Sample records for monotectics
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Solidification studies of monotectic systems
NASA Technical Reports Server (NTRS)
Chang, K.
1982-01-01
Described is an attempt to determine critical wetting temperatures in monotectic systems and to investigate the wetting phase on container walls and the phase preferential wetting of a monotectic solid.
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Cellular solidification in a monotectic system
NASA Technical Reports Server (NTRS)
Kaukler, W. F.; Curreri, P. A.
1987-01-01
Succinonitrile-glycerol, SN-G, transparent organic monotectic alloy is studied with particular attention to cellular growth. The phase diagram is determined, near the monotectic composition, with greater accuracy than previous studies. A solidification interface stability diagram is determined for planar growth. The planar-to-cellular transition is compared to predictions from the Burton, Primm, Schlichter theory. A new technique to determine the solute segregation by Fourier transform infrared spectroscopy is developed. Proposed models that involve the cellular interface for alignment of monotectic second-phase spheres or rods are compared with observations.
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Solidification processing of monotectic alloy matrix composites
NASA Technical Reports Server (NTRS)
Frier, Nancy L.; Shiohara, Yuh; Russell, Kenneth C.
1989-01-01
Directionally solidified aluminum-indium alloys of the monotectic composition were found to form an in situ rod composite which obeys a lambda exp 2 R = constant relation. The experimental data shows good agreement with previously reported results. A theoretical boundary between cellular and dendritic growth conditions was derived and compared with experiments. The unique wetting characteristics of the monotectic alloys can be utilized to tailor the interface structure in metal matrix composites. Metal matrix composites with monotectic and hypermonotectic Al-In matrices were made by pressure infiltration, remelted and directionally solidified to observe the wetting characteristics of the alloys as well as the effect on structure of solidification in the constrained field of the fiber interstices. Models for monotectic growth are modified to take into account solidification in these constrained fields.
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NASA Astrophysics Data System (ADS)
Bo, Lin; Li, Shanshan; Wang, Lin; Wu, Di; Zuo, Min; Zhao, Degang
2018-03-01
The cooling rate has a significant effect on the solidification behavior and microstructure of monotectic alloy. In this study, different cooling rate was designed through casting in the copper mold with different bore diameters. The effects of different cooling rate on the solidification behavior of Al55Bi36Cu9 (at.%) immiscible alloy have been investigated. The liquid-liquid phase separation of Al55Bi36Cu9 immiscible alloy melt was investigated by resistivity test. The solidification microstructure and phase analysis of Al55Bi36Cu9 immiscible alloy were performed by the SEM and XRD, respectively. The results showed that the liquid-liquid phase separation occurred in the solidification of Al55Bi36Cu9 monotectic melt from 917 °C to 653 °C. The monotectic temperature, liquid phase separation temperature and immiscibility zone of Al55Bi36Cu9 monotectic alloy was lower than those of Al-Bi binary monotectic alloy. The solidification morphology of Al55Bi36Cu9 monotectic alloy was very sensitive to the cooling rate. The Al/Bi core-shell structure formed when Al55Bi36Cu9 melt was cast in the copper mold with a 8 mm bore diameter.
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NASA Technical Reports Server (NTRS)
Kaukler, William F.
1988-01-01
The purpose of this work was to resolve a scientific controversy in the understanding of how second phase particles become aligned during unidirectional growth of a monotectic alloy. A second aspect was to make the first systematic observations of the solidification behavior of a monotectic alloy during cellular growth in-situ. This research provides the first systematic transparent model study of cellular solidification. An interface stability diagram was developed for the planar to cellular transition of the succinonitrile glycerol (SNG) system. A method was developed utilizing Fourier Transform Infrared Spectroscopy which allows quantitative compositional analysis of directionally solidified SNG along the growth axis. To determine the influence of cellular growth front on alignment for directionally solidified monotectic alloys, the planar and cellular growth morphology was observed in-situ for SNG between 8 and 17 percent glycerol and for a range of over two orders of magnitude G/R.
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Nickel-Silver Monotectic in Alumina Crucible for Use with Contact Thermometry
NASA Astrophysics Data System (ADS)
Gotoh, M.; Dedyulin, S. N.
2017-07-01
Previously, the authors have published work describing a pure Ni fixed point within alumina crucibles. The success of this study stimulated working with the Ni-Ag monotectic point in alumina crucibles. Similar to eutectic points, the Ni-Ag monotectic temperature is an invariant point but it differs from a eutectic reaction in such a way that the monotectic phase change takes place from Ni-Ag liquid solution to Ni-Ag solid solution and Ag rich Ni-Ag liquid solution. In the phase diagram references, the Ni-Ag monotectic phase transition temperature is assigned to be about 20°C below the pure Ni melting/freezing point. As is the case for pure Ni, mechanical stability is one of the concerns. Therefore, proper cell design is necessary to avoid breakage of the alumina crucible. The techniques used for the fabrication and measurement of the pure Ni cell were applied to the Ni-Ag cell as well. The cells have been successfully fabricated and the temperature measurement at the fixed point was carried out for more than 20 thermal cycles in total. A Pt/Pd thermocouple was used to measure the temperature and was calibrated from the tin point to the gold point to measure the ITS-90. Freezing plateaus are realized with the technique of "recurrent offset freezing method with reserved solid". The duration of each freezing plateau is a minimum of 30 min. The monotectic transformation temperature for the best performed cell is determined as 1428.27°C with a combined uncertainty of ±0.06°C ({k}=1).
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Liquid-liquid phase separation and core-shell structure of ternary Al-In-Sn immiscible alloys
NASA Astrophysics Data System (ADS)
Zhao, Degang; Bo, Lin; Wang, Lin; Li, Shanshan
2018-04-01
In this study, the liquid-liquid phase separation of four kinds of ternary immiscible Al-In-Sn melts was investigated with resistivity and thermodynamics method. The nonlinear changes in ρ-T and DSC curves of Al-In-Sn immiscible alloys above monotectic reaction temperature revealed the occurrence of liquid-liquid phase separation of Al-In-Sn melts. The monotectic temperature, liquid phase separation temperature and immiscible gap of ternary Al-In-Sn alloys were lower than those of binary Al-In alloy. With the Al content decreasing, the immiscible gap of Al-In-Sn alloy decreased. The composition of Al80In10Sn10, Al70In15Sn15, Al60In20Sn20 and Al50In25Sn25 was located in the immiscible zone of Al-In-Sn system. Due to the differences of Stokes effect, Marangoni convection and immiscible gap, the solidification morphology of four kinds of Al-In-Sn monotectic alloy was different. The core–shell structure of Al-In-Sn monotectic alloy can form within a certain range of composition.
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NASA Technical Reports Server (NTRS)
Parr, R. A.; Johnston, M. H.; Mcclure, J. C.
1980-01-01
Monotectic alloys having aligned spherical particles of rods of the minor component dispersed in a matrix of the major component are prepared by forming a melt containing predetermined amounts of the major and minor components of a chosen monotectic system, providing in the melt a dopant capable of breaking down the liquid solid interface for the chosen alloy, and directionally solidfying the melt at a selected temperature gradient and a selected rate of movement of the liquid-solid interface (growth rate). Shaping of the minor component into spheres or rods and the spacing between them are controlled by the amount of dopant and the temperature gradient and growth rate values. Specific alloy systems include Al Bi, Al Pb and Zn Bi, using a transition element such as iron.
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NASA Technical Reports Server (NTRS)
Kaukler, W. F.; Frazier, D. O.; Facemire, B.
1984-01-01
Equilibrium temperature-composition diagrams were determined for the two organic systems, succinonitrile-benzene and succinonitrile-cyclohexanol. Measurements were made using the common thermal analysis methods and UV spectrophotometry. Succinonitrile-benzene monotectic was chosen for its low affinity for water and because UV analysis would be simplified. Succinonitrile-cyclohexanol was chosen because both components are transparent models for metallic solidification, as opposed to the other known succinonitrile-based monotectics.
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Immiscible phase incorporation during directional solidification of hypermonotectics
NASA Technical Reports Server (NTRS)
Andrews, J. Barry; Merrick, Roger A.
1993-01-01
Solidification processes in immiscible samples were investigated by directly observing the events taking place at the solid-liquid interface during directional solidification. Visualization of these events was made possible through the use of a transparent metal analog system and a temperature gradient stage assembly fitted to an optical microscope. The immiscible transparent analog system utilized was the succinonitrile-glycerol system. This system has been shown to exhibit the same morphological transitions as observed in metallic alloys of monotectic composition. Both monotectic and hypermonotectic composition samples were directionally solidified in order to gain an improved understanding of the manner in which the excess hypermonotectic liquid is incorporated into the solidifying structure. The processing conditions utilized prevented sedimentation of the excess hypermonotectic liquid by directionally solidifying the samples in very thin (13 microns), horizontally oriented cells. High thermal gradient to growth rate ratios (G/R) were used in an effort to prevent constitutional supercooling and the subsequent formation of L(sub 2) droplets in advance of the solidification front during the growth of fibrous composite structures. Results demonstrated that hypermonotectic composites could be produced in samples up to two weight percent off of the monotectic composition by using a G/R ratio greater than or equal to 4.6 x 10(exp 4) C(s)/mm(sup 2) to avoid constitutional supercooling. For hypermonotectic samples processed with G/R ratios below 4.6 x 10(exp 4) C(s)/mm(sup 2), constitutional supercooling occurred and resulted in slight interfacial instability. For these samples, two methods of incorporation of the hypermonotectic liquid were observed and are reported. The correlation between the phase spacing, lambda, and the growth rate, R, was examined and was found to obey a relationship generally associated with a diffusion controlled coupled growth process. For samples with compositions ranging from the monotectic composition up to 2 percent off of the monotectic composition, data indicated that the square of the phase spacing (lambda) varied linearly with the inverse of the growth rate (R).
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NASA Technical Reports Server (NTRS)
Curreri, P. A.; Kaukler, W. F.
1986-01-01
Five hypermonotectic Al-In-Sn compositions were directionally solidified in a Bridgman-type furnace at normal gravity and during aircraft low-gravity maneuvers. The tendency of the Al-30In alloy to form an indium-rich band at the start of unidirectional growth (SUG) made it difficult to study the integration of L sub 2 into the solidification interface. Hypermonotectic compositions closer to monotectic slightly hypermonotectic caused only a partial band on L sub 2 to form at SUG and allowed the study of such variables as gravity, composition, and monotectic dome height on integration of excess L sub 2 into the solid plus L sub 2 interface. It was found that formation of aligned composite structures for the Al-In-Sn system is not only a function of G and R but also of the degree to which the composition varies from monotectic. Most of the aligned fibrous structures formed from hypermonotectic Al-In-Sn had spacings that were of the order of irregular fibrous structures reported for on monotectic Al-In-Sn. The spacings for the large fibers and aligned globules found for ground and low-gravity processed Al-In-18-Sn-22, respectively, were significantly larger than the others measured and were of the order expected for cell spacings under the growth conditions utilized. It was found that the integration into the solidification front of excess L sub 2 in low gravity was a function of the Sn composition of the alloy.
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Real-Time X-Ray Transmission Microscopy of Solidifying Al-In Alloys
NASA Technical Reports Server (NTRS)
Curreri, Peter A.; Kaukler, William F.
1997-01-01
Real-time observations of transparent analog materials have provided insight, yet the results of these observations are not necessarily representative of opaque metallic systems. In order to study the detailed dynamics of the solidification process, we develop the technologies needed for real-time X ray microscopy of solidifying metallic systems, which has not previously been feasible with the necessary resolution, speed, and contrast. In initial studies of Al-In monotectic alloys unidirectionally solidified in an X-ray transparent furnace, in situ records of the evolution of interface morphologies, interfacial solute accumulation, and formation of the monotectic droplets were obtained for the first time: A radiomicrograph of Al-30In grown during aircraft parabolic maneuvers is presented, showing the volumetric phase distribution in this specimen. The benefits of using X-ray microscopy for postsolidification metallography include ease of specimen preparation, increased sensitivity, and three-dimensional analysis of phase distribution. Imaging of the solute boundary layer revealed that the isoconcentration lines are not parallel (as is often assumed) to the growth interface. Striations in the solidified crystal did not accurately decorate the interface position and shape. The monotectic composition alloy under some conditions grew in an uncoupled manner.
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Abdelkader, Hamdy; Abdallah, Ossama Y; Salem, Hesham; Alani, Adam W G; Alany, Raid G
2014-10-01
The solid-state interactions of fused mixtures nimesulide (ND) with polyethylene glycol (PEG) 4000, urea or mannitol were studied through constructing thaw-melt phase equilibrium diagrams. The solid-state characteristics were investigated using differential scanning calorimetry (DSC) and X-ray diffraction (XRD). Various types of interactions were identified such as the formation of a eutectic system of ND-PEG 4000, monotectic system of ND-urea and complete solid immiscibility of ND with mannitol. The effects of carrier concentrations on the equilibrium solubility and in-vitro dissolution characteristics were studied. Linear increases (R(2) > 0.99) in the aqueous solubility of ND in various concentrations of PEG 4000 and urea were obtained, whereas mannitol did not exhibit any effect on the solubility of ND. Similar trends were obtained with the dissolution efficiency of the fused mixtures of ND with PEG 4000 and urea compared with the corresponding physical mixtures and untreated drug. The analgesic effects of untreated ND and the selected formulations were investigated by evaluating the drug's ability to inhibit the acetic acid-induced writhing response. The analgesic effect of ND in a eutectic mixture with PEG 4000 and a monotectic mixture with urea was potentiated by 3.2 and 2.7-fold respectively compared with the untreated drug. © 2014 Royal Pharmaceutical Society.
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A study of surface tension driven segregation in monotectic alloy systems
NASA Technical Reports Server (NTRS)
Andrews, J. Barry; Andrews, Rosalia N.; Gowens, Terrell F.
1988-01-01
The compatibilities of various monotectic alloy systems with several different crucible materials were evaluated. The study was carried out using small candidate alloy samples of compositions that produced fifty volume percent of each liquid phase at the monotectic temperature. Compatibility was based on the evaluation of the wetting tendency of the two immiscible phases with the crucible material in a one-g solidified sample. Three types of wetting phenomena were observed during the evaluation. Type 1 indicates an alloy-crucible combination where the L2 phase preferentially wets the crucible material. Since L2 is usually the minority phase in desirable alloys, this material combination would be difficult to process and is therefore considered incompatible. Type 2 behavior indicates an alloy-crucible combination where the L1 phase preferentially wets the crucible material. This type of combination is considered compatible since surface tension effects should aid in processing the alloy to a useful form. Type 3 indicates any combination that leads to major reactions between the alloy and crucible material, gas entrapment, or separation of the metal from the crucible wall. Additional compatibility evaluations would have to be carried out on combinations of this category. The five alloy systems studied included aluminum-bismuth, copper-lead, aluminum-indium, aluminum-lead and cadmium-gallium. The systems were combined with crucibles of alumina, boron nitride, mullite, quartz, silicon carbide and zirconia.
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Fluid flow in solidifying monotectic alloys
NASA Technical Reports Server (NTRS)
Ecker, A.; Frazier, D. O.; Alexander, J. Iwan D.
1989-01-01
Use of a two-wavelength holographic technique results in a simultaneous determination of temperature and composition profiles during directional solidification in a system with a miscibility gap. The relationships among fluid flow, phase separation, and mass transport during the solidification of the monotectic alloy are discussed. The primary sources of fluid motion in this system are buoyancy and thermocapillary forces. These forces act together when phase separation results in the formation of droplets (this occurs at the solid-liquid interface and in the bulk melt). In the absence of phase separation, buoyancy results from density gradients related to temperature and compositional gradients in the single-phase bulk melt. The effects of buoyancy are especially evident in association with water- or ethanol-rich volumes created at the solid-liquid growth interface.
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Cellular solidification of transparent monotectics
NASA Technical Reports Server (NTRS)
Kaulker, W. F.
1986-01-01
Understanding how liquid phase particles are engulfed or pushed during freezing of a monotectic is addressed. The additional complication is that the solid-liquid interface is nonplanar due to constitutional undercooling. Some evidence of particle pushing where the particles are the liquid phase of the montectic was already observed. Cellular freezing of the succinonitrile-glycerol system also occurred. Only a few compositions were tested at that time. The starting materials were not especially pure so that cellular interface observed was likely due to the presence of unkown impurities, the major portion of which was water. Topics addressed include: the effort of modeling the particle pushing process using the computer, establishing an apparatus for the determination of phase diagrams, and the measurement of the temperature gradients with a specimen which will solidify on the temperature gradient microscope stage.
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FNAS modify matric and transparent experiments
NASA Technical Reports Server (NTRS)
Smith, Guy A.; Kosten, Sue E.; Workman, Gary L.
1992-01-01
Monotectic alloy materials are created by rapid melt/rapid solidification processing on the NASA KC-135. Separation of the uniform liquid into two liquids may occur by either of two processes; spinodal decomposition or nucleation followed by growth. In the first case, the liquid is unstable to composition waves, which form and grow, giving liquids of two different compositions. In the latter process discrete particles of the second liquid phase form via thermal fluctuations and then grow by diffusion. The two processes are very different, with the determining process being dictated by temperature, composition, and thermodynamic characteristics of the alloy. The first two quantities are process variables, while the third is determined by electronic interactions between the atoms in the alloy. In either case the initial alloy decomposition is followed by coarsening, resulting in growth of the particle size at nearly constant volume fraction. In particular, reduced gravity experiments on monotectic solutions have shown a number of interesting results in the KC-135. Monotectic solutions exhibit a miscibility gap in the liquid state, and consequently, gravity driven forces can dominate the solidification parameters at 1 g. In reduced gravity however, the distribution of the phases is different, resulting in new and interesting microstructures. The Rapid Melt/Rapid Quench Furnace allows one to melt a sample and resolidify it in one parabola of the KC-135's flight path, thus eliminating any accumulative influence of multiple parabolas to affect the microstructure of the material.
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Separation processes during binary monotectic alloy production
NASA Technical Reports Server (NTRS)
Frazier, D. O.; Facemire, B. R.; Kaukler, W. F.; Witherow, W. K.; Fanning, U.
1984-01-01
Observation of microgravity solidification processes indicates that outside of sedimentation, at least two other important effects can separate the phases: critical-point wetting and spreading; and thermal migration of second-phase droplets due to interfacial tension gradients. It is difficult to study these surface tension effects while in a unit gravity field. In order to investigate the processes occurring over a temperature range, i.e., between a consolute point and the monotectic temperature, it is necessary to use a low-gravity environment. The MSFC drop tube (and tower), the ballistic trajectory KC-135 airplane, and the Space Shuttle are ideal facilities to aid formation and testing of hypotheses. Much of the early work in this area focuses on transparent materials so that process dynamics may be studied by optical techniques such as photography for viewing macro-processes; holography for studying diffusional growth; spinodal decomposition and coalescence; ellipsometry for surface wetting and spreading effects; and interferometry and spectroscopy for small-scale spatial resolution of concentration profiles.
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Specific heat and related thermophysical properties of liquid Fe-Cu-Mo alloy
NASA Astrophysics Data System (ADS)
Wang, Haipeng; Luo, Bingchi; Chang, Jian; Wei, Bingbo
2007-08-01
The specific heat and related thermophysical properties of liquid Fe77.5Cu13Mo9.5 monotectic alloy were investigated by an electromagnetic levitation drop calorimeter over a wide temperature range from 1482 to 1818 K. A maximum undercooling of 221 K (0.13 T m) was achieved and the specific heat was determined as 44.71 J·mol-1·K-1. The excess specific heat, enthalpy change, entropy change and Gibbs free energy difference of this alloy were calculated on the basis of experimental results. It was found that the calculated results by traditional estimating methods can only describe the solidification process under low undercooling conditions. Only the experimental results can reflect the reality under high undercooling conditions. Meanwhile, the thermal diffusivity, thermal conductivity, and sound speed were derived from the present experimental results. Furthermore, the solidified microstructural morphology was examined, which consists of (Fe) and (Cu) phases. The calculated interface energy was applied to exploring the correlation between competitive nucleation and solidification microstructure within monotectic alloy.
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Ellipsometric measurement of liquid film thickness
NASA Technical Reports Server (NTRS)
Chang, Ki Joon; Frazier, D. O.
1989-01-01
The immediate objective of this research is to measure liquid film thickness from the two equilibrium phases of a monotectic system in order to estimate the film pressure of each phase. Thus liquid film thicknesses on the inside walls of the prism cell above the liquid level have been measured elliposmetrically for the monotectic system of succinonitrile and water. The thickness varies with temperature and composition of each plane. The preliminary results from both layers at 60 deg angle of incidence show nearly uniform thickness from about 21 to 23 C. The thickness increases with temperature but near 30 C the film appears foggy and scatters the laser beam. As the temperature of the cell is raised beyond room temperature it becomes increasingly difficult to equalize the temperature inside and outside the cell. The fogging may also be an indication that solution, not pure water, is adsorbed onto the substrate. Nevertheless, preliminary results suggest that ellipsometric measurement is feasible and necessary to measure more accurately and rapidly the film thickness and to improve thermal control of the prism walls.
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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.
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Liquid-liquid phase separation of freely falling undercooled ternary Fe-Cu-Sn alloy
NASA Astrophysics Data System (ADS)
Wang, W. L.; Wu, Y. H.; Li, L. H.; Zhai, W.; Zhang, X. M.; Wei, B.
2015-11-01
The active modulation and control of the liquid phase separation for high-temperature metallic systems are still challenging the development of advanced immiscible alloys. Here we present an attempt to manipulate the dynamic process of liquid-liquid phase separation for ternary Fe47.5Cu47.5Sn5 alloy. It was firstly dispersed into numerous droplets with 66 ~ 810 μm diameters and then highly undercooled and rapidly solidified under the containerless microgravity condition inside drop tube. 3-D phase field simulation was performed to explore the kinetic evolution of liquid phase separation. Through regulating the combined effects of undercooling level, phase separation time and Marangoni migration, three types of separation patterns were yielded: monotectic cell, core shell and dispersive structures. The two-layer core-shell morphology proved to be the most stable separation configuration owing to its lowest chemical potential. Whereas the monotectic cell and dispersive microstructures were both thermodynamically metastable transition states because of their highly active energy. The Sn solute partition profiles of Fe-rich core and Cu-rich shell in core-shell structures varied only slightly with cooling rate.
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Study on solidification of immisible alloys (M-10)
NASA Technical Reports Server (NTRS)
Kamio, Akihiko
1993-01-01
Alloying of immiscible alloys under microgravity is of interest in metallurgical processes. Several experiments investigating the alloying of immiscible alloys, such as Al-In, Al-Bi, Zn-Bi, and Zn-Pb, were done in space. Homogeneous distribution of small L2 particles in the matrix, such as an emulsion structure, was expected in the space-solidifed alloys. However, the alloys demonstrated an extremely segregated structure. To date insufficient information was obtained to explain these unexpected results. Our experiment was proposed to clarify the solidification manner of immiscible alloys and to obtain fundamental information concerning structural control of the alloys. In space, density differences between the two liquids separated in immiscible regions can be neglected, so that no sedimentation of L(sub 2) phase will take place. When the growth of the alloys is interrupted and this status is frozen by an adequate rapid cooling procedure, it will provide much information concerning decomposing homogeneous liquid and the interaction between the monotectic growth front morphology and the distribution of L(sub 2) phase. It is anticipated that the results will be useful for elucidating the monotectic solidification manner and it will be instructive to explain the segregated structures obtained in the past space experiments.
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Law, Devalina; Wang, Weili; Schmitt, Eric A; Long, Michelle A
2002-03-01
To define an index based on the van't Hoff equation that can be used as a screening tool for predicting poly(ethylene) glycol (PEG)-drug eutectic composition. Phase diagrams of PEG with ritonavir, ibuprofen, fenofibrate. naproxen, and griseofulvin were constructed using differential scanning calorimetry, hot stage microscopy and powder X-ray diftractometry. Previously reported phase diagrams were also used to test the predictive capability of the index. This work shows that a modified van't Hoff equation can be used to model the drug liquidus line of these phase diagrams. The slope of the liquidus line depends on the melting point (T(f)d) and heat of fusion (deltaH(f)d) of the drug and describes the initial rate at which the eutectic or monotectic point is approached. Based on this finding, a dimensionless index Ic was defined. The index can be calculated from the melting points of the pure components and heat of fusion of the drug. In addition to the compounds listed above, the index was found to predict the eutectic composition for flurbiprofen, temazepam and indomethacin. These compounds range over 150 degrees C in T(f)d, and from 25-65 kJ/mole in deltaH(f)d. Using Ic the approximate eutectic composition for eight different compounds was predicted. The index provides a useful screening tool for assessing the maximum drug loading in a drug-polymer eutectic/monotectic formulation.
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NASA Astrophysics Data System (ADS)
Yakovleva, A. O.; Belov, N. A.; Bazlova, T. A.; Shkalei, I. V.
2018-01-01
The effect of low-melting metals (Pb, Bi, Cd, In) on the structure, phase composition, and properties of the Al-5% Si-4% Cu alloy was studied using calculations. Polythermal sections have been reported, which show that the considered systems are characterized by the presence of liquid regions and monotectic reactions. The effect of low-melting metals on the microstructure and hardening of base alloy in the cast and heat-treated states has been studied.
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Metal-halide mixtures for latent heat energy storage
NASA Astrophysics Data System (ADS)
Chen, K.; Manvi, R.
Some candidates for alkali metal and alkali halide mixtures suitable for thermal energy storage at temperatures 600 C are identified. A solar thermal system application which offer advantages such as precipitation of salt crystals away from heat transfer surfaces, increased thermal conductivity of phase change materials, corrosion inhibition, and a constant monotectic temperature, independent of mixture concentrations. By using the lighters, metal rich phase as a heat transfer medium and the denser, salt rich phase as a phase change material for latent heat storage, undesirable solidification on the heat transfer surface may be prevented, is presented.
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Metal-halide mixtures for latent heat energy storage
NASA Technical Reports Server (NTRS)
Chen, K.; Manvi, R.
1981-01-01
Some candidates for alkali metal and alkali halide mixtures suitable for thermal energy storage at temperatures 600 C are identified. A solar thermal system application which offer advantages such as precipitation of salt crystals away from heat transfer surfaces, increased thermal conductivity of phase change materials, corrosion inhibition, and a constant monotectic temperature, independent of mixture concentrations. By using the lighters, metal rich phase as a heat transfer medium and the denser, salt rich phase as a phase change material for latent heat storage, undesirable solidification on the heat transfer surface may be prevented, is presented.
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Investigations on transparent liquid-miscibility gap systems
NASA Technical Reports Server (NTRS)
Lacy, L. L.; Nishioka, G.; Ross, S.
1979-01-01
Sedimentation and phase separation is a well known occurrence in monotectic or miscibility gap alloys. Previous investigations indicate that it may be possible to prepare such alloys in a low-gravity space environment but recent experiments indicate that there may be nongravity dependent phase separation processes which can hinder the formation of such alloys. Such phase separation processes are studied using transparent liquid systems and holography. By reconstructing holograms into a commercial-particle-analysis system, real time computer analysis can be performed on emulsions with diameters in the range of 5 micrometers or greater. Thus dynamic effects associated with particle migration and coalescence can be studied. Characterization studies on two selected immiscible systems including an accurate determination of phase diagrams, surface and interfacial tension measurements, surface excess and wetting behavior near critical solution temperatures completed.
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Factors affecting the formation of eutectic solid dispersions and their dissolution behavior.
Vippagunta, Sudha R; Wang, Zeren; Hornung, Stefanie; Krill, Steven L
2007-02-01
The objective of this work was to obtain a fundamental understanding of the factors, specifically the properties of poorly water-soluble drugs and water-soluble carriers, which influence predominantly, the formation of eutectic or monotectic crystalline solid dispersion and their dissolution behavior. A theoretical model was applied on five poorly water-soluble drugs (fenofibrate, flurbiprofen, griseofulvin, naproxen, and ibuprofen) having diverse physicochemical properties and water-soluble carrier (polyethylene glycol (PEG) 8000) for the evaluation of these factors. Of these, two drugs, fenofibrate and flurbiprofen, and PEG of different molecular weights (3350, 8000, and 20000), were chosen as model drugs and carriers for further investigation. Experimental phase diagrams were constructed and dissolution testing was performed to assess the performance of the systems. The theoretical model predicted the formation of eutectic or monotectic solid dispersions of fenofibrate, griseofulvin, ibuprofen, and naproxen with PEG, holding the contribution of specific intermolecular interactions between compound and carrier to zero. In the case of the flurbiprofen-PEG eutectic system, intermolecular interactions between drug and polymer needed to be taken into consideration to predict the experimental phase diagram. The results of the current work suggest that the thermodynamic function of melting point and heat of fusion (as a measure of crystal energy of drug) plays a significant role in the formation of a eutectic system. Lipophilicity of the compound (as represented by cLog P) was also demonstrated to have an effect. Specific interactions between drug and carrier play a significant role in influencing the eutectic composition. Molar volume of the drug did not seem to have an impact on eutectic formation. The polymer molecular weight appeared to have an impact on the eutectic composition for flurbiprofen, which exhibits specific interactions with PEG, whereas no such impact of polymer molecular weight on eutectic composition was observed for fenofibrate, which does not exhibit specific interactions with PEG. The impact of polymer molecular weight on dissolution of systems where specific drug-polymer interactions are exhibited was also observed. The current work provides valuable insight into factors affecting formation and dissolution of eutectic systems, which can facilitate the rational selection of suitable water-soluble carriers. Copyright (c) 2006 Wiley-Liss, Inc.
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NASA Astrophysics Data System (ADS)
Stinn, Caspar; Nose, Katsuhiro; Okabe, Toru; Allanore, Antoine
2017-12-01
The phase diagram of the barium sulfide-copper(I) sulfide system was investigated above 873 K (600 °C) using a custom-built differential thermal analysis (DTA) apparatus. The melting point of barium sulfide was determined utilizing a floating zone furnace. Four new compounds, Ba2Cu14S9, Ba2Cu2S3, Ba5Cu4S7, and Ba9Cu2S10, were identified through quench experiments analyzed with wavelength dispersive X-ray spectroscopy (WDS) and energy dispersive X-ray analysis (EDS). A miscibility gap was observed between 72 and 92 mol pct BaS using both DTA experiments and in situ melts observation in a floating zone furnace. A monotectic was observed at 94.5 mol pct BaS and 1288 K (1015 °C).
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Bootello, Miguel A; Hartel, Richard W; Garcés, Rafael; Martínez-Force, Enrique; Salas, Joaquín J
2012-10-01
Cocoa butter equivalents (CBEs) are produced from vegetable fats by blending palm mid fraction (PMF) and tropical butters coming from shea, mango kernel or kokum fat. In this regard, high oleic-high stearic (HOHS) sunflower hard stearins from solvent fractionation can be used in CBE production since their compositions and physical properties are similar to those found in the above-mentioned tropical butters. In this work, three sunflower hard stearins (SHS) ranging from 65% to 95% of disaturated triacylglycerols and a shea stearin (used as reference) were blended with PMF to evaluate their potential use in CBEs formulation. Isosolid phase diagrams of mixtures of PMF/SHS showed eutectic formation for SHS 65 and SHS 80, but monotectic behaviour with softening effect for SHS 95. Three CBEs from SHS and shea stearin were formulated according to phase behaviour diagrams and solid fat content data at 25 °C. Isosolid phase diagrams of mixtures of these CBEs with cocoa butter showed no eutectic behaviour. Therefore, CBEs elaborated from SHS exhibited full compatibility with cocoa butter. Copyright © 2012 Elsevier Ltd. All rights reserved.
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NASA Astrophysics Data System (ADS)
Wang, Chao-hong; Kuo, Chun-yi; Yang, Nian-cih
2015-11-01
The isothermal section of the ternary Sn-Pb-Co system at 250°C was experimentally determined through a series of the equilibrated Sn-Pb-Co alloys of various compositions. The equilibrium phases were identified on the basis of compositional analysis. For the Sn-Co intermetallic compounds (IMCs), CoSn3, CoSn2, CoSn and Co3Sn2, the Pb solubility was very limited. There exist five tie-triangle regions. The Co-Pb system involves one monotectic reaction, so the phase separation of liquid alloys near the Co-Pb side occurred prior to solidification. The immiscibility field was also determined. Additionally, interfacial reactions between Co and Sn-Pb alloys were conducted. The reaction phase for the Sn-48 at.%Pb and Sn-58 at.%Pb at 250°C was CoSn3 and CoSn2, respectively. Both of them were simultaneously formed in the Sn-53 at.%Pb/Co. The formed IMCs were closely associated to the phase equilibria relationship of the liquid-CoSn3-CoSn2 tie-triangle. Furthermore, with increasing temperatures, the phase formed in equilibrium with Sn-37 wt.%Pb was found to transit from CoSn3 to CoSn2 at 275°C. We propose a simple method of examining the phase transition temperature in the interfacial reactions to determine the boundaries of the liquid-CoSn3-CoSn2 tie-triangles at different temperatures.
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Real Time Characterization of Solid/Liquid Interfaces During Directional Solidification
NASA Technical Reports Server (NTRS)
Sen, S.; Kaukler, W. K.; Curreri, P. A.; Peters, P.
1997-01-01
A X-Ray Transmission Microscope (XTM) has been developed to observe in real time and in-situ solidification phenomenon at the solid/liquid interface. Recent improvements in the horizontal Bridgman furnace design provides real-time magnification (during solidification) up to 12OX. The increased magnification has enabled for the first time the XTM imaging of real-time growth of fibers and particles with diameters of 3-6 micrometers. Further, morphological transitions from planar to cellular interfaces have also been imaged. Results from recent XTM studies on Al-Bi monotectic system, Al-Au eutectic system and interaction of insoluble particles with s/I interfaces in composite materials will be presented. An important parameter during directional solidification of molten metal is the interfacial undercooling. This parameter controls the morphology and composition at the s/I interface. Conventional probes such as thermocouples, due to their large bead size, do not have sufficient resolution for measuring undercooling at the s/I interface. Further, the intrusive nature of the thermocouples also distorts the thermal field at the s/I interface. To overcome these inherent problems we have recently developed a compact furnace which utilizes a non-intrusive technique (Seebeck) to measure undercooling at the S/I interface. Recent interfacial undercooling measurements obtained for the Pb-Sn system will be presented. The Seebeck measurement furnace in the future will be integrated with the XTM to provide the most comprehensive tool for real time characterization of s/I interfaces during solidification.
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Effects of cooling rate and Al on MnS formation in medium-carbon non-quenched and tempered steels
NASA Astrophysics Data System (ADS)
Li, Meng-long; Wang, Fu-ming; Li, Chang-rong; Yang, Zhan-bing; Meng, Qing-yong; Tao, Su-fen
2015-06-01
The effect of Al on the morphology of MnS in medium-carbon non-quenched and tempered steel was investigated at three different cooling rates of 0.24, 0.43, and 200°C·s-1. The formation mechanisms of three types of MnS were elucidated based on phase diagram information combined with crystal growth models. The morphology of MnS is governed by the precipitation mode and the growth conditions. A monotectic reaction and subsequent fast solidification lead to globular Type I MnS. Type II MnS inclusions with different morphological characteristics form as a result of a eutectic reaction followed by the growth in the Fe matrix. Type III MnS presents a divorced eutectic morphology. At the cooling rate of 0.24°C·s-1, the precipitation of dispersed Type III MnS is significantly enhanced by the addition of 0.044wt% acid-soluble Al (Als), while Type II MnS clusters prefer to form in steels with either 0.034wt% or 0.052wt% Als. At the relatively higher cooling rates of 200°C·s-1 and 0.43°C·s-1, the formation of Type I and Type II MnS inclusions is promoted, and the influence of Al is negligible. The results of this work are expected to be employed in practice to improve the mechanical properties of non-quenched and tempered steels.
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Fundamental Studies of Solidification in Microgravity Using Real-Time X-Ray Microscopy
NASA Technical Reports Server (NTRS)
Curreri, Peter A.; Kaukler, William; Sen, Subhayu; Bhat, Biliyar N.
1999-01-01
This research applies a state of the art X-ray Transmission Microscope, XTM, to image (with resolutions up to 3 micrometers) the solidification of metallic or semiconductor alloys in real-time. We have successfully imaged in real-time: interfacial morphologies, phase growth, coalescence, incorporation of phases into the growing interface, and the solute boundary layer in the liquid at the solid-liquid interface. We have also measured true local growth rates and can evaluate segregation structures in the solid; a form of in-situ metallography. During this study, the growth of secondary phase fibers and lamellae from eutectic and monotectic alloys have been imaged during solidification, in real-time, for the first time in bulk metal alloys. Current high resolution X-ray sources and high contrast X-ray detectors have advanced to allow systematic study of solidification dynamics and the resulting microstructure. We have employed a state-of-the-art sub-micron source with acceleration voltages of 10-100 kV to image solidification of metals. One useful strength of the XTM stems from the manner an image is formed. The radiographic image is a shadow formed by x-ray photons that are not absorbed as they pass through the specimen. Composition gradients within the specimen cause variations in absorption of the flux such that the final image represents a spatial integral of composition (or thickness). The ability to image these features in real-time enables more fundamental and detailed understanding of solidification dynamics than has previously been possible. Hence, application of this technique towards microgravity experiments will allow rigorous testing of critical solidification models.
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Solution based synthesis of mixed-phase materials in the Li2TiO3-Li4SiO4 system
NASA Astrophysics Data System (ADS)
Hanaor, Dorian A. H.; Kolb, Matthias H. H.; Gan, Yixiang; Kamlah, Marc; Knitter, Regina
2015-01-01
As candidate tritium breeder materials for use in the ITER helium cooled pebble bed, ceramic multiphasic compounds lying in the region of the quasi-binary lithium metatitanate-lithium orthosilicate system may exhibit mechanical and physical advantages relative to single phase materials. Here we present an organometallic solution-based synthesis procedure for the low-temperature fabrication of compounds in the Li2TiO3-Li4SiO4 region and investigate phase stability and transformations through temperature varied X-ray diffraction and scanning calorimetry. Results demonstrate that the metatitanate and metasilicate phases Li2TiO3 and Li2SiO3 readily crystallise in nanocrystalline form at temperatures below 180 °C. Lithium deficiency in the region of 5% results from Li sublimation from Li4SiO4 and/or from excess Li incorporation in the metatitanate phase and brings about a stoichiometry shift, with product compounds exhibiting mixed lithium orthosilicate/metasilicate content towards the Si rich region and predominantly Li2TiO3 content towards the Ti rich region. Above 1150 °C the transformation of monoclinic to cubic γ-Li2TiO3 disordered solid-solution occurs while the melting of silicate phases indicates a likely monotectic type system with a solidus line in the region 1050-1100 °C. Synthesis procedures involving a lithium chloride precursor are not likely to be a viable option for breeder pebble synthesis as this route was found to yield materials with a more significant Li-deficiency exhibiting the crystallisation of the Li2TiSiO5 phase at intermediate compositions.
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Coupled Growth in Hypermonotectics
NASA Technical Reports Server (NTRS)
Andrews, J. Barry; Coriell, Sam R.
2001-01-01
The overall objective of this project is to obtain a fundamental understanding of the physics controlling solidification processes in immiscible alloy systems. The investigation involves both experimentation and the development of a model describing solidification in monotectic systems. The experimental segment was designed to first demonstrate that it is possible to obtain interface stability and steady state coupled growth in hypermonotectic alloys through microgravity processing. Microgravity results obtained to date have verified this possibility. Future flights will permit experimental determination of the limits of interface stability and the influence of alloy composition and growth rate on microstructure. The objectives of the modeling segment of the investigation include prediction of the limits of interface stability, modeling of convective flow due to residual acceleration, and the influence of surface tension driven flows at the solidification interface. The study of solidification processes in immiscible alloy systems is hindered by the inherent convective flow that occurs on Earth and by the possibility of sedimentation of the higher density immiscible liquid phase. It has been shown that processing using a high thermal gradient and a low growth rate can lead to a stable macroscopically planar growth front even in hypermonotectic alloys. Processing under these growth conditions can avoid constitutional supercooling and prevent the formation of the minor immiscible liquid phase in advance of the solidification front. However, the solute depleted boundary layer that forms in advance of the solidification front is almost always less dense than the liquid away from the solidification front. As a result, convective instability is expected. Ground based testing has indicated that convection is a major problem in these alloy systems and leads to gross compositional variations along the sample and difficulties maintaining interface stability. Sustained low gravity processing conditions are necessary in order to minimize these problems and obtain solidification conditions which approach steady state.
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NASA Technical Reports Server (NTRS)
deGroh, Henry C., III
1999-01-01
This is a survey of the published works of Prof. Bingbo Wei of the Department of Applied Physics at Northwestern Polytechnical University, Xian P.R. China. Transformations among solid - liquid - and vapor are fundamental to the foundations of life and culture on Earth. The development and understanding of materials has lead the evolution and advancement of the human race since antiquity. Materials and fluids research is continuing today, with us standing on the shoulders of those that have gone before us. Technological and scientific breakthroughs continue due to studies of greater and greater complexity, that include for example, research done at high pressures, in high magnetic fields, at temperatures near absolute zero, and in the low gravity environment of low Earth orbit. Of particular technological importance is the liquid to solid transformation of metals and alloys. Solidification processing is generally the most important factor in the final properties of objects made of metal; and undercooling is the fundamental driving force for all solidification. The interest and resources dedicated to the study of solidification and undercooling are great and World wide. For many years B. Wei and his coworkers have been studying undercooling and rapid solidification and have amassed a significant body of published research in this important field, contributing to the leading edge of the state-of-the-art. It is the goal of this memorandum to provide a review of the research of B. Wei et al.; publications in Chinese are included in the reference list but are not discussed. The bulk of Wei's work has been in the area of undercooling and rapid solidification [1-11, 13-16, 24-36] with papers dating back to 1989, the same year he earned his Ph.D. Below, discussions of Wei's undercooling and rapid solidification research have been grouped together mostly on the basis of alloy type, such as eutectic, intermetallic, or monotectic.