mmol) and D,L-glutamic acid (Glu: 2 mmol) were dissolved in 10 ml of hot water, and the resulting solution was divided in 5 vessels. After recrystallization, the crystals were collected from each vessel, and the enantiomeric excess (ee) of Glu was determined with chemical derivatization using 1-fluoro-2,4-dinitrophenyl- 5-L-leucinamide followed by high-performance liquid chromatography. Ten crystallizations provided all D-rich Glu with ee values of 2.69 % ± 0.81 % (mean ± standard deviation), and those using R-Iva provided all L-rich Glu with ee values of 6.24 % ± 2.20 %. Five recrystallizations of D,L-Glu alone provided ee values of 0.474 % ± 0.33 %. The differences among these three ee values were statistically significant, showing that S-Iva, which was present in meteorites caused a significant induction of ee in this physiological amino acid. This is the first outcome that S-Iva induced ee changes in a physiological amino acid. S-Iva did not induce any ee changes in D,L-asparagine, leucine, valine, methionine, phenylalanine, tryptophan, glutamine, tyrosine, aspartic acid, or histidine under similar recrystallizations.

Small molecule ice recrystallization inhibitors mitigate red blood cell lysis during freezing, transient warming and thawing

PubMed Central

Briard, Jennie G.; Poisson, Jessica S.; Turner, Tracey R.; Capicciotti, Chantelle J.; Acker, Jason P.; Ben, Robert N.

2016-01-01

During cryopreservation, ice recrystallization is a major cause of cellular damage. Conventional cryoprotectants such as dimethyl sulfoxide (DMSO) and glycerol function by a number of different mechanisms but do not mitigate or control ice recrystallization at concentrations utilized in cryopreservation procedures. In North America, cryopreservation of human red blood cells (RBCs) utilizes high concentrations of glycerol. RBC units frozen under these conditions must be subjected to a time-consuming deglycerolization process after thawing in order to remove the glycerol to <1% prior to transfusion thus limiting the use of frozen RBC units in emergency situations. We have identified several low molecular mass ice recrystallization inhibitors (IRIs) that are effective cryoprotectants for human RBCs, resulting in 70–80% intact RBCs using only 15% glycerol and slow freezing rates. These compounds are capable of reducing the average ice crystal size of extracellular ice relative to a 15% glycerol control validating the positive correlation between a reduction in ice crystal size and increased post-thaw recovery of RBCs. The most potent IRI from this study is also capable of protecting frozen RBCs against the large temperature fluctuations associated with transient warming. PMID:27021850

Effect of storage conditions on the recrystallization of drugs in solid dispersions with crospovidone.

PubMed

Shibata, Yusuke; Fujii, Makiko; Suzuki, Ayako; Koizumi, Naoya; Kanada, Ken; Yamada, Masaki; Watanabe, Yoshiteru

2014-06-01

The physical stability of amorphous solid dispersions (SDs) is influenced by their storage conditions. The goal of this work was to investigate the factors affecting the recrystallization of drugs in SDs after storage under conditions of high temperature and high humidity. SDs of three drugs (dipyridamole, nifedipine and indomethacin) with different functional groups (amino, carbonyl and hydroxyl) and onset times for crystallization of the amorphous state were prepared using crospovidone (CrosPVP). All of the drugs in the SDs remained in an amorphous state at 25 °C/50% relative humidity (RH) in closed glass bottles for at least six months. Under conditions of high temperature (40 °C/75%RH/closed and 60 °C/open), differences in interactions between the hydrogen bond donors of the drugs and the amide carbonyl group of CrosPVP are essential factors for recrystallization of the drugs in the SDs. On the other hand, under condition of high humidity (40 °C/75%RH/open), in addition to the difference in the interaction between the drug and CrosPVP, the rate of increase in moisture content affects their recrystallization in SDs.

Reduced graphene oxide-induced recrystallization of NiS nanorods to nanosheets and the improved Na-storage properties.

PubMed

Pan, Qin; Xie, Jian; Zhu, Tiejun; Cao, Gaoshao; Zhao, Xinbing; Zhang, Shichao

2014-04-07

Preparation of two-dimensional (2D) graphene-like materials is currently an emerging field in materials science since the discovery of single-atom-thick graphene prepared by mechanical cleavage. In this work, we proposed a new method to prepare 2D NiS, where reduced graphene oxide (rGO) was found to induce the recrystallization of NiS from nanorods to nanosheets in a hydrothermal process. The process and mechanism of recrystallization have been clarified by various characterization techniques, including scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive X-ray spectroscopy (EDS) mapping, and X-ray photoelectron spectroscopy (XPS). The characterization of ex situ NiS/rGO products by SEM and EDS mapping indicates that the recrystallization of NiS from nanorods to nanosheets is realized actually through an exfoliation process, while the characterization of in situ NiS/rGO products by SEM, TEM, and EDS mapping reveals the exfoliation process. The XPS result demonstrates that hydrothermally assisted chemical bonding occurs between NiS and rGO, which induces the exfoliation of NiS nanorods into nanosheets. The obtained NiS/rGO composite shows promising Na-storage properties.

Small molecule ice recrystallization inhibitors mitigate red blood cell lysis during freezing, transient warming and thawing.

PubMed

Briard, Jennie G; Poisson, Jessica S; Turner, Tracey R; Capicciotti, Chantelle J; Acker, Jason P; Ben, Robert N

2016-03-29

During cryopreservation, ice recrystallization is a major cause of cellular damage. Conventional cryoprotectants such as dimethyl sulfoxide (DMSO) and glycerol function by a number of different mechanisms but do not mitigate or control ice recrystallization at concentrations utilized in cryopreservation procedures. In North America, cryopreservation of human red blood cells (RBCs) utilizes high concentrations of glycerol. RBC units frozen under these conditions must be subjected to a time-consuming deglycerolization process after thawing in order to remove the glycerol to <1% prior to transfusion thus limiting the use of frozen RBC units in emergency situations. We have identified several low molecular mass ice recrystallization inhibitors (IRIs) that are effective cryoprotectants for human RBCs, resulting in 70-80% intact RBCs using only 15% glycerol and slow freezing rates. These compounds are capable of reducing the average ice crystal size of extracellular ice relative to a 15% glycerol control validating the positive correlation between a reduction in ice crystal size and increased post-thaw recovery of RBCs. The most potent IRI from this study is also capable of protecting frozen RBCs against the large temperature fluctuations associated with transient warming.

LLNL small-scale static spark machine: static spark sensitivity test

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

Foltz, M F; Simpson, L R

1999-08-23

Small-scale safety testing of explosives and other energetic materials is done in order to determine their sensitivity to various stimuli, such as friction, static spark, and impact. Typically this testing is done to discover potential handling problems that may exist for either newly synthesized materials of unknown behavior, or materials that have been stored for long periods of time. This report describes the existing ''Static Spark Test Apparatus'' at Lawrence Livermore National Laboratory (LLNL), as well as the method used to evaluate the relative static spark sensitivity of energetic materials. The basic design, originally developed by the Picatinny Arsenal inmore » New Jersey, is discussed. The accumulated data for the materials tested to date is not included here, with the exception of specific examples that have yielded interesting or unusual results during the tests.« less

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

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.

A re-evaluation of the mechanism of SIBM

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

Bate, P.; Hutchinson, B.

The process for creating a new recrystallized grain by the bulging out of an existing grain boundary within the deformed structure was recognized by Beck and Sperry and described as strain induced boundary migration, often now as SIBM. For many years SIBM seemed to be accorded less significance than the subgrain growth models for nucleation of recrystallization. However, the importance of SIBM is increasingly recognized, for example in the case of cube texture development in aluminum alloys. There is increasing evidence that high angle boundaries in deformed metals are not only residues of the prior grain structure but may alsomore » be generated by the deformation itself. These also participate in the nucleation of recrystallization on annealing and must do so by some form of SIBM mechanism.« less

Etude de la texture des rubans EPR de silicium polycristallin photovoltaïque

NASA Astrophysics Data System (ADS)

Chibani, A.; Gauthier, R.; Pinard, P.; Andonov, P.

1991-09-01

EPR polysilicon ribbons are obtained from a 5N-6N purity grade silicon powder melting followed by a recrystallization step. Being assigned to the photocell manufacture, we study the texture by X-ray diffraction method to reveal the majority of the crystal orientations and prove the eventual existence of specific orientations adapted to the best photovoltaic conversion efficiencies such as (100), (110) or (111). Moreover, we tested the possibility to induce the (111) orientation with a monocrystalline seed having this orientation. It appears that the crystal growth is essentially anisotropic and that only the orientation of the grains with their (331) planes parallel to the ribbon surface may be considered as dominant after the recrystallization step; finally, the (111) starting seed has an effect only at the recrystallization onset.

Aging and loading rate effects on the mechanical behavior of equine bone

NASA Astrophysics Data System (ADS)

Kulin, Robb M.; Jiang, Fengchun; Vecchio, Kenneth S.

2008-06-01

Whether due to a sporting accident, high-speed impact, fall, or other catastrophic event, the majority of clinical bone fractures occur under dynamic loading conditions. However, although extensive research has been performed on the quasi-static fracture and mechanical behavior of bone to date, few high-quality studies on the fracture behavior of bone at high strain rates have been performed. Therefore, many questions remain regarding the material behavior, including not only the loading-rate-dependent response of bone, but also how this response varies with age. In this study, tests were performed on equine femoral bone taken post-mortem from donors 6 months to 28 years of age. Quasi-static and dynamic tests were performed to determine the fracture toughness and compressive mechanical behavior as a function of age at varying loading rates. Fracture paths were then analyzed using scanning confocal and scanning-electron microscopy techniques to assess the role of various microstructural features on toughening mechanisms.

Artificial neural network prediction of aircraft aeroelastic behavior

NASA Astrophysics Data System (ADS)

Pesonen, Urpo Juhani

An Artificial Neural Network that predicts aeroelastic behavior of aircraft is presented. The neural net was designed to predict the shape of a flexible wing in static flight conditions using results from a structural analysis and an aerodynamic analysis performed with traditional computational tools. To generate reliable training and testing data for the network, an aeroelastic analysis code using these tools as components was designed and validated. To demonstrate the advantages and reliability of Artificial Neural Networks, a network was also designed and trained to predict airfoil maximum lift at low Reynolds numbers where wind tunnel data was used for the training. Finally, a neural net was designed and trained to predict the static aeroelastic behavior of a wing without the need to iterate between the structural and aerodynamic solvers.

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.

Programmable Phase Transitions in a Photonic Microgel System: Linking Soft Interactions to a Temporal pH Gradient.

PubMed

Go, Dennis; Rommel, Dirk; Chen, Lisa; Shi, Feng; Sprakel, Joris; Kuehne, Alexander J C

2017-02-28

Soft amphoteric microgel systems exhibit a rich phase behavior. Crystalline phases of these material systems are of interest because they exhibit photonic stop-gaps, giving rise to iridescent color. Such microgel systems are promising for applications in soft, switchable, and programmable photonic filters and devices. We here report a composite microgel system consisting of a hard and fluorescently labeled core and a soft, amphoteric microgel shell. At pH above the isoelectric point (IEP), these colloids easily crystallize into three-dimensional colloidal assemblies. By adding a cyclic lactone to the system, the temporal pH profile can be controlled, and the microgels can be programmed to melt, while they lose charge. When the microgels gain the opposite charge, they recrystallize into assemblies of even higher order. We provide a model system to study the dynamic phase behavior of soft particles and their switchable and programmable photonic effects.