Hybrid Contactless Heating and Levitation

NASA Technical Reports Server (NTRS)

Lee, M. C.

1985-01-01

Acoustic and electromagnetic fields applied. In contactless processing apparatus, acoustic and electromagnetic levitating fields employed alternately or simultaneously with amplitude of each controlled to produce various combinations of heating, cooling, and levitation. Apparatus provides rapid heating and cooling or slow heating and cooling for such processes as nucleation, crystallization, incubation, deep undercooling, and heterogeneity control.

Treatment of TNT red water by layer melt crystallization.

PubMed

Jo, Jeong-Hyeon; Ernest, Takyi; Kim, Kwang-Joo

2014-09-15

Treatment of the red water, which is wastewater of 2,4,6- trinitrotoluene (TNT) manufacturing process has been explored using ice crystallization. This study focuses on the formation of ice crystals from the red water in a layer crystallizer under various operating conditions. Among the parameters which affect layer crystallization, attention was given to cooling rate, cooling temperature, sweating rate and concentration of the red water. The study highlights the effect of subcooling and growth rate on purity of the ice crystalline layers produced. After sweating, the COD value of crystalline ice layer was significantly reduced from 10,000 mg/L to below 20mg/L. Most organic contaminants were removed in sweating fractions of 0.5. Eventually, the red water was treated by layer crystallization combined with the sweating process. Copyright © 2014 Elsevier B.V. All rights reserved.

On the morphological and chemical stability of vitamin C crystals

NASA Astrophysics Data System (ADS)

Halász, Susan; Bodor, Beáta

1993-03-01

Mass cooling crystallization of aqueous vitamin C solution was studied by applying different cooling rates, initial supersaturations and mixing intensity. The morphology of the products (size, habit and colour) well followed the changes of process parameters. Comparing a high purity (99.9%) standard with a yellow coloured heterodisperse product and a slowly grown single crystal, HPLC chromatography detected decreasing purity of the bigger single crystals, while X-ray and NMR analysis did not show any perceptible difference. It has been concluded that not the surface oxidation (chemical degredation), but rather the inclusions are the main sources of impurities within the crystals.

Spectroscopic and laser cooling results on Yb3+-doped BaY2F8 single crystal

NASA Astrophysics Data System (ADS)

Bigotta, Stefano; Parisi, Daniela; Bonelli, Lucia; Toncelli, Alessandra; Tonelli, Mauro; Di Lieto, Alberto

2006-07-01

Anti-Stokes cooling has been observed in an Yb3+-doped BaY2F8 single crystal. Single crystals have been grown by the Czochralski technique. The absorption spectra and the emission properties have been measured at room temperature and at 10K. The energy positions of the Stark sublevels of the ground and the excited state manifolds have been determined and separated from the vibronic substructure. The intrinsic decay time of the F5/22 level has been measured taking care of avoiding the effect of multiple reabsorption processes. The theoretical and experimental cooling efficiencies of Yb:BaY2F8 are evaluated and compared with respect to those of the most frequently investigated materials for laser cooling. A temperature drop of almost 4K was measured by pumping the crystal with 3W of laser radiation at ˜1025nm in single pass configuration with a cooling efficiency of ˜3%.

The Effect of the Wall Contact and Post-Growth C001-Down on Defects in CdTe Crystals Grown by Contactless PVT

NASA Technical Reports Server (NTRS)

Palosz, W.; Grasza, K.; Dudley, M.; Raghothamachar, B.; Cai, L.; Durose, K.; Halliday, D.; Boyall, N. M.; Rose, M. Franklin (Technical Monitor)

2001-01-01

In crystal growth, the quality of the final material may depend, among other factors, on its interaction with the walls of the ampoule during and after the growth, and on the rate of the crystal cool-down at the end of ate the process. To investigate the above phenomena, a series of CdTe crystal growth processes was carried out, The crystals were grown by physical vapor transport without contact with the side walls of the silica glass ampoules, applying the Low Supersaturation Nucleation technique. The source temperature was 930 C, the undercooling was a few degrees. The crystals, having the diameter of 25 mm, grew at the rate of a few mm per day. The post-growth cool-down to the room temperature was conducted at different rates, and lasted from a few minutes to four days. The crystals were characterized using chemical etching low temperature luminescence, and Synchrotron White Beam X-ray Topography techniques. The dislocation (etch pit) density was measured and its distribution was analyzed by comparison with Poisson curves and with the Normalized Radial Distribution Correlation Function. It was found that the contact of the crystal with silica leads to a strain field and high (in the 105 sq cm range) dislocation (etch pit) density. Similar defect concentrations were found in crystals subjected to fast post-growth cool-down. Typical EPD values for lower cool-down rates and in regions not affected by wall interactions are in the lower 10(exp 4) sq cm range. In some areas the actual dislocation density was about 10(exp 3) sq cm or even less. No apparent effect of the cool-down rate on polygonization was observed. A fine structure could be discerned in low-temperature PL spectra of crystals with low dislocation density.

Device for isolation of seed crystals during processing of solution

DOEpatents

Montgomery, K.E.; Zaitseva, N.P.; Deyoreo, J.J.; Vital, R.L.

1999-05-18

A device is described for isolation of seed crystals during processing of solutions. The device enables a seed crystal to be introduced into the solution without exposing the solution to contaminants or to sources of drying and cooling. The device constitutes a seed protector which allows the seed to be present in the growth solution during filtration and overheating operations while at the same time preventing the seed from being dissolved by the under saturated solution. When the solution processing has been completed and the solution cooled to near the saturation point, the seed protector is opened, exposing the seed to the solution and allowing growth to begin. 3 figs.

Kinetic Controls on Formation of Textures in Rapidly Cooled Rocks

NASA Technical Reports Server (NTRS)

Lofgren, Gary E.

2006-01-01

The crystallization of silicate melts is a complex process involving melts usually produced by partial melting and cooling environments that are rapid in volcanic lavas or so slow as to be auto-metamorphic in plutonic regimes. The volcanic lavas are amenable to laboratory study as are chondrules that comprise the bulk of chondritic meteorites. Dynamic crystallization studies of basalt and chondrule melts have shown that nucleation has a more profound effect on the final texture than the cooling or crystal growth rates. The sequence of crystal shapes grown at increasing degrees of supercooling (DELTA T) or cooling rate demonstrates the effect of increasing growth rate. Equant or euhedral crystals become skeletal, then dendritic and ultimately spherulitic indicating the nucleation temperature and the DELTA T when growth began. Because crystals cannot grow until they nucleate, cooling rate does not always correlate with crystal growth rate and thus crystal shape. Silicate melts cooled at the same rate can have drastically different textures depending on the temperature of nucleation. A dynamic crystallization study of basaltic rocks shows that basaltic lavas must erupt with sufficient crystals present in the melt to act as nuclei and foster growth. With nuclei present, growth will begin when the temperature drops below the liquidus temperature and typical basaltic textures such as intersertal, intergranular or subophitic will form. If nuclei are not present, crystallization will not begin immediately and the DELTA T will increase until embryos in the melts become nuclei. The DELTA T present when grow begins dictates the growth rate and the crystal shapes and thus the rock texture. If nucleation is delayed, growth will take place at high DELTA T and the crystals will favor skeletal or dendritic shapes. Chondrules are usually considered crystallized melt droplets and clearly some are, but most are not. Most chondrules have porphyritic textures that cannot develop from totally melted droplets because nucleation is delayed during cooling and growth occurs at high DELTA T and the resulting textures are dendritic or spherulitic. The porphyritic textures will develop only if the chondrule is partially molten and begins to crystallize immediately upon cooling. Chondrule compositions are close to komatiites and these studies bear on the origin of their textures as well.

Measuring and modelling the structure of chocolate

NASA Astrophysics Data System (ADS)

Le Révérend, Benjamin J. D.; Fryer, Peter J.; Smart, Ian; Bakalis, Serafim

2015-01-01

The cocoa butter present in chocolate exists as six different polymorphs. To achieve the desired crystal form (βV), traditional chocolate manufacturers use relatively slow cooling (<2°C/min). A newer generation of rapid cooling systems has been suggested requiring further understanding of fat crystallisation. To allow better control and understanding of these processes and newer rapid cooling processes, it is necessary to understand both heat transfer and crystallization kinetics. The proposed model aims to predict the temperature in the chocolate products during processing as well as the crystal structure of cocoa butter throughout the process. A set of ordinary differential equations describes the kinetics of fat crystallisation. The parameters were obtained by fitting the model to a set of DSC curves. The heat transfer equations were coupled to the kinetic model and solved using commercially available CFD software. A method using single crystal XRD was developed using a novel subtraction method to quantify the cocoa butter structure in chocolate directly and results were compared to the ones predicted from the model. The model was proven to predict phase change temperature during processing accurately (±1°C). Furthermore, it was possible to correctly predict phase changes and polymorphous transitions. The good agreement between the model and experimental data on the model geometry allows a better design and control of industrial processes.

Kinetic study on the isothermal and nonisothermal crystallization of monoglyceride organogels.

PubMed

Meng, Zong; Yang, Lijun; Geng, Wenxin; Yao, Yubo; Wang, Xingguo; Liu, Yuanfa

2014-01-01

The isothermal and nonisothermal crystallization kinetics of monoglyceride (MAG) organogels were studied by pulsed nuclear magnetic resonance (pNMR) and differential scanning calorimetry (DSC), respectively. The Avrami equation was used to describe the isothermal crystallization kinetics and experimental data fitted the equation fairly well. Results showed that the crystal growth of MAG organogels was a rod-like growth of instantaneous nuclei at higher degrees of supercooling and a plate-like form with high nucleation rate at lower degrees of supercooling. The exothermic peak in nonisothermal DSC curves for the MAG organogels became wider and shifted to lower temperature when the cooling rate increased, and nonisothermal crystallization was analyzed by Mo equation. Results indicated that at the same crystallization time, to get a higher degree of relative crystallinity, a higher cooling rate was necessary. The activation energy of nonisothermal crystallization was calculated as 739.59 kJ/mol according to the Kissinger method. Therefore, as the results of the isothermal and nonisothermal crystallization kinetics for the MAG organogels obtained, the crystallization rate, crystal nucleation, and growth during the crystallization process could be preliminarily monitored through temperature and cooling rate regulation, which laid the foundation for the real industrial manufacture and application of the MAG organogels.

The effect factors of potassium dihydrogen phosphate crystallization in aqueous solution

NASA Astrophysics Data System (ADS)

Zhou, Cun; Sun, Fei; Liu, Xuzhao

2017-01-01

The effects of cooling rate and pH on the potassium dihydrogen phosphate crystallization process were studied by means of batch crystallization process. The experiment shows that with the increase of cooling rate, the metastable zone width increase and the induction period decrease. When the pH is 3.0, the metastable zone width and induction period are both the minimum, while the crystallization rate is the highest. The crystallization products were characterized by scanning election microscope. Potassium Dihydrogen Phosphate (KDP) is a kind of excellent nonlinear optical materials, and belongs to tetragonal system, and ideal shape is aggregate of tetragonal prism and tetragonal dipyramid, the (100) cone is alternating accumulation by double positive ions and double negative ions [1-4]. The crystals of aqueous solution method to grow have large electro-optical nonlinear coefficient and high loser-damaged threshold, and it is the only nonlinear optical crystal could be used in inertial confinement fusion (ICF), KDP crystals are the ideal system to study the native defects of complex oxide insulating material [5-7]. With the development of photovoltaic technology, KDP crystals growth and performance have become a research focus worldwide [8, 9]. The merits of the crystallization process directly affect the quality of KDP products, so the study of the effect of crystallization conditions has an important significance on industrial production. This paper studied the change rule of metastable zone width, induction period, crystallization rate and particle size distribution in crystal process, and discussed the technical condition of KDP crystallization.

Magma oceanography. II - Chemical evolution and crustal formation. [lunar crustal rock fractional crystallization model

NASA Technical Reports Server (NTRS)

Longhi, J.

1977-01-01

A description is presented of an empirical model of fractional crystallization which predicts that slightly modified versions of certain of the proposed whole moon compositions can reproduce the major-element chemistry and mineralogy of most of the primitive highland rocks through equilibrium and fractional crystallization processes combined with accumulation of crystals and trapping of residual liquids. These compositions contain sufficient Al to form a plagioclase-rich crust 60 km thick on top of a magma ocean that was initially no deeper than about 300 km. Implicit in the model are the assumptions that all cooling and crystallization take place at low pressure and that there are no compositional or thermal gradients in the liquid. Discussions of the cooling and crystallization of the proposed magma ocean show these assumptions to be disturbingly naive when applied to the ocean as a whole. However, the model need not be applied to the whole ocean, but only to layers of cooling liquid near the surface.

Optimization of cooling strategy and seeding by FBRM analysis of batch crystallization

NASA Astrophysics Data System (ADS)

Zhang, Dejiang; Liu, Lande; Xu, Shijie; Du, Shichao; Dong, Weibing; Gong, Junbo

2018-03-01

A method is presented for optimizing the cooling strategy and seed loading simultaneously. Focused beam reflectance measurement (FBRM) was used to determine the approximating optimal cooling profile. Using these results in conjunction with constant growth rate assumption, modified Mullin-Nyvlt trajectory could be calculated. This trajectory could suppress secondary nucleation and has the potential to control product's polymorph distribution. Comparing with linear and two step cooling, modified Mullin-Nyvlt trajectory have a larger size distribution and a better morphology. Based on the calculating results, the optimized seed loading policy was also developed. This policy could be useful for guiding the batch crystallization process.

An Investigation into the Polymorphism and Crystallization of Levetiracetam and the Stability of its Solid Form.

PubMed

Xu, Kailin; Xiong, Xinnuo; Guo, Liuqi; Wang, Lili; Li, Shanshan; Tang, Peixiao; Yan, Jin; Wu, Di; Li, Hui

2015-12-01

Levetiracetam (LEV) crystals were prepared using different solvents at different temperatures. The LEV crystals were systematically characterized by X-ray powder diffraction (XRPD) and morphological analysis. The results indicated that many kinds of crystal habits exist in a solid form of LEV. To investigate the effects of LEV concentration, crystallization temperature, and crystallization type on crystallization and solid phase transformation of LEV, multiple methods were performed for LEV aqueous solution to determine if a new solid form exists in solid-state LEV. However, XRPD data demonstrate that the LEV solid forms possess same spatial arrangements that are similar to the original solid form. This result indicates that the LEV concentration, crystallization temperature, and crystallization type in aqueous solution have no influence on the crystallization and solid phase transformation of LEV. Moreover, crystallization by sublimation, melt cooling, and quench cooling, as well as mechanical effect, did not result in the formation of new LEV solid state. During melt cooling, the transformation of solid form LEV is a direct process from melting amorphous phase to the original LEV crystal phase, and the conversion rate is very quick. In addition, stability investigation manifested that LEV solid state is very stable under various conditions. © 2015 Wiley Periodicals, Inc. and the American Pharmacists Association.

A Kinetic Study of the Effect of Basicity on the Mold Fluxes Crystallization

NASA Astrophysics Data System (ADS)

Zhou, Lejun; Wang, Wanlin; Ma, Fanjun; Li, Jin; Wei, Juan; Matsuura, Hiroyuki; Tsukihashi, Fumitaka

2012-04-01

The effect of basicity on the mold fluxes crystallization was investigated in this article. The time-temperature-transformation (TTT) diagrams and continuous-cooling-transformation (CCT) diagrams of mold fluxes with different basicity were constructed by using single, hot thermocouple technology (SHTT). The results showed that with the increase of basicity, the incubation time of isothermal crystallization became shorter, the crystallization temperature was getting higher, and the critical cooling rate of continuous cooling crystallization became faster. The X-ray diffraction analysis suggested that calcium silicate (CaO·SiO2) was precipitated at the upper part of the TTT diagram and cuspidine (Ca4Si2O7F2) was formed at the lower part, when the basicity of mold fluxes was within 1.0 to 1.2. However, when basicity was 0.8, only the cuspidine phase was formed. A kinetic study of isothermal crystallization process indicated that the increase of the basicity tended to enhance the mold flux crystallization, and the crystallization activation energy became smaller. The crystallization mechanism of cupsidine was changing from one-dimensional growth to three-dimensional growth with a constant number of nuclei, when the basicity of mold fluxes varied from 0.8 to 1.2.

Thermo-mechanical characterization of a thermoplastic composite and prediction of the residual stresses and lamina curvature during cooling

NASA Astrophysics Data System (ADS)

Péron, Mael; Jacquemin, Frédéric; Casari, Pascal; Orange, Gilles; Bailleul, Jean-Luc; Boyard, Nicolas

2017-10-01

The prediction of process induced stresses during the cooling of thermoplastic composites still represents a challenge for the scientific community. However, a precise determination of these stresses is necessary in order to optimize the process conditions and thus lower the stresses effects on the final part health. A model is presented here, that permits the estimation of residual stresses during cooling. It relies on the nonlinear laminate theory, which has been adapted to arbitrary layup sequences. The developed model takes into account the heat transfers through the thickness of the laminate, together with the crystallization kinetics. The development of the composite mechanical properties during cooling is addressed by an incremental linear elastic constitutive law, which also considers thermal and crystallization strains. In order to feed the aforementioned model, a glass fiber and PA6.6 matrix unidirectional (UD) composite has been characterized. This work finally focuses on the identification of the material and process related parameters that lower the residual stresses level, including the ply sequence, the fiber volume fraction and the cooling rate.

Kinetic Study on the Isothermal and Nonisothermal Crystallization of Monoglyceride Organogels

PubMed Central

Meng, Zong; Yang, Lijun; Geng, Wenxin; Yao, Yubo; Wang, Xingguo; Liu, Yuanfa

2014-01-01

The isothermal and nonisothermal crystallization kinetics of monoglyceride (MAG) organogels were studied by pulsed nuclear magnetic resonance (pNMR) and differential scanning calorimetry (DSC), respectively. The Avrami equation was used to describe the isothermal crystallization kinetics and experimental data fitted the equation fairly well. Results showed that the crystal growth of MAG organogels was a rod-like growth of instantaneous nuclei at higher degrees of supercooling and a plate-like form with high nucleation rate at lower degrees of supercooling. The exothermic peak in nonisothermal DSC curves for the MAG organogels became wider and shifted to lower temperature when the cooling rate increased, and nonisothermal crystallization was analyzed by Mo equation. Results indicated that at the same crystallization time, to get a higher degree of relative crystallinity, a higher cooling rate was necessary. The activation energy of nonisothermal crystallization was calculated as 739.59 kJ/mol according to the Kissinger method. Therefore, as the results of the isothermal and nonisothermal crystallization kinetics for the MAG organogels obtained, the crystallization rate, crystal nucleation, and growth during the crystallization process could be preliminarily monitored through temperature and cooling rate regulation, which laid the foundation for the real industrial manufacture and application of the MAG organogels. PMID:24701138

Nucleation control and separation of paracetamol polymorphs through swift cooling crystallization process

NASA Astrophysics Data System (ADS)

Sudha, C.; Srinivasan, K.

2014-09-01

Polymorphic nucleation behavior of pharmaceutical solid paracetamol has been investigated by performing swift cooling crystallization process. Saturated aqueous solution prepared at 318 K was swiftly cooled to 274 K in steps of every 1 K in the temperature range from 274 K to 313 K with uniform stirring of 100 rpm. The resultant supersaturation generated in the mother solution favours the nucleation of three different polymorphs of paracetamol. Lower supersaturation region σ=0.10-0.83 favours stable mono form I; the intermediate supersaturation region σ=0.92-1.28 favours metastable ortho form II and the higher supersaturation region σ=1.33-1.58 favours unstable form III polymorphic nucleation. Depending upon the level of supersaturation generated during swift cooling process and the corresponding solubility limit and metastable zone width (MSZW) of each polymorph, the nucleation of a particular polymorph occurs in the system. The type of polymorphs was identified by in-situ optical microscopy and the internal structure was confirmed by Powder X-ray diffraction (PXRD) study. By this novel approach, the preferred nucleation regions of all the three polymorphs of paracetamol are optimized in terms of different cooling ranges employed during the swift cooling process. Also solution mediated polymorphic transformations from unstable to mono and ortho to mono polymorphs have been studied by in-situ.

Effects of cooling interval and MnO2, TiO2, CdO, NiO additions on spheluritic willemite crystals

NASA Astrophysics Data System (ADS)

Coşkun, Nihal Derin; Uz, Veli; Issi, Ali; Genç, Soner; Çakı, Münevver

2017-01-01

Macro crystal production in crystal glaze systems is a very important topic in ceramic art and science. In this study, crystal growth was obtained in two different firing regimes. Recipes were prepared by adding MnO, TiO, NiO and CdO into the frit. The first firing regime, which is used in artistic ceramics, has a 100 °C cooling temperature interval. The second regime that has a 580 °C cooling temperature interval, was determined by DTA analysis. Then, the development of crystals was compared between these two firing regimes. According to the results, spheluritic willemite crystals up to three cm in the glazes doped MnO2 have been obtained by cooling it in a wide cooling interval. Larger willemite crystals were not formed in the narrow cooling temperature interval. It was determined that larger crystals can be produced by cooling at wide cooling temperature intervals and holding at lower temperature which involves nucleating the temperature of the crystal.

Influence of other rare earth ions on the optical refrigeration efficiency in Yb:YLF crystals.

PubMed

Di Lieto, Alberto; Sottile, Alberto; Volpi, Azzurra; Zhang, Zhonghan; Seletskiy, Denis V; Tonelli, Mauro

2014-11-17

We investigated the effect of rare earth impurities on the cooling efficiency of Yb³⁺:LiYF₄ (Yb:YLF). The refrigeration performance of two single crystals, doped with 5%-at. Yb and with identical history but with different amount of contaminations, have been compared by measuring the cooling efficiency curves. Spectroscopic and elemental analyses of the samples have been carried out to identify the contaminants, to quantify their concentrations and to understand their effect on the cooling efficiencies. A model of energy transfer processes between Yb and other rare earth ions is suggested, identifying Erbium and Holmium as elements that produce a detrimental effect on the cooling performance.

Vacuum electrolysis of quartz

DOEpatents

King, James Claude

1976-01-13

The disclosure is directed to a method for processing quartz used in fabricating crystal resonators such that transient frequency change of resonators exposed to pulse irradiation is virtually eliminated. The method involves heating the crystal quartz in a hydrogen-free atmosphere while simultaneously applying an electric field in the Z-axis direction of the crystal. The electric field is maintained during the cool-down phase of the process.

Mathematical modeling of static layer crystallization for propellant grade hydrogen peroxide

NASA Astrophysics Data System (ADS)

Hao, Lin; Chen, Xinghua; Sun, Yaozhou; Liu, Yangyang; Li, Shuai; Zhang, Mengqian

2017-07-01

Hydrogen peroxide (H2O2) is an important raw material widely used in many fields. In this work a mathematical model of heat conduction with a moving boundary was proposed to study the melt crystallization process of hydrogen peroxide which was carried out outside a cylindrical crystallizer. Considering the effects of the temperature of the cooling fluid on the thermal conductivity of crude crystal, the model is an improvement of Guardani's research and can be solved by analytic iteration method. An experiment was designed to measure the thickness of crystal layer with time under different conditions. A series of analysis, including the effects of different refrigerant temperature on crystal growth rate, the effects of different cooling rates on crystal layer growth rate, the effects of crystallization temperature on heat transfer and the model's application scope were conducted based on the comparison between experimental results and simulation results of the model.

Development of Casting Process for Pressings of Pistons of Car Augmented Engines

NASA Astrophysics Data System (ADS)

Korostelev, V. F.; Denisov, M. S.

2017-01-01

Results of a study aimed at formation of a single-phase fine-grained structure in pistons during their production process involving isostatic pressing of liquid metal prior to the start of crystallization, pressing of the crystallizing metal, and holding under pressure in the process of cooling to the shop temperature are presented.

Supersaturation Control using Analytical Crystal Size Distribution Estimator for Temperature Dependent in Nucleation and Crystal Growth Phenomena

NASA Astrophysics Data System (ADS)

Zahari, Zakirah Mohd; Zubaidah Adnan, Siti; Kanthasamy, Ramesh; Saleh, Suriyati; Samad, Noor Asma Fazli Abdul

2018-03-01

The specification of the crystal product is usually given in terms of crystal size distribution (CSD). To this end, optimal cooling strategy is necessary to achieve the CSD. The direct design control involving analytical CSD estimator is one of the approaches that can be used to generate the set-point. However, the effects of temperature on the crystal growth rate are neglected in the estimator. Thus, the temperature dependence on the crystal growth rate needs to be considered in order to provide an accurate set-point. The objective of this work is to extend the analytical CSD estimator where Arrhenius expression is employed to cover the effects of temperature on the growth rate. The application of this work is demonstrated through a potassium sulphate crystallisation process. Based on specified target CSD, the extended estimator is capable of generating the required set-point where a proposed controller successfully maintained the operation at the set-point to achieve the target CSD. Comparison with other cooling strategies shows a reduction up to 18.2% of the total number of undesirable crystals generated from secondary nucleation using linear cooling strategy is achieved.

DKDP crystal growth controlled by cooling rate

NASA Astrophysics Data System (ADS)

Xie, Xiaoyi; Qi, Hongji; Shao, Jianda

2017-08-01

The performance of deuterated potassium dihydrogen phosphate (DKDP) crystal directly affects beam quality, energy and conversion efficiency in the Inertial Confinement Fusion（ICF）facility, which is related with the initial saturation temperature of solution and the real-time supersaturation during the crystal growth. However, traditional method to measure the saturation temperature is neither efficient nor accurate enough. Besides, the supersaturation is often controlled by experience, which yields the higher error and leads to the instability during the crystal growth. In this paper, DKDP solution with 78% deuteration concentration is crystallized in different temperatures. We study the relation between solubility and temperature of DKDP and fit a theoretical curve with a parabola model. With the model, the measurement of saturation temperature is simplified and the control precision of the cooling rate is improved during the crystal growth, which is beneficial for optimizing the crystal growth process.

Crystal-field effects in fluoride crystals for optical refrigeration

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

Hehlen, Markus P

2010-01-01

The field of optical refrigeration of rare-earth-doped solids has recently seen an important breakthrough. The cooling of a YLiF{sub 4} (YLF) crystal doped with 5 mol% Yb3+ to 155 K by Seletskiy et al [NPhot] has surpassed the lowest temperatures ({approx}170 K for {approx}100 mW cooling capacity) that are practical with commercial multi-stage thermoelectric coolers (TEC) [Glaister]. This record performance has advanced laser cooling into an application relevant regime and has put first practical optical cryocoolers within reach. The result is also relevant from a material perspective since for the first time, an Yb3+-doped crystal has outperformed an Yb3+-doped glass.more » The record temperature of 208 K was held by the Yb3+-doped fluorozirconate glass ZBLAN. Advanced purification and glass fabrication methods currently under development are expected to also advance ZBLAN:Yb3+ to sub-TEC temperatures. However, recent achievements with YLF:Yb3+ illustrate that crystalline materials may have two potentially game-changing advantajes over glassy materials. First, the crystalline environment reduces the inhomogeneous broadening of the Yb3+ electronic transitions as compared to a glassy matrix. The respective sharpening of the crystal-field transitions increases the peak absorption cross section at the laser excitation wavelength and allows for more efficient pumping of the Yb3+ ions, particularly at low temperatures. Second, many detrimental impurities present in the starting materials tend to be excluded from the crystal during its slow growth process, in contrast to a glass where all impurities present in the starting materials are included in the glass when it is formed by temperature quenching a melt. The ultra high purity required for laser cooling materials [PRB] therefore may be easier to realize in crystals than in glasses. Laser cooling occurs by laser excitation of a rare-earth ion followed by anti-Stokes luminescence. Each such laser-cooling cycle extracts thermal energy from the solid and carries it away as high-entropy light, thereby cooling the material. In the ideal case, the respective laser-cooling power is given by the pump wavelength ({lambda}{sub p}), the mean fluorescence wavelength ({bar {lambda}}{sub L}), and the absorption coefficient (a{sub r}) of the pumped transition. These quantities are solely determined by crystal field interactions. On one hand, a large crystal-field splitting offers a favorably large difference of {lambda}{sub p} - {bar {lambda}}{sub L} and thus a high cooling efficiency {eta}{sub cool} = ({lambda}{sub p} - {bar {lambda}}{sub L})/{bar {lambda}}{sub L}. On the other hand, a small crystal-field splitting offers a high thermal population (n{sub i}) of the initial state of the pumped transition, giving a high pump absorption coefficient and thus high laser cooling power, particularly at low temperatures. A quantitative description of crystal-field interactions is therefore critical to the understanding and optimization of optical refrigeration. In the case of Yb3+ as the laser cooling ion, however, development of a crystal-field model is met with substantial difficulties. First, Yb3+ has only two 4/multiplets, {sup 2}F{sub 7/2} and {sup 2}F{sub 5/2}, which lead to at most 7 crystal-field levels. This makes it difficult, and in some cases impossible, to evaluate the crystal-field Hamiltonian, which has at least 4 parameters for any Yb3+ point symmety lower than cubic. Second, {sup 2}F{sub 7/2}{leftrightarrow}{sup 2}F{sub 5/2} transitions exhibit an exceptionally strong electron-phonon coupling compared to 4f transitions of other rare earths. This makes it difficult to distinguish electronic from vibronic transitions in the absorption and luminescence spectra and to reliably identify the crystal-field levels. Yb3+ crystal-field splittings reported in the literature should thus generally be viewed with caution. This paper explores the effects of crystal-field interactions on the laser cooling performance of Yb3+-doped fluoride crystals. It is shown that the total crystal-field splitting of the {sup 2}F{sub 7/2} and {sup 2}F{sub 5/2} multiplets of Yb3+ can be estimated from crystal-field splittings of other rare-earth-doped fluoride crystals. This approach takes advantage of an extensive body of experimental work from which Yb3+ doped fluoride crystals with favorable laser cooling properties might be identified. Section 2 reviews the crystal-field splitting of the 4f electronic states and introduces the crystal-field strength as a means to predict the total crystal-field splitting of the {sup 2}F{sub 7/2} and {sup 2}F{sub 5/2} multiplets. Section 3 illustrates the effect of the total {sup 2}F{sub 7/2} crystal field splitting on the laser cooling power. Finally, Section 4 compiles literature data on crystal-field splittings in fluoride crystals from which the {sup 2}F{sub 7/2} splitting is predicted.« less

Effects of high pressure on microstructure evolution and crystallization mechanisms during solidification of nickel

NASA Astrophysics Data System (ADS)

Zhang, Hai-Tao; Mo, Yun-Fei; Liu, Rang-Su; Tian, Ze-An; Liu, Hai-Rong; Hou, Zhao-Yang; Zhou, Li-Li; Liang, Yong-Chao; Peng, Ping

2018-03-01

To deeply understand the effects of high pressure on microstructural evolutions and crystallization mechanisms of liquid metal Ni during solidification process, MD simulation studies have been performed under 7 pressures of 0 ˜ 30 GPa, at cooling rate of 1.0 × 1011 K s-1. Adopting several microstructural analyzing methods, especially the cluster-type index method (CTIM-2) to analyze the local microstructures in the system. It is found that the pressure has important influence on the formation and evolution of microstructures, especially of the main basic clusters in the system. All the simulation systems are directly solidified into crystal structures, and the 1421, 1422, 1441 and 1661 bond-types, as well the FCC (12 0 0 0 12 0), HCP (12 0 0 0 6 6) and BCC (14 6 0 8 0 0) clusters play a key role in the microstructure transitions from liquid to crystal structures. The crystallization temperature T c is enhanced almost linearly with the increase of pressure. Highly interesting, it is found for the first time that there is an important phase transformation point from FCC to BCC structures between 20 ˜ 22.5 GPa during the solidification processes from the same initial liquid system at the same cooling rate. And the effect of increasing pressure is similar to that of decreasing cooling rate for the phase transformation of microstructures during solidification process of liquid metal Ni system, though they have different concrete effecting mechanisms.

Numerical simulation of crystal fractionation in shergottite meteorites

NASA Astrophysics Data System (ADS)

Grimm, R. E.; McSween, H. Y., Jr.

Cumulus clinopyroxenes in the Shergotty and Zagami meteorites suggest crystal fractionation occurred, possibly by gravitative settling. Numerical models of this process in a nonconvecting environment argue that the small phenocrysts can segregate only under extreme conditions of cooling time or gravitational field strength. Since textures indicate that cooling time was not excessive, a large (planetary) g is required by these models, in agreement with other suggestions that the shergottite parent body may be Mars. Other calculations indicate that it is extremely difficult to produce the observed textures in a convecting environment, unless crystal setting occurred in a quiescent zone at the bottom of the magma chamber.

Numerical simulation of crystal fractionation in shergottite meteorites

NASA Technical Reports Server (NTRS)

Grimm, R. E.; Mcsween, H. Y., Jr.

1982-01-01

Cumulus clinopyroxenes in the Shergotty and Zagami meteorites suggest crystal fractionation occurred, possibly by gravitative settling. Numerical models of this process in a nonconvecting environment argue that the small phenocrysts can segregate only under extreme conditions of cooling time or gravitational field strength. Since textures indicate that cooling time was not excessive, a large (planetary) g is required by these models, in agreement with other suggestions that the shergottite parent body may be Mars. Other calculations indicate that it is extremely difficult to produce the observed textures in a convecting environment, unless crystal setting occurred in a quiescent zone at the bottom of the magma chamber.

Laser Cooling of 2-6 Semiconductors

DTIC Science & Technology

2016-08-12

practical optical refrigeration . The challenge is the stoichiometric defect in bulk crystal which introduces mid-gap states that manifest as broad-band...cooling in semiconductor has stimulated strong interest in further scaling up towards practical optical refrigeration . The challenge is the...energy. The upconversion process is facilitated by the annihilation of phonons and leads to cooling of the matter. The concept of optical refrigeration

Rutilated quartz: combining Ti-in-quartz thermometry and lattice diffusion

NASA Astrophysics Data System (ADS)

Tailby, N.; Towbin, H.; Ackerson, M. R.

2017-12-01

The Ti content of quartz can be used to evaluate crystallization temperatures in silicic magmas like the S-type Jillamatong granodiorite of the Lachlan Fold Belt. Additionally, the presence of crystallographically-aligned exsolved rutile needles in quartz from this granodiorite suggests that post-crystallization modification of Ti in quartz can be used to assess magmatic cooling rates. In this study we report Ti-in-quartz temperatures that indicate crystallization between 600-700 °C at this location (i.e., 25-60 ppmw Ti, P = 5 kbar, aTiO2= 0.46-0.66). After crystallization, Ti in quartz can be reset via lattice diffusion, a process that can be quantified or evaluated from experimentally-determined values [Cherniak et al., 2007; where DTi = 7x10-8exp (-273±12kJmol-1/RT) m2sec-1)]. The slow diffusivity of Ti through the quartz lattice is one factor that contributes to the general use of quartz thermometry - this is to say that unrealistically long time periods are required in order for a cooling quartz crystal to re-equilibrate with the new thermal regime. This is particularly true of crystal cores (generally on the mm scale), where the diffusive length scale from the core to rim of the crystal could be used to suggest core retention is likely in even the slowest cooling granitic systems. In the Jillamatong pluton - as we predict is possible in a significant body of granitoids - coupling of slow diffusion and decreasing Ti solubility in quartz upon cooling can lead to a situation where a quartz crystal becomes saturated in Ti (i.e., aTiO2=1) and rutile exsolutions develop. The radius ( 0.6 microns) and distribution of these needles, coupled with the diffusive draw down well ( 11 microns) around these exsolutions, can be used to evaluate the cooling history of the pluton, thus providing a comprehensive time-integrated crystallization and cooling history of plutonic rocks. ReferencesCherniak et al., 2007. Chem. Geol. 236, 65-74 Thomas et al., 2010. Contrib. Mineral. Petr. 160, 743-759

Stamp forming optimization for formability and crystallinity

NASA Astrophysics Data System (ADS)

Donderwinkel, T. G.; Rietman, B.; Haanappel, S. P.; Akkerman, R.

2016-10-01

The stamp forming process is well suited for high volume production of thermoplastic composite parts. The process can be characterized as highly non-isothermal as it involves local quench-cooling of a molten thermoplastic composite blank where it makes contact with colder tooling. The formability of the thermoplastic composite depends on the viscoelastic material behavior of the matrix material, which is sensitive to temperature and degree of crystallinity. An experimental study was performed to determine the effect of temperature and crystallinity on the storage modulus during cooling for a woven glass fiber polyamide-6 composite material. An increase of two decades in modulus was observed during crystallization. As this will significantly impede the blank formability, the onset of crystallization effectively governs the time available for forming. Besides the experimental work, a numerical model is developed to study the temperature and crystallinity throughout the stamp forming process. A process window can be determined by feeding the model with the experimentally obtained data on crystallization.

Improving crystal size distribution by internal seeding combined cooling/antisolvent crystallization with a cooling/heating cycle

NASA Astrophysics Data System (ADS)

Lenka, Maheswata; Sarkar, Debasis

2018-03-01

This work investigates the effect of internal seeding and an initial cooling/heating cycle on the final crystal size distribution (CSD) during a combined cooling/antisolvent crystallization of L-asparagine monohydrate from it's aqueous solution using isopropyl-alcohol as antisolvent. Internal seeds were generated by one-pot addition of various amounts of antisolvent to the crystallizer. It was then followed by a cooling/heating cycle to dissolve the fines produced and thus obtain a suitable initial seed. A combined cooling/antisolvent crystallization was then followed by employing a linear cooling profile with simultaneous addition of antisolvent with a constant mass flow rate to promote the growth of the internally generated seeds. The amount of initial antisolvent influences the characteristics of the internal seeds generated and the effect of initial amount of antisolvent on the final CSD is investigated. It was found that the introduction of a single cooling/heating cycle significantly improves the reproducibility of final CSD as well as the mean size. Overall, the study indicates that the application of internal seeding with a single cooling/heating cycle for fines dissolution is an effective technique to tailor crystal size distribution.

Crystallization history of lunar picritic basalt sample 12002 - Phase-equilibria and cooling-rate studies

NASA Technical Reports Server (NTRS)

Walker, D.; Kirkpatrick, R. J.; Longhi, J.; Hays, J. F.

1976-01-01

Experimental crystallization of a lunar picrite composition (sample 12002) at controlled linear cooling rates produces systematic changes in the temperature at which crystalline phases appear, in the texture, and in crystal morphology as a function of cooling rate. Phases crystallize in the order olivine, chromium spinel, pyroxene, plagioclase, and ilmenite during equilibrium crystallization, but ilmenite and plagioclase reverse their order of appearance and silica crystallizes in the groundmass during controlled cooling experiments. The partition of iron and magnesium between olivine and liquid is independent of cooling rate, temperature, and pressure. Comparison of the olivine nucleation densities in the lunar sample and in the experiments indicates that the sample began cooling at about 1 deg C/hr. Pyroxene size, chemistry, and growth instability spacings, as well as groundmass coarseness, all suggest that the cooling rate subsequently decreased by as much as a factor of 10 or more. The porphyritic texture of this sample, then, is produced at a decreasing, rather than a discontinuously increasing, cooling rate.

Crystal growth of intermetallic clathrates: Floating zone process and ultra rapid crystallization

NASA Astrophysics Data System (ADS)

Prokofiev, A.; Yan, X.; Ikeda, M.; Löffler, S.; Paschen, S.

2014-09-01

We studied the crystal growth process of type-I transition metal clathrates in two different regimes: a regime of moderate cooling rate, realized with the floating zone technique, and a regime of ultra rapid cooling, realized by the melt spinning technique. In the former regime, bulk Ba8AuxSi46-x and Ba8Cu4.8GaxGe41.2-x single crystals were grown. We investigated segregation effects of the constituting elements by measurements of the composition profiles along the growth direction. The compositional non-uniformity results in a spatial variation of the electrical resistivity which is discussed as well. Structural features of clathrates and their extremely low thermal conductivities imply specifics in growth behavior which manifest themselves most pronouncedly in a rapid crystallization process. Our melt spinning experiments on Ba8Au5Si41 and Ba8Ni3.5Si42.5 (and earlier on some other clathrates) have revealed surprisingly large grains of at least 1 μm. Because of the anomalously high growth rate of the clathrate phase the formation of impurity phases is considerably kinetically suppressed. We present our scanning and transmission electron microscopy investigations of melt spun samples and discuss structural, thermodynamic and kinetic aspects of the unusual clathrate nucleation and crystallization.

Optimization of anisotropic photonic density of states for Raman cooling of solids

NASA Astrophysics Data System (ADS)

Chen, Yin-Chung; Ghosh, Indronil; Schleife, André; Carney, P. Scott; Bahl, Gaurav

2018-04-01

Optical refrigeration of solids holds tremendous promise for applications in thermal management. It can be achieved through multiple mechanisms including inelastic anti-Stokes Brillouin and Raman scattering. However, engineering of these mechanisms remains relatively unexplored. The major challenge lies in the natural unfavorable imbalance in transition rates for Stokes and anti-Stokes scattering. We consider the influence of anisotropic photonic density of states on Raman scattering and derive expressions for cooling in such photonically anisotropic systems. We demonstrate optimization of the Raman cooling figure of merit considering all possible orientations for the material crystal and two example photonic crystals. We find that the anisotropic description of the photonic density of states and the optimization process is necessary to obtain the best Raman cooling efficiency for systems having lower symmetry. This general result applies to a wide array of other laser cooling methods in the presence of anisotropy.

Rheological Characterization of Molten Polymer-Drug Dispersions as a Predictive Tool for Pharmaceutical Hot-Melt Extrusion Processability.

PubMed

Van Renterghem, Jeroen; Vervaet, Chris; De Beer, Thomas

2017-11-01

The aim of this study was to investigate (i) the influence of drug solid-state (crystalline or dissolved in the polymer matrix) on the melt viscosity and (ii) the influence of the drug concentration, temperature and shear rate on polymer crystallization using rheological tests. Poly (ethylene oxide) (PEO) (100.000 g/mol) and physical mixtures (PM) containing 10-20-30-40% (w/w) ketoprofen or 10% (w/w) theophylline in PEO were rheologically characterized. Rheological tests were performed (frequency and temperature sweeps in oscillatory shear as well as shear-induced crystallization experiments) to obtain a thorough understanding of the flow behaviour and crystallization of PEO-drug dispersions. Theophylline did not dissolve in PEO as the complex viscosity (η*) of the drug-polymer mixture increased as compared to that of neat PEO. In contrast, ketoprofen dissolved in PEO and acted as a plasticizer, decreasing η*. Acting as a nucleating agent, theophylline induced the crystallization of PEO upon cooling from the melt. On the other hand, ketoprofen inhibited crystallization upon cooling. Moreover, higher concentrations of ketoprofen in the drug-polymer mixture increasingly inhibited polymer crystallization. However, shear-induced crystallization was observed for all tested mixtures containing ketoprofen. The obtained rheological results are relevant for understanding and predicting HME processability (e.g., barrel temperature selection) and downstream processing such as injection moulding (e.g., mold temperature selection).

Molecular rotation-vibration dynamics of low-symmetric hydrate crystal in the terahertz region.

PubMed

Fu, Xiaojian; Wu, Hongya; Xi, Xiaoqing; Zhou, Ji

2014-01-16

The rotational and vibrational dynamics of molecules in copper sulfate pentahydrate crystal are investigated with terahertz dielectric spectra. It is shown that the relaxation-like dielectric dispersion in the low frequency region is related to the reorientation of water molecules under the driving of terahertz electric field, whereas the resonant dispersion can be ascribed to lattice vibration. It is also found that, due to the hydrogen-bond effect, the vibrational mode at about 1.83 THz along [-111] direction softens with decreasing temperature, that is, the crystal expands in this direction when cooled. On the contrary, the mode hardens in the direction perpendicular to [-111] during the cooling process. This contributes to the further understanding of the molecular structure and bonding features of hydrate crystals.

Temperature nonuniformity occurring during the cooling process of a KDP crystal and its effects on second-harmonic generation.

PubMed

Liang, Yingchun; Su, Ruifeng; Lu, Lihua; Liu, Haitao

2014-08-10

The temperature nonuniformity occurring during the cooling process of a KDP crystal is studied, along with its effects on the second-harmonic generation (SHG) of a high-average-power laser. A comprehensive model is proposed incorporating principles of thermodynamics, mechanics, and optics, and it is applied to investigate the temperature nonuniformity and its effects. The temperature rise caused by linear absorption is calculated, while the temperature nonuniformity occurring during the cooling process is analyzed using the finite-element method (FEM). The stress induced by the nonuniformity is then studied using the FEM, and the trend of its change is determined. Moreover, the changes in refractive index caused by the stress are calculated, the results of which are used to determine the variations in the induced phase mismatch. The SHG efficiency considering the phase mismatch is eventually obtained by solving the coupling wave equations. The results demonstrate that the temperature nonuniformity has negative effects on the SHG efficiency.

Solid-state transformations in the β-form of chlorpropamide on cooling to 100 K.

PubMed

Drebushchak, Tatiana N; Drebushchak, Valeri A; Boldyreva, Elena V

2011-04-01

A single-crystal X-ray diffraction study of the effect of cooling down to 100 K on the β-form of chlorpropamide, 4-chloro-N-(propylaminocarbonyl)benzenesulfonamide, has revealed reversible phase transitions at ∼257 K and between 150 and 125 K: β (Pbcn, Z' = 1) ⇔ β(II) (P2/c, Z' = 2) ⇔ β(III) (P2/n, a' = 2a, Z' = 4); the sequence corresponds to cooling. Despite changes in the space group and number of symmetry-independent molecules, the volume per molecule changes continuously in the temperature range 100-300 K. The phase transition at ∼257 K is accompanied by non-merohedral twinning, which is preserved on further cooling and through the second phase transition, but the original single crystal does not crack. DSC (differential scanning calorimetry) and X-ray powder diffraction investigations confirm the phase transitions. Twinning disappears on heating as the reverse transformations take place. The second phase transition is related to a change in conformation of the alkyl tail from trans to gauche in 1/4 of the molecules, regularly distributed in the space. Possible reasons for the increase in Z' upon cooling are discussed in comparison to other reported examples of processes (crystallization, phase transitions) in which organic crystals with Z' > 1 have been formed. Implications for pharmaceutical applications are discussed. © 2011 International Union of Crystallography

Atomistic insights into the nanosecond long amorphization and crystallization cycle of nanoscale G e2S b2T e5 : An ab initio molecular dynamics study

NASA Astrophysics Data System (ADS)

Branicio, Paulo S.; Bai, Kewu; Ramanarayan, H.; Wu, David T.; Sullivan, Michael B.; Srolovitz, David J.

2018-04-01

The complete process of amorphization and crystallization of the phase-change material G e2S b2T e5 is investigated using nanosecond ab initio molecular dynamics simulations. Varying the quench rate during the amorphization phase of the cycle results in the generation of a variety of structures from entirely crystallized (-0.45 K/ps) to entirely amorphized (-16 K/ps). The 1.5-ns annealing simulations indicate that the crystallization process depends strongly on both the annealing temperature and the initial amorphous structure. The presence of crystal precursors (square rings) in the amorphous matrix enhances nucleation/crystallization kinetics. The simulation data are used to construct a combined continuous-cooling-transformation (CCT) and temperature-time-transformation (TTT) diagram. The nose of the CCT-TTT diagram corresponds to the minimum time for the onset of homogenous crystallization and is located at 600 K and 70 ps. That corresponds to a critical cooling rate for amorphization of -4.5 K/ps. The results, in excellent agreement with experimental observations, suggest that a strategy that utilizes multiple quench rates and annealing temperatures may be used to effectively optimize the reversible switching speed and enable fast and energy-efficient phase-change memories.

A Differential Scanning Calorimetry Method for Construction of Continuous Cooling Transformation Diagram of Blast Furnace Slag

NASA Astrophysics Data System (ADS)

Gan, Lei; Zhang, Chunxia; Shangguan, Fangqin; Li, Xiuping

2012-06-01

The continuous cooling crystallization of a blast furnace slag was studied by the application of the differential scanning calorimetry (DSC) method. A kinetic model describing the correlation between the evolution of the degree of crystallization with time was obtained. Bulk cooling experiments of the molten slag coupled with numerical simulation of heat transfer were conducted to validate the results of the DSC methods. The degrees of crystallization of the samples from the bulk cooling experiments were estimated by means of the X-ray diffraction (XRD) and the DSC method. It was found that the results from the DSC cooling and bulk cooling experiments are in good agreement. The continuous cooling transformation (CCT) diagram of the blast furnace slag was constructed according to crystallization kinetic model and experimental data. The obtained CCT diagram characterizes with two crystallization noses at different temperature ranges.

Crystallization Behavior of Perovskite in the Synthesized High-Titanium-Bearing Blast Furnace Slag Using Confocal Scanning Laser Microscope

NASA Astrophysics Data System (ADS)

Hu, Meilong; Liu, Lu; Lv, Xuewei; Bai, Chenguang; Zhang, Shengfu

2014-01-01

The isothermal phase composition of high-titanium-bearing slag (23 mass pct TiO2) under an argon atmosphere during cooling process from 1723 K (1450 °C) was calculated by FactSage.6.3 (CRCT-ThermFact Inc., Montréal, Canada). Three main phases, which were perovskite, titania spinel, and clinopyroxene, could form during the cooling process and they precipitated at 1713 K, 1603 K, and 1498 K (1440 °C, 1330 °C, and 1225 °C), respectively. The nonisothermal crystallization process of perovskite in synthesized high-titanium-bearing slag was studied in situ by a confocal scanning laser microscope (CSLM) with cooling rate of 30 K/min. The results showed that the primary phase was perovskite that precipitated at 1703 K (1430 °C). The whole precipitation and growth process of perovskite was obtained, whereas other phases formed as glass under the current experimental conditions. Perovskite grew along a specific growth track and finally appeared with snowflake morphology. The growing kinetics of perovskite formation from molten slag were also mentioned.

Engineering evaluation of magma cooling-tower demonstration at Nevada Power Company's Sunrise Station

NASA Astrophysics Data System (ADS)

1980-11-01

The Magma Cooling Tower (MCT) process utilizes a falling film heat exchanger integrated into an induced draft cooling tower to evaporate waste water. A hot water source such as return cooling water provides the energy for evaporation. Water quality control is maintained by removing potential scaling constituents to make concentrations of the waste water possible without scaling heat transfer surfaces. A pilot-scale demonstration test of the MCT process was performed from March 1979 through June 1979 at Nevada Power Company's Sunrise Station in Las Vegas, Nevada. The pilot unit extracted heat from the powerplant cooling system to evaporate cooling tower blowdown. Two water quality control methods were employed: makeup/sidestream softening and fluidized bed crystallization. The 11 week softening mode test was successful.

Production of crystalline refractory metal oxides containing colloidal metal precipitates and useful as solar-effective absorbers

DOEpatents

Narayan, Jagdish; Chen, Yok

1983-01-01

This invention is a new process for producing refractory crystalline oxides having improved or unusual properties. The process comprises the steps of forming a doped-metal crystal of the oxide; exposing the doped crystal in a bomb to a reducing atmosphere at superatmospheric pressure and a temperature effecting precipitation of the dopant metal in the crystal lattice of the oxide but insufficient to effect net diffusion of the metal out of the lattice; and then cooling the crystal. Preferably, the cooling step is effected by quenching. The process forms colloidal precipitates of the metal in the oxide lattice. The process may be used, for example, to produce thermally stable black MgO crystalline bodies containing magnetic colloidal precipitates consisting of about 99% Ni. The Ni-containing bodies are solar-selective absorbers, having a room-temperature absorptivity of about 0.96 over virtually all of the solar-energy spectrum and exhibiting an absorption edge in the region of 2 .mu.m. The process parameters can be varied to control the average size of the precipitates. The process can produce a black MgO crystalline body containing colloidal Ni precipitates, some of which have the face-centered-cubic structure and others of which have the body-centered cubic structure. The products of the process are metal-precipitate-containing refractory crystalline oxides which have improved or unique optical, mechanical, magnetic, and/or electronic properties.

Solid state optical refrigeration using stark manifold resonances in crystals

DOEpatents

Seletskiy, Denis V.; Epstein, Richard; Hehlen, Markus P.; Sheik-Bahae, Mansoor

2017-02-21

A method and device for cooling electronics is disclosed. The device includes a doped crystal configured to resonate at a Stark manifold resonance capable of cooling the crystal to a temperature of from about 110K to about 170K. The crystal host resonates in response to input from an excitation laser tuned to exploit the Stark manifold resonance corresponding to the cooling of the crystal.

The Vitrification and Determination of the Crystallization Time Scales of a Zr58.5Nb2.8Cu15.6Ni12.8Al10.3 Bulk Metallic Glass Forming Liquid

NASA Technical Reports Server (NTRS)

Hays, C. C.; Schroers, J.; Johnson, W. L.; Rathz, T. J.; Hyers, R. W.; Rogers, J. R.; Robinson, M. B.; Whitaker, Ann F. (Technical Monitor)

2001-01-01

Zr58.5Nb2.8Cul5.6Nil2.8All0.3 is the first bulk glass forming liquid that does not contain beryllium to be vitrified by purely radiative cooling in the containerless electrostatic levitation process. The measured critical cooling rate is 1.75 K/s. The sluggish crystallization kinetics enable the determination of the time-temperature-transformation (TTT) diagram between the liquidus and the glass transition temperatures. At the nose of the TTT diagram, the shortest time to reach crystallization in an isothermal experiment is 32 seconds. In contrast to other bulk metallic glasses the scatter in the crystallization onset times are small at both high and low temperatures.

Experimental study of the rotational magnetocaloric effect in KTm(MoO4)2

NASA Astrophysics Data System (ADS)

Tarasenko, Róbert; Tkáč, Vladimír; Orendáčová, Alžbeta; Orendáč, Martin; Feher, Alexander

2018-06-01

An experimental study is presented of the rotational magnetocaloric effect in a KTm(MoO4)2 single crystal at temperatures above 2 K associated with the rotation of a single crystal between the magnetic easy and hard axis in constant magnetic fields up to 5 T. The magnetocaloric properties of KTm(MoO4)2 single crystals are investigated by isothermal magnetization measurements. The maximal rotational entropy change -ΔSR ≈ 9.8 J/(kgK) is achieved at 10 K in a magnetic field of 5 T. The adiabatic rotation of a single crystal in a field of 5 T at an initial temperature of 4.2 K causes cooling of the sample down to 0.5 K, which indicates an interesting possibility of using this material for cooling processes at low temperatures.

Physical and Structural Studies on the Cryo-cooling of Insulin Crystals

NASA Technical Reports Server (NTRS)

Lovelace, J.; Bellamy, H.; Snell, E. H.; Borgstahl, G.

2003-01-01

Reflection profiles were analyzed from microgravity-(mg) and earth-grown insulin crystals to measure mosaicity (h) and to reveal mosaic domain structure and composition. The effects of cryocooling on single and multi-domain crystals were compared. The effects of cryocooling on insulin structure were also re-examined. Microgravity crystals were larger, more homogeneous, and more perfect than earth crystals. Several mg crystals contained primarily a single mosaic domain with havg of 0.005deg. The earth crystals varied in quality and all contained multiple domains with havg of 0.031deg. Cryocooling caused a 43-fold increase in h for mg crystals (havg=0.217deg) and an %fold increase for earth crystals (havg=0.246deg). These results indicate that very well-ordered crystals are not completely protected from the stresses associated with cryocooling, especially when structural perturbations occur. However, there were differences in the reflection profiles. For multi-mosaic domain crystals, each domain individually broadened and separated from the other domains upon cryo-cooling. Cryo-cooling did not cause an increase in the number of domains. A crystal composed of a single domain retained this domain structure and the reflection profiles simply broadened. Therefore, an improved signal-to-noise ratio for each reflection was measured from cryo-cooled single domain crystals relative to cryo-cooled multi-domain crystals. This improved signal, along with the increase in crystal size, facilitated the measurement of the weaker high- resolution reflections. The observed broadening of reflection profiles indicates increased variation in unit cell dimensions which may be linked to cryo-cooling-associated structural changes and disorder.

Long-term stability of crystal-stabilized water-in-oil emulsions.

PubMed

Ghosh, Supratim; Pradhan, Mamata; Patel, Tejas; Haj-Shafiei, Samira; Rousseau, Dérick

2015-12-15

The impact of cooling rate and mixing on the long-term kinetic stability of wax-stabilized water-in-oil emulsions was investigated. Four cooling/mixing protocols were investigated: cooling from 45°C to either 25°C or 4°C with/without stirring and two cooling rates - slow (1°C/min) and fast (5°C/min). The sedimentation behaviour of the emulsions was significantly affected by cooling protocol. Stirring was critical to the stability of all emulsions, with statically-cooled (no stirring) emulsions suffering from extensive aqueous phase separation. Emulsions stirred while cooling showed sedimentation of a waxy emulsion layer leaving a clear oil layer at the top, with a smaller separation and droplet size distribution at 4°C compared to 25°C, indicating the importance of the amount of crystallized wax on emulsion stability. Light microscopy revealed that crystallized wax appeared both on the droplet surface and in the continuous phase, suggesting that stirring ensured dispersibility of the water droplets during cooling as the wax was crystallizing. Wax crystallization on the droplet surface provided stability against droplet coalescence while continuous phase wax crystals minimized inter-droplet collisions. The key novel aspect of this research is in the simplicity to tailor the spatial distribution of wax crystals, i.e., either at the droplet surface or in the continuous phase via use of a surfactant and judicious stirring and/or cooling. Knowledge gained from this research can be applied to develop strategies for long-term storage stability of crystal-stabilized W/O emulsions. Copyright © 2015 Elsevier Inc. All rights reserved.

Ultrasound assisted crystallization of mefenamic acid: Effect of operating parameters and comparison with conventional approach.

PubMed

Iyer, Sneha R; Gogate, Parag R

2017-01-01

The current work investigates the application of low intensity ultrasonic irradiation for improving the cooling crystallization of Mefenamic Acid for the first time. The crystal shape and size has been analyzed with the help of optical microscope and image analysis software respectively. The effect of ultrasonic irradiation on crystal size, particle size distribution (PSD) and yield has been investigated, also establishing the comparison with conventional approach. It has been observed that application of ultrasound not only enhances the yield but also reduces the induction time for crystallization as compared to conventional cooling crystallization technique. In the presence of ultrasound, the maximum yield was obtained at optimum conditions of power dissipation of 30W and ultrasonic irradiation time of 10min. The yield was further improved by application of ultrasound in cycles where the formed crystals are allowed to grow in the absence of ultrasonic irradiation. It was also observed that the desired crystal morphology was obtained for the ultrasound assisted crystallization. The conventionally obtained needle shaped crystals transformed into plate shaped crystals for the ultrasound assisted crystallization. The particle size distribution was analyzed using statistical means on the basis of skewness and kurtosis values. It was observed that the skewness and excess kurtosis value for ultrasound assisted crystallization was significantly lower as compared to the conventional approach. XRD analysis also revealed better crystal properties for the processed mefenamic acid using ultrasound assisted approach. The overall process intensification benefits of mefenamic acid crystallization using the ultrasound assisted approach were reduced particle size, increase in the yield and uniform PSD coupled with desired morphology. Copyright © 2016 Elsevier B.V. All rights reserved.

Incorporation of cooling-induced crystallization into a 2-dimensional axisymmetric conduit heat flow model

NASA Astrophysics Data System (ADS)

Heptinstall, David; Bouvet de Maisonneuve, Caroline; Neuberg, Jurgen; Taisne, Benoit; Collinson, Amy

2016-04-01

Heat flow models can bring new insights into the thermal and rheological evolution of volcanic 3 systems. We shall investigate the thermal processes and timescales in a crystallizing, static 4 magma column, with a heat flow model of Soufriere Hills Volcano (SHV), Montserrat. The latent heat of crystallization is initially computed with MELTS, as a function of pressure and temperature for an andesitic melt (SHV groundmass starting composition). Three fractional crystallization simulations are performed; two with initial pressures of 34MPa (runs 1 & 2) and one of 25MPa (run 3). Decompression rate was varied between 0.1MPa/° C (runs 1 & 3) and 0.2MPa/° C (run 2). Natural and experimental matrix glass compositions are accurately reproduced by all MELTS runs. The cumulative latent heat released for runs 1, 2 and 3 differs by less than 9% (8.69E5 J/kg*K, 9.32E5 J/kg*K, and 9.49E5 J/kg*K respectively). The 2D axisymmetric conductive cooling simulations consider a 30m-diameter conduit that extends from the surface to a depth of 1500m (34MPa). The temporal evolution of temperature is closely tracked at depths of 10m, 750m and 1400m in the centre of the conduit, at the conduit walls, and 20m from the walls into the host rock. Following initial cooling by 7-15oC at 10m depth inside the conduit, the magma temperature rebounds through latent heat release by 32-35oC over 85-123 days to a maximum temperature of 1002-1005oC. At 10m depth, it takes 4.1-9.2 years for the magma column to cool by 108-131oC and crystallize to 75wt%, at which point it cannot be easily remobilized. It takes 11-31.5 years to reach the same crystallinity at 750-1400m depth. We find a wide range in cooling timescales, particularly at depths of 750m or greater, attributed to the initial run pressure and the dominant latent heat producing crystallizing phase, Albite-rich Plagioclase Feldspar. Run 1 is shown to cool fastest and run 3 cool the slowest, with surface emissivity having the strongest cooling influence in the upper tens of meters of the conduit in all runs.

An ion microprobe study of the intra-crystalline behavior of REE and selected trace elements in pyroxene from mare basalts with different cooling and crystallization histories

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

Shearer, C.K.; Papike, J.J.; Simon, S.B.

1989-05-01

To study the effects of crystallization sequence and rate on trace element zoning characteristics of pyroxenes, the authors used combined electron microprobe-ion microprobe techniques on four nearly isochemical Apollo 12 and 15 pigeonite basalts with different cooling rates and crystallization histories. Major and minor element zoning characteristics are nearly identical to those reported in the literature. All the pyroxenes have similar chondrite-normalized REE patterns: negative Eu anomalies, positive slopes as defined by Yb/Ce, and slopes of REE patterns from Ce to Sm much steeper than from Gd to Yb. These trace element zoning characteristics in pyroxene and the partitioning ofmore » trace elements between pyroxene and the melt are intimately related to the interplay among the efficiency of the crystallization process, the kinetics at the crystal-melt interface, the kinetics of plagioclase nucleation and the characteristics of the crystal chemical substitutions within both the pyroxene and the associated crystallizing phases (i.e. plagioclase).« less

Vitrification and devitrification of micro-droplets

NASA Astrophysics Data System (ADS)

Ryoun Youn, Jae; Song, Young Seok

2012-11-01

Vitrification can be achieved by flash freezing and thawing (i.e. quenching) when ice crystal formation is inhibited in a cryogenic environment. Such ultra-rapid cooling and rewarming occurs due to the large temperature difference between the liquid and its surrounding medium. Here, we analyze the crystallization behavior of a droplet (i.e. vitrification and devitrification) by using a numerical model. The numerical results were found to explain the experimental observations successfully. The findings showed that for successful cryopreservation not only sufficiently fast cooling, but also rewarming processes should be designed and controlled to avoid devitrification of a droplet.

Three-dimensional analysis of dislocation multiplication during thermal process of grown silicon with different orientations

NASA Astrophysics Data System (ADS)

Gao, B.; Nakano, S.; Harada, H.; Miyamura, Y.; Kakimoto, K.

2017-09-01

We used an advanced 3D model to study the effect of crystal orientation on the dislocation multiplication in single-crystal silicon under accurate control of the cooling history of temperature. The incorporation of the anisotropy effect of the crystal lattice into the model has been explained in detail, and an algorithm for accurate control of the temperature in the furnace has also been presented. This solver can dynamically track the history of dislocation generation for different orientations during thermal processing of single-crystal silicon. Four orientations, [001], [110], [111], and [112], have been examined, and the comparison of dislocation distributions has been provided.

Non-isothermal crystallization of poly(etheretherketone) aromatic polymer composite

NASA Technical Reports Server (NTRS)

Cebe, Peggy

1988-01-01

The nonisothermal crystallization kinetics of PEEK APC-2 and of 450G neat resin PEEK material were compared using a differential scanning calorimeter to monitor heat flow during crystallization; the effects of cooling rate on the crystallization temperature, the degree of crystallinity, and the conversion rate were investigated. A modified Avrami (1940) analysis was used to describe nonisothermal crystallization kinetics. It was found that, compared with the 450G neat resin PEEK, the nonisothermal crystallization of the PEEK APC-2 composite is characterized by higher initiation temperature, higher heat flow maximum temperature, and greater relative conversion by primary processes.

The initial cooling of pahoehoe flow lobes

USGS Publications Warehouse

Keszthelyi, L.; Denlinger, R.

1996-01-01

In this paper we describe a new thermal model for the initial cooling of pahoehoe lava flows. The accurate modeling of this initial cooling is important for understanding the formation of the distinctive surface textures on pahoehoe lava flows as well as being the first step in modeling such key pahoehoe emplacement processes as lava flow inflation and lava tube formation. This model is constructed from the physical phenomena observed to control the initial cooling of pahoehoe flows and is not an empirical fit to field data. We find that the only significant processes are (a) heat loss by thermal radiation, (b) heat loss by atmospheric convection, (c) heat transport within the flow by conduction with temperature and porosity-dependent thermal properties, and (d) the release of latent heat during crystallization. The numerical model is better able to reproduce field measurements made in Hawai'i between 1989 and 1993 than other published thermal models. By adjusting one parameter at a time, the effect of each of the input parameters on the cooling rate was determined. We show that: (a) the surfaces of porous flows cool more quickly than the surfaces of dense flows, (b) the surface cooling is very sensitive to the efficiency of atmospheric convective cooling, and (c) changes in the glass forming tendency of the lava may have observable petrographic and thermal signatures. These model results provide a quantitative explanation for the recently observed relationship between the surface cooling rate of pahoehoe lobes and the porosity of those lobes (Jones 1992, 1993). The predicted sensitivity of cooling to atmospheric convection suggests a simple field experiment for verification, and the model provides a tool to begin studies of the dynamic crystallization of real lavas. Future versions of the model can also be made applicable to extraterrestrial, submarine, silicic, and pyroclastic flows.

Assessment of the Dehydration-Greenhouse Feedback Over the Arctic During Winter

NASA Astrophysics Data System (ADS)

Girard, E.; Stefanof, A.; Peltier-Champigny, M.; Munoz-Alpizar, R.; Dueymes, G.; Jean-Pierre, B.

2007-12-01

The effect of pollution-derived sulphuric acid aerosols on the aerosol-cloud-radiation interactions is investigated over the Arctic for February 1990. Observations suggest that acidic aerosols can decrease the heterogeneous nucleation rate of ice crystals and lower the homogeneous freezing temperature of haze droplets. Based on these observations, we hypothesize that the cloud thermodynamic phase is modified in polluted air mass (Arctic haze). Cloud ice number concentration is reduced, thus promoting further ice crystal growth by the Bergeron-Findeisen process. Hence, ice crystals reach larger sizes and low-level ice crystal precipitation from mixed-phase clouds increases. Enhanced dehydration of the lower troposphere contributes to decrease the water vapour greenhouse effect and cool the surface. A positive feedback is created between surface cooling and air dehydration, accelerating the cold air production. This process is referred to as the dehydration-greenhouse feedback (DGF). Simulations performed using an arctic regional climate model for February 1990, February and March 1985 and 1995 are used to assess the potential effect of the DGF on the Arctic climate. Results show that the DGF has an important effect over the Central and Eurasian Arctic, which is the coldest part of the Arctic with a surface cooling ranging between 0 and -3K. Moreover, the lower tropospheric cooling over the Eurasian and Central Arctic strengthens the atmospheric circulation at upper level, thus increasing the aerosol transport from the mid-latitudes and enhancing the DGF. Over warmer areas, the increased aerosol concentration (caused by the DGF) leads to longer cloud lifetime, which contributes to warm these areas. It is also shown that the maximum ice nuclei reduction must be of the order of 100 to get a significant effect.

Comparative analysis of thermal behavior, isothermal crystallization kinetics and polymorphism of palm oil fractions.

PubMed

Zhang, Xia; Li, Lin; Xie, He; Liang, Zhili; Su, Jianyu; Liu, Guoqin; Li, Bing

2013-01-15

Thermal behavior of palm stearin (PS) and palm olein (PO) was explored by monitoring peak temperature transitions by differential scanning calorimetry (DSC). The fatty acid composition (FAC), isothermal crystallization kinetics studied by pulsed Nuclear Magnetic Resonance (pNMR) and isothermal microstructure were also compared. The results indicated that the fatty acid composition had an important influence on the crystallization process. PS and PO both exhibited more multiple endotherms than exotherms which showed irregular peak shapes. An increasing in cooling rate, generally, was associated with an increase in peak size. Application of the Avaimi equation to isothermal crystallization of PS and PO revealed different nucleation and growth mechanisms based on the Avrami exponents. PS quickly reached the end of crystallization because of more saturated triacylglycerol (TAG). The Avrami index of PS were the same as PO under the same isothermal condition at lower temperatrue, indicating that the crystallization mechanism of the two samples based on super-cooling state were the same. According to the polarized light microscope (PLM) images, crystal morphology of PS and PO was different. With the temperature increased, the structure of crystal network of both PS and PO gradually loosened.

Hot zone design for controlled growth to mitigate cracking in laser crystal growth

NASA Astrophysics Data System (ADS)

Zhang, Hui; Zheng, Lili; Fang, Haisheng

2011-03-01

Cracking is a major problem during large diameter crystal growth. The objective of this work is to design an effective hot zone for a controlled growth of Yb:S-FAP [Yb3+:Sr5(PO4)3F] laser crystal by the Czochralski technology and effective cooling that can reduce stress. Theoretical and numerical analyses are performed to study the causes of cracking, mitigate the major cracking, as well as reduce cooling time. In the current system, three locations in the crystal are prone to crack, such as the top shoulder of the crystal, the middle portion above the crucible edge, and the bottom tail portion. Based on numerical simulations, we propose a new hot zone design and cooling procedure to grow and cool large diameter crystal without cracking.

Hindered settling and the formation of layered intrusions

NASA Astrophysics Data System (ADS)

Bons, Paul D.; Baur, Albrecht; Elburg, Marlina A.; Lindhuber, Matthias J.; Marks, Michael A. W.; Soesoo, Alvar; van Milligen, Boudewijn P.; Walte, Nicolas P.

2015-04-01

Layered intrusions are characterized by (often repetitive) layering on a range of scales. Many explanations for the formation of such layering have been proposed over the past decades. We investigated the formation of "mats" by hindered crystal settling, a model that was first suggested by Lauder (1964). The interaction of sinking and rising crystals leads to the amplification of perturbations in crystal density within a magma chamber, a process similar to the formation of traffic jams in dense traffic (Bons et al., 2015). Once these "crystal traffic jams" form they constitute a barrier for further settling of crystals. Between these barriers, the magma evolves in a semi-closed system in which stratification may develop by gravitational sorting. Barriers, and therefore layers, form sequentially during inward cooling of the magma chamber. Barring later equilibration, mineralogical and geochemical trends within the layers are repetitive, but with variations due to the random process of initial perturbation formation. Layers can form in the transition between two end-member regimes: (1) in a fast cooling and/or viscous magma crystals cannot sink or float a significant distance and minerals are distributed homogeneously throughout the chamber; (2) in a slow cooling and/or low-viscosity magma crystals can quickly settle at the top and bottom of the chamber and crystals concentrations are never high enough to form "traffic jams". As a result, heavy and light minerals get fully separated in the chamber. Between these two end members, crystals can sink and float a significant distance, but not the whole height of the magma chamber before entrapment in "traffic jams". We illustrate the development of layers with numerical models and compare the results with the layered nepheline syenites (kakortokites) of the Ilímaussaq intrusion in SW Greenland. References: Bons, P.D., Baur, A., Elburg, M.A., Lindhuber, M.J., Marks, M.A.W., Soesoo, A., van Milligen, B.P., Walte, N.P. 2015. Layered intrusions and traffic jams. Geology 43, 71-74 Lauder, W. 1964. Mat formation and crystal settling in magma. Nature 202, 1100-1101.

Preparation of cerium halide solvate complexes

DOEpatents

Vasudevan, Kalyan V; Smith, Nickolaus A; Gordon, John C; McKigney, Edward A; Muenchaussen, Ross E

2013-08-06

Crystals of a solvated cerium(III) halide solvate complex resulted from a process of forming a paste of a cerium(III) halide in an ionic liquid, adding a solvent to the paste, removing any undissolved solid, and then cooling the liquid phase. Diffusing a solvent vapor into the liquid phase also resulted in crystals of a solvated cerium(III) halide complex.

A study on ice crystal formation behavior at intracellular freezing of plant cells using a high-speed camera.

PubMed

Ninagawa, Takako; Eguchi, Akemi; Kawamura, Yukio; Konishi, Tadashi; Narumi, Akira

2016-08-01

Intracellular ice crystal formation (IIF) causes several problems to cryopreservation, and it is the key to developing improved cryopreservation techniques that can ensure the long-term preservation of living tissues. Therefore, the ability to capture clear intracellular freezing images is important for understanding both the occurrence and the IIF behavior. The authors developed a new cryomicroscopic system that was equipped with a high-speed camera for this study and successfully used this to capture clearer images of the IIF process in the epidermal tissues of strawberry geranium (Saxifraga stolonifera Curtis) leaves. This system was then used to examine patterns in the location and formation of intracellular ice crystals and to evaluate the degree of cell deformation because of ice crystals inside the cell and the growing rate and grain size of intracellular ice crystals at various cooling rates. The results showed that an increase in cooling rate influenced the formation pattern of intracellular ice crystals but had less of an effect on their location. Moreover, it reduced the degree of supercooling at the onset of intracellular freezing and the degree of cell deformation; the characteristic grain size of intracellular ice crystals was also reduced, but the growing rate of intracellular ice crystals was increased. Thus, the high-speed camera images could expose these changes in IIF behaviors with an increase in the cooling rate, and these are believed to have been caused by an increase in the degree of supercooling. Copyright © 2016 Elsevier Inc. All rights reserved.

Destabilization of mayonnaise induced by lipid crystallization upon freezing.

PubMed

Miyagawa, Yayoi; Ogawa, Takenobu; Nakagawa, Kyuya; Adachi, Shuji

2016-01-01

The thermal and rheological history of mayonnaise during freezing and its dispersion stability after the freeze-thaw process were investigated. Mayonnaise was cooled to freeze and stored at -20 to -40 °C while monitoring the temperature; penetration tests were conducted on the mayonnaise, which was sampled at selected times during isothermal storage at -20 °C. Significant increases in the temperature and stress values due to water-phase crystallization and subsequent oil-phase crystallization were observed. The water phase crystallized during the cooling step in all the tested mayonnaise samples. The oil phases of the prepared mayonnaise (with rapeseed oil) and commercial mayonnaise crystallized during isothermal storage after 6 and 4 h, respectively, at -20 °C. The dispersion stability was evaluated from the separation ratio, which was defined as the weight ratio of separated oil after centrifuging to the total amount of oil in the commercial mayonnaise. The separation ratio rapidly increased after 4 h of freezing. This result suggests that crystallization of the oil phase is strongly related to the dispersion stability of mayonnaise.

Does Warming a Lysozyme Solution Cook Ones Data?

NASA Technical Reports Server (NTRS)

Pusey, Marc; Burke, Michael; Judge, Russell

2000-01-01

Chicken egg white lysozyme has a well characterized thermally driven phase transition. Between pH 4.0 and 5.2, the transition temperature, as defined by the point where the tetragonal and orthorhombic solubility are equal, is a function of the pH, salt (precipitant) type and concentration, and most likely of the buffer concentration as well. This phase transition can be carried out with protein solution alone, prior to the initiation of the crystallization process. We have now measured the kinetics of this process and investigated its reversibility. An aliquot of a stock protein solution is held at a given temperature, and at periodic intervals used to set up batch crystallization experiments. The batch solutions were incubated at 20 C until macroscopic crystals were obtained, at which point the number of crystals in each well were counted. The transition effects increased with temperature, slowly falling off at 30 C with a half time (time to approx. 1/2 the t = 0 number of crystals) of approx. 5 hours, and an estimated half time of approx. 0.5 hours at 43 C. Further, the process was not reversible by simple cooling. After holding a lysozyme solution at 37 C (prior to addition of precipitant) for 16 hours, then cooling and holding it at 4 C, no return to the pre-warmed nucleation kinetics are observed after at least 4 weeks. Thus every thermal excursion above the phase transition point results in a further decrease in the nucleation rate of that solution, the extent being a function of the time and temperature. Orthorhombic lysozyme crystals apparently do not undergo the flow-induced growth cessation of tetragonal lysozyme crystals. We have previously shown that putting the protein in the orthorhombic form does not affect the averaged face growth kinetics, only nucleation, for tetragonal crystals. We may be able to use this differential behavior to elucidate how flow affects tile lysozyme crystal growth process.

The influence of cooling parameters on the speed of continuous steel casting

NASA Astrophysics Data System (ADS)

Tirian, G. O.; Gheorghiu, C. A.; Hepuţ, T.; Chioncel, C. P.

2018-01-01

This paper analyzes the cooling parameters of the continuous casting speed. In the researches carried out we aimed to establish some correlation equations between the parameters characterizing the continuous casting process, the temperature of the steel at the entrance to the crystallizer, the superheating of the steel and the flow of the cooling water in the crystallizer and different zones of the secondary cooling. Parallel to these parameters were also the values for the casting speed. The research was made for the casting of round ϕ270mm semi-finished steel products. The steel was developed in an electric EBT furnace with a capacity of 100t, treated in L.F. (Ladle - Furnace) and VD (Vacuum-Degassing) and poured in a 5-wire continuous casting plant. The obtained data was processed in MATLAB using three types of correlation equations. The obtained results are presented both in the analytical and graphical form, each correlation being analyzed from the technological point of view, indicating the optimal values for the independent parameters monitored. In the analysis we present a comparison between the results obtained after the three types of equations for each correlation.

Optimization of the cooling profile to achieve crack-free Yb:S-FAP crystals

NASA Astrophysics Data System (ADS)

Fang, H. S.; Qiu, S. R.; Zheng, L. L.; Schaffers, K. I.; Tassano, J. B.; Caird, J. A.; Zhang, H.

2008-08-01

Yb:S-FAP [Yb 3+:Sr 5(PO 4) 3F] crystals are an important gain medium for diode-pumped laser applications. Growth of 7.0 cm diameter Yb:S-FAP crystals utilizing the Czochralski (CZ) method from SrF 2-rich melts often encounters cracks during the post-growth cool-down stage. To suppress cracking during cool-down, a numerical simulation of the growth system was used to understand the correlation between the furnace power during cool-down and the radial temperature differences within the crystal. The critical radial temperature difference, above which the crystal cracks, has been determined by benchmarking the simulation results against experimental observations. Based on this comparison, an optimal three-stage ramp-down profile was implemented, which produced high-quality, crack-free Yb:S-FAP crystals.

Relationships between molecular structure and kinetic and thermodynamic controls in lipid systems. Part III. Crystallization and phase behavior of 1-palmitoyl-2,3-stearoyl-sn-glycerol (PSS) and tristearoylglycerol (SSS) binary system.

PubMed

Bouzidi, Laziz; Narine, Suresh S

2012-01-01

The phase behavior of 1-palmitoyl-2,3-distearoyl-sn-glycerol (PSS)/tristearoylglycerol (SSS) binary system was investigated in terms of polymorphism, crystallization and melting behavior, microstructure and solid fat content (SFC) using widely different constant cooling rates. Kinetic phase diagrams were experimentally determined from the DSC heating thermograms and analyzed using a thermodynamic model to account for non-ideality of mixing. The kinetic phase diagram presented a typical eutectic behavior with a eutectic point at the 0.5(PSS) mixture with a probable precipitation line from 0.5(PSS) to 1.0(PSS), regardless of the rate at which the sample was cooled. The eutectic temperature decreased only slightly with increasing cooling rate. PSS has a strong effect on the physical properties of the PSS-SSS mixtures. In fact, the overall phase behavior of the PSS-SSS binary system was determined, for a very large part, by the asymmetrical TAG. Moreover, PSS is a key driver of the high stability observed in crystal growth, polymorphism and phase development. Levels as low as 10% PSS, when cooled slowly, and 30% when cooled rapidly, were found to be sufficient to suppress the effect of thermal processing. Copyright © 2011 Elsevier Ireland Ltd. All rights reserved.

Method for single crystal growth of photovoltaic perovskite material and devices

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

Huang, Jinsong; Dong, Qingfeng

Systems and methods for perovskite single crystal growth include using a low temperature solution process that employs a temperature gradient in a perovskite solution in a container, also including at least one small perovskite single crystal, and a substrate in the solution upon which substrate a perovskite crystal nucleates and grows, in part due to the temperature gradient in the solution and in part due to a temperature gradient in the substrate. For example, a top portion of the substrate external to the solution may be cooled.

Abstracts, Third Space Processing Symposium, Skylab results

NASA Technical Reports Server (NTRS)

1974-01-01

Skylab experiments results are reported in abstracts of papers presented at the Third Space Processing Symposium. Specific areas of interest include: exothermic brazing, metals melting, crystals, reinforced composites, glasses, eutectics; physics of the low-g processes; electrophoresis, heat flow, and convection demonstrations flown on Apollo missions; and apparatus for containerless processing, heating, cooling, and containing materials.

Thermal properties of poly(3-hydroxybutyrate)/vegetable fiber composites

NASA Astrophysics Data System (ADS)

Vitorino, Maria B. C.; Reul, Lízzia T. A.; Carvalho, Laura H.; Canedo, Eduardo L.

2015-05-01

The present work studies the thermal properties of composites of poly(3-hydroxybutyrate) (PHB) - a fully biodegradable semi-crystalline thermo-plastic obtained from renewable resources through low-impact biotechno-logical process, biocompatible and non-toxic - and vegetable fiber from the fruit (coconut) of babassu palm tree. PHB is a highly crystalline resin and this characteristic leads to suboptimal properties in some cases. Consequently, thermal properties, in particular those associated with the crystallization of the matrix, are important to judge the suitability of the compounds for specific applications. PHB/babassu composites with 0-50% load were prepared in an internal mixer. Two different types of babassu fibers with two different particle size ranges were compounded with PHB and test specimens molded by compression. Melting and crystallization behavior were studied by differential scanning calorimetry (DSC) at heating/cooling rates between 2 and 30°C/min. Several parameters, including melting point, crystallization temperature, crystallinity, and rate of crystallization, were estimated as functions of load and heating/cooling rates. Results indicate that fibers do not affect the melting process, but facilitate crystallization from the melt. Crystallization temperatures are 30 to 40°C higher for the compounds compared with the neat resin. However, the amount of fiber added has little effect on crystallinity and the degree of crystallinity is hardly affected by the load. Fiber type and initial particle size do not have a significant effect on thermal properties.

Rapid hydrothermal cooling above the axial melt lens at fast-spreading mid-ocean ridge

NASA Astrophysics Data System (ADS)

Zhang, Chao; Koepke, Juergen; Kirchner, Clemens; Götze, Niko; Behrens, Harald

2014-09-01

Axial melt lenses sandwiched between the lower oceanic crust and the sheeted dike sequences at fast-spreading mid-ocean ridges are assumed to be the major magma source of oceanic crust accretion. According to the widely discussed ``gabbro glacier'' model, the formation of the lower oceanic crust requires efficient cooling of the axial melt lens, leading to partial crystallization and crystal-melt mush subsiding down to lower crust. These processes are believed to be controlled by periodical magma replenishment and hydrothermal circulation above the melt lens. Here we quantify the cooling rate above melt lens using chemical zoning of plagioclase from hornfelsic recrystallized sheeted dikes drilled from the East Pacific at the Integrated Ocean Drilling Program Hole 1256D. We estimate the cooling rate using a forward modelling approach based on CaAl-NaSi interdiffusion in plagioclase. The results show that cooling from the peak thermal overprint at 1000-1050°C to 600°C are yielded within about 10-30 years as a result of hydrothermal circulation above melt lens during magma starvation. The estimated rapid hydrothermal cooling explains how the effective heat extraction from melt lens is achieved at fast-spreading mid-ocean ridges.

Incorporation of cooling-induced crystallisation into a 2-dimensional axisymmetric conduit heat flow model

NASA Astrophysics Data System (ADS)

Heptinstall, D. A.; Neuberg, J. W.; Bouvet de Maisonneuve, C.; Collinson, A.; Taisne, B.; Morgan, D. J.

2015-12-01

Heat flow models can bring new insights into the thermal and rheological evolution of volcanic systems. We shall investigate the thermal processes and timescales in a crystallizing, static magma column, with a heat flow model of Soufriere Hills Volcano (SHV), Montserrat. The latent heat of crystallization is initially computed with MELTS, as a function of pressure and temperature for an andesitic melt (SHV groundmass starting composition). Three fractional crystallization simulations are performed; two with initial pressures of 34MPa (runs 1 & 2) and one of 25MPa (run 3). Decompression rate was varied between 0.1MPa/°C (runs 1 & 3) and 0.2MPa/°C (run 2). Natural and experimental matrix glass compositions are accurately reproduced by all MELTS runs. The cumulative latent heat released for runs 1, 2 and 3 differs by less than 9% (8.69e5 J/kg*K, 9.32e5 J/kg*K, and 9.49e5 J/kg*K respectively). The 2D axisymmetric conductive cooling simulations consider a 30m-diameter conduit that extends from the surface to a depth of 1500m (34MPa). The temporal evolution of temperature is closely tracked at depths of 10m, 750m and 1400m in the center of the conduit, at the conduit walls, and 20m from the walls into the host rock. Following initial cooling by 7-15oC at 10m depth inside the conduit, the magma temperature rebounds through latent heat release by 32-35oC over 85-123 days to a maximum temperature of 1002-1005oC. At 10 m depth, it takes 4.1-9.2 years for the magma column to cool over 108-130oC and crystallize to 75wt%, at which point it cannot be easily remobilized. It takes 11-31.5 years to reach the same crystallinity at 750-1400m depth. We find a wide range in cooling timescales, particularly at depths of 750m or greater, attributed to the initial run pressure and dominant latent heat producing crystallizing phases (Quartz), where run 1 cools fastest and run 3 cools slowest. Surface cooling by comparison has the strongest influence on the upper tens of meters in all runs.

On-line monitoring of the crystallization process: relationship between crystal size and electrical impedance spectra

NASA Astrophysics Data System (ADS)

Zhao, Yanlin; Yao, Jun; Wang, Mi

2016-07-01

On-line monitoring of crystal size in the crystallization process is crucial to many pharmaceutical and fine-chemical industrial applications. In this paper, a novel method is proposed for the on-line monitoring of the cooling crystallization process of L-glutamic acid (LGA) using electrical impedance spectroscopy (EIS). The EIS method can be used to monitor the growth of crystal particles relying on the presence of an electrical double layer on the charged particle surface and the polarization of double layer under the excitation of alternating electrical field. The electrical impedance spectra and crystal size were measured on-line simultaneously by an impedance analyzer and focused beam reflectance measurement (FBRM), respectively. The impedance spectra were analyzed using the equivalent circuit model and the equivalent circuit elements in the model can be obtained by fitting the experimental data. Two equivalent circuit elements, including capacitance (C 2) and resistance (R 2) from the dielectric polarization of the LGA solution and crystal particle/solution interface, are in relation with the crystal size. The mathematical relationship between the crystal size and the equivalent circuit elements can be obtained by a non-linear fitting method. The function can be used to predict the change of crystal size during the crystallization process.

Fate of a perched crystal layer in a magma ocean

NASA Technical Reports Server (NTRS)

Morse, S. A.

1992-01-01

The pressure gradients and liquid compressibilities of deep magma oceans should sustain the internal flotation of native crystals owing to a density crossover between crystal and liquid. Olivine at upper mantle depths near 250 km is considered. The behavior of a perched crystal layer is part of the general question concerning the fate of any transient crystal carried away from a cooling surface, whether this be a planetary surface or the roof of an intrusive magma body. For magma bodies thicker than a few hundred meters at modest crustal depths, the major cooling surface is the roof even when most solidification occurs at the floor. Importation of cool surroundings must also be invoked for the generation of a perched crystal layer in a magma ocean, but in this case the perched layer is deeply embedded in the hot part of the magma body, and far away from any cooling surface. Other aspects of this study are presented.

Optimization of the cooling profile to achieve crack-free Yb:S-FAP crystals

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

Fang, H; Qiu, S; Kheng, L

Yb:S-FAP [Yb{sup 3+}:Sr{sub 5}(PO{sub 4}){sub 3}F] crystals are an important gain medium for diode-pumped laser applications. Growth of 7.0 cm diameter Yb:S-FAP crystals utilizing the Czochralski (CZ) method from SrF{sub 2}-rich melts often encounter cracks during the post growth cool down stage. To suppress cracking during cool down, a numerical simulation of the growth system was used to understand the correlation between the furnace power during cool down and the radial temperature differences within the crystal. The critical radial temperature difference, above which the crystal cracks, has been determined by benchmarking the simulation results against experimental observations. Based on thismore » comparison, an optimal three-stage ramp-down profile was implemented and produced high quality, crack-free Yb:S-FAP crystals.« less

Crystal growth in a microgravity environment

NASA Technical Reports Server (NTRS)

Kroes, Roger L. (Inventor); Reiss, Donald A. (Inventor); Lehoczky, Sandor L. (Inventor)

1992-01-01

Gravitational phenomena, including convection, sedimentation, and interactions of materials with their containers all affect the crystal growth process. If they are not taken into consideration they can have adverse effects on the quantity and quality of crystals produced. As a practical matter, convection, and sedimentation can be completely eliminated only under conditions of low gravity attained during orbital flight. There is, then, an advantage to effecting crystallization in space. In the absence of convection in a microgravity environment cooling proceeds by thermal diffusion from the walls to the center of the solution chamber. This renders control of nucleation difficult. Accordingly, there is a need for a new improved nucleation process in space. Crystals are nucleated by creating a small localized region of high relative supersaturation in a host solution at a lower degree of supersaturation.

Thermal deformation of cryogenically cooled silicon crystals under intense X-ray beams: measurement and finite-element predictions of the surface shape

PubMed Central

Zhang, Lin; Sánchez del Río, Manuel; Monaco, Giulio; Detlefs, Carsten; Roth, Thomas; Chumakov, Aleksandr I.; Glatzel, Pieter

2013-01-01

X-ray crystal monochromators exposed to white-beam X-rays in third-generation synchrotron light sources are subject to thermal deformations that must be minimized using an adequate cooling system. A new approach was used to measure the crystal shape profile and slope of several cryogenically cooled (liquid nitrogen) silicon monochromators as a function of beam power in situ and under heat load. The method utilizes multiple angular scans across the Bragg peak (rocking curve) at various vertical positions of a narrow-gap slit downstream from the monochromator. When increasing the beam power, the surface of the liquid-nitrogen-cooled silicon crystal deforms from a concave shape at low heat load to a convex shape at high heat load, passing through an approximately flat shape at intermediate heat load. Finite-element analysis is used to calculate the crystal thermal deformations. The simulated crystal profiles and slopes are in excellent agreement with experiments. The parameters used in simulations, such as material properties, absorbed power distribution on the crystal and cooling boundary conditions, are described in detail as they are fundamental for obtaining accurate results. PMID:23765298

Liquid encapsulated crystal growth

NASA Technical Reports Server (NTRS)

Morrison, Andrew D. (Inventor)

1989-01-01

Low-defect crystals are grown in a closed ampoule under a layer of encapsulant. After crystal growth, the crystal is separated from the melt and moved into the layer of encapsulant and cooled to a first temperature at which crystal growth stops. The crystal is then moved into the inert gas ambient in the ampoule and further cooled. The crystal can be separated from the melt by decanting the melt into an adjacent reservoir or by rotating the ampoule to rotate the crystal into the encapsulant layer.

Liquid encapsulated crystal growth

NASA Technical Reports Server (NTRS)

Morrison, Andrew D. (Inventor)

1987-01-01

Low-defect crystals are grown in a closed ampoule under a layer of encapsulant. After crystal growth, the crystal is separated from the melt and moved into the layer of encapsulant and cooled to a first temperature at which crystal growth stops. The crystal is then moved into the inert gas ambient in the ampoule and further cooled. The crystal can be separated from the melt by decanting the melt into and adjacent reservoir or by rotating the ampoule to rotate the crystal into the encapsulant layer.

Hot Views on Cold Crystals: The Application of Thermal Imaging in Cryo-crystallography

NASA Technical Reports Server (NTRS)

Snell, E. H.; vanderWoerd, M. J.; Deacon, A.

2003-01-01

In the past we have used thermal imaging techniques to visualize the cryocooling processes of macromolecular crystals. From these images it was clear that a cold wave progresses through a crystal starting at the face closest to the origin of the cold stream and ending at the point furthest away. During these studies we used large volume crystals, which were clearly distinguished from the loop holding them. These large crystals, originally grown for neutron diffraction studies, were chosen deliberately to enhance the imaging. As an extension to this work, we present used thermal imaging to study small crystals, held in a cryo-loop, in the presence of vitrified mother liquor. The different infrared transmission and reflectance properties of the crystal in comparison to the mother liquor surrounding it are thought to be the parameter that produces the contrast that makes the crystal visible. An application of this technology may be the determination of the exact location of small crystals in a cryo-loop. Data from initial tests in support of application development was recorded for lysozyme crystals and for bFGF/dna complex crystals, which were cryo-cooled and imaged in large loops, both with visible light and with infrared radiation. The crystals were clearly distinguished from the vitrified solution in the infrared spectrum, while in the case of the bFGF/dna complex the illumination had to be carefully manipulated to make the crystal visible in the visible spectrum. These results suggest that the thermal imaging may be more sensitive than visual imaging for automated location of small crystals. However, further work on small crystals robotically mounted at SSRL did not clearly visualize those crystals. The depth of field of the camera proved to be limiting and a different cooling geometry was used, compared to the previous, successful experiments. Analysis to exploit multiple images to improve depth of field and experimental work to understand cooling geometry effects is ongoing. These results will be presented along with advantages and disadvantages of the technique and a discussion of how it might be applied.

Hot Views on Cold Crystals: The Application of Thermal Imaging in Cryocrystallography

NASA Technical Reports Server (NTRS)

Snell, Eddie H.

2003-01-01

In the past we have used thermal imaging techniques to visualize the cryocooling processes of macromolecular crystals. From these images it was clear that a cold wave progresses through a crystal starting at the face closest to the origin of the cold stream and ending at the point furthest away. During these studies we used large volume crystals, which were clearly distinguished from the loop holding them. These large crystals, originally grown for neutron diffraction studies, were chosen deliberately to enhance the imaging. As an extension to this work, we used thermal imaging to study small crystals, held in a cryo- loop, in the presence of vitrified mother liquor. The different infrared transmission and reflectance properties of the crystal in comparison to the mother liquor surrounding it are thought to be the parameter that produces the contrast that makes the crystal visible. An application of this technology may be the determination of the exact location of small crystals in a cryo-loop. Data from initial tests in support of application development was recorded for lysozyme crystals and for bFGF/dna complex crystals, which were cryo-cooled and imaged in large loops, both with visible light and with infrared radiation. The crystals were clearly distinguished from the vitrified solution in the infrared spectrum, while in the case of the bFGF/dna complex the illumination had to be carefully manipulated to make the crystal visible in the visible spectrum. These results suggest that the thermal imaging may be more sensitive than visual imaging for automated location of small crystals. However, further work on small crystals robotically mounted at SSRL did not clearly visualize those crystals. The depth of field of the camera proved to be limiting and a different cooling geometry was used, compared to the previous, successful experiments. Analysis to exploit multiple images to improve depth of field and experimental work to understand cooling geometry effects is ongoing. These results will be presented along with advantages and disadvantages of the technique and a discussion of how it might be applied .

An experimental study of pyroxene crystallization during rapid cooling in a thermal gradient; applications to komatiites and chondrites

NASA Astrophysics Data System (ADS)

Bouquain, S.; Arndt, N. T.; Faure, F.; Libourel, G.

2013-03-01

To investigate the crystallization of pyroxene in spinifex-textured komatiites and in chondrites we undertook a series of experiments in which compositions in the CMAS system were cooling rapidly in a thermal gradient. Cooling rates were generally between 5 to 10 °C h-1 but some runs were made at 100-200 °C h-1; thermal gradients were between 10 and 20 °C cm-1. These conditions reproduced those at various levels in the crust of komatiitic lava flow. The starting composition was chosen to have pigeonite on the liquidus and a majority of the experiments crystallized zoned pigeonite-diopside crystals like those in komatiite lavas. A~conspicuous aspect of the experimental results was their lack of reproduceability. Some experiments crystallized forsterite whereas others that were run under similar conditions crystallized two pyroxenes and no forsterite; some experiments were totally glassy but others totally crystallized to pyroxene. The degree of supercooling at the onset of pyroxene crystallization was variable, from less than 25 °C to more than 110 °C. We attribute these results to the difficulty of nucleation of pyroxene. In some cases forsterite crystallized metastably and modified the liquid composition to inhibit pyroxene crystallization; in others no nucleation took place until a large degree of supercooling was achieved, then pyroxene crystallized rapidly. Pigeonite crystallized under a wide range of conditions, at cooling rates from 3 to 100 °C h-1. The notion that this mineral only forms at low cooling rates is not correct.

Solubility and crystallization of xylose isomerase from Streptomyces rubiginosus

NASA Astrophysics Data System (ADS)

Vuolanto, Antti; Uotila, Sinikka; Leisola, Matti; Visuri, Kalevi

2003-10-01

We have studied the crystallization and crystal solubility of xylose isomerase (XI) from Streptomyces rubiginosus. In this paper, we show a rational approach for developing a large-scale crystallization process for XI. Firstly, we measured the crystal solubility in salt solutions with respect to salt concentration, temperature and pH. In ammonium sulfate the solubility of XI decreased logarithmically when increasing the salt concentration. Surprisingly, the XI crystals had a solubility minimum at low concentration of magnesium sulfate. The solubility of XI in 0.17 M magnesium sulfate was less than 0.5 g l -1. The solubility of XI increased logarithmically when increasing the temperature. We also found a solubility minimum around pH 7. This is far from the isoelectric point of XI (pH 3.95). Secondly, based on the solubility study, we developed a large-scale crystallization process for XI. In a simple and economical cooling crystallization of XI from 0.17 M magnesium sulfate solution, the recovery of crystalline active enzyme was over 95%. Moreover, we developed a process for production of uniform crystals and produced homogenous crystals with average crystal sizes between 12 and 360 μm.

An investigation of the effect of processing conditions on the lamellar and spherulitic morphology of polyhydroxyalkanoates

NASA Astrophysics Data System (ADS)

Xie, Yuping; Akpalu, Yvonne A.

2007-03-01

Polyhydroxyalkanoates (PHAs) have recently attracted much interest because of their biodegradability and biocompatibility. Since the ultimate properties of polymers can be controlled by processing conditions, particularly cooling rates, the systematic and thorough understanding of the effects of cooling rates on the final morphology and the resulting mechanical properties of PHAs is necessary and important. In this presentation, the lamellar (tens of nanometers), fibrillar (several hundred nanometers) and spherulitic (˜μm) morphologies of poly (3-hydroxybutyric acid) (PHB) and the copolymer poly (3-hydroxybutyric acid-co-3-hydroxyvaleric acid) (PHBV) crystallized under different cooling rates were studied using small angle X-ray scattering, ultra small angle X-ray scattering, and polarized optical microscopy, respectively. The morphology was observed to depend strongly on cooling rate. The influence of cooling rate on the morphology and mechanical properties such as toughness, tensile strength and overall stress-strain behavior will be discussed.

Demonstration of Crystal Structure.

ERIC Educational Resources Information Center

Neville, Joseph P.

1985-01-01

Describes an experiment where equal parts of copper and aluminum are heated then cooled to show extremely large crystals. Suggestions are given for changing the orientation of crystals by varying cooling rates. Students are more receptive to concepts of microstructure after seeing this experiment. (DH)

Astigmatic Herriott cell for optical refrigeration

NASA Astrophysics Data System (ADS)

Gragossian, Aram; Meng, Junwei; Ghasemkhani, Mohammadreza; Albrecht, Alexander R.; Sheik-Bahae, Mansoor

2017-01-01

Cooling rare-earth-doped crystals to the lowest temperature possible requires enhanced resonant absorption and high-purity crystals. Since resonant absorption decreases as the crystal is cooled, the only path forward is to increase the number of roundtrips that the laser makes inside the crystal. To achieve even lower temperatures than previously reported, we have employed an astigmatic Herriott cell to improve laser absorption at low temperatures. Preliminary results indicate improvement over previous designs. This cavity potentially enables us to use unpolarized high-power fiber lasers, and to achieve much higher cooling power for practical applications.

Dynamics of melt crystal interface and thermal stresses in rotational Bridgman crystal growth process

NASA Astrophysics Data System (ADS)

Ma, Ronghui; Zhang, Hui; Larson, David J.; Mandal, Krishna C.

2004-05-01

The growth process of potassium bromide (KBr) single crystals in a vertical Bridgman furnace has been studied numerically using an integrated model that combines formulation of global heat transfer and thermal elastic stresses. The global heat transfer sub-model accounts for conduction, convection and interface movement in the multiphase system. Using the elastic stress sub-model, thermal stresses in the growing crystal caused by the non-uniform temperature distribution is predicted. Special attention is directed to the interaction between the crystal and the ampoule. The global temperature distribution in the furnace, the flow pattern in the melt and the interface shapes are presented. We also investigate the effects of the natural convection and rotational forced convection on the shape of the growth fronts. Furthermore, the state of the thermal stresses in the crystal is studied to understand the plastic deformation mechanisms during the cooling process. The influence of the wall contact on thermal stresses is also addressed.

Novel approach for solid state cryocoolers.

PubMed

Volpi, Azzurra; Di Lieto, Alberto; Tonelli, Mauro

2015-04-06

Laser cooling in solids is based on anti-Stokes luminescence, via the annihilation of lattice phonons needed to compensate the energy of emitted photons, higher than absorbed ones. Usually the anti-Stokes process is obtained using a rare-earth active ion, like Yb. In this work we demonstrate a novel approach for optical cooling based not only to Yb anti-Stokes cycle but also to virtuous energy-transfer processes from the active ion, obtaining an increase of the cooling efficiency of a single crystal LiYF(4) (YLF) doped Yb at 5at.% with a controlled co-doping of 0.0016% Thulium ions. A model for efficiency enhancement based on Yb-Tm energy transfer is also suggested.

Semiconductor-to-metal phase change in MoTe2 layers (Conference Presentation)

NASA Astrophysics Data System (ADS)

Davydov, Albert V.; Krylyuk, Sergiy; Kalish, Irina; Meshi, Louisa; Beams, Ryan; Kalanyan, Berc; Sharma, Deepak K.; Beck, Megan; Bergeron, Hadallia; Hersam, Mark C.

2016-09-01

Molybdenum ditelluride (MoTe2), which can exist in a semiconducting prismatic hexagonal (2H) or a metallic distorted octahedral (1T') phases, is one of the very few materials that exhibit metal-semiconductor transition. Temperature-driven 2H - 1T' phase transition in bulk MoTe2 occurs at high temperatures (above 900 °C) and it is usually accompanied by Te loss. The latter can exacerbate the control over reversibility of the phase transition. Here, we study effects of high-temperature annealing on phase transition in MoTe2 single crystals. First, MoTe2 were grown in sealed evacuated quartz ampoules from polycrystalline MoTe2 powder in an iodine-assisted chemical vapor transport process at 1000 °C. The 2H and 1T' phases were stabilized by controlling the cooling rate after the growth. In particular, slow cooling at 10 °C/h rate yielded the 2H phase whereas the 1T' phase was stabilized by ice-water quenching. Next, the phase conversion was achieved by annealing MoTe2 single crystals in vacuum-sealed ampoules at 1000 °C with or without additional poly-MoTe2 powder followed by fast or slow cooling. Similarly to the CVT growth, slow cooling and quenching consistently produced 2H and 1T' phases, respectively, regardless of the initial MoTe2 crystal structure. We will discuss structural and optical properties of the as-grown and phase-converted MoTe2 single crystals using TEM, SEM/EDS, XRD, XPS and Raman. Electrical characteristics of two-terminal devices made from metallic 1T' and bottom-gated FETs made from 2H exfoliated crystals will also be presented.

Sideband cooling of small ion Coulomb crystals in a Penning trap

NASA Astrophysics Data System (ADS)

Stutter, G.; Hrmo, P.; Jarlaud, V.; Joshi, M. K.; Goodwin, J. F.; Thompson, R. C.

2018-03-01

We have recently demonstrated the laser cooling of a single ? ion to the motional ground state in a Penning trap using the resolved-sideband cooling technique on the electric quadrupole transition S? D?. Here we report on the extension of this technique to small ion Coulomb crystals made of two or three ? ions. Efficient cooling of the axial motion is achieved outside the Lamb-Dicke regime on a two-ion string along the magnetic field axis as well as on two- and three-ion planar crystals. Complex sideband cooling sequences are required in order to cool both axial degrees of freedom simultaneously. We measure a mean excitation after cooling of ? for the centre of mass (COM) mode and ? for the breathing mode of the two-ion string with corresponding heating rates of 11(2) ? and ? at a trap frequency of 162 kHz. The occupation of the ground state of the axial modes (?) is above 75% for the two-ion planar crystal and the associated heating rates 0.8(5) ? at a trap frequency of 355 kHz.

Method of synthesizing and growing copper-indium-diselenide (CuInSe/sub 2/) crystals

DOEpatents

Ciszek, T.F.

1984-11-29

A process for preparing CuInSe/sub 2/ crystals includes melting a sufficient quantity of B/sub 2/O/sub 2/ along with stochiometric quantities of Cu, In, and Se in a crucible in a high-pressure atmosphere of inert gas to encapsulate the CuInSe/sub 2/ melt and confine the Se to the crucible. Additional Se in the range of 1.8 to 2.2% over the stochiometric quantity is preferred to make up for small amounts of Se lost in the process. The melt can then be cooled slowly to form the crystal as direct solidification, or the crystal can be grown by inserting a seed crystal through the B/sub 2/O/sub 3/ encapsulate into contact with the CuInSe/sub 2/ melt and withdrawing the seed upwardly to grow the crystal thereon from the melt.

Erythritol: crystal growth from the melt.

PubMed

Lopes Jesus, A J; Nunes, Sandra C C; Ramos Silva, M; Matos Beja, A; Redinha, J S

2010-03-30

The structural changes occurring on erythritol as it is cooled from the melt to low temperature, and then heated up to the melting point have been investigated by differential scanning calorimetry (DSC), polarized light thermal microscopy (PLTM), X-ray powder diffraction (PXRD) and Fourier transform infrared spectroscopy (FTIR). By DSC, it was possible to set up the conditions to obtain an amorphous solid, a crystalline solid, or a mixture of both materials in different proportions. Two crystalline forms have been identified: a stable and a metastable one with melting points of 117 and 104 degrees C, respectively. The fusion curve decomposition of the stable form revealed the existence of three conformational structures. The main paths of the crystallization from the melt were followed by PLTM. The texture and colour changes allowed the characterization of the different phases and transitions in which they are involved on cooling as well as on heating processes. The type of crystallization front and its velocity were also followed by microscopic observation. These observations, together with the data provided by PXRD, allowed elucidating the transition of the metastable form into the stable one. The structural changes occurring upon the cooling and subsequent heating processes, namely those arising from intermolecular hydrogen bonds, were also accompanied by infrared spectroscopy. Particular attention was given to the spectral changes occurring in the OH stretching region. Copyright (c) 2009 Elsevier B.V. All rights reserved.

Single Crystal Casting with Fluidized Carbon Bed Cooling: A Process Innovation for Quality Improvement and Cost Reduction

NASA Astrophysics Data System (ADS)

Hofmeister, M.; Franke, M. M.; Koerner, C.; Singer, R. F.

2017-12-01

Superalloy gas turbine blades are being produced by investment casting and directional solidification. A new process, Fluidized Carbon Bed Cooling (FCBC), has been developed and is now being optimized in a prototype casting unit with 10 kg pouring weight. In early test runs with still rather simple mold cluster geometries, a reduction of the primary dendrite arm spacing of around 40 pct compared to the standard radiation cooling process (HRS) could be demonstrated. The improvement is mainly attributed to higher temperature gradients driving solidification, made possible by a functioning Dynamic Baffle. Compared to earlier development efforts in the literature, contamination of the melt and damage to the equipment are avoided using carbon-based fluidized bed materials and the so-called "counter pressure concept."

An experimental study of pyroxene crystallization during rapid cooling in a thermal gradient: application to komatiites

NASA Astrophysics Data System (ADS)

Bouquain, S.; Arndt, N. T.; Faure, F.; Libourel, G.

2014-07-01

To investigate the crystallization of pyroxene in spinifex-textured komatiites, we undertook a series of experiments in which compositions in the CaO-MgO-Al2O3-SiO2 CMAS system were cooled rapidly in a thermal gradient. Cooling rates were generally between 5 and 10 °C h-1, but some runs were made at 100-200 °C h-1; thermal gradients were between 10 and 20 °C cm-1. These conditions reproduced those at various depths in the crust of komatiite lava flow. The starting composition was chosen to have pigeonite on the liquidus, and most of the experimental charges crystallized zoned pigeonite-diopside crystals like those in komatiite lavas. An intriguing aspect of the experimental results was their lack of reproducibility. Some experiments crystallized forsterite, whereas others that were run under similar conditions crystallized two pyroxenes and no forsterite; some experiments were totally glassy, but others crystallized entirely to pyroxene. The degree of supercooling at the onset of pyroxene crystallization was variable, from less than 25 °C to more than 110 °C. We attribute these results to the difficulty of nucleation of pyroxene under the conditions of the experiments. In some cases forsterite crystallized metastably and modified the liquid composition to inhibit pyroxene crystallization; in others no nucleation took place until a large degree of supercooling was achieved, and then pyroxene crystallized rapidly. Pigeonite crystallized under a wide range of conditions, at cooling rates from 3 to 100 °C h-1. The notion that this mineral only forms at low cooling rates is not correct.

Rapid cooling and cold storage in a silicic magma reservoir recorded in individual crystals.

PubMed

Rubin, Allison E; Cooper, Kari M; Till, Christy B; Kent, Adam J R; Costa, Fidel; Bose, Maitrayee; Gravley, Darren; Deering, Chad; Cole, Jim

2017-06-16

Silicic volcanic eruptions pose considerable hazards, yet the processes leading to these eruptions remain poorly known. A missing link is knowledge of the thermal history of magma feeding such eruptions, which largely controls crystallinity and therefore eruptability. We have determined the thermal history of individual zircon crystals from an eruption of the Taupo Volcanic Zone, New Zealand. Results show that although zircons resided in the magmatic system for 10 3 to 10 5 years, they experienced temperatures >650° to 750°C for only years to centuries. This implies near-solidus long-term crystal storage, punctuated by rapid heating and cooling. Reconciling these data with existing models of magma storage requires considering multiple small intrusions and multiple spatial scales, and our approach can help to quantify heat input to and output from magma reservoirs. Copyright © 2017, American Association for the Advancement of Science.

Forward to cryogenic temperature: laser cooling of Yb: LuLiF crystal

NASA Astrophysics Data System (ADS)

Zhong, Biao; Luo, Hao; Lei, Yongqing; Shi, Yanling; Yin, Jianping

2017-06-01

The high quality Yb-doped fluoride crystals have broad prospects for optical refrigeration. We have laser cooled the Yb:LuLiF crystal to a temperature below the limit of current thermoelectric coolers ( 180 K). The 5% Yb:LuLiF crystal sample has a geometry of 2 mm×2 mm×5 mm and was supported by two fibers of 200 μm in diameter. They were placed in a 2×10-4 Pa vacuum chamber with an environment temperature of 294.5 K. The 1019 nm CW laser of power 38.7 W was adopted to irradiate the sample. The temperature of the sample was measured utilizing the DLT methods. After 20 minutes of laser irradiation, the 5% Yb:LuLiF crystal sample was cooled down to 182.4 K. By further optimizing experimental conditions and increasing the doped Yb concentration, the Yb:LuLiF crystal might be optically cooled below the cryogenic temperature of 123K in the near future.

The Effects of Thermal History on Nucleation of Tetragonal Lysozyme Crystals, or Hot Protein and Cold Nucleation

NASA Technical Reports Server (NTRS)

Burke, Michael; Judge, Russell; Pusey, Marc

2000-01-01

Chicken egg white lysozyme has a well characterized thermally driven phase transition. Between pH 4.2 and 5.2, the transition temperature, as defined by the point where the tetragonal and orthorhombic solubilities are equal, is a function of the pH, salt (precipitant) type and concentration, and most likely of the buffer concentration as well. This phase transition can be carried out with protein solution alone, prior to addition of precipitant solution. Warming a lysozyme solution above the phase transition point, then cooling it back below this point, has been shown to affect the subsequent nucleation rate, as determined by the numbers and size of crystals formed, but not the growth rate for the tetragonal crystal form . We have now measured the kinetics of this process and investigated its reversibility. The transition effects are progressive with temperature, having a half time of about 1 hour at 37C at pH 4.8. After holding a lysozyme solution at 37C (prior to addition of precipitant) for 16 hours, then cooling it back to 4C no return to the pre-warmed nucleation kinetics are observed after at least 4 weeks. Orthorhombic lysozyme crystals apparently do not undergo the flow-induced growth cessation of tetragonal lysozyme crystals. Putting the protein in the orthorhombic form does not affect the averaged face growth kinetics, only nucleation, for tetragonal crystals. This differential behaviour may be exploited to elucidate how and where flow affects the lysozyme crystal growth process. The presentation will focus on the results of these and ongoing studies in this area.

Fast ion swapping for quantum-information processing

NASA Astrophysics Data System (ADS)

Kaufmann, H.; Ruster, T.; Schmiegelow, C. T.; Luda, M. A.; Kaushal, V.; Schulz, J.; von Lindenfels, D.; Schmidt-Kaler, F.; Poschinger, U. G.

2017-05-01

We demonstrate a swap gate between laser-cooled ions in a segmented microtrap via fast physical swapping of the ion positions. This operation is used in conjunction with qubit initialization, manipulation, and readout and with other types of shuttling operations such as linear transport and crystal separation and merging. Combining these operations, we perform quantum process tomography of the swap gate, obtaining a mean process fidelity of 99.5(5)%. The swap operation is demonstrated with motional excitations below 0.05(1) quantum for all six collective modes of a two-ion crystal for a process duration of 42 μ s . Extending these techniques to three ions, we reverse the order of a three-ion crystal and reconstruct the truth table for this operation, resulting in a mean process fidelity of 99.96(13)% in the logical basis.

Cold crucible Czochralski for solar cells

NASA Technical Reports Server (NTRS)

Trumble, T. M.

1982-01-01

The efficiency and radiation resistance of present silicon solar cells are a function of the oxygen and carbon impurities and the boron doping used to provide the proper resistivity material. The standard Czochralski process used grow single crystal silicon contaminates the silicon stock material due to the use of a quartz crucible and graphite components. The use of a process which replaces these elements with a water cooled copper to crucible has provided a major step in providing gallium doped (100) crystal orientation, low oxygen, low carbon, silicon. A discussion of the Cold Crucible Czochralski process and recent float Zone developments is provided.

Cold crucible Czochralski for solar cells

NASA Astrophysics Data System (ADS)

Trumble, T. M.

The efficiency and radiation resistance of present silicon solar cells are a function of the oxygen and carbon impurities and the boron doping used to provide the proper resistivity material. The standard Czochralski process used grow single crystal silicon contaminates the silicon stock material due to the use of a quartz crucible and graphite components. The use of a process which replaces these elements with a water cooled copper to crucible has provided a major step in providing gallium doped (100) crystal orientation, low oxygen, low carbon, silicon. A discussion of the Cold Crucible Czochralski process and recent float Zone developments is provided.

Crystallization Behavior of the CaO-Al2O3-MgO System Studied with a Confocal Laser Scanning Microscope

NASA Astrophysics Data System (ADS)

Jung, Sung Suk; Sohn, Il

2012-12-01

The crystallization behavior of a calcium-aluminate system with various MgO content from 2.5 to 7.5 wt pct and CaO/Al2O3 ratios between 0.8 and 1.2 has been examined using a confocal laser scanning microscope (CLSM). CCT (continuous cooling transformation) and time temperature transformation (TTT) diagrams were constructed to identify the primary crystal phase of slag at different compositions and at cooling rates between 25 and 800 K/minutes. In the slag at a CaO/Al2O3 ratio of 1.0, crystallization temperature increased during isothermal and continuous cooling with higher MgO content, and the shortest incubation time was observed at 5 wt pct MgO. When MgO content was fixed to be 5 wt pct, crystallization temperature increased with lower CaO/Al2O3 ratio. According to the slag composition, cooling rates and temperature, the primary phase could be CA, or C5A3, or C3A, or C3MA2, or MgO, and the crystal morphology changes from dendrites to faceted crystals to columnar crystals in this composition range.

Nucleated Poly(L-lactic acid) with N, N‧-oxalyl bis(benzoic acid) dihydrazide

NASA Astrophysics Data System (ADS)

Tian, Liang-Liang; Cai, Yan-Hua

2018-04-01

One of the major challenges in the field of Poly(L-lactic acid) (PLLA) is the enhancement of crystallization. In the present work, the evaluation of the influence of N, N‧-oxalyl bis(benzoic acid) dihydrazide (TBOD), as a novel organic nucleating agent, on the non-isothermal crystallization, melting behavior, and thermal stability of PLLA was performed using differential scanning calorimeter and thermogravimetric analysis. Non-isothermal crystallization measurement revealed that TBOD had an excellent accelerating effect for the crystallization of PLLA in cooling, and upon the addition of 3 wt% TBOD, PLLA exhibited the highest onset crystallization temperature and the crystallization peak temperature, as well as the largest non-isothermal crystallization enthalpy. In particular, when the TBOD concentration was 1 wt% ∼ 3 wt%, the onset crystallization temperatures were higher than the theoretical ceiling temperature of crystallization, thoroughly demonstrating the powerful crystallization promoting ability of TBOD. Additionally, the non-isothermal crystallization behavior of PLLA/TBOD depended on the TBOD concentration, cooling rate as well as the final melting temperature. The melting behavior of PLLA/TBOD after non-isothermal crystallization further confirmed the effect of TBOD on the crystallization process and crystal structure of PLLA, and the appearance of the double melting peaks during melting stages was attribute to the melting-recrystallization. For melting behavior after isothermal crystallization, the crystallization temperature and crystallization time significantly affected the melting behavior of PLLA/TBOD. The addition of TBOD could not change the thermal decomposition profile of the PLLA, but the thermal stability did not regularly decrease with increasing of TBOD concentration, indicating that there might exist intermolecular interaction between PLLA and TBOD.

Investigation of Artificial Forced Cooling in the Bridgman Crystal Growth of Cadmium Zinc Telluride

NASA Astrophysics Data System (ADS)

Liu, Juncheng; Li, Jiao; Zhang, Guodong; Li, Changxing; Lennon, Craig; Sivananthan, Siva

2007-08-01

The effects of artificial forced cooling on the solid liquid interface and on solute segregation were investigated by modeling the vertical Bridgman method for the single-crystal growth of CdZnTe, taking into consideration effects such as increasing the axial outward heat flux from the crucible bottom, the radial outward heat flux from the crucible wall, and the carbon film thickness on the crucible inner wall. Axial artificially forced cooling noticeably increases convection and the temperature gradient in the melt next to the solid liquid interface, and substantially reduces interface concavity at the initial solidification stage. Interface concavity increases a little when the solidification proceeds further, however. Axial artificially forced cooling reduces radial solute segregation of the initial segment of the grown crystal and slightly increases the solute iso-concentration segment. Radial artificially forced cooling enhances melt convection substantially, affects solid liquid interface concavity only slightly, and hardly affects solute segregation in the grown crystal. Doubling the carbon film thickness weakens convection of the melt in front of the interface, substantially increases interface concavity, and hardly affects solute segregation in the grown crystal.

Thermal evolution of old white dwarfs

NASA Astrophysics Data System (ADS)

Kozhberov, Andrew

2017-11-01

This work is devoted to a description of thermodynamic properties of Coulomb crystals which are expected to form in white dwarf interiors. Effects of magnetic field, isotopic impurities, polarization of the electron background and crystal lattice type on the thermal evolution of white dwarfs are discussed. It is shown that the electron polarization could play a noticeable role in the cooling process. While other parameters in concern do not make a significant impact.

Morphological diversity of nitroguanidine crystals with enhanced mechanical performance and thermodynamic stability

NASA Astrophysics Data System (ADS)

Luo, Zhilong; Cui, Yingdan; Dong, Weibing; Xu, Qipeng; Zou, Gaoxing; Kang, Chao; Hou, Baohong; Chen, Song; Gong, Junbo

2017-12-01

Nitroguanidine (NQ) is a commonly used explosive, which has been widely used for both civilian and military explosive applications. However, the weak flowability and mechanical performance limit its application. In this work, mechanical performance and thermodynamic stability of NQ crystals were improved by controlling crystal morphologies in the crystallization process. Typical NQ crystals with multiple morphologies and single crystal form were obtained in the presence of additives during the cooling crystallization. The morphology controlled NQ crystals showed higher density, unimodal crystal size distribution and enhanced flowability. The additives showed the inhibitory effect on the nucleation of NQ crystals by in-situ FBRM and PVM determination, and the mechanism was analyzed by means of morphological prediction and molecular simulation. Furthermore, the morphology controlled NQ crystals suggested higher thermodynamic stability according to the calculation of entropy, enthalpy, Gibbs free energy and apparent activation energy on the basis of DSC results.

Microgravity

NASA Image and Video Library

2004-04-15

Comparison of Germanium Telluride (GeTe) Crystals grown on Earth (left) and in space (right) during the Skylab SL-3 mission. These crystals were grown using a vapor transport crystal growth method in the Multipurpose Electric Furnace System (MEFS). Crystals grown on earth are needles and platelettes with distorted surfaces and hollow growth habits. The length of the ground-based needle is approximately 2 mm and the average lenth of the platelets is 1 mm. The dull appearance of the Skylab crystals resulted from condensation of the transport agent during the long cooling period dictated by the Skylab furnace. In a dedicated process, this would be prevented by removing the ampoule from the furnace and quenching the vapor source.

Crystallization and Cooling of a Deep Silicate Magma Ocean

NASA Astrophysics Data System (ADS)

Wolf, A. S.; Bower, D. J.

2015-12-01

Impact and accretion simulations of terrestrial planet formation suggest that giant impacts are both common and expected to produce extensive melting. The moon-forming impact, for example, likely melted the majority of Earth's mantle to produce a global magma ocean that subsequently cooled and crystallized (e.g. Nakajima and Stevenson, 2015). Understanding the cooling process is critical to determining magma ocean lifetimes and recognizing possible remnant signatures of the magma ocean in present-day mantle heterogeneities (i.e. Labrosse et al., 2007). Modeling this evolution is challenging, however, due to the vastly different timescales and lengthscales associated with turbulent convection (magma ocean) and viscous creep (present-day mantle), in addition to uncertainties in material properties and chemical partitioning. We consider a simplified spherically-symmetric (1-D) magma ocean to investigate both its evolving structure and cooling timescale. Extending the work of Abe (1993), mixing-length theory is employed to determine convective heat transport, producing a high resolution model that captures the ultra-thin boundary layer (few cms) at the surface of the magma ocean. The thermodynamics of mantle melting are represented using a pseudo-one-component model, which retains the simplicity of a standard one-component model while introducing a finite temperature interval for melting (important for multi-component systems). We derive a new high P-T equation of state (EOS) formulation designed to capture the energetics and physical properties of the partially molten system using parameters that are readily interpreted in the context of magma ocean crystallization. This model is used to determine the cooling timescale for a variety of plausible thermodynamic models, with special emphasis on comparing the center-outwards vs bottom-up cooling scenarios that arise from the assumed EOS (e.g., Mosenfelder et al., 2009; Stixrude et al., 2009).

Evidence of monotropic hexatic tilted smectic phase in the phase sequence of ferroelectric liquid crystal

NASA Astrophysics Data System (ADS)

Różycka, Anna; Deptuch, Aleksandra; Jaworska-Gołąb, Teresa; Węgłowska, Dorota; Marzec, Monika

2018-02-01

Physical properties of a new ferroelectric liquid crystal have been studied by complementary methods: differential scanning calorimetry, polarizing optical microscopy, dielectric and X-ray diffraction. It was found that next to enantiotropic ferroelectric smectic C* phase, the monotropic smectic phase appears at cooling. X-ray diffraction measurements allowed to identify this phase as hexatic tilted smectic. Temperature dependence of spontaneous polarization, tilt angle of molecules and switching time were found in both liquid crystalline phases at cooling. Based on the dielectric results, the dielectric processes were identified as Goldstone mode in the smectic C* phase, whereas as the bond-orientation-like phason and the bulk domain mode in the monotropic hexatic tilted smectic phase.

Dynamic crystallization of silicate melts

NASA Technical Reports Server (NTRS)

Russell, W. J.

1984-01-01

Two types of furnaces with differing temperature range capabilities were used to provide variations in melt temperatures and cooling rates in a study of the effects of heterogeneous nucleation on crystallization. Materials of chondrule composition were used to further understanding of how the disequilibrium features displayed by minerals in rocks are formed. Results show that the textures of natural chondrules were duplicated. It is concluded that the melt history is dominant over cooling rate and composition in controlling texture. The importance of nuclei, which are most readily derived from preexisting crystalline material, support an origin for natural chondrules based on remelting of crystalline material. This would be compatible with a simple, uniform chondrule forming process having only slight variations in thermal histories resulting in the wide range of textures.

The role of superheating in the formation of Glass Mountain obsidians (Long Valley, CA) inferred through crystallization of sanidine

NASA Astrophysics Data System (ADS)

Waters, Laura E.; Andrews, Benjamin J.

2016-10-01

The Glass Mountain obsidians (Long Valley, CA) are crystal poor (<8 vol%) and highly evolved (high SiO2, low Sr), and therefore, their formation required extremely efficient separation of melts from a crystal-rich source. A petrologic and experimental investigation of the mineral phases in Glass Mountain lavas identifies conditions under which phenocrysts grew and the driving mechanism for crystallization, which places constraints on the possible processes that generated the obsidians. The obsidian in this study (GM-11) is saturated in nine phases (sanidine + quartz + plagioclase + titanomagnetite + ilmenite + zircon + apatite + allanite + biotite), and results of high-resolution SEM compositional mapping and electron microprobe analysis reveal that individual sanidine crystals are normally zoned and span a range of compositions (Or40-78). Sanidines have a "granophyric" texture, characterized by intergrowths of quartz and sanidine. Mineral phases in the natural sample are compared to H2O-saturated phase equilibrium experiments conducted in cold-seal pressure vessels, over a range of conditions (700-850 °C; 75-225 MPa), and all are found to be plausible phenocrysts. Comparison of sanidine compositions from the natural sample with those grown in phase equilibrium experiments demonstrates that sanidine in the natural sample occurs in a reduced abundance. Further comparison with phase equilibrium experiments suggests that sanidine compositions track progressive loss of dissolved melt water (±cooling), suggesting that crystallization in the natural obsidian was driven predominantly by degassing resulting from decompression. It is paradoxical that an effusively (slowly) erupted lava should contain multiple phenocryst phases, including sanidine crystals that span a range of compositions with granophyric textures, and yet remain so crystal poor. To resolve this paradox, it is necessary that the solidification mechanism (degassing or cooling) that produced the sanidine crystals (and other mineral phases) must have an associated kinetic effect(s) that efficiently hinders crystal nucleation and growth. Decompression experiments conducted in this study and from the literature collectively demonstrate that the simplest way to inhibit nucleation during degassing-induced crystallization is to initiate degassing ± cooling from superliquidus conditions, and therefore, the Glass Mountain obsidians were superheated prior to crystallization.

Flash crystallization kinetics of methane (sI) hydrate in a thermoelectrically-cooled microreactor.

PubMed

Chen, Weiqi; Pinho, Bruno; Hartman, Ryan L

2017-09-12

The crystallization kinetics of methane (sI) hydrate were investigated in a thermoelectrically-cooled microreactor with in situ Raman spectroscopy. Step-wise and precise control of the temperature allowed acquisition of reproducible data within minutes, while the nucleation of methane hydrates can take up to 24 h in traditional batch reactors. The propagation rates of methane hydrate (from 3.1-196.3 μm s -1 ) at the gas-liquid interface were measured for different Reynolds' numbers (0.7-68.9), pressures (30.0-80.9 bar), and sub-cooling temperatures (1.0-4.0 K). The precise measurement of the propagation rates and their subsequent analyses revealed a transition from mixed heat-transfer-crystallization-rate-limited to mixed heat-transfer-mass-transfer-crystallization-rate-limited kinetics. A theoretical model, based on heat transfer, mass transfer, and intrinsic crystallization kinetics, was derived for the first time to understand the non-linear relationship between the propagation rate and sub-cooling temperature. The molecular diffusivity of methane within a stagnant film (ahead of the propagation front) was discovered to follow Stokes-Einstein, while calculated Hatta (0.50-0.68), Lewis (128-207), and beta (0.79-116) numbers also confirmed that the diffusive flux influences crystal growth. Understanding methane hydrate crystal growth is important to the atmospheric, oceanic, and planetary sciences and to energy production, storage, and transportation. Our discoveries could someday advance the science of other multiphase, high-pressure, and sub-cooled crystallizations.

Unique nucleation activity of inorganic fullerene-like WS2 nanoparticles in polyphenylene sulfide nanocomposites: isokinetic and isoconversional study of dynamic crystallization kinetics.

PubMed

Naffakh, Mohammed; Marco, Carlos; Gómez, Marián A; Jiménez, Ignacio

2009-05-21

The dynamic crystallization kinetics of polyphenylene sulfide (PPS) nanocomposites with inorganic fullerene WS2 nanopartices (IF-WS2) content varying from 0.05 to 8 wt % has been studied using differential scanning calorimetry (DSC). The analysis of the crystallization at different cooling rates demonstrates that the completely isokinetic description of the crystallization process is not possible. However, the isoconversional methods in combination with the JMAEK equation provide a better understanding of the kinetics of the dynamic crystallization process. The addition of IF-WS2 influences the crystallization kinetics of PPS but in ways unexpected for polymer nanocomposites. A drastic change from retardation to promotion of crystallization is observed with increasing nanoparticle content. In the same way, the results of the nucleation activity and the effective energy barrier confirmed the unique dependence of the crystallization behavior of PPS on composition. In addition, the morphological data obtained from the polarized optical microscopy (POM) and time-resolved synchrotron X-ray diffraction is consistent with results of the crystallization kinetics of PPS/IF-WS2 nanocomposites.

Vapor Saturation as The Cause of Volcanic Eruptions at the Lassen Volcanic Center, California, as Inferred from Crystallization Pressures and Temperatures

NASA Astrophysics Data System (ADS)

De Los Reyes, A. M. A.; Putirka, K. D.; Clynne, M. A.; Scruggs, M. A.

2015-12-01

The last three silicic eruptions at the Lassen Volcanic Center occurred at Lassen Peak (27 ka and 1915-17) and Chaos Crags (1103 yrs BP). Klemetti and Clynne (2014) showed that felsic eruptions at Lassen reflect remobilization of resident rhyodacitic crystal mush by intrusion of mafic magma. To better understand the rejuvenation and eruption triggering process, we calculate crystallization temperatures and pressures from clinopyroxene-liquid equilibria on mafic enclaves that provide our closest approach to the composition of mafic magmas delivered to the shallow system. Our goal is to examine whether and to what extent cooling and crystallization occur after recharge, which bears on whether recharge, mixing, or partial crystallization (and consequent vapor saturation) provide the trigger for eruption. We use results from the cpx-liq barometer (1.7 kbar) as input to calculate T for other phases (plagioclase, olivine and amphibole) found in mafic enclave samples. Cpx crystallizes at 1100-1150 oC and olivine precipitates at similar to slightly higher temperatures. Cpx and ol are followed by plagioclase (1000-1050 oC), amphibole (875-1000 oC), and Fe-Ti oxides (1030-1050 oC). These temperatures indicate that recharge magmas are incompletely crystallized as they enter the shallow reservoir of cooler (~725-750 oC, Quinn et al., 2013) felsic crystal mush, and that significant cooling of the mafic magma occurs during mixing and prior to eruption. Such cooling intervals indicate that recharge is not the proximal cause of eruption, but rather that vapor saturation, following a period of mixing and cooling, leads to increased magma overpressure that causes eruption. Interestingly, the Lassen Peak 27 ka volcanics (at 2.09 km3), have a greater volume than either of Chaos Crags (1.2 km3) and the 1915 (0.03 km3) eruption, but our results indicate that their thermal histories are similar. This suggests that while volumes of mafic recharge may control the degree of interaction with felsic crystal mush (e.g., Clynne, 1999), and eventually the volume of erupted magma, recharge volumes do not affect eruption triggering mechanisms. Clynne MA (1999) J. Petrol, 40: 105-132.Klemetti and Clynne, 2014, PLoS One (/12:e113157. doi10.1371/journal.pone0113157)Quinn et al., 2013, AGU Fall Annual Meeting V23C-2848

The effect of growth temperature on the irreversibility line of MPMG YBCO bulk with Y2O3 layer

NASA Astrophysics Data System (ADS)

Kurnaz, Sedat; Çakır, Bakiye; Aydıner, Alev

2017-07-01

In this study, three kinds of YBCO samples which are named Y1040, Y1050 and Y1060 were fabricated by Melt-Powder-Melt-Growth (MPMG) method without a seed crystal. Samples seem to be single crystal. The compacted powders were located on a crucible with a buffer layer of Y2O3 to avoid liquid to spread on the furnace plate and also to support crystal growth. YBCO samples were investigated by magnetoresistivity (ρ-T) and magnetization (M-T) measurements in dc magnetic fields (parallel to c-axis) up to 5 T. Irreversibility fields (Hirr) and upper critical fields (Hc2) were obtained using 10% and 90% criteria of the normal state resistivity value from ρ-T curves. M-T measurements were carried out using the zero field cooling (ZFC) and field cooling (FC) processes to get irreversible temperature (Tirr). Fitting of the irreversibility line results to giant flux creep and vortex glass models were discussed. The results were found to be consistent with the results of the samples fabricated using a seed crystal. At the fabrication of MPMG YBCO, optimized temperature for crystal growth was determined to be around 1050-1060 °C.

Silicon crystals: Process for manufacturing wafer-like silicon crystals with a columnar structure

NASA Technical Reports Server (NTRS)

Authier, B.

1978-01-01

Wafer-like crystals suitable for making solar cells are formed by pouring molten Si containing suitable dopants into a mold of the desired shape and allowing it to solidify in a temperature gradient, whereby the large surface of the melt in contact with the mold is kept at less than 200 D and the free surface is kept at a temperature of 200-1000 D higher, but below the melting point of Si. The mold can also be made in the form of a slit, whereby the 2 sides of the mold are kept at different temperatures. A mold was milled in the surface of a cylindrical graphite block 200 mm in diameter. The granite block was induction heated and the bottom of the mold was cooled by means of a water-cooled Cu plate, so that the surface of the mold in contact with one of the largest surfaces of the melt was held at approximately 800 D. The free surface of the melt was subjected to thermal radiation from a graphite plate located 2 mm from the surface and heated to 1500 D. The Si crystal formed after slow cooling to room temperature had a columnar structure and was cut with a diamond saw into wafers approximately 500 mm thick. Solar cells prepared from these wafers had efficiencies of 10 to 11%.

Specific Features of the Domain Structure of BaTiO3 Crystals during Thermal Heating and Cooling

NASA Astrophysics Data System (ADS)

Kiselev, D. A.; Ilina, T. S.; Malinkovich, M. D.; Sergeeva, O. N.; Bolshakova, N. N.; Semenova, E. M.; Kuznetsova, Yu. V.

2018-04-01

This paper presents the results of the study of the domain structure of barium titanate crystals in a wide temperature range including the Curie point ( T C) using the polarization-optical method in the reflected light and the force microscopy of the piezoelectric response. It is shown that a new a-c domain structure forms during cyclic heating of the crystal above T C and subsequent cooling to the ferroelectric phase. The role of uncompensated charges appeared on the crystal surface during the phase transition and their influence on the formation of the domain structure during cooling are discussed.

Estimation of the growth kinetics for the cooling crystallisation of paracetamol and ethanol solutions

NASA Astrophysics Data System (ADS)

Mitchell, Niall A.; Ó'Ciardhá, Clifford T.; Frawley, Patrick J.

2011-08-01

This work details the estimation of the growth kinetics of paracetamol in ethanol solutions for cooling crystallisation processes, by means of isothermal seeded batch experiments. The growth kinetics of paracetamol crystals were evaluated in isolation, with the growth rate assumed to be size independent. Prior knowledge of the Metastable Zone Width (MSZW) was required, so that supersaturation ratios of 1.7-1.1 could be induced in solution without the occurrence of nucleation. The technique involved the utilisation of two in-situ Process Analytical Techniques (PATs), with a Focused Beam Reflectance Measurement (FBRM ®) utilised to ensure that negligible nucleation occurred and an Attenuated Total Reflectance-Fourier Transform Infrared (ATR-FTIR) probe employed for online monitoring of solute concentration. Initial Particle Size Distributions (PSDs) were used in conjunction with desupersaturation profiles to determine the growth rate as a function of temperature and supersaturation. Furthermore, the effects of seed loading and size on the crystal growth rate were investigated. A numerical model, incorporating the population balance equation and the method of moments, was utilised to describe the crystal growth process. Experimental parameters were compared to the model simulation, with the accuracy of the model validated by means of the final product PSDs and solute concentration.

Laboratory duplication of comb layering in the Rhum pluton. [igneous rocks with comb layered texture

NASA Technical Reports Server (NTRS)

Donaldson, C. H.

1977-01-01

A description is provided of the texture of harrisite comb layers, taking into account the results of crystallization experiments at controlled cooling rates, which have reproduced the textural change from 'cumulate' to comb-layered harrisite. Melted samples of harrisite were used in the dynamic crystallization experiments considered. The differentiation of a cooling rate run with respect to olivine grain size and shape is shown and three possible origins of hopper olivine in differentiated crystallization runs are considered. It is found that olivine nucleation occurred throughout cooling, except for the incubation period during early cooling. The elongate combed olivines in harrisite apparently grew as the magma locally supercooled to at least 30 C. It is suggested that the branching crystals in most comb layers, including comb-layered harrisite, probably grew along thermal gradients.

Crystallization of Synthetic Blast Furnace Slags Pertaining to Heat Recovery

NASA Astrophysics Data System (ADS)

Esfahani, Shaghayegh

Heat recovery from blast furnace slags is often contradicted by another requirement, to generate amorphous slag for its use in cement production. As both the rate and extent of heat recovery and slag structure are determined by its cooling rate, a relation between the crystallization kinetics and the cooling conditions is highly desired. In this study, CaO-SiO2-Al2O3-MgO (CSAM) slags with different basicities were studied by Single Hot Thermocouple Technique (SHTT) during isothermal treatment and non-isothermal cooling. Their time-temperature-transformation (TTT) and continuous-cooling-transformation (CCT) diagrams were plotted and compared with each other. Furthermore, kinetic parameters such as the Avrami exponent (n), rate coefficient (K) and effective activation energy of crystallization (EA) were found by analysis of data obtained from in-situ observation of glassy to crystalline transformation and image analysis. Also, the dependence of nucleation and growth rates of crystalline phases were quantified as a function of time, temperature, and slag basicity. Together with the observations of crystallization front, they facilitated establishing the dominant mechanisms of crystallization. In addition to the experimental work, a mathematical model was developed and validated that predicts the amount of crystallization during cooling. A second mathematical model that calculates temperature history of slag during its cooling was coupled with the above model, to allow studying the effect of parameters such as the slag/air ratio and granule size on the heat recovery and glass content of slag.

Building Magnetic Fields in White Dwarfs

NASA Astrophysics Data System (ADS)

Kohler, Susanna

2017-03-01

White dwarfs, the compact remnants left over at the end of low- and medium-mass stars lifetimes, are often found to have magnetic fields with strengths ranging from thousands to billions of times that of Earth. But how do these fields form?MultiplePossibilitiesAround 1020% of white dwarfs have been observed to have measurable magnetic fields with a wide range of strengths. There are several theories as to how these fields might be generated:The fields are fossil.The original weak magnetic fields of the progenitor stars were amplified as the stars cores evolved into white dwarfs.The fields are caused by binary interactions.White dwarfs that formed in the merger of a binary pair might have had a magnetic field amplified as a result of a dynamo that was generated during the merger.The fields were produced by some other internal physical mechanism during the cooling of the white dwarf itself.In a recent publication, a team of authors led by Jordi Isern (Institute of Space Sciences, CSIC, and Institute for Space Studies of Catalonia, Spain) explored this third possibility.Dynamos from CrystallizationThe inner and outer boundaries of the convective mantle of carbon/oxygen white dwarfs of two different masses (top vs. bottom panel) as a function of luminosity. As the white dwarf cools (toward the right), the mantle grows thinner due to the crystallization and settling of material. [Isern et al. 2017]As white dwarfs have no nuclear fusion at their centers, they simply radiate heat and gradually cool over time. The structure of the white dwarf undergoes an interesting change as it cools, however: though the object begins as a fluid composed primarily of an ionized mixture of carbon and oxygen (and a few minor species like nickel and iron), it gradually crystallizes as its temperature drops.The crystallized phase of the white dwarf is oxygen-rich which is denser than the liquid, so the crystallized material sinks to the center of the dwarf as it solidifies. As a result, the white dwarf forms a solid, oxygen-rich core with a liquid, carbon-rich mantle thats Rayleigh-Taylor unstable: as crystallization continues, the solids continue to sink out of the mantle.By analytically modeling this process, Isern and collaborators demonstrate that the Rayleigh-Taylor instabilities in the convective mantle can drive a dynamo large enough to generate the magnetic field strengths weve observed in white dwarfs.Magnetic field density as a function of the dynamo energy density. The plots show Earth and Jupiter (black dots), T Tauri stars (cyan), M dwarf stars (magenta), and two types of white dwarfs (blue and red). Do these lie on the same scaling relation? [Isern et al. 2017]A Universal Process?This setup the solid core with an unstable liquid mantle on top is exactly the structure expected to occur in planets such as Earth and Jupiter. These planets magnetic fields are similarly thought to be generated by convective dynamos powered by the cooling and chemical separation of their interiors and the process can also be scaled up to account for the magnetic fields of fully convective objects like T Tauri stars, as well.If white-dwarf magnetic fields are generated by the same type of dynamo, this may be a universal process for creating magnetic fields in astrophysical objects though other processes may well be at work too.CitationJordi Isern et al 2017 ApJL 836 L28. doi:10.3847/2041-8213/aa5eae

Phase determinations and crystal growth of Pb 2KNb 5O 15 (PKN)

NASA Astrophysics Data System (ADS)

Kramer, W. E.; Roland, G. W.

1982-07-01

Two problems must be addressed before good quality crystals of Pb 2KNb 5O 15 (PKN) can be grown: first, the compound does not melt congruently and therefore growth must be slow to avoid inclusions in the crystal; and second, cracking of crystals occurs during cooling due to anisotropic behavior of the thermal expansion coefficients at the Curie temperature. Extremely slow cooling in a uniform temperature gradient is necessary to get good quality, uncracked crystals.

19. RW Meyer Sugar: 18761889. Cooling Shed Interior, 1881. View: ...

Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

19. RW Meyer Sugar: 1876-1889. Cooling Shed Interior, 1881. View: Looking toward west end of cooling shed. After the concentrated syrup flowed out of the sorghum pan it cooled and crystallized in large sugar coolers. The humidity and vapors caused by the sorghum pan would have retarded the crystallizing and cooling of the sugar in the boiling house. In 1881 this shed was constructed to house the coolers and the sugar before it was dried in the centrifugals. - R. W. Meyer Sugar Mill, State Route 47, Kualapuu, Maui County, HI

Orbicules and Comb Layers: Igneous Layering in Shallow Plutons as a Result of Mineral Growth in Subvolcanic Conduits

NASA Astrophysics Data System (ADS)

McCarthy, A. J.; Müntener, O.

2017-12-01

Different processes have been proposed to explain the variety of igneous layering in plutonic rocks. Vertical layering in particular has been described as resulting from various processes such as Ostwald ripening, oscillatory crystallization or reactive mush infiltration in cooling plutons. Comb layers and orbicules are formed by the growth of elongated, feather-like minerals growing ±perpendicular to the layering and nucleating either on dyke walls (comb layers) or on xenoliths (orbicules) at the contact between homogenous plutons. Through a detailed study of the mineralogy, bulk chemistry and the size-frequency distribution of representative comb layers and orbicules of the 110Ma Fisher Lake Pluton (Sierra Nevada, USA), we show that comb layers and orbicules show no evidence of forming through a self-organizing, oscillatory crystallization process, but represent crystallization fronts resulting from in-situ crystallization and extraction of evolved melt fractions during decompression-driven crystallization of superheated melts in subvolcanic conduits. The microstructures are dominated by the formation of a plagioclase-dominated cres-cumulate at the mm- to m-scale. We propose that the crystal content of the melt and the dynamics of the magmatic system control the mechanisms responsible for vertical igneous layering in shallow reservoirs. Moreover, the mineralogical and compositional variation of orbicules rims and comb layers can be ascribed to variations in pressure, temperature and cooling rates within the subvolcanic conduit, with estimated growth timescales of mm- to m-thick orbicules and comb layers ranging from weeks to years. Moreover, though plagioclase-glomerocrysts found in erupted volcanic products are generally interpreted as remobilized crystal-mush, we propose that some glomerocrysts might represent "failed" orbicules forming within vertical conduits upon eruption. Such glomerocrysts, as well as orbicules found in erupted volcanic products, might allow for unique insights into the dynamics, timescales and P-T conditions within volcanic conduits upon eruption.

Example of a Fluid-Phase Change Examined with MD Simulation: Evaporative Cooling of a Nanoscale Droplet.

PubMed

Ao, Takashi; Matsumoto, Mitsuhiro

2017-10-24

We carried out a series of molecular dynamics simulations in order to examine the evaporative cooling of a nanoscale droplet of a Lennard-Jones liquid. After thermally equilibrating a droplet at a temperature T ini /T t ≃ 1.2 (T t is the triple-point temperature), we started the evaporation into vacuum by removing vaporized particles and monitoring the change in droplet size and the temperature inside. As free evaporation proceeds, the droplet reaches a deep supercooled liquid state of T/T t ≃ 0.7. The temperature was found to be uniform in spite of the fast evaporative cooling on the surface. The time evolution of the evaporating droplet properties was satisfactorily explained with a simple one-dimensional phase-change model. After a sufficiently long run, the supercooled droplet was crystallized into a polycrystalline fcc structure. The crystallization is a stochastic nucleation process. The time and the temperature of inception were evaluated over 42 samples, which indicate the existence of a stability limit.

First demonstration of an all-solid-state optical cryocooler

DOE PAGES

Hehlen, Markus P.; Meng, Junwei; Albrecht, Alexander R.; ...

2018-06-06

Solid-state optical refrigeration uses anti-Stokes fluorescence to cool macroscopic objects to cryogenic temperatures without vibrations. Crystals such as Yb 3+-doped YLiF 4 (YLF:Yb) have previously been laser-cooled to 91 K. In this study, we show for the first time laser cooling of a payload connected to a cooling crystal. A YLF:Yb crystal was placed inside a Herriott cell and pumped with a 1020-nm laser (47 W) to cool a HgCdTe sensor that is part of a working Fourier Transform Infrared (FTIR) spectrometer to 135 K. This first demonstration of an all-solid-state optical cryocooler was enabled by careful control of themore » various desired and undesired heat flows. Fluorescence heating of the payload was minimized by using a single-kink YLF thermal link between the YLF:Yb cooling crystal and the copper coldfinger that held the HgCdTe sensor. The adhesive-free bond between YLF and YLF:Yb showed excellent thermal reliability. This laser-cooled assembly was then supported by silica aerogel cylinders inside a vacuum clamshell to minimize undesired conductive and radiative heat loads from the warm surroundings. Our structure can serve as a baseline for future optical cryocooler devices.« less

First demonstration of an all-solid-state optical cryocooler

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

Hehlen, Markus P.; Meng, Junwei; Albrecht, Alexander R.

Solid-state optical refrigeration uses anti-Stokes fluorescence to cool macroscopic objects to cryogenic temperatures without vibrations. Crystals such as Yb 3+-doped YLiF 4 (YLF:Yb) have previously been laser-cooled to 91 K. In this study, we show for the first time laser cooling of a payload connected to a cooling crystal. A YLF:Yb crystal was placed inside a Herriott cell and pumped with a 1020-nm laser (47 W) to cool a HgCdTe sensor that is part of a working Fourier Transform Infrared (FTIR) spectrometer to 135 K. This first demonstration of an all-solid-state optical cryocooler was enabled by careful control of themore » various desired and undesired heat flows. Fluorescence heating of the payload was minimized by using a single-kink YLF thermal link between the YLF:Yb cooling crystal and the copper coldfinger that held the HgCdTe sensor. The adhesive-free bond between YLF and YLF:Yb showed excellent thermal reliability. This laser-cooled assembly was then supported by silica aerogel cylinders inside a vacuum clamshell to minimize undesired conductive and radiative heat loads from the warm surroundings. Our structure can serve as a baseline for future optical cryocooler devices.« less

Continuous-Flow In-Line Solvent-Swap Crystallization of Vitamin D3

PubMed Central

2017-01-01

A continuous tandem in-line evaporation–crystallization is presented. The process includes an in-line solvent-swap step, suitable to be coupled to a capillary based cooler. As a proof of concept, this setup is tested in a direct in-line acetonitrile mediated crystallization of Vitamin D3. This configuration is suitable to be coupled to a new end-to-end continuous microflow synthesis of Vitamin D3. By this procedure, vitamin particles can be crystallized in continuous flow and isolated using an in-line continuous filtration step. In one run in just 1 min of cooling time, ∼50% (w/w) crystals of Vitamin D3 are directly obtained. Furthermore, the polymorphic form as well as crystals shape and size properties are described in this paper.

A Polymer Visualization System with Accurate Heating and Cooling Control and High-Speed Imaging

PubMed Central

Wong, Anson; Guo, Yanting; Park, Chul B.; Zhou, Nan Q.

2015-01-01

A visualization system to observe crystal and bubble formation in polymers under high temperature and pressure has been developed. Using this system, polymer can be subjected to a programmable thermal treatment to simulate the process in high pressure differential scanning calorimetry (HPDSC). With a high-temperature/high-pressure view-cell unit, this system enables in situ observation of crystal formation in semi-crystalline polymers to complement thermal analyses with HPDSC. The high-speed recording capability of the camera not only allows detailed recording of crystal formation, it also enables in situ capture of plastic foaming processes with a high temporal resolution. To demonstrate the system’s capability, crystal formation and foaming processes of polypropylene/carbon dioxide systems were examined. It was observed that crystals nucleated and grew into spherulites, and they grew at faster rates as temperature decreased. This observation agrees with the crystallinity measurement obtained with the HPDSC. Cell nucleation first occurred at crystals’ boundaries due to CO2 exclusion from crystal growth fronts. Subsequently, cells were nucleated around the existing ones due to tensile stresses generated in the constrained amorphous regions between networks of crystals. PMID:25915031

Experimental and textural constraints on mafic enclave formation in volcanic rocks

USGS Publications Warehouse

Coombs, M.L.; Eichelberger, J.C.; Rutherford, M.J.

2002-01-01

We have used experiments and textural analysis to investigate the process of enclave formation during magma mixing at Southwest Trident volcano, Alaska. Andesite enclaves are present throughout the four dacite lava flows produced by the eruption, and resemble mafic enclaves commonly found in other volcanic rocks. Our experiments replicate the pressure-temperature-time path taken by enclave-forming andesite magma as it is engulfed in dacite during magma mixing. Pressure and temperature information for the andesite and dacite are from [Coombs et al., Contrib. Mineral. Petrol. 140 (2000) 99-118]. The andesite was annealed at 1000??C, and then cooled to 890??C at rates of 110??C h1, 10??C h1 and 2??C h1. Once cooled to 890??C, andesite was held at this lower temperature from times ranging from 1 to 40 h. The andesite that was cooled at the slower rates of 2??C h1 and 10??C h1 most resembles enclave groundmass texturally and compositionally. Based on simple thermal calculations, these rates are more consistent with cooling of the andesite groundmass below an andesite-dacite interface than with cooling of enclave-sized spheres. If enclaves do crystallize as spheres, post-crystallization disaggregation must occur. Calculations using the MELTS algorithm [Ghiorso and Sack, Contrib. Mineral. Petrol. 119 (1995) 197-212] show that for incoming andesite to become less dense than the dacite to become less dense ???34 volume % of its groundmass must crystallize to undergo~18 volume % vesiculation; these values are similar to those determined for Southwest Trident enclaves. Thus such crystallization may lead to 'flotation' of enclaves and be a viable mechanism for enclave formation and dispersal. The residual melt in the cooling experiments did not evolve to rhyolitic compositions such as seen in natural enclaves due to a lack of a decompression step in the experiments. Decompression experiments on Southwest Trident dacite suggest an average ascent rate for the eruption of ???2-3 MPa h1. An andesite experiment that was cooled and then decompressed at this rate contains melt that matches that of the natural enclaves. It is apparent that decompression (ascent)-induced crystallization occurs in enclaves, but not in the form of microlites as happens in the dacite host, due either to insufficient residence time at chamber temperatures or to the pre-existing microphenocrysts which act as sites for new growth. ?? 2002 Elsevier Science B.V. All rights reserved.

Heat load studies of a water-cooled minichannel monochromator for synchrotron x-ray beams

NASA Astrophysics Data System (ADS)

Freund, Andreas K.; Arthur, John R.; Zhang, Lin

1997-12-01

We fabricated a water-cooled silicon monochromator crystal with small channels for the special case of a double-crystal fixed-exit monochromator design where the beam walks across the crystal when the x-ray energy is changed. The two parts of the cooled device were assembled using a new technique based on low melting point solder. The bending of the system produced by this technique could be perfectly compensated by mechanical counter-bending. Heat load tests of the monochromator in a synchrotron beam of 75 W total power, 3 mm high and 15 mm wide, generated by a multipole wiggler at SSRL, showed that the thermal slope error of the crystal is 1 arcsec/40 W power, in full agreement with finite element analysis. The cooling scheme is adequate for bending magnet beamlines at the ESRF and present wiggler beamlines at the SSRL.

Effect of Cooling Rate and Oxygen Fugacity on the Crystallization of the Queen Alexandra Range 94201 Martian Melt Composition

NASA Technical Reports Server (NTRS)

Koizumi, E.; Mikouchi, T.; McKay, G.; Schwandt, C.; Monkawa, A.; Miyamoto, M.

2002-01-01

Although many basaltic shergottites have been recently found in north African deserts, QUE94201 basaltic shergottite (QUE) is still important because of its particular mineralogical and petrological features. This meteorite is thought to represent its parent melt composition [1 -3] and to crystallize under most reduced condition in this group [1,4]. We performed experimental study by using the synthetic glass that has the same composition as the bulk of QUE. After homogenization for 48 hours at 1300 C, isothermal and cooling experiments were done under various conditions (e.g. temperature, cooling rates, and redox states). Our goals are (1) to verify that QUE really represents its parent melt composition, (2) to estimate a cooling rate of this meteorite, (3) to clarify the crystallization sequences of present minerals, and (4) to verity that this meteorite really crystallized under reduced condition.

Analysis of Dependence of the Properties of Alloy V95 on the Pressure Applied to Crystallizing Metal

NASA Astrophysics Data System (ADS)

Korostelev, V. F.; Khromova, L. P.; Denisov, M. S.

2017-05-01

Results of a study aimed at formation of a single-phase fine-grained structure in pistons from aluminum alloy V95 in the process of their fabrication, which involves isostatic pressing of liquid metal before the start of crystallization, application of pressure to the crystallizing metal, and holding under pressure in the process of cooling to the shop temperature, are presented. The ultimate strength and the structure of alloy V95 after casting with imposition of pressure are determined. An example of application of the method suggested for fabricating cast billets ∅ 82 × 70 mm in size with a uniform dense structure without gas shrinkage defects, volume and dendritic segregation is considered.

TEM study on a new Zr-(Fe, Cu) phase in furnace-cooled Zr-1.0Sn-0.3Nb-0.3Fe-0.1Cu alloy

NASA Astrophysics Data System (ADS)

Liu, Yushun; Qiu, Risheng; Luan, Baifeng; Hao, Longlong; Tan, Xinu; Tao, Boran; Zhao, Yifan; Li, Feitao; Liu, Qing

2018-06-01

A new Zr-(Fe, Cu) phase was found in furnace-cooled Zr-1.0Sn-0.3Nb-0.3Fe- 0.1Cu alloy and alloys aged at 580 °C for 10min, 2 h and 10 h. Electron diffraction experiment shows the crystal structure of this phase to be body-centered tetragonal with unit cell dimensions determined to be a = b = 6.49 Å, c = 5.37 Å. Its possible space groups have been discussed and the reason accounting for its formation is believed to be the addition of Cu according to the atom-level images. In addition, no crystal structural or chemical composition changes were observed throughout the aging process.

Crucible-free pulling of germanium crystals

NASA Astrophysics Data System (ADS)

Wünscher, Michael; Lüdge, Anke; Riemann, Helge

2011-03-01

Commonly, germanium crystals are grown after the Czochralski (CZ) method. The crucible-free pedestal and floating zone (FZ) methods, which are widely used for silicon growth, are hardly known to be investigated for germanium. The germanium melt is more than twice as dense as liquid silicon, which could destabilize a floating zone. Additionally, the lower melting point and the related lower radiative heat loss is shown to reduce the stability especially of the FZ process with the consequence of a screw-like crystal growth. We found that the lower heat radiation of Ge can be compensated by the increased convective cooling of a helium atmosphere instead of the argon ambient. Under these conditions, the screw-like growth could be avoided. Unfortunately, the helium cooling deteriorates the melting behavior of the feed rod. Spikes appear along the open melt front, which touch on the induction coil. In order to improve the melting behavior, we used a lamp as a second energy source as well as a mixture of Ar and He. With this, we found a final solution for growing stable crystals from germanium by using both gases in different parts of the furnace. The experimental work is accompanied by the simulation of the stationary temperature field. The commercially available software FEMAG-FZ is used for axisymmetric calculations. Another tool for process development is the lateral photo-voltage scanning (LPS), which can determine the shape of the solid-liquid phase boundary by analyzing the growth striations in a lateral cut of a grown crystal. In addition to improvements of the process, these measurements can be compared with the calculated results and, hence, conduce to validate the calculation.

Microgravity

NASA Image and Video Library

1991-09-01

The Advanced Automated Directional Solidification Furnace (AADSF) flew during the USMP-2 mission. During USMP-2, the AADSF was used to study the growth of mercury cadmium telluride crystals in microgravity by directional solidification, a process commonly used on earth to process metals and grow crystals. The furnace is tubular and has three independently controlled temperature zones. The sample travels from the hot zone of the furnace (1600 degrees F) where the material solidifies as it cools. The solidification region, known as the solid/liquid interface, moves from one end of the sample to the other at a controlled rate, thus the term directional solidification.

Ordered iron aluminide alloys having an improved room-temperature ductility and method thereof

DOEpatents

Sikka, Vinod K.

1992-01-01

A process is disclosed for improving the room temperature ductility and strength of iron aluminide intermetallic alloys. The process involves thermomechanically working an iron aluminide alloy by means which produce an elongated grain structure. The worked alloy is then heated at a temperature in the range of about 650.degree. C. to about 800.degree. C. to produce a B2-type crystal structure. The alloy is rapidly cooled in a moisture free atmosphere to retain the B2-type crystal structure at room temperature, thus providing an alloy having improved room temperature ductility and strength.

Melting behavior and phase relations of lunar samples. [Apollo 12 rock samples

NASA Technical Reports Server (NTRS)

Hays, J. F.

1975-01-01

Cooling rate studies of 12002 were conducted and the results interpreted in terms of the crystallization history of this rock and certain other picritic Apollo 12 samples. Calculations of liquid densities and viscosities during crystallization, crystal settling velocities, and heat loss by the parent rock body are discussed, as are petrographic studies of other Apollo 12 samples. The process of magmatic differentiation that must have accompanied the early melting and chemical fractionation of the moon's outer layers was investigated. The source of regions of both high- and low-titanium mare basalts were also studied.

A Novel Compact Pyroelectric X-Ray and Neutron Source

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

Yaron Danon

2007-08-31

This research was focused on the utilization of pyroelectric crystals for generation of radiation. When in constant temperature pyroelectric crystals are spontaneously polarized. The polarization causes internal charges to accumulate near the crystal faces and masking charges from the environment are attracted to the crystal faces and neutralize the charge. When a pyroelectric crystal is heated or cooled it becomes depolarized and the surface charges become available. If the heating or cooling is done on a crystal in vacuum where no masking charges are available, the crystal becomes a charged capacitor and because of its small capacitance large potential developsmore » across the faces of the crystal.« less

Three-Dimensional Microstructure of Biological Tissues during Freezing and Thawing

NASA Astrophysics Data System (ADS)

Ishiguro, Hiroshi; Horimizu, Takashi; Kataori, Akinobu; Kajigaya, Hiroshi

Three-dimensional behavior of ice crystals and cells during the freezing and thawing of biological tissues was investigated microscopically in real time by using a confocal laser scanning microscope(CLSM) and a fluorescent dye, acridine orange (AO). Fresh tender meat (2nd pectoral muscles) of chicken was stained with the AO in physiological saline to distinguish ice crystals and cells by their different colors, and then frozen and thawed under two different thermal protocols: a) slow-cooling and rapid-warming and b) rapid-cooling and rapid-warming. The CLSM noninvasively produced optical tomograms of the tissues to clarify the pattern of freezing, morphology of ice crystals in the tissues, and the interaction between ice crystals and cells. Also, the tissues were morphologically investigated by pathological means after the freezing and thawing. Typical freezing pattern during the slow-cooling was extracellular-freezing, and those during the rapid-cooling were extracellular-freezing and intracellular freezing with a lot of fine ice crystals in the cells. Cracks caused by the extracellular and intracellular ice crystals remained in the muscle tissues after the thawing. The results obtained by using the CLSM/dye method were consistent with pathologically morphological changes in the tissues through freezing and thawing.

Cooling and crystallization of lava in open channels, and the transition of Pāhoehoe Lava to 'A'ā

NASA Astrophysics Data System (ADS)

Cashman, Katharine V.; Thornber, Carl; Kauahikaua, James P.

Samples collected from a lava channel active at Kīlauea Volcano during May 1997 are used to constrain rates of lava cooling and crystallization during early stages of flow. Lava erupted at near-liquidus temperatures ( 1150 °C) cooled and crystallized rapidly in upper parts of the channel. Glass geothermometry indicates cooling by 12-14 °C over the first 2km of transport. At flow velocities of 1-2m/s, this translates to cooling rates of 22-50 °C/h. Cooling rates this high can be explained by radiative cooling of a well-stirred flow, consistent with observations of non-steady flow in proximal regions of the channel. Crystallization of plagioclase and pyroxene microlites occurred in response to cooling, with crystallization rates of 20-50% per hour. Crystallization proceeded primarily by nucleation of new crystals, and nucleation rates of 104/cm3s are similar to those measured in the 1984 open channel flow from Mauna Loa Volcano. There is no evidence for the large nucleation delays commonly assumed for plagioclase crystallization in basaltic melts, possibly a reflection of enhanced nucleation due to stirring of the flow. The transition of the flow surface morphology from pāhoehoe to 'a'ā occurred at a distance of 1.9km from the vent. At this point, the flow was thermally stratified, with an interior temperature of 1137 °C and crystallinity of 15%, and a flow surface temperature of 1100 °C and crystallinity of 45%. 'A'ā formation initiated along channel margins, where crust was continuously disrupted, and involved tearing and clotting of the flow surface. Both observations suggest that the transition involved crossing of a rheological threshold. We suggest this threshold to be the development of a lava yield strength sufficient to prevent viscous flow of lava at the channel margin. We use this concept to propose that 'a'ā formation in open channels requires both sufficiently high strain rates for continued disruption of surface crusts and sufficient groundmass crystallinity to generate a yield strength equivalent to the imposed stress. In Hawai'i, where lava is typically microlite poor on eruption, these combined requirements help to explain two common observations on 'a'ā formation: (a) 'a'ā flow fields are generated when effusion rates are high (thus promoting crustal disruption); and (b) under most eruption conditions, lava issues from the vent as pāhoehoe and changes to 'a'ā only after flowing some distance, thus permitting sufficient crystallization.

Magnetism out of antisite disorder in the J =0 compound Ba2YIrO6

NASA Astrophysics Data System (ADS)

Chen, Q.; Svoboda, C.; Zheng, Q.; Sales, B. C.; Mandrus, D. G.; Zhou, H. D.; Zhou, J.-S.; McComb, D.; Randeria, M.; Trivedi, N.; Yan, J.-Q.

2017-10-01

We systematically investigate the magnetic properties and local structure of Ba2YIrO6 to demonstrate that Y and Ir lattice defects in the form of antiphase boundary or clusters of antisite disorder affect the magnetism observed in this 5 d4 compound. The experimental investigation involved comparison of the magnetic properties and atomic imaging of (1) a slow-cooled crystal, (2) a crystal quenched from 900°C after growth, and (3) a crystal grown using a faster cooling rate during growth than the slow-cooled one. Atomic-scale imaging by scanning transmission electron microscopy (STEM) shows that quenching from 900°C introduces Ir-rich antiphase boundaries in the crystals, and a faster cooling rate during crystal growth leads to clusters of Y and Ir antisite disorder. Compared to the slow-cooled crystals, Ba2YIrO6 crystals with clusters of antisite defects have a larger effective moment and a larger saturation moment, while quenched crystals with Ir-rich antiphase boundary show a slightly suppressed moment. Our DFT and model magnetic Hamiltonian calculations suggest magnetic condensation is unlikely, as the energy to be gained from superexchange is small compared to the spin-orbit gap. However, once Y is replaced by Ir in the antisite disordered region, the picture of local nonmagnetic singlets breaks down and magnetism can be induced. This is because of (a) enhanced interactions due to increased orbital overlap and (b) increased number of orbitals mediating the interactions. Our work highlights the importance of lattice defects in understanding the experimentally observed magnetism in Ba2YIrO6 and other J =0 systems.

Magnetism out of antisite disorder in the J = 0 compound Ba 2 YIrO 6

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

Chen, Qiang; Svoboda, Chris; Zheng, Qiang

Here, we systematically investigate the magnetic properties and local structure of Ba 2YIrO 6 to demonstrate that Y and Ir lattice defects in the form of antiphase boundary or clusters of antisite disorder affect the magnetism observed in this 5d 4 compound. The experimental investigation involved comparison of the magnetic properties and atomic imaging of (1) a slow-cooled crystal, (2) a crystal quenched from 900°C after growth, and (3) a crystal grown using a faster cooling rate during growth than the slow-cooled one. Atomic-scale imaging by scanning transmission electron microscopy (STEM) shows that quenching from 900°C introduces Ir-rich antiphase boundariesmore » in the crystals, and a faster cooling rate during crystal growth leads to clusters of Y and Ir antisite disorder. Compared to the slow-cooled crystals, Ba 2YIrO 6 crystals with clusters of antisite defects have a larger effective moment and a larger saturation moment, while quenched crystals with Ir-rich antiphase boundary show a slightly suppressed moment. Our DFT and model magnetic Hamiltonian calculations suggest magnetic condensation is unlikely, as the energy to be gained from superexchange is small compared to the spin-orbit gap. However, once Y is replaced by Ir in the antisite disordered region, the picture of local nonmagnetic singlets breaks down and magnetism can be induced. This is because of (a) enhanced interactions due to increased orbital overlap and (b) increased number of orbitals mediating the interactions. Our work highlights the importance of lattice defects in understanding the experimentally observed magnetism in Ba 2YIrO 6 and other J = 0 systems.« less

Magnetism out of antisite disorder in the J = 0 compound Ba 2 YIrO 6

DOE PAGES

Chen, Qiang; Svoboda, Chris; Zheng, Qiang; ...

2017-10-18

Here, we systematically investigate the magnetic properties and local structure of Ba 2YIrO 6 to demonstrate that Y and Ir lattice defects in the form of antiphase boundary or clusters of antisite disorder affect the magnetism observed in this 5d 4 compound. The experimental investigation involved comparison of the magnetic properties and atomic imaging of (1) a slow-cooled crystal, (2) a crystal quenched from 900°C after growth, and (3) a crystal grown using a faster cooling rate during growth than the slow-cooled one. Atomic-scale imaging by scanning transmission electron microscopy (STEM) shows that quenching from 900°C introduces Ir-rich antiphase boundariesmore » in the crystals, and a faster cooling rate during crystal growth leads to clusters of Y and Ir antisite disorder. Compared to the slow-cooled crystals, Ba 2YIrO 6 crystals with clusters of antisite defects have a larger effective moment and a larger saturation moment, while quenched crystals with Ir-rich antiphase boundary show a slightly suppressed moment. Our DFT and model magnetic Hamiltonian calculations suggest magnetic condensation is unlikely, as the energy to be gained from superexchange is small compared to the spin-orbit gap. However, once Y is replaced by Ir in the antisite disordered region, the picture of local nonmagnetic singlets breaks down and magnetism can be induced. This is because of (a) enhanced interactions due to increased orbital overlap and (b) increased number of orbitals mediating the interactions. Our work highlights the importance of lattice defects in understanding the experimentally observed magnetism in Ba 2YIrO 6 and other J = 0 systems.« less

Pd-Ag chronometry of IVA iron meteorites and the crystallization and cooling of a protoplanetary core

DOE PAGES

Matthes, M.; Fischer-Godde, M.; Kruijer, T. S.; ...

2017-09-07

To constrain the timescales and processes involved in the crystallization and cooling of protoplanetary cores, we examined the Pd-Ag isotope systematics of the IVA iron meteorites Muonionalusta and Gibeon. A Pd-Ag isochron for Muonionalusta provides an initial 107Pd/ 108Pd = (2.57 ± 0.07) × 10 -5. The three metal samples analyzed from Gibeon plot below the Muonionalusta isochron, but these samples also show significant effects of cosmic ray-induced neutron capture reactions, as is evident from 196Pt excesses in the Gibeon samples. After correction for neutron capture effects on Ag isotopes, the Gibeon samples plot on the Muonionalusta isochron, indicating thatmore » these two IVA irons have indistinguishable initial 107Pd/ 108Pd. Collectively, the Pd-Ag data indicate cooling of the IVA core below Pd-Ag closure between 2.9 ± 0.4 Ma and 8.9 ± 0.6 Ma after CAI formation, where this age range reflects uncertainties in the initial 107Pd/ 108Pd ratios of the solar system, which in turn result from uncertainties in the Pb-Pb age of Muonionalusta. The Ag isotopic data indicate that the IVA core initially evolved with a modestly elevated Pd/Ag, but the low Ag concentrations measured for some metal samples indicate derivation from a source with much lower Ag contents and, hence, higher Pd/Ag. These contrasting observations can be reconciled if the IVA irons crystallized from an initially more Ag-rich core, followed by extraction of Fe-S melts during compaction of the nearly solidified core. Owing to its strong tendency to partition into Fe-S melts, Ag was removed from the IVA core during compaction, leading to the very low Ag concentration observed in metal samples of IVA irons. Alternatively, Ag was lost by evaporation from a still molten metallic body just prior to the onset of crystallization. The Pd-Ag isotopic data indicate that Muonionalusta cooled at >500 K/Ma through the Pd-Ag closure temperature of ~900 K, consistent with the rapid cooling inferred from metallographic cooling rates for IVA irons. Finally, combined, these observations are consistent with cooling of IVA irons in a metallic body with little or no silicate mantle.« less

Pd-Ag chronometry of IVA iron meteorites and the crystallization and cooling of a protoplanetary core

NASA Astrophysics Data System (ADS)

Matthes, M.; Fischer-Gödde, M.; Kruijer, T. S.; Kleine, T.

2018-01-01

To constrain the timescales and processes involved in the crystallization and cooling of protoplanetary cores, we examined the Pd-Ag isotope systematics of the IVA iron meteorites Muonionalusta and Gibeon. A Pd-Ag isochron for Muonionalusta provides an initial 107Pd/108Pd = (2.57 ± 0.07) × 10-5. The three metal samples analyzed from Gibeon plot below the Muonionalusta isochron, but these samples also show significant effects of cosmic ray-induced neutron capture reactions, as is evident from 196Pt excesses in the Gibeon samples. After correction for neutron capture effects on Ag isotopes, the Gibeon samples plot on the Muonionalusta isochron, indicating that these two IVA irons have indistinguishable initial 107Pd/108Pd. Collectively, the Pd-Ag data indicate cooling of the IVA core below Pd-Ag closure between 2.9 ± 0.4 Ma and 8.9 ± 0.6 Ma after CAI formation, where this age range reflects uncertainties in the initial 107Pd/108Pd ratios of the solar system, which in turn result from uncertainties in the Pb-Pb age of Muonionalusta. The Ag isotopic data indicate that the IVA core initially evolved with a modestly elevated Pd/Ag, but the low Ag concentrations measured for some metal samples indicate derivation from a source with much lower Ag contents and, hence, higher Pd/Ag. These contrasting observations can be reconciled if the IVA irons crystallized from an initially more Ag-rich core, followed by extraction of Fe-S melts during compaction of the nearly solidified core. Owing to its strong tendency to partition into Fe-S melts, Ag was removed from the IVA core during compaction, leading to the very low Ag concentration observed in metal samples of IVA irons. Alternatively, Ag was lost by evaporation from a still molten metallic body just prior to the onset of crystallization. The Pd-Ag isotopic data indicate that Muonionalusta cooled at >500 K/Ma through the Pd-Ag closure temperature of ∼900 K, consistent with the rapid cooling inferred from metallographic cooling rates for IVA irons. Combined, these observations are consistent with cooling of IVA irons in a metallic body with little or no silicate mantle.

Pd-Ag chronometry of IVA iron meteorites and the crystallization and cooling of a protoplanetary core

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

Matthes, M.; Fischer-Godde, M.; Kruijer, T. S.

To constrain the timescales and processes involved in the crystallization and cooling of protoplanetary cores, we examined the Pd-Ag isotope systematics of the IVA iron meteorites Muonionalusta and Gibeon. A Pd-Ag isochron for Muonionalusta provides an initial 107Pd/ 108Pd = (2.57 ± 0.07) × 10 -5. The three metal samples analyzed from Gibeon plot below the Muonionalusta isochron, but these samples also show significant effects of cosmic ray-induced neutron capture reactions, as is evident from 196Pt excesses in the Gibeon samples. After correction for neutron capture effects on Ag isotopes, the Gibeon samples plot on the Muonionalusta isochron, indicating thatmore » these two IVA irons have indistinguishable initial 107Pd/ 108Pd. Collectively, the Pd-Ag data indicate cooling of the IVA core below Pd-Ag closure between 2.9 ± 0.4 Ma and 8.9 ± 0.6 Ma after CAI formation, where this age range reflects uncertainties in the initial 107Pd/ 108Pd ratios of the solar system, which in turn result from uncertainties in the Pb-Pb age of Muonionalusta. The Ag isotopic data indicate that the IVA core initially evolved with a modestly elevated Pd/Ag, but the low Ag concentrations measured for some metal samples indicate derivation from a source with much lower Ag contents and, hence, higher Pd/Ag. These contrasting observations can be reconciled if the IVA irons crystallized from an initially more Ag-rich core, followed by extraction of Fe-S melts during compaction of the nearly solidified core. Owing to its strong tendency to partition into Fe-S melts, Ag was removed from the IVA core during compaction, leading to the very low Ag concentration observed in metal samples of IVA irons. Alternatively, Ag was lost by evaporation from a still molten metallic body just prior to the onset of crystallization. The Pd-Ag isotopic data indicate that Muonionalusta cooled at >500 K/Ma through the Pd-Ag closure temperature of ~900 K, consistent with the rapid cooling inferred from metallographic cooling rates for IVA irons. Finally, combined, these observations are consistent with cooling of IVA irons in a metallic body with little or no silicate mantle.« less

Use of thulium-sensitized rare earth-doped low phonon energy crystalline hosts for IR sources.

PubMed

Ganem, Joseph; Bowman, Steven R

2013-11-01

Crystalline hosts with low phonon energies enable novel energy transfer processes when doped with rare earth ions. Two applications of energy transfer for rare earth ions in thulium-sensitized low phonon energy crystals that result in infrared luminescence are discussed. One application is an endothermic, phonon-assisted cross-relaxation process in thulium-doped yttrium chloride that converts lattice phonons to infrared emission, which raises the possibility of a fundamentally new method for achieving solid-state optical cooling. The other application is an optically pumped mid-IR phosphor using thulium-praseodymium-doped potassium lead chloride that converts 805-nm diode light to broadband emission from 4,000 to 5,500 nm. These two applications in chloride crystals are discussed in terms of critical radii calculated from Forster-Dexter energy transfer theory. It is found that the critical radii for electric dipole-dipole interactions in low phonon energy chloride crystals are comparable to those in conventional oxide and fluoride crystals. It is the reduction in multi-phonon relaxation rates in chloride crystals that enable these additional energy transfer processes and infrared luminescence.

Use of thulium-sensitized rare earth-doped low phonon energy crystalline hosts for IR sources

NASA Astrophysics Data System (ADS)

Ganem, Joseph; Bowman, Steven R.

2013-11-01

Crystalline hosts with low phonon energies enable novel energy transfer processes when doped with rare earth ions. Two applications of energy transfer for rare earth ions in thulium-sensitized low phonon energy crystals that result in infrared luminescence are discussed. One application is an endothermic, phonon-assisted cross-relaxation process in thulium-doped yttrium chloride that converts lattice phonons to infrared emission, which raises the possibility of a fundamentally new method for achieving solid-state optical cooling. The other application is an optically pumped mid-IR phosphor using thulium-praseodymium-doped potassium lead chloride that converts 805-nm diode light to broadband emission from 4,000 to 5,500 nm. These two applications in chloride crystals are discussed in terms of critical radii calculated from Forster-Dexter energy transfer theory. It is found that the critical radii for electric dipole-dipole interactions in low phonon energy chloride crystals are comparable to those in conventional oxide and fluoride crystals. It is the reduction in multi-phonon relaxation rates in chloride crystals that enable these additional energy transfer processes and infrared luminescence.

Use of thulium-sensitized rare earth-doped low phonon energy crystalline hosts for IR sources

PubMed Central

2013-01-01

Crystalline hosts with low phonon energies enable novel energy transfer processes when doped with rare earth ions. Two applications of energy transfer for rare earth ions in thulium-sensitized low phonon energy crystals that result in infrared luminescence are discussed. One application is an endothermic, phonon-assisted cross-relaxation process in thulium-doped yttrium chloride that converts lattice phonons to infrared emission, which raises the possibility of a fundamentally new method for achieving solid-state optical cooling. The other application is an optically pumped mid-IR phosphor using thulium-praseodymium-doped potassium lead chloride that converts 805-nm diode light to broadband emission from 4,000 to 5,500 nm. These two applications in chloride crystals are discussed in terms of critical radii calculated from Forster-Dexter energy transfer theory. It is found that the critical radii for electric dipole-dipole interactions in low phonon energy chloride crystals are comparable to those in conventional oxide and fluoride crystals. It is the reduction in multi-phonon relaxation rates in chloride crystals that enable these additional energy transfer processes and infrared luminescence. PMID:24180684

Thin-Film Evaporative Cooling for Side-Pumped Laser

NASA Technical Reports Server (NTRS)

Stewart, Brian K. (Inventor)

2010-01-01

A system and method are provided for cooling a crystal rod of a side-pumped laser. A transparent housing receives the crystal rod therethrough so that an annular gap is defined between the housing and the radial surface of the crystal rod. A fluid coolant is injected into the annular gap such the annular gap is partially filled with the fluid coolant while the radial surface of the crystal rod is wetted as a thin film all along the axial length thereof.

Practical macromolecular cryocrystallography

PubMed Central

Pflugrath, J. W.

2015-01-01

Cryocrystallography is an indispensable technique that is routinely used for single-crystal X-ray diffraction data collection at temperatures near 100 K, where radiation damage is mitigated. Modern procedures and tools to cryoprotect and rapidly cool macromolecular crystals with a significant solvent fraction to below the glass-transition phase of water are reviewed. Reagents and methods to help prevent the stresses that damage crystals when flash-cooling are described. A method of using isopentane to assess whether cryogenic temperatures have been preserved when dismounting screened crystals is also presented. PMID:26057787

Reversible thermosalience of 4-aminobenzonitrile.

PubMed

Alimi, Lukman O; van Heerden, Dewald P; Lama, Prem; Smith, Vincent J; Barbour, Leonard J

2018-05-31

Crystals of 4-aminobenzonitrile grown by sublimation undergo reversible thermosalient phase changes during cooling and subsequent heating. Single-crystal diffraction studies have been carried out at 20 K intervals during cooling from 300 to 100 K in order to explain the structural change that occurs.

Film-Cooling Heat-Transfer Measurements Using Liquid Crystals

NASA Technical Reports Server (NTRS)

Hippensteele, Steven A.

1997-01-01

The following topics are discussed: (1) The Transient Liquid-Crystal Heat-Transfer Technique; (2) 2-D Film-Cooling Heat-Transfer on an AlliedSignal Vane; and (3) Effects of Tab Vortex Generators on Surface Heat Transfer. Downstream of a Jet in Crossflow.

Monitoring of antisolvent crystallization of sodium scutellarein by combined FBRM-PVM-NIR.

PubMed

Liu, Xuesong; Sun, Di; Wang, Feng; Wu, Yongjiang; Chen, Yong; Wang, Longhu

2011-06-01

Antisolvent crystallization can be used as an alternative to cooling or evaporation for the separation and purification of solid product in the pharmaceutical industry. To improve the process understanding of antisolvent crystallization, the use of in-line tools is vital. In this study, the process analytical technology (PAT) tools including focused beam reflectance measurement (FBRM), particle video microscope (PVM), and near-infrared spectroscopy (NIRS) were utilized to monitor antisolvent crystallization of sodium scutellarein. FBRM was used to monitor chord count and chord length distribution of sodium scutellarein particles in the crystallizer, and PVM, as an in-line video camera, provided pictures imaging particle shape and dimension. In addition, a quantitative model of PLS was established by in-line NIRS to detect the concentration of sodium scutellarein in the solvent and good calibration statistics were obtained (r(2) = 0.976) with the residual predictive deviation value of 11.3. The discussion over sensitivities, strengths, and weaknesses of the PAT tools may be helpful in selection of suitable PAT techniques. These in-line techniques eliminate the need for sample preparation and offer a time-saving approach to understand and monitor antisolvent crystallization process. Copyright © 2011 Wiley-Liss, Inc.

Studies of the Crystallization Process of Aluminum-Silicon Alloys Using a High Temperature Microscope. Thesis

NASA Technical Reports Server (NTRS)

Justi, S.

1985-01-01

It is shown that primary silicon crystals grow polyhedral in super-eutectic AlSi melts and that phosphorus additives to the melt confirm the strong seeding capacity. Primary silicon exhibits strong dendritic seeding effects in eutectic silicon phases of various silicon alloys, whereas primary aluminum does not possess this capacity. Sodium addition also produces a dendritic silicon network growth in the interior of the sample that is attributed to the slower silicon diffusion velocity during cooling.

Focused beam reflectance measurement as a tool for in situ monitoring of the lactose crystallization process.

PubMed

Pandalaneni, K; Amamcharla, J K

2016-07-01

Lactose accounts for about 75 and 85% of the solids in whey and deproteinized whey, respectively. Production of lactose is usually carried out by a process called crystallization. Several factors including rate of cooling, presence of impurities, and mixing speed influence the crystal size characteristics. To optimize the lactose crystallization process parameters to maximize the lactose yield, it is important to monitor the crystallization process. However, efficient in situ tools to implement at concentrations relevant to the dairy industry are lacking. The objective of the present work was to use a focused beam reflectance measurement (FBRM) system for in situ monitoring of lactose crystallization at supersaturated concentrations (wt/wt) 50, 55, and 60% at 20 and 30°C. The FBRM data were compared with Brix readings collected using a refractometer during isothermal crystallization. Chord length distributions obtained from FBRM in the ranges of <50 µm (fine crystals) and 50 to 300 µm (coarse crystals) were recorded and evaluated in relation to the extent of crystallization and rate constants deduced from the refractometer measurements. Extent of crystallization and rate constants increased with increasing supersaturation concentration and temperature. The measured fine crystal counts from FBRM increased at higher supersaturated concentration and temperature during isothermal crystallization. On the other hand, coarse counts were observed to increase with decreasing supersaturated concentration and temperature. Square weighted chord length distribution obtained from FBRM showed that as concentration increased, a decrease in chord lengths occurred at 20°C and similar observations were made from microscopic images. The robustness of FBRM in understanding isothermal lactose crystallization at various concentrations and temperatures was successfully assessed in the study. Copyright © 2016 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

Thermal and convection analyses of the dendrite remelting rocket experiment; Experiment 74-21 in the space processing rocket program

NASA Technical Reports Server (NTRS)

Grodzka, P. G.; Pond, J. E.; Spradley, J. W.; Johnson, M. H.

1976-01-01

The Dendrite Remelting Rocket Experiment was performed aboard a Black Brant VC Sounding Rocket during a period which gravity levels of approximately 0.00001 g prevailed. The experiment consisted of cooling an aqueous ammonium chloride solution in a manner such that crystallization of ammonium chloride crystals proceeded throughout a three minute period of zero-g. The crystallization process during flight was recorded on 35 mm panatomic-x film. A number of ground crystallizations were similarly recorded for comparison purposes. The convective and thermal conditions in aqueous and metallic liquid systems were assessed under conditions of the flight experiment to help establish the relevance of the rocket experiment to metals casting phenomena. The results indicate that aqueous or metallic convective velocities in the Dendrite Remelting Rocket Experiment cell are of insignificant magnitudes at the 0.0001 to 0.00001 g levels of the experiment. The crystallization phenomena observed in the Rocket Experiment, therefore, may be indicative of how metals will solidify in low-g.

A stress-induced phase transition model for semi-crystallize shape memory polymer

NASA Astrophysics Data System (ADS)

Guo, Xiaogang; Zhou, Bo; Liu, Liwu; Liu, Yanju; Leng, Jinsong

2014-03-01

The developments of constitutive models for shape memory polymer (SMP) have been motivated by its increasing applications. During cooling or heating process, the phase transition which is a continuous time-dependent process happens in semi-crystallize SMP and the various individual phases form at different temperature and in different configuration. Then, the transformation between these phases occurred and shape memory effect will emerge. In addition, stress applied on SMP is an important factor for crystal melting during phase transition. In this theory, an ideal phase transition model considering stress or pre-strain is the key to describe the behaviors of shape memory effect. So a normal distributed model was established in this research to characterize the volume fraction of each phase in SMP during phase transition. Generally, the experiment results are partly backward (in heating process) or forward (in cooling process) compared with the ideal situation considering delay effect during phase transition. So, a correction on the normal distributed model is needed. Furthermore, a nonlinear relationship between stress and phase transition temperature Tg is also taken into account for establishing an accurately normal distributed phase transition model. Finally, the constitutive model which taking the stress as an influence factor on phase transition was also established. Compared with the other expressions, this new-type model possesses less parameter and is more accurate. For the sake of verifying the rationality and accuracy of new phase transition and constitutive model, the comparisons between the simulated and experimental results were carried out.

An unusual type of polymorphism in a liquid crystal

DOE PAGES

Li, Lin; Salamonczyk, Miroslaw; Shadpour, Sasan; ...

2018-02-19

Polymorphism is a remarkable concept in chemistry, materials science, computer science, and biology. Whether it is the ability of a material to exist in two or more crystal structures, a single interface connecting to two different entities, or alternative phenotypes of an organism, polymorphism determines function and properties. In materials science, polymorphism can be found in an impressively wide range of materials, including crystalline materials, minerals, metals, alloys, and polymers. Here in this paper we report on polymorphism in a liquid crystal. A bent-core liquid crystal with a single chiral side chain forms two structurally and morphologically significantly different liquidmore » crystal phases solely depending on the cooling rate from the isotropic liquid state. On slow cooling, the thermodynamically more stable oblique columnar phase forms, and on rapid cooling, a not heretofore reported helical microfilament phase. Since structure determines function and properties, the structural color for these phases also differs.« less

An unusual type of polymorphism in a liquid crystal

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

Li, Lin; Salamonczyk, Miroslaw; Shadpour, Sasan

Polymorphism is a remarkable concept in chemistry, materials science, computer science, and biology. Whether it is the ability of a material to exist in two or more crystal structures, a single interface connecting to two different entities, or alternative phenotypes of an organism, polymorphism determines function and properties. In materials science, polymorphism can be found in an impressively wide range of materials, including crystalline materials, minerals, metals, alloys, and polymers. Here in this paper we report on polymorphism in a liquid crystal. A bent-core liquid crystal with a single chiral side chain forms two structurally and morphologically significantly different liquidmore » crystal phases solely depending on the cooling rate from the isotropic liquid state. On slow cooling, the thermodynamically more stable oblique columnar phase forms, and on rapid cooling, a not heretofore reported helical microfilament phase. Since structure determines function and properties, the structural color for these phases also differs.« less

Ultrasonically controlled particle size distribution of explosives: a safe method.

PubMed

Patil, Mohan Narayan; Gore, G M; Pandit, Aniruddha B

2008-03-01

Size reduction of the high energy materials (HEM's) by conventional methods (mechanical means) is not safe as they are very sensitive to friction and impact. Modified crystallization techniques can be used for the same purpose. The solute is dissolved in the solvent and crystallized via cooling or is precipitated out using an antisolvent. The various crystallization parameters such as temperature, antisolvent addition rate and agitation are adjusted to get the required final crystal size and morphology. The solvent-antisolvent ratio, time of crystallization and yield of the product are the key factors for controlling antisolvent based precipitation process. The advantages of cavitationally induced nucleation can be coupled with the conventional crystallization process. This study includes the effect of the ultrasonically generated acoustic cavitation phenomenon on the solvent antisolvent based precipitation process. CL20, a high-energy explosive compound, is a polyazapolycyclic caged polynitramine. CL-20 has greater energy output than existing (in-use) energetic ingredients while having an acceptable level of insensitivity to shock and other external stimuli. The size control and size distribution manipulation of the high energy material (CL20) has been successfully carried out safely and quickly along with an increase in the final mass yield, compared to the conventional antisolvent based precipitation process.

Temperature distribution of laser crystal in end-pumped DPSSL

NASA Astrophysics Data System (ADS)

Zheng, Yibo; Jia, Liping; Zhang, Lei; Wen, Jihua; Kang, Junjian

2009-11-01

The temperature distribution in different cooling system was studied. A thermal distribution model of laser crystal was established. Based on the calculation, the temperature distribution and deformation of ND:YVO4 crystal in different cooling system were obtained. When the pumping power is 2 W and the radius of pumping beams is 320μm, the temperature distribution and end face distortion of the laser crystal are lowest by using side directly hydrocooling method. The study shows that, the side directly hydrocooling method is a more efficient method to control the crystal temperature distribution and reduce the thermal effect.

Investigations into the low temperature behavior of jet fuels: Visualization, modeling, and viscosity studies

NASA Astrophysics Data System (ADS)

Atkins, Daniel L.

Aircraft operation in arctic regions or at high altitudes exposes jet fuel to temperatures below freeze point temperature specifications. Fuel constituents may solidify and remain within tanks or block fuel system components. Military and scientific requirements have been met with costly, low freeze point specialty jet fuels. Commercial airline interest in polar routes and the use of high altitude unmanned aerial vehicles (UAVs) has spurred interest in the effects of low temperatures and low-temperature additives on jet fuel. The solidification of jet fuel due to freezing is not well understood and limited visualization of fuel freezing existed prior to the research presented in this dissertation. Consequently, computational fluid dynamics (CFD) modeling that simulates jet fuel freezing and model validation were incomplete prior to the present work. The ability to simulate jet fuel freezing is a necessary tool for fuel system designers. An additional impediment to the understanding and simulation of jet fuel freezing has been the absence of published low-temperature thermo-physical properties, including viscosity, which the present work addresses. The dissertation is subdivided into three major segments covering visualization, modeling and validation, and viscosity studies. In the first segment samples of jet fuel, JPTS, kerosene, Jet A and Jet A containing additives, were cooled below their freeze point temperatures in a rectangular, optical cell. Images and temperature data recorded during the solidification process provided information on crystal habit, crystallization behavior, and the influence of the buoyancy-driven flow on freezing. N-alkane composition of the samples was determined. The Jet A sample contained the least n-alkane mass. The cooling of JPTS resulted in the least wax formation while the cooling of kerosene yielded the greatest wax formation. The JPTS and kerosene samples exhibited similar crystallization behavior and crystal habits during cooling. Low-temperature additives modified the crystal habit of the Jet A fuel. Crystal shapes and sizes were recorded for use in future computational modeling. In the second segment, a computational fluid dynamics model was developed that simulates the solidification of jet fuel due to freezing in a buoyancy-driven flow. Flow resistance caused by porous crystal structures that exist in liquid-solid regions is simulated through the use of a momentum resistance source term. (Abstract shortened by UMI.)

Numerical simulation of flow and melting characteristics of seawater-ice crystals two-phase flow in inlet straight pipe of shell and tube heat exchanger of polar ship

NASA Astrophysics Data System (ADS)

Xu, Li; Huang, Chang-Xu; Huang, Zhen-Fei; Sun, Qiang; Li, Jie

2018-05-01

The ice crystal particles are easy to enter into the seawater cooling system of polar ship together with seawater when it sails in the Arctic. They are easy to accumulate in the pipeline, causing serious blockage of the cooling pipe. In this study, the flow and melting characteristics of ice particles-seawater two-phase flow in inlet straight pipe of shell-and-tube heat exchanger were numerically simulated by using Eulerian-Eulerian two-fluid model coupled with the interphase heat and mass transfer model. The influences of inlet ice packing factor, ice crystal particle diameter, and inlet velocity on the distribution and melting characteristics of ice crystals were investigated. The degree of asymmetry of the distribution of ice crystals in the cross section decreases gradually when the IPF changes from 5 to 15%. The volume fractions of ice crystals near the top of the outlet cross section are 19.59, 19.51, and 22.24% respectively for ice packing factor of 5, 10 and 15%. When the particle diameter is 0.5 mm, the ice crystals are gradually stratified during the flow process. With particle diameters of 1.0 and 2.0 mm, the region with the highest volume fraction of ice crystals is a small circle and the contours in the cloud map are compact. The greater the inlet flow velocity, the less stratified the ice crystals and the more obvious the turbulence on the outlet cross section. The average volume fraction of ice crystals along the flow direction is firstly rapidly reduced and then stabilized after 300 mm.

Synthesis of renewable diesel through hydrodeoxygenation reaction from nyamplung oil (Calophyllum Inophyllum oil) using NiMo/Z and NiMo/C catalysts with rapid heating and cooling method

NASA Astrophysics Data System (ADS)

Susanto, B. H.; Prakasa, M. B.; Shahab, M. H.

2016-11-01

The synthesis of metal nanocrystal was conducted by modification preparation from simple heating method which heating and cooling process run rapidly. The result of NiMo/Z 575 °C characterizations are 33.73 m2/gram surface area and 31.80 nm crystal size. By used NiMo/C 700 °C catalyst for 30 minutes which had surface area of 263.21 m2/gram, had 31.77 nm crystal size, and good morphology, obtained catalyst with high activity, selectivity, and stability. After catalyst activated, synthesis of renewable diesel performed in hydrogenation reactor at 375 °C, 12 bar, and 800 rpm. The result of conversion was 81.99%, yield was 68.08%, and selectivity was 84.54%.

Atomic and electronic structure transformations of silver nanoparticles under rapid cooling conditions.

PubMed

Lobato, I; Rojas, J; Landauro, C V; Torres, J

2009-02-04

The structural evolution and dynamics of silver nanodrops Ag(2869) (4.4 nm in diameter) under rapid cooling conditions have been studied by means of molecular dynamics simulations and electronic density of state calculations. The interaction of silver atoms is modelled by a tight-binding semiempirical interatomic potential proposed by Cleri and Rosato. The pair correlation functions and the pair analysis technique are used to reveal the structural transition in the process of solidification. It is shown that Ag nanoparticles evolve into different nanostructures under different cooling processes. At a cooling rate of 1.5625 × 10(13) K s(-1) the nanoparticles preserve an amorphous-like structure containing a large amount of 1551 and 1541 pairs which correspond to icosahedral symmetry. For a lower cooling rate (1.5625 × 10(12) K s(-1)), the nanoparticles transform into a crystal-like structure consisting mainly of 1421 and 1422 pairs which correspond to the face centred cubic and hexagonal close packed structures, respectively. The variations of the electronic density of states for the differently cooled nanoparticles are small, but in correspondence with the structural changes.

A white dwarf cooling age of 8 Gyr for NGC 6791 from physical separation processes.

PubMed

García-Berro, Enrique; Torres, Santiago; Althaus, Leandro G; Renedo, Isabel; Lorén-Aguilar, Pablo; Córsico, Alejandro H; Rohrmann, René D; Salaris, Maurizio; Isern, Jordi

2010-05-13

NGC 6791 is a well studied open cluster that it is so close to us that can be imaged down to very faint luminosities. The main-sequence turn-off age ( approximately 8 Gyr) and the age derived from the termination of the white dwarf cooling sequence ( approximately 6 Gyr) are very different. One possible explanation is that as white dwarfs cool, one of the ashes of helium burning, (22)Ne, sinks in the deep interior of these stars. At lower temperatures, white dwarfs are expected to crystallize and phase separation of the main constituents of the core of a typical white dwarf ((12)C and (16)O) is expected to occur. This sequence of events is expected to introduce long delays in the cooling times, but has not hitherto been proven. Here we report that, as theoretically anticipated, physical separation processes occur in the cores of white dwarfs, resolving the age discrepancy for NGC 6791.

Zaoyang chondrite cooling history from pyroxene Fe(2+)-Mg intracrystalline ordering and exolutions

NASA Technical Reports Server (NTRS)

Molin, G. M.; Tribaudino, M.; Brizi, E.

1993-01-01

The Zaoyang ordinary chondrite fell as a single 14.15-kg mass in Hubey province (China) in October 1984 and was classified as a non-brecciated H5 chondrite, shock facies b. Cooling rate in pyroxenes can be calculated down to about 1000 C by using fine textures and at still lower temperatures (700 to 200 C) by intracrystalline ordering processes. The crystal chemistry of clinopyroxene and orthopyroxene from the matrix of the H5 Zaoyang chondrite has been investigated by X-ray structure refinement and detailed microprobe analysis. By comparison with terrestrial pyroxenes cell and polyhedral volumes in clino- and orthopyroxenes show a low crystallization pressure. Fe(2+) and Mg are rather disordered in M1 and M2 sites of clino- and orthopyroxenes; the closure temperatures of the exchange reaction are 600 and 512 C respectively, which is consistent with a quite fast cooling rate, estimated of the order of one degree per day. The closure temperature for the intercrystalline Ca-Mg exchange reaction for clino- and orthopyroxene showing clinopyroxene lamellae about 10 microns thick. Kinetic evaluations based on the thickness of exolved lamellae give a cooling rate of not more than a few degrees per 10(exp 4) years. The different cooling rates obtained from Fe(2+)-Mg intracrystalline partitioning and exolution lamellae suggest an initial episode of slow cooling at 900 C, followed by faster cooling at temperatures of 600-500 C at low pressure conditions. The most probable scenario of the meteorite history seems that the exolved orthopyroxene entered the parental chondrite body after exolution had taken place at high temperature. Subsequent fast cooling occurred at low temperature after the formation of the body.

Examining the role of canister cooling conditions on the formation of nepheline from nuclear waste glasses

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

Christian, J. H.

2015-09-01

Nepheline (NaAlSiO₄) crystals can form during slow cooling of high-level waste (HLW) glass after it has been poured into a waste canister. Formation of these crystals can adversely affect the chemical durability of the glass. The tendency for nepheline crystallization to form in a HLW glass increases with increasing concentrations of Al₂O₃ and Na₂O.

Cryo-cooling in macromolecular crystallography: advantages, disadvantages and optimization.

PubMed

Juers, Douglas H; Matthews, Brian W

2004-05-01

The flash-cooling of crystals in macromolecular crystallography has become commonplace. The procedure makes it possible to collect data from much smaller specimens than was the case in the past Also, flash-cooled crystals are much less prone to radiation damage than their room-temperature counterparts, allowing data to be accumulated over extended periods of time. Notwithstanding the attractiveness of the technique, it does have potential disadvantages. First, better methods need to be developed to prevent damage to crystals on freezing. There is also a risk that structures determined at low temperature may suggest conclusions based on aspects of the structure that are not necessarily relevant at room temperature.

Investigation of the Evolution of Crystal Size and Shape during Temperature Cycling and in the Presence of a Polymeric Additive Using Combined Process Analytical Technologies

PubMed Central

2017-01-01

Crystal size and shape can be manipulated to enhance the qualities of the final product. In this work the steady-state shape and size of succinic acid crystals, with and without a polymeric additive (Pluronic P123) at 350 mL, scale is reported. The effect of the amplitude of cycles as well as the heating/cooling rates is described, and convergent cycling (direct nucleation control) is compared to static cycling. The results show that the shape of succinic acid crystals changes from plate- to diamond-like after multiple cycling steps, and that the time required for this morphology change to occur is strongly related to the type of cycling. Addition of the polymer is shown to affect both the final shape of the crystals and the time needed to reach size and shape steady-state conditions. It is shown how this phenomenon can be used to improve the design of the crystallization step in order to achieve more efficient downstream operations and, in general, to help optimize the whole manufacturing process. PMID:28867966

Microgravity

NASA Image and Video Library

1992-03-12

The Advanced Automated Directional Solidification Furnace (AADSF) with the Experimental Apparatus Container (EAC) removed flew during the USMP-2 mission. During USMP-2, the AADSF was used to study the growth of mercury cadmium telluride crystals in microgravity by directional solidification, a process commonly used on earth to process metals and grow crystals. The furnace is tubular and has three independently controlled temperature zones . The sample travels from the hot zone of the furnace (1600 degrees F) where the material solidifies as it cools. The solidification region, known as the solid/liquid interface, moves from one end of the sample to the other at a controlled rate, thus the term directional solidification.

Formation of Superhard Chromium Carbide Crystal Microrods in Ni-Cr-C Systems

NASA Astrophysics Data System (ADS)

Val'chuk, V. P.; Zmienko, D. S.; Kolesov, V. V.; Chernozatonskii, L. A.

2018-04-01

Ni-Cr-C materials with a high hardness determined by the presence of regions consisting of Cr3C2 microrods with a record microhardness reaching 3200 kg/mm2 have been obtained. Their self-organization in a powder consisting of Ni, Cr, and carbon microparticles with a high weight percentage occurs in the process of its sintering at a temperature of 1300°C and the subsequent sharp cooling of the resulting alloy. A model has been proposed for the process of formation of such crystal microrods whose characteristics have been determined by hardness measurement, electron microscopy, and microchemical and X-ray diffraction analyses.

Growth of triglycine sulfate (TGS) crystals by solution technique

NASA Technical Reports Server (NTRS)

Lal, R. B.; Kroes, R. L.; Wilcox, W. R.

1982-01-01

The growth of crystals from solution is greatly influenced by buoyancy driven convection. In a low-g environment, convection is greatly suppressed and diffusion becomes the predominant mechanism for thermal and mass transport. An experiment to grow TGS crystals by solution technique during the orbital Spacelab III mission has been designed. Crystals are grown by a new and unique technique of extracting heat from the crystal through a sting. The cooling at the sting tip is responsible for the desired supersaturation near the growing crystal. Calculations indicate that the cooled sting technique for solution crystal growth is necessary in low-g to maintain a maximum growth rate of 1 mm/day. Results of groundbased work in support of the flight experiment are discussed.

Low field magnetocaloric effect in bulk and ribbon alloy La(Fe0.88Si0.12)13

NASA Astrophysics Data System (ADS)

Vuong, Van-Hiep; Do-Thi, Kim-Anh; Nguyen, Duy-Thien; Nguyen, Quang-Hoa; Hoang, Nam-Nhat

2018-03-01

Low-field magnetocaloric effect occurred in itinerant metamagnetic materials is at core for magnetic cooling application. This works reports the magnetocaloric responses obtained at 1.35 T for the silicon-doped iron-based binary alloy La(Fe0.88Si0.12)13 in the bulk and ribbon form. Both samples possess a same symmetry but with different crystallite sizes and lattice parameters. The ribbon sample shows a larger maximum entropy change (nearly 8.5 times larger) and a higher Curie temperature (5 K higher) in comparison with that of the bulk sample. The obtained relative cooling power for the ribbon is also larger and very promising for application (RCP = 153 J/kg versus 25.2 J/kg for the bulk). The origin of the effect observed is assigned to the occurrence of negative magnetovolume effect in the ribbon structure with limit crystallization, caused by rapid cooling process at the preparation, which induced smaller crystallite size and large lattice constant at the overall weaker local crystal field.

Water-cooled probe technique for the study of freeze lining formation

NASA Astrophysics Data System (ADS)

Verscheure, Karel; Campforts, Mieke; Verhaeghe, Frederik; Boydens, Eddy; Blanpain, Bart; Wollants, Patrick; van Camp, Maurits

2006-12-01

Furnace protection by water-cooled freeze linings becomes increasingly important as the metal producing industry attempts to achieve higher process intensities. Systematic investigations of the growth and the resulting microstructure and compositional profile of freeze linings are necessary to understand the behavior of freeze linings, their relation with the industrial process, and their interaction with the wall cooling system. We have developed a technique based on the submergence of a water-cooled probe into a liquid slag bath. Freeze linings of two industrial nonferrous slags have been produced using this technique and their growth, microstructural, and compositional profiles as a function of submergence time were determined. Thermodynamic equilibrium for the investigated slag systems was calculated and compared with the observed microstructures. The freeze linings form in approximately 15 minutes. Close to the water cooling, the freeze linings are predominantly amorphous in structure. With increasing distance from the water cooling, the proportion of crystalline phases increases and bath material is entrapped in the microstructure. Cellular crystals are observed close to the bath. The freeze linings exhibit an approximate homogeneous composition. The results demonstrate that the technique is a successful tool in obtaining information on the growth, microstructure, and composition of freeze linings in industrial water-cooled furnaces.

Fractionation of lithium isotopes in magmatic systems as a natural consequence of cooling

NASA Astrophysics Data System (ADS)

Gallagher, Kerry; Elliott, Tim

2009-02-01

High-temperature, diffusive fractionation has been invoked to account for striking Li isotopic variability recently observed within individual phenocrysts and xenolith minerals. It has been argued that chemical potential gradients required to drive such diffusion arise from changes in Li partitioning between coexisting phases during cooling. If so, Li isotopic zoning should be a common occurrence but the role of temperature-dependent partition coefficients in generating Li isotopic variability remains to be tested in a quantitative manner. Here we consider a basic scenario of a phenocryst in a cooling lava, using simple parameterisations of the temperature dependence of Li partitioning and diffusivity in clinopyroxene. Our model initially produces an asymmetric isotope profile across the crystal with a δ7Li minimum that remains close to the edge of a crystal. Such a distinctive shape mimics Li isotopic profiles documented in some olivine and clinopyroxene phenocrysts, which have isotopically normal cores but anomalously light rims. The temperature dependence of both the diffusivity and the partition coefficient of Li are key factors in generating this form of diffusion profile. Continued diffusion leads to an inversion in the sense of isotopic change between core and rim and results in the whole phenocryst attaining markedly light isotopic values. Our calculations show that significant Li isotopic zoning can occur as a natural consequence of cooling magmatic systems. Crystals that have experienced more complex thermal histories (e.g. re-entrained cumulates versus true phenocrysts) will therefore exhibit contrasting isotopic profiles and, as such, these data may be useful for tracing sub-volcanic processes.

Apparatus and method for heating a material in a transparent ampoule. [crystal growth

NASA Technical Reports Server (NTRS)

Holland, L. R. (Inventor)

1983-01-01

An improved process for heating a material within a fused silica ampoule by radiation through the wall of the ampoule, while simultaneously passing a cooling gas around the ampoule is described. The radiation passes through a screen of fused silica so as to remove those components capable of directly heating the silica, therby increasing the temperature of the material within the ampoule above the strain point of the ampoule, while maintaining the exterior of the ampoule cool enough to prevent rupturing the amp.

[Standardization of cryopreservation process of Saccharomyces boulardii yeasts for usage in collections and banks of industrial microorganism strains].

PubMed

Gurina, T M; Vysekantsev, I P; Babinets, O M

2013-01-01

New implementation principle of freeze-thawing during cryopreservation of microorganisms, initiation of the process of crystal formation at cooling and thawing stage with the controlled rate of heating was experimentally substantiated. This allows increasing the cell viability, guaranteeing their equal number in each preparation, decreasing the contamination risk of the samples at thawing stage.

Constraints on crystallization of basaltic magma: observations from Kilauea Iki lava lake, Hawaii

NASA Astrophysics Data System (ADS)

Helz, Rosalind

2013-04-01

Kilauea Iki lava lake is a picritic (average MgO = 15.5%) magma body, approximately 135 m thick, which underwent extensive internal differentiation as it cooled and crystallized from its formation during the eruption of 1959 until final solidification in the mid-nineties. Observations of its initial state include data on the stages of filling of the lava lake, plus the sequence and temperature of lava compositions erupted. Drilling and core recovery (from 1960 to 1988) have documented the state of the lake at specific times, showing that the rate of growth of the upper crust was nearly linear (~2.5 m per year between 1962 and 1979), and that the overall pattern of cooling of the lava lake is consistent with conductive heat loss. Recovery and analysis of partially molten drill core has provided a detailed view of the cooling and differentiation history of the melts and minerals within the lake. Observations that may be relevant to older systems include: (1) documentation of when and to what extent olivine settling occurred in the lake; (2) the observation that the most differentiated part of the lake, which lies within the upper crust at a depth of 20-40 m, had completely crystallized by 1975, and (3) the observation that the position of the last interstitial melt was at 80-85 m down, or 62% of the way down in the lake, as would be predicted from conductive cooling. The lava lake lost heat through its roof faster than through the floor, with the result that the position of most-differentiated horizon is grossly offset from the position of the final melt. Circulation patterns in Kilauea Iki were initially driven by lava input during the eruption plus extensive loss of volatiles. These processes significantly affected the location of foundered crust within the lake, as well as the accumulation of coarse, pre-existing olivine phenocrysts between 50 and 95 m. Subsequently, two other major differentiation processes within the lake were driven by upward movement of low-density melts (compositional convection) or of vesicle plumes + melts. These two processes operated vertically, with large-scale motion perpendicular to the (sub-horizontal) isothermal surfaces in the crystallizing mush zones. They have also influenced the grainsize of groundmass minerals throughout the lake. These processes, together with limited olivine settling, have created the existing chemically zoned body. Because of the real-time constraints on when and by what processes the differentiated body that now exists at Kilauea Iki was produced, we can begin to better understand other, older lava lakes and sills, where only the final state is available to us.

Monoclinic MB phase and phase instability in [110] field cooled Pb(Zn1/3Nb2/3)O3-4.5%PbTiO3 single crystals

NASA Astrophysics Data System (ADS)

Yao, Jianjun; Cao, Hu; Ge, Wenwei; Li, Jiefang; Viehland, D.

2009-08-01

We report the finding of a monoclinic MB phase in Pb(Zn1/3Nb2/3)O3-4.5%PbTiO3 single crystals. High precision x-ray diffraction investigations of [110] field cooled crystals have shown a transformation sequence of cubic(C)→tetragonal(T)→orthorhombic(O)→monoclinic(MB), which is different from that previously reported [A.-E. Renault et al., J. Appl. Phys. 97, 044105 (2005)]. Beginning in the zero-field-cooled condition at 383 K, a rhombohedral (R)→MB→O sequence was observed with increasing field. Coexisting MB and O phases were then found upon removal of field, which fully transformed to MB on cooling to room temperature.

Improved thermoelectrically cooled quartz crystal microbalance

NASA Technical Reports Server (NTRS)

Mckeown, W. E.; Corbin, W. E., Jr.; Fox, M. G.

1974-01-01

Design changes in the thermoelectrically-cooled quartz microbalance, which is used to monitor surface contamination in space simulation chambers, is described in terms of its extended temperature range, increased temperature control, mass sensitivity, and cooling power. The mass sensor uses 20 MHz quartz crystals having a sensitivity of 8.8 x 10 to the minus tenth power g/sq cm - Hz. The crystals are optically polished, metal plated, and overplated with magnesium fluoride to simulate an optical surface. The microbalance temperature circuitry is designed to readout and control surface temperature between 100 C and minus 59 C to plus or minus 0.5 C, and readout only temperature between minus 60 C and minus 199 C using auxiliary liquid nitrogen cooling. Data is included on the measurement of oil contamination of surfaces as a function of temperature in space simulation chambers.

Models and Experiments of Melt-Rock Interaction in the Lower Oceanic Crust

NASA Astrophysics Data System (ADS)

Orton, W. H., II; Liang, Y.; Sanfilippo, A.

2017-12-01

Understanding the processes of melt-rock interaction in the lower oceanic crust isimportant to the interpretation of mid-ocean ridge basalt (MORB) and the petrogenesis of lowercrustal cumulates. Petrologic and geochemical studies of cumulates from the lower crustalregions of oceanic lithosphere have identified a number of textural and chemical features that arepertinent to melt-rock reaction (e.g., high-Mg# clinopyroxene oikocrysts within local gabbroicregions in troctolite bodies). The purpose of the present study is to provide some referenceexamples of MORB melt and cumulate mush interaction under controlled conditions. Suchsimple experiments are useful in sorting out crystallization, dissolution, re-precipitation, anddiffusion processes in the cumulate mush and in developing better models for melt transport andmelt-rock interaction in the lower oceanic crust.We performed piston cylinder experiments at 0.5-0.7 GPa and 1000-1250°C reacting anolivine or olivine + plagioclase cumulate mush and an intruding MORB melt in a graphite-linedmolybdenum capsule. Our experiments consist of two steps: (1) reaction at 1250°C for 10 to 24hours; and (2) reactive crystallization to a lower temperature through controlled cooling overseveral days. Cooling promotes in situ crystallization of interstitial melts, allowing us to bettercharacterize the mineral compositional trends produced and observed by melt-rock reaction andcrystallization. Reaction at 1250°C produced an olivine + melt mush with small rounded crystalscharacteristic of dissolution. Significant crystal settling was also observed at large melt-to- rockratio. Cooling with continued reaction resulted in the formation of a plagioclase matrix withpoikilitic clinopyroxene oikocrysts containing plagioclase and relict olivine as chadacrysts.Clinopyroxenes were in a reaction relationship with both plagioclase and olivine. In somesamples, multiple phases of clinopyroxene and plagioclase were present, each with differentcompositions, similar to those observed in the field-based studies. With these insights, a modelfor melt transport and melt-rock interaction in the lower oceanic crust has been developed andwill be used to study major and trace element fractionation during reactive melt migration in thecumulate mush.

A local heat transfer analysis of lava cooling in the atmosphere: application to thermal diffusion-dominated lava flows

NASA Astrophysics Data System (ADS)

Neri, Augusto

1998-05-01

The local cooling process of thermal diffusion-dominated lava flows in the atmosphere was studied by a transient, one-dimensional heat transfer model taking into account the most relevant processes governing its behavior. Thermal diffusion-dominated lava flows include any type of flow in which the conductive-diffusive contribution in the energy equation largely overcomes the convective terms. This type of condition is supposed to be satisfied, during more or less extended periods of time, for a wide range of lava flows characterized by very low flow-rates, such as slabby and toothpaste pahoehoe, spongy pahoehoe, flow at the transition pahoehoe-aa, and flows from ephemeral vents. The analysis can be useful for the understanding of the effect of crust formation on the thermal insulation of the lava interior and, if integrated with adequate flow models, for the explanation of local features and morphologies of lava flows. The study is particularly aimed at a better knowledge of the complex non-linear heat transfer mechanisms that control lava cooling in the atmosphere and at the estimation of the most important parameters affecting the global heat transfer coefficient during the solidification process. The three fundamental heat transfer mechanisms with the atmosphere, that is radiation, natural convection, and forced convection by the wind, were modeled, whereas conduction and heat generation due to crystallization were considered within the lava. The magma was represented as a vesiculated binary melt with a given liquidus and solidus temperature and with the possible presence of a eutectic. The effects of different morphological features of the surface were investigated through a simplified description of their geometry. Model results allow both study of the formation in time of the crust and the thermal mushy layer underlying it, and a description of the behavior of the temperature distribution inside the lava as well as radiative and convective fluxes to the atmosphere. The analysis, performed by using parameters typical of Etnean lavas, particularly focuses on the non-intuitive relations between superficial cooling effects and inner temperature distribution as a function of the major variables involved in the cooling process. Results integrate recent modelings and measurements of the cooling process of Hawaiian pahoehoe flow lobes by Hon et al. (1994) and Keszthelyi and Denlinger (1996) and highlight the critical role played by surface morphology, lava thermal properties, and crystallization dynamics. Furthermore, the reported description of the various heat fluxes between lava and atmosphere can be extended to any other type of lava flows in which atmospheric cooling is involved.

Enhanced electrocaloric cooling in ferroelectric single crystals by electric field reversal

NASA Astrophysics Data System (ADS)

Ma, Yang-Bin; Novak, Nikola; Koruza, Jurij; Yang, Tongqing; Albe, Karsten; Xu, Bai-Xiang

2016-09-01

An improved thermodynamic cycle is validated in ferroelectric single crystals, where the cooling effect of an electrocaloric refrigerant is enhanced by applying a reversed electric field. In contrast to the conventional adiabatic heating or cooling by on-off cycles of the external electric field, applying a reversed field is significantly improving the cooling efficiency, since the variation in configurational entropy is increased. By comparing results from computer simulations using Monte Carlo algorithms and experiments using direct electrocaloric measurements, we show that the electrocaloric cooling efficiency can be enhanced by more than 20% in standard ferroelectrics and also relaxor ferroelectrics, like Pb (Mg1 /3 /Nb2 /3)0.71Ti0.29O3 .

Microstructural properties and evolution of nanoclusters in liquid Si during a rapid cooling process

NASA Astrophysics Data System (ADS)

Gao, T.; Hu, X.; Li, Y.; Tian, Z.; Xie, Q.; Chen, Q.; Liang, Y.; Luo, X.; Ren, L.; Luo, J.

2017-11-01

The formation of amorphous structures in Si during the rapid quenching process was studied based on molecular dynamics simulation by using the Stillinger-Weber potential. The evolution characteristics of nanoclusters during the solidification were analyzed by several structural analysis methods. The amorphous Si has been formed with many tetrahedral clusters and few nanoclusters. During the solidification, tetrahedral polyhedrons affect the local structures by their different positions and connection modes. The main kinds of polyhedrons randomly linked with one another to form an amorphous network structures in the system. The structural evolution of crystal nanocluster demonstrates that the nanocluster has difficulty to growth because of the high cooling rate of 1012 K/s.

Accessing protein conformational ensembles using room-temperature X-ray crystallography

PubMed Central

Fraser, James S.; van den Bedem, Henry; Samelson, Avi J.; Lang, P. Therese; Holton, James M.; Echols, Nathaniel; Alber, Tom

2011-01-01

Modern protein crystal structures are based nearly exclusively on X-ray data collected at cryogenic temperatures (generally 100 K). The cooling process is thought to introduce little bias in the functional interpretation of structural results, because cryogenic temperatures minimally perturb the overall protein backbone fold. In contrast, here we show that flash cooling biases previously hidden structural ensembles in protein crystals. By analyzing available data for 30 different proteins using new computational tools for electron-density sampling, model refinement, and molecular packing analysis, we found that crystal cryocooling remodels the conformational distributions of more than 35% of side chains and eliminates packing defects necessary for functional motions. In the signaling switch protein, H-Ras, an allosteric network consistent with fluctuations detected in solution by NMR was uncovered in the room-temperature, but not the cryogenic, electron-density maps. These results expose a bias in structural databases toward smaller, overpacked, and unrealistically unique models. Monitoring room-temperature conformational ensembles by X-ray crystallography can reveal motions crucial for catalysis, ligand binding, and allosteric regulation. PMID:21918110

Spherical crystals of Pb 1 - xSn xTe grown in microgravity

NASA Astrophysics Data System (ADS)

Kinoshita, Kyoichi; Yamada, Tomoaki

1996-07-01

Pb 1- xSn xTe spherical crystals were unintentionally obtained along with a cylindrical Pb 1 - xSn xTe crystal grown during the {SL-J}/{FMPT} mission on board the space shuttle "Endeavor". About 25 spherical crystals ranged from 0.5 to 11 mm in diameter. Melt leaked from the melt reservoir into the spring that plays the role of pushing the melt toward a seed crystal and eliminating free surface areas of the melt. Because of the surface tension of the melt, spherical melt drops formed in the hollow of the spring, then solidified into spherical crystals during the cooling process. Some of the crystals had lower dislocation densities, in the order of 10 4 cm -2, two orders smaller than those of terrestrially grown crystals from a melt. The experiment showed a way of stably positioning a large volume of liquid in microgravity without touching the crucible wall and a way of reducing crystalline defects by such growth.

Finding the Cold Needle in a Warm Haystack: Infrared Imaging Applied to Locating Cryo-cooled Crystals in Loops

NASA Technical Reports Server (NTRS)

Snell, Edward; vanderWoerd, Mark

2003-01-01

Thermally imaging the cryocooling processes of crystals has been demonstrated showing the progression of a cold wave through a crystal from the face closest to the origin of the coldstream ending at the point furthest away. During these studies large volume crystals were clearly distinguished from the loop holding them. Large volume crystals, used for neutron studies, were chosen deliberately to enhance the imaging. The different infrared transmission and reflectance properties of the crystal in comparison to the cryo-protectant are thought to be the parameter that produces the contrast making the crystal visible. As an application of the technology to locating crystals, more small crystals of lysozyme and a bFGF/dna complex were cryo-protected and imaged in large loops. The crystals were clearly distinguished from the vitrified solution. In the case of the bFGF/dna complex the illumination had to be carefully manipulated to enable the crystal to be seen in the visible spectrum. These preliminary results will be presented along with advantages and disadvantages of the technique and a discussion of how it might be applied.

DNA-mediated nanoparticle crystallization into Wulff polyhedra

NASA Astrophysics Data System (ADS)

Auyeung, Evelyn; Li, Ting I. N. G.; Senesi, Andrew J.; Schmucker, Abrin L.; Pals, Bridget C.; de La Cruz, Monica Olvera; Mirkin, Chad A.

2014-01-01

Crystallization is a fundamental and ubiquitous process much studied over the centuries. But although the crystallization of atoms is fairly well understood, it remains challenging to predict reliably the outcome of molecular crystallization processes that are complicated by various molecular interactions and solvent involvement. This difficulty also applies to nanoparticles: high-quality three-dimensional crystals are mostly produced using drying and sedimentation techniques that are often impossible to rationalize and control to give a desired crystal symmetry, lattice spacing and habit (crystal shape). In principle, DNA-mediated assembly of nanoparticles offers an ideal opportunity for studying nanoparticle crystallization: a well-defined set of rules have been developed to target desired lattice symmetries and lattice constants, and the occurrence of features such as grain boundaries and twinning in DNA superlattices and traditional crystals comprised of molecular or atomic building blocks suggests that similar principles govern their crystallization. But the presence of charged biomolecules, interparticle spacings of tens of nanometres, and the realization so far of only polycrystalline DNA-interconnected nanoparticle superlattices, all suggest that DNA-guided crystallization may differ from traditional crystal growth. Here we show that very slow cooling, over several days, of solutions of complementary-DNA-modified nanoparticles through the melting temperature of the system gives the thermodynamic product with a specific and uniform crystal habit. We find that our nanoparticle assemblies have the Wulff equilibrium crystal structure that is predicted from theoretical considerations and molecular dynamics simulations, thus establishing that DNA hybridization can direct nanoparticle assembly along a pathway that mimics atomic crystallization.

Numerical Study of the Features of Ti-Nb Alloy Crystallization during Selective Laser Sintering

NASA Astrophysics Data System (ADS)

Dmitriev, A. I.; Nikonov, A. Y.

2016-07-01

The demand for implants with individual shape requires the development of new methods and approaches to their production. The obvious advantages of additive technologies and selective laser sintering are the capabilities to form both the external shape of the product and its internal structure. Recently appeared and attractive from the perspective of biomechanical compatibility are beta alloys of titanium-niobium that have similar mechanical properties to those of cortical bone. This paper studies the processes occurring at different stages of laser sintering using computer simulation on atomic scale. The effect of cooling rate on the resulting crystal structure of Ti-Nb alloy was analysed. Also, the dependence of tensile strength of sintered particles on heating time and cooling rate was studied. It was shown that the main parameter, which determines the adhesive properties of sintered particles, is the contact area obtained during sintering process. The simulation results can both help defining the technological parameters of the process to provide the desired mechanical properties of the resulting products and serve as a necessary basis for calculations on large scale levels in order to study the behaviour of actually used implants.

Method of processing "BPS" glass ceramic and seals made therewith

DOEpatents

Reed, Scott T.; Stone, Ronald G.; McCollister, Howard L.; Wengert, deceased, Paul R.

1998-01-01

A glass ceramic composition, a glass ceramic-to-metal seal, and more specifically a hermetic glass ceramic-to-metal seal prepared by subjecting a glass composition comprising, by weight percent, SiO.sub.2 (65-80%), LiO.sub.2 (8-16%), Al.sub.2 O.sub.3 (2-8%), K.sub.2 O (1-8%), P.sub.2 O.sub.5 (1-5%), B.sub.2 O.sub.3 (0.5-7%), and ZnO (0-5%) to the following processing steps: 1) heating the glass composition in a belt furnace to a temperature sufficient to melt the glass and crystallize lithium phosphate, 2) holding at a temperature and for a time sufficient to create cristobalite nuclei, 3) cooling at a controlled rate and to a temperature to cause crystallization of lithium silicates and growth of cristobalite, and 4) still further cooling in stages to ambient temperature. This process produces a glass ceramic whose high coefficient of thermal expansion (up to 200.times.10.sup.-7 in/in/.degree.C.) permits the fabrication of glass ceramic-to-metal seals, and particularly hermetic glass ceramic seals to nickel-based and stainless steel alloys and copper.

Method of processing ``BPS`` glass ceramic and seals made therewith

DOEpatents

Reed, S.T.; Stone, R.G.; McCollister, H.L.; Wengert, P.R.

1998-10-13

A glass ceramic composition, a glass ceramic-to-metal seal, and more specifically a hermetic glass ceramic-to-metal seal prepared by subjecting a glass composition comprising, by weight percent, SiO{sub 2} (65--80%), LiO{sub 2} (8--16%), Al{sub 2}O{sub 3} (2--8%), K{sub 2}O (1--8%), P{sub 2}O{sub 5} (1--5%), B{sub 2}O{sub 3} (0.5--7%), and ZnO (0--5%) to the following processing steps: (1) heating the glass composition in a belt furnace to a temperature sufficient to melt the glass and crystallize lithium phosphate, (2) holding at a temperature and for a time sufficient to create cristobalite nuclei, (3) cooling at a controlled rate and to a temperature to cause crystallization of lithium silicates and growth of cristobalite, and (4) still further cooling in stages to ambient temperature. This process produces a glass ceramic whose high coefficient of thermal expansion (up to 200{times}10{sup {minus}7} in/in/C) permits the fabrication of glass ceramic-to-metal seals, and particularly hermetic glass ceramic seals to nickel-based and stainless steel alloys and copper. 5 figs.

Tuning the functional properties of PMN-PT single crystals via doping and thermoelectrical treatments

NASA Astrophysics Data System (ADS)

Luo, Laihui; Dietze, Matthias; Solterbeck, Claus-Henning; Luo, Haosu; Es-Souni, Mohammed

2013-12-01

Single crystals based on solid solutions of lead-magnesium-niobate (PMN) and lead titanate (PT) have emerged as highly promising multifunctional systems combining piezoelectric, pyroelectric, and electro-optic properties that surpass by far those of the best known lead-zirkonium-titanate ceramics. In this paper we present new findings on how the phase transition temperature and the dielectric and ferroelectric properties can be tuned depending on crystal composition, orientation, and thermoelectrical treatment. Mn-doped and pure 0.72PbMg1/3Nb2/3O3-0.28PbTiO3 (0.72PMN-0.28PT) single crystals with ⟨111⟩ and ⟨001⟩ orientations were investigated. A special attention was devoted to field cooling (FC), i.e., cooling under electric field from different temperatures. The results illustrate different findings that were not reported before: the Curie temperature, i.e., ferroelectric-paraelectric transition temperature, is enhanced after field cooling of the Mn-doped, ⟨001⟩-oriented crystal while such a shift is not observed in the ⟨111⟩-oriented and the non-doped crystals. In addition, substantial polarization suppression occurs in the Mn-doped crystals upon FC from high temperature regardless of orientation. Based on piezoforce microscopy of the domain structure that shows suppression of domain growth following field cooling from 200 °C, we propose a mechanism for polarization suppression based on domain pinning by charged defects. The practical importance of our results lies in showing the opportunity offered by a proper choice of crystal composition and poling conditions for tuning the functional properties of PMN-PT single crystals for a specific application. This should contribute to the understanding of their properties towards advanced sensor and transducers devices.

Chromite in komatiites: 3D morphologies with implications for crystallization mechanisms

NASA Astrophysics Data System (ADS)

Godel, Bélinda; Barnes, Stephen J.; Gürer, Derya; Austin, Peter; Fiorentini, Marco L.

2013-01-01

High-resolution X-ray computed tomography has been carried out on a suite of komatiite samples representing a range of volcanic facies, chromite contents and degrees of alteration and metamorphism, to reveal the wide range of sizes, shapes and degrees of clustering that chromite grains display as a function of cooling history. Dendrites are spectacularly skeletal chromite grains formed during very rapid crystallization of supercooled melt in spinifex zones close to flow tops. At slower cooling rates in the interiors of thick flows, chromite forms predominantly euhedral grains. Large clusters (up to a dozen of grains) are characteristic of liquidus chromite, whereas fine dustings of mostly individual ~20-μm grains form by in situ crystallization from trapped intercumulus liquid. Chromite in coarse-grained olivine cumulates from komatiitic dunite bodies occurs in two forms: as clusters or chains of euhedral crystals, developing into "chicken-wire" texture where chromite is present in supra-cotectic proportions; and as strongly dendritic, semi-poikilitic grains. These dendritic grains are likely to have formed by rapid crescumulate growth from magma that was close to its liquidus temperature but supersaturated with chromite. In some cases, this process seems to have been favoured by nucleation of chromite on the margins of sulphide liquid blebs. This texture is a good evidence for the predominantly cumulus origin of oikocrysts and in situ origin of heteradcumulate textures. Our 3D textural analysis confirms that the morphology of chromite crystals is a distinctive indicator of crystallization environment even in highly altered rocks.

Structural evolution in the crystallization of rapid cooling silver melt

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

Tian, Z.A., E-mail: ze.tian@gmail.com; Laboratory for Simulation and Modelling of Particulate Systems School of Materials Science and Engineering, University of New South Wales, Sydney, NSW 2052; Dong, K.J.

2015-03-15

The structural evolution in a rapid cooling process of silver melt has been investigated at different scales by adopting several analysis methods. The results testify Ostwald’s rule of stages and Frank conjecture upon icosahedron with many specific details. In particular, the cluster-scale analysis by a recent developed method called LSCA (the Largest Standard Cluster Analysis) clarified the complex structural evolution occurred in crystallization: different kinds of local clusters (such as ico-like (ico is the abbreviation of icosahedron), ico-bcc like (bcc, body-centred cubic), bcc, bcc-like structures) in turn have their maximal numbers as temperature decreases. And in a rather wide temperaturemore » range the icosahedral short-range order (ISRO) demonstrates a saturated stage (where the amount of ico-like structures keeps stable) that breeds metastable bcc clusters. As the precursor of crystallization, after reaching the maximal number bcc clusters finally decrease, resulting in the final solid being a mixture mainly composed of fcc/hcp (face-centred cubic and hexagonal-closed packed) clusters and to a less degree, bcc clusters. This detailed geometric picture for crystallization of liquid metal is believed to be useful to improve the fundamental understanding of liquid–solid phase transition. - Highlights: • A comprehensive structural analysis is conducted focusing on crystallization. • The involved atoms in our analysis are more than 90% for all samples concerned. • A series of distinct intermediate states are found in crystallization of silver melt. • A novelty icosahedron-saturated state breeds the metastable bcc state.« less

Lead magnesium niobate actuator for micropositioning

DOEpatents

Swift, Charles D.; Bergum, John W.

1994-01-01

An improved lead magnesium niobate actuator is disclosed comprising a cylindrical lead magnesium niobate crystal stack mounted in a cylindrical casing wherein a bias means, such as one or more belleville washers, is located between one end of the crystal stack and a partially closed end of the casing; and adjustment means are provided which bear against the opposite end of the crystal stack, whereby an adjustable compressive force is constantly applied against the crystal stack, whether the crystal stack is actuated in an extended position, or is in an unactuated contracted position. In a preferred embodiment, cooling ports are provided for the circulation of coolant in the actuator to cool the crystal stack, and provision is made for removal and replacement of the crystal stack without disconnecting the actuator from the external device being actuated.

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

Righettoni, Marco; Pratsinis, Sotiris E., E-mail: sotiris.pratsinis@ptl.mavt.ethz.ch

Highlights: • Flame-made WO{sub 3} nanoparticles with closely controlled crystal and grain size. • Dynamic phase transition of annealing of pure and Si-doped WO{sub 3} by in situ XRD. • Irreversible evolution of WO{sub 3} crystallinity by heating/cooling during its annealing. • Si-doping alters the WO{sub 3} crystallinity dynamics and stabilizes nanosized WO{sub 3}. • Flame-made nano-WO{sub 3} can sense NO at the ppb level. - Abstract: Tungsten trioxide is a semiconductor with distinct applications in gas sensors, catalysis, batteries and pigments. As such the transition between its different crystal structures during its annealing are of interest, especially for sensormore » applications. Here, WO{sub 3} nanoparticles with closely controlled crystal and grain size (9–15 nm) and phase composition are made by flame spray pyrolysis and the formation of different WO{sub 3} phases during annealing is investigated. Most notably, the dynamic phase transition and crystal size evolution of WO{sub 3} during heating and cooling is monitored by in situ X-ray diffraction revealing how metastable WO{sub 3} phases can be captured stably. The effect of Si-doping is studied since it is used in practise to control crystal growth and phase transition during metal oxide synthesis and processing. Finally the influence of annealing on the WO{sub 3} sensing performance of NO, a lung inflammation tracer in the human breath, is explored at the ppb-level.« less

Optimization of the Processing Parameters of High Temperature Superconducting Glass-Ceramics: Center Director's Discretionary Fund Final Report

NASA Technical Reports Server (NTRS)

Ethridge, E. C.; Kaukler, W. F.

1993-01-01

A number of promising glass forming compositions of high Tc superconducting Ba-Sr-Ca-Cu-O (BSCCO) materials were evaluated for their glass-ceramic crystallization ability. The BSCCO ceramics belonging to the class of superconductors in the Ba-Sr-Ca-Cu-O system were the focus of this study. By first forming the superconducting material as a glass, subsequent devitrification into the crystalline (glass-ceramic) superconductor can be performed by thermal processing of the glass preform body. Glass formability and phase formation were determined by a variety of methods in another related study. This study focused on the nucleation and crystallization of the materials. Thermal analysis during rapid cooling aids in the evaluation of nucleation and crystallization behavior. Melt viscosity is used to predict glass formation ability.

Vapor Growth of Binary and Ternary Chalcogenides in Preparation for Microgravity Experiments

NASA Technical Reports Server (NTRS)

Su, C.; Whitaker, Ann F. (Technical Monitor)

2001-01-01

In the bulk crystal growth of some technologically important semiconducting chalcopyrites, such as ZnTe, CdS, ZnSe and ZnS, vapor growth techniques have significant advantages over melt growth techniques due to the high melting points of these materials. The realization of routine production of high-quality single crystals of these semiconductors requires a fundamental, systematic and in-depth study on the PVT growth process and crystal growth by vapor transport in low gravity offers a set of unique conditions for this study. Previously, two reasons have been put forward to account for this. The first is weight-related reductions in crystal strain and defects. These are thought to be caused by the weight of the crystals during processing at elevated temperatures and retained on cooling, particularly for materials with a low yield strength. The second, and more general, reason is related to the reduction in density-gradient driven convection. The PVT crystal growth process consists of essentially three processes: sublimation of the source material, transport of the vapor species and condensation of the vapor species to form the crystal. The latter two processes can be affected by the convection caused by gravitational accelerations on Earth. Reductions in such convection in low gravity is expected to yield a nearly diffusion-limited growth condition which results in more uniform growth rates (on the microscopic scale) and hence greater crystalline perfection and compositional homogeneity. The reduction of convective contamination by performing flight experiments in a reduced gravity environment will help to understand the relation between fluid phase processes (growth parameters) and defect and impurity incorporation in grown crystals.

Pushing the boundaries of high power lasers: low loss, large area CVD diamond

NASA Astrophysics Data System (ADS)

Wickham, Benjamin; Schoofs, Frank; Olsson-Robbie, Stefan; Bennett, Andrew; Balmer, Richard

2018-02-01

Synthetic CVD diamond has exceptional properties, including broad spectral transmission, physical and chemical robustness, and the highest thermal conductivity of any known material, making diamond an attractive material for medium to high power optical and laser applications, minimizing the detrimental effects of thermal lensing and radiation damage. Example applications include ATR prisms, Raman laser crystals, extra- and intra-cavity laser cooling. In each case the demands on the fundamental material properties and fabrication routes are slightly different. In recent years, there has been good progress in the development of low-loss, single crystal diamond, suitable for higher power densities, higher pulse rates and more demanding intra- and extra-cavity thermal management. The adoption of single crystal diamond in this area has however, been hindered by the availability of large area, low birefringence plates. To address this, we report a combination of CVD growth and processing methods that have enabled the manufacture of large, low defect substrates. A final homoepitaxial, low absorption synthesis stage has produced plates with large area (up to 16 mm edge length), low absorption (α<0.005 cm-1 at 1064 nm), and low birefringence (Δn <10-5), suitable for double-sided intra-cavity cooling. We demonstrate the practical advances in synthesis, including increasing the size while reducing in-use losses compared to previous generations of single crystal material, and practical developments in processing and implementation of the single crystal diamond parts, optimizing them for use in a state-of-the-art femto-second pulsed Ti:Sa thin disk gain module, all made in collaboration with the wider European FP7 funded Ti:Sa TD consortium.

Properties of tetrahedral clusters and medium range order in GaN during rapid solidification

NASA Astrophysics Data System (ADS)

Gao, Tinghong; Li, Yidan; Yao, Zhenzhen; Hu, Xuechen; Xie, Quan

2017-12-01

The solidification process of liquid gallium nitride has been studied by molecular dynamics simulation using the Stillinger-Weber potential at cooling rate of 10 K/ps. The structural properties of gallium nitride during the rapid cooling process were investigated in detail by the radial distribution functions, Voronoi polyhedron index and the visualization technology. The amorphous structures were formed with many medium range order structures at 200 K. The <4 0 0 0> polyhedron as the main polyhedron was more stable than other polyhedron in GaN during the quenching process. The cubic and hexahedral medium range order structures were formed by the close link between <4 0 0 0> polyhedron. The cubic crystal structures grew up through the crystalline surface by a layer-by-layer method to become more stable structures during the quenching process.

Crystallization of calcia-gallia-silica glasses

NASA Technical Reports Server (NTRS)

Ray, C. S.; Day, D. E.

1984-01-01

A thermal image furance is presently used to study the critical cooling rate for glass formation, and the kinetics of crystallization, of the compositions 18.4CaO-(81.6-X)Ga2O3-XSiO2, where X = 3, 6, 9, and 13.8. Crystallization was studied nonisothermally, and the data were analyzed in light of the Avrami (1939) equation. Critical cooling rate and crystallization activation energy are both found to decrease with increasing silica content, and the results obtained by the present technique are noted to agree with those obtained on the basis of differential thermal analysis measurements.

Novel casting processes for single-crystal turbine blades of superalloys

NASA Astrophysics Data System (ADS)

Ma, Dexin

2018-03-01

This paper presents a brief review of the current casting techniques for single-crystal (SC) blades, as well as an analysis of the solidification process in complex turbine blades. A series of novel casting methods based on the Bridgman process were presented to illustrate the development in the production of SC blades from superalloys. The grain continuator and the heat conductor techniques were developed to remove geometry-related grain defects. In these techniques, the heat barrier that hinders lateral SC growth from the blade airfoil into the extremities of the platform is minimized. The parallel heating and cooling system was developed to achieve symmetric thermal conditions for SC solidification in blade clusters, thus considerably decreasing the negative shadow effect and its related defects in the current Bridgman process. The dipping and heaving technique, in which thinshell molds are utilized, was developed to enable the establishment of a high temperature gradient for SC growth and the freckle-free solidification of superalloy castings. Moreover, by applying the targeted cooling and heating technique, a novel concept for the three-dimensional and precise control of SC growth, a proper thermal arrangement may be dynamically established for the microscopic control of SC growth in the critical areas of large industrial gas turbine blades.

The role of diffusion-controlled oscillatory nucleation in the formation of line rock in pegmatite-aplite dikes

USGS Publications Warehouse

Webber, K.L.; Falster, A.U.; Simmons, W.B.; Foord, E.E.

1997-01-01

The George Ashley Block (GAB), located in the Pala Pegmatite District, San Diego County, California, is a composite pegmatite-aplite dike of 8 m thickness displaying striking mineralogical layering in the aphte portion of the dike, referred to as line rock. Rhythmic layering is characterized by garnet-rich bands alternating with albite-quartz-muscovite-rich bands. Cumulus textures are notably absent from the layered portion of the dike. Elongated quartz, megacrysts are oriented perpendicular to the garnet-rich layers and poikilitically include garnet, albite, and muscovite. Calculated crystal-free magma viscosity with 3% H2O is 106.2 Pa s and the calculated settling velocity for garnet is 0??51 cm/year. Conductive cooling calculations based on emplacement of a 650??C dike into 150?? C fractured gabbroic country rock at 1??5 kbar, and accounting for latent heat of crystallization, demonstrate that the line rock portion of the dike cools to 550?? C in about 1 year. Crystal size distribution studies also suggest very rapid nucleation and crystallization. Diffusion-controlled gel crystallization experiments yield textures virtually identical to those observed in the layered aplite, including rhythmic banding, colloform layering, and band discontinuities. Thus, observed textures and calculated magmatic parameters suggest that mineralogical layering in the GAB results from an in situ diffusion-controlled process of oscillatory nucleation and crystallization. We propose that any event that promotes strong undercooling has the potential to initiate rapid heterogeneous nucleation and oscillatory crystal growth, leading to the development of a layer of excluded components in front of the crystallization front, and the formation of line rock.

History Dependence of the Microstructure on Time-Dependent Deformation During In-Situ Cooling of a Nickel-Based Single-Crystal Superalloy

NASA Astrophysics Data System (ADS)

Panwisawas, Chinnapat; D'Souza, Neil; Collins, David M.; Bhowmik, Ayan; Roebuck, Bryan

2018-05-01

Time-dependent plastic deformation through stress relaxation and creep deformation during in-situ cooling of the as-cast single-crystal superalloy CMSX-4® has been studied via neutron diffraction, transmission electron microscopy, electro-thermal miniature testing, and analytical modeling across two temperature regimes. Between 1000 °C and 900 °C, stress relaxation prevails and gives rise to softening as evidenced by a decreased dislocation density and the presence of long segment stacking faults in γ phase. Lattice strains decrease in both the γ matrix and γ' precipitate phases. A constitutive viscoplastic law derived from in-situ isothermal relaxation test under-estimates the equivalent plastic strain in the prediction of the stress and strain evolution during cooling in this case. It is thereby shown that the history dependence of the microstructure needs to be taken into account while deriving a constitutive law and which becomes even more relevant at high temperatures approaching the solvus. Higher temperature cooling experiments have also been carried out between 1300 °C and 1150 °C to measure the evolution of stress and plastic strain close to the γ' solvus temperature. In-situ cooling of samples using ETMT shows that creep dominates during high-temperature deformation between 1300 °C and 1220 °C, but below a threshold temperature, typically 1220 °C work hardening begins to prevail from increasing γ' fraction and resulting in a rapid increase in stress. The history dependence of prior accumulated deformation is also confirmed in the flow stress measurements using a single sample while cooling. The saturation stresses in the flow stress experiments show very good agreement with the stresses measured in the cooling experiments when viscoplastic deformation is dominant. This study demonstrates that experimentation during high-temperature deformation as well as the history dependence of the microstructure during cooling plays a key role in deriving an accurate viscoplastic constitutive law for the thermo-mechanical process during cooling from solidification.

Method for harvesting rare earth barium copper oxide single crystals

DOEpatents

Todt, V.R.; Sengupta, S.; Shi, D.

1996-04-02

A method of preparing high temperature superconductor single crystals is disclosed. The method of preparation involves preparing precursor materials of a particular composition, heating the precursor material to achieve a peritectic mixture of peritectic liquid and crystals of the high temperature superconductor, cooling the peritectic mixture to quench directly the mixture on a porous, wettable inert substrate to wick off the peritectic liquid, leaving single crystals of the high temperature superconductor on the porous substrate. Alternatively, the peritectic mixture can be cooled to a solid mass and reheated on a porous, inert substrate to melt the matrix of peritectic fluid while leaving the crystals melted, allowing the wicking away of the peritectic liquid. 2 figs.

Method for harvesting rare earth barium copper oxide single crystals

DOEpatents

Todt, Volker R.; Sengupta, Suvankar; Shi, Donglu

1996-01-01

A method of preparing high temperature superconductor single crystals. The method of preparation involves preparing precursor materials of a particular composition, heating the precursor material to achieve a peritectic mixture of peritectic liquid and crystals of the high temperature superconductor, cooling the peritectic mixture to quench directly the mixture on a porous, wettable inert substrate to wick off the peritectic liquid, leaving single crystals of the high temperature superconductor on the porous substrate. Alternatively, the peritectic mixture can be cooled to a solid mass and reheated on a porous, inert substrate to melt the matrix of peritectic fluid while leaving the crystals melted, allowing the wicking away of the peritectic liquid.

Monitoring of Batch Industrial Crystallization with Growth, Nucleation, and Agglomeration. Part 1: Modeling with Method of Characteristics.

PubMed

Porru, Marcella; Özkan, Leyla

2017-05-24

This paper develops a new simulation model for crystal size distribution dynamics in industrial batch crystallization. The work is motivated by the necessity of accurate prediction models for online monitoring purposes. The proposed numerical scheme is able to handle growth, nucleation, and agglomeration kinetics by means of the population balance equation and the method of characteristics. The former offers a detailed description of the solid phase evolution, while the latter provides an accurate and efficient numerical solution. In particular, the accuracy of the prediction of the agglomeration kinetics, which cannot be ignored in industrial crystallization, has been assessed by comparing it with solutions in the literature. The efficiency of the solution has been tested on a simulation of a seeded flash cooling batch process. Since the proposed numerical scheme can accurately simulate the system behavior more than hundred times faster than the batch duration, it is suitable for online applications such as process monitoring tools based on state estimators.

Monitoring of Batch Industrial Crystallization with Growth, Nucleation, and Agglomeration. Part 1: Modeling with Method of Characteristics

PubMed Central

2017-01-01

This paper develops a new simulation model for crystal size distribution dynamics in industrial batch crystallization. The work is motivated by the necessity of accurate prediction models for online monitoring purposes. The proposed numerical scheme is able to handle growth, nucleation, and agglomeration kinetics by means of the population balance equation and the method of characteristics. The former offers a detailed description of the solid phase evolution, while the latter provides an accurate and efficient numerical solution. In particular, the accuracy of the prediction of the agglomeration kinetics, which cannot be ignored in industrial crystallization, has been assessed by comparing it with solutions in the literature. The efficiency of the solution has been tested on a simulation of a seeded flash cooling batch process. Since the proposed numerical scheme can accurately simulate the system behavior more than hundred times faster than the batch duration, it is suitable for online applications such as process monitoring tools based on state estimators. PMID:28603342

Fluoride glass: Crystallization, surface tension

NASA Technical Reports Server (NTRS)

Doremus, R. H.

1988-01-01

Fluoride glass was levitated acoustically in the ACES apparatus on STS-11, and the recovered sample had a different microstructure from samples cooled in a container. Further experiments on levitated samples of fluoride glass are proposed. These include nucleation, crystallization, melting observations, measurement of surface tension of molten glass, and observation of bubbles in the glass. Ground experiments are required on sample preparation, outgassing, and surface reactions. The results should help in the development and evaluation of containerless processing, especially of glass, in the development of a contaminent-free method of measuring surface tensions of melts, in extending knowledge of gas and bubble behavior in fluoride glasses, and in increasing insight into the processing and properties of fluoride glasses.

KREEP basalt petrogenesis: Insights from 15434,181

NASA Astrophysics Data System (ADS)

Cronberger, Karl; Neal, Clive R.

2017-05-01

Returned lunar KREEP basalts originated through impact processes or endogenous melting of the lunar interior. Various methods have been used to distinguish between these two origins, with varying degrees of success. Apollo 15 KREEP basalts are generally considered to be endogenous melts of the lunar interior. For example, sample 15434,181 is reported to have formed by a two-stage cooling process, with large orthopyroxene (Opx) phenocrysts forming first and eventually cocrystalizing with smaller plagioclase crystals. However, major and trace element analyses of Opx and plagioclase coupled with calculated equilibrium liquids are inconsistent with the large orthopyroxenes being a phenocryst phase. Equilibrium liquid rare earth element (REE) profiles are enriched relative to the whole rock (WR) composition, inconsistent with Opx being an early crystallizing phase, and these are distinct from the plagioclase REE equilibrium liquids. Fractional crystallization modeling using the Opx equilibrium liquids as a parental composition cannot reproduce the WR values even with crystallization of late-stage phosphates and zircon. This work concludes that instead of being a phenocryst phase, the large Opx crystals are actually xenocrysts that were subsequently affected by pyroxene overgrowths that formed intergrowths with cocrystallizing plagioclase.

Cooling rates and crystallization dynamics of shallow level pegmatite-aplite dikes, San Diego County, California

USGS Publications Warehouse

Webber, Karen L.; Simmons, William B.; Falster, Alexander U.; Foord, Eugene E.

1999-01-01

Pegmatites of the Pala and Mesa Grande Pegmatite Districts, San Diego County, California are typically thin, sheet-like composite pegmatite-aplite dikes. Aplitic portions of many dikes display pronounced mineralogical layering referred to as "line rock," characterized by fine-grained, garnet-rich bands alternating with albite- and quartz-rich bands. Thermal modeling was performed for four dikes in San Diego County including the 1 m thick Himalaya dike, the 2 m thick Mission dike, the 8 m thick George Ashley dike, and the 25 m thick Stewart dike. Calculations were based on conductive cooling equations accounting for latent heat of crystallization, a melt emplacement temperature of 650 °C into 150 °C fractured, gabbroic country rock at a depth of 5 km, and an estimated 3 wt% initial H2O content in the melt. Cooling to -5 cm/s. Crystal size distribution (CSD) studies of garnet from layered aplites suggest growth rates of about 10-6 cm/s. These results indicate that the dikes cooled and crystallized rapidly, with variable nucleation rates but high overall crystal-growth rates. Initial high nucleation rates coincident with emplacement and strong undercooling can account for the millimeter-size aplite grains. Lower nucleation rates coupled with high growth rates can explain the decimeter-size minerals in the hanging walls, cores, and miarolitic cavities of the pegmatites. The presence of tourmaline and/or lepidolite throughout these dikes suggests that although the melts were initially H2O-undersaturated, high melt concentrations of incompatible (or fluxing) components such as B, F, and Li (±H2O), aided in the development of large pegmatitic crystals that grew rapidly in the short times suggested by the conductive cooling models.

Looking through the Zircon Kaleidoscope: Durations, Rates, and Fluxes in Silicic Magmatic System

NASA Astrophysics Data System (ADS)

Schaltegger, U.; Wotzlaw, J. F.

2014-12-01

The crystallization rate of zircon in a cooling magma depends on the cooling rate through the saturation interval in addition to compositional and kinetic factors. Repeated influx of hot magma over 10-20 ka leads to short-amplitude temperature oscillations, which are recorded by resorption/crystallization cycles of zircon. Plotting the number of dated zircons versus their high-precision U-Pb date results in curves that qualitatively relate to the evolution of magma temperature over time [1], [2]. The trace elemental, O and Hf isotopic composition of zircon gives indications about the degree of magma homogenization and thermal evolution. Zircons from systems with small volumes and magma fluxes record non-systematic chemical and Hf isotopic heterogeneity, suggesting crystallization in non-homogenized ephemeral magma batches. Such systems typically lead to small, mid-upper crustal plutons [3]. Zircons from large-volume crystal-poor rhyolites record initial heterogeneities and rapid amalgamation of smaller magma batches over 10 ka [4], while zircons from monotonous intermediates record magma evolution over several 100 ka with coherent fractionation trends suggesting homogenization and a coherent thermal evolution [2]. In both cases, volumes and flux rates were sufficient to produce large volumes of eruptible magma on very contrasting time scales. Zircon is therefore recording cyclic crystallization-rejuvenation processes during temperature fluctuations in intermediate to upper crustal magma reservoirs but may not relate to the physical pluton emplacement or eruption. We can quantify volumes, rates of magma influx, rates of cooling and crystallization, and the degree of convective homogenization from zircon data, and infer reservoir assembly and eruption trigger mechanisms. These parameters largely control the evolution of long-lived, low-flux silicic magmatic system typical for mid-to-upper crustal plutons, monotonous intermediates are characterized by intermediate durations and fluxes while short-lived, high-flux systems preferentially produce crystal-poor rhyolites. References: [1] Caricchi et al. (2014) Nature 511, 457-461; [2] Wotzlaw et al. (2013) Geology 41, 867-870; [3] Broderick (2013) PhD thesis, Univ. of Geneva; [3] Wotzlaw et al. (2014) Geology, doi:10.1130/G35979.1

Efficient rotational cooling of Coulomb-crystallized molecular ions by a helium buffer gas.

PubMed

Hansen, A K; Versolato, O O; Kłosowski, L; Kristensen, S B; Gingell, A; Schwarz, M; Windberger, A; Ullrich, J; López-Urrutia, J R Crespo; Drewsen, M

2014-04-03

The preparation of cold molecules is of great importance in many contexts, such as fundamental physics investigations, high-resolution spectroscopy of complex molecules, cold chemistry and astrochemistry. One versatile and widely applied method to cool molecules is helium buffer-gas cooling in either a supersonic beam expansion or a cryogenic trap environment. Another more recent method applicable to trapped molecular ions relies on sympathetic translational cooling, through collisional interactions with co-trapped, laser-cooled atomic ions, into spatially ordered structures called Coulomb crystals, combined with laser-controlled internal-state preparation. Here we present experimental results on helium buffer-gas cooling of the rotational degrees of freedom of MgH(+) molecular ions, which have been trapped and sympathetically cooled in a cryogenic linear radio-frequency quadrupole trap. With helium collision rates of only about ten per second--that is, four to five orders of magnitude lower than in typical buffer-gas cooling settings--we have cooled a single molecular ion to a rotational temperature of 7.5(+0.9)(-0.7) kelvin, the lowest such temperature so far measured. In addition, by varying the shape of, or the number of atomic and molecular ions in, larger Coulomb crystals, or both, we have tuned the effective rotational temperature from about 7 kelvin to about 60 kelvin by changing the translational micromotion energy of the ions. The extremely low helium collision rate may allow for sympathetic sideband cooling of single molecular ions, and eventually make quantum-logic spectroscopy of buffer-gas-cooled molecular ions feasible. Furthermore, application of the present cooling scheme to complex molecular ions should enable single- or few-state manipulations of individual molecules of biological interest.

Lead magnesium niobate actuator for micropositioning

DOEpatents

Swift, C.D.; Bergum, J.W.

1994-10-25

An improved lead magnesium niobate actuator is disclosed comprising a cylindrical lead magnesium niobate crystal stack mounted in a cylindrical casing wherein a bias means, such as one or more belleville washers, is located between one end of the crystal stack and a partially closed end of the casing; and adjustment means are provided which bear against the opposite end of the crystal stack, whereby an adjustable compressive force is constantly applied against the crystal stack, whether the crystal stack is actuated in an extended position, or is in an unactuated contracted position. In a preferred embodiment, cooling ports are provided for the circulation of coolant in the actuator to cool the crystal stack, and provision is made for removal and replacement of the crystal stack without disconnecting the actuator from the external device being actuated. 3 figs.

Migration of Amphitheater-Headed Valleys in Kauai Basalts: Wailua Falls as a Case Example

NASA Astrophysics Data System (ADS)

Pederson, D. T.; Blay, C.

2006-12-01

Amphitheater-headed valleys in Kauai basalts migrate upstream primarily because of weathering processes. Basalt weathering rates are enhanced by the presence of water and/or vegetation. When both weathering process are present, weathering rates are greater than the sum of the two processes. Because waterfalls can create an environment where vegetation growth is greatly inhibited by the impact of falling water, weathering rates may be much greater on each side of the falls where vegetation can grow. Sources of water for weathering include groundwater discharge, waterfall spray, and condensation of atmospheric water. Because basalts weather rapidly in tropical environments, streams require only the capability to transport smaller particle sizes to sustain amphitheater migration. It should be noted that most waterfalls occupy only a small fraction of the amphitheater head which further supports weathering as the principal agent in amphitheater development and migration. Lava flows building shield volcanos are usually episodic with crystallization and possible weathering occurring before the next flow. The rate of cooling of a flow determines the crystal size of minerals and in combination with the magma chemistry the susceptibility of a flow to weathering process as well as the strength of the rock. With time, soils and topography will develop on the now crystallized flow. Because clays are a product of basalt weathering, soils when buried by later flows, represent low permeability layers. Additionally, new flows may follow (and bury) surface drainage systems resulting in localized thicker flows that cool more slowly and have different properties then the adjacent thinner flows. Consequently, most amphitheater heads have significant heterogenieties, especially in a vertical section representing multiple basalt flows. Wailua Falls on Kauai will be used as a field example of amphitheater weathering processes and migration.

Numerical and Experimental Studies of Transient Natural Convection with Density Inversion

NASA Astrophysics Data System (ADS)

Mizutani, Satoru; Ishiguro, Tatsuji; Kuwahara, Kunio

1996-11-01

In beer manufacturing process, we cool beer in storage tank down from 8 to -1 ^circC. The understanding of cooling process is very important for designing a fermentation tank. In this paper, flow and temperature distribution in a rectangular enclosure was studied. The unsteady incompressible Navier-Stokes equations were integrated by using the multi-directional third-order upwind finite difference method(MUFDM). A parabolic density-temperature relationship was assumed in water which has the maximum density at 3.98 ^circC. Cooling down from 8 to 0 ^circC of water in 10 cm cubical enclosure (Ra=10^7) was numerically done by keeping a vertical side wall at 0 ^circC. Vortex was caused by density inversion of water which was cooled bellow 4 ^circC, and it rose near the cold wall and reached water surface after 33 min from the start of cooling. Finally, cooling proceeded from upper surface. At the aim of verifing the accuracy of the numerical result, temperature distribution under the same condition was experimentally visualized using temperature sensitive liquid crystal. The results will be presented by using video movie. Comparison between the computation and the experiment showed that the present direct simulation based on the MUFDM was powerful tool for the understanding of the natural convection with density inversion and the application of cooling phenomenon to the design of beer storage tanks.

In situ crystallization and transformation kinetics of polymorphic forms of saturated-unsaturated-unsaturated triacylglycerols: 1-palmitoyl-2,3-dioleoyl glycerol, 1-stearoyl-2,3-dioleoyl glycerol, and 1-palmitoyl-2-oleoyl-3-linoleoyl glycerol.

PubMed

Bayés-García, L; Calvet, T; Cuevas-Diarte, M A; Ueno, S

2016-07-01

We examined the influence of dynamic thermal treatment (variation of cooling/heating rates) on the polymorphic crystallization and transformation pathways of 1-palmitoyl-2,3-dioleoyl glycerol (POO), 1-stearoyl-2,3-dioleoyl glycerol (SOO), and 1-palmitoyl-2-oleoyl-3-linoleoyl glycerol (POL), which are major saturated-unsaturated-unsaturated (SUU) triacylglycerols (TAGs) of vegetable oils and animal fats (e.g., palm oil, olive oil, and Iberian ham fat). Using mainly a combination of differential scanning calorimetry (DSC) and synchrotron radiation X-ray diffraction (SR-XRD), we analyzed the polymorphic behavior of TAGs when high (15°Cmin -1 ), intermediate (2°Cmin -1 ), and low (0.5°Cmin -1 ) cooling and heating rates were applied. Multiple polymorphic forms were detected in POO, SOO, and POL (sub-α, α, β' 2 , and β' 1 ). Transient disordered phases, defined as kinetic liquid crystal (KLC) phases, were determined in POO and SOO for the first time. The results demonstrated that more stable forms were directly obtained from the melt by decreasing the cooling rates, whereas less stable forms predominated at high cooling rates, as confirmed in our previous work. Regarding heating rate variation, we confirmed that the nature of the polymorphic transformations observed (solid-state, transformation through KLC phase, or melt-mediation) depended largely on the heating rate. These results were discussed considering the activation energies involved in each process and compared with previous studies on TAGs with different saturated-unsaturated structures (1,3-dioleoyl-2-palmitoylglycerol, 1,3-dipalmitoyl-2-oleoyl-glycerol, trioleoyl glycerol, and 1,2-dioleoyl-3-linoleoyl glycerol). Copyright © 2016 Elsevier Ltd. All rights reserved.

Interface Shape and Growth Rate Analysis of Se/GaAs Bulk Crystals Grown in the NASA Crystal Growth Furnace (CGF)

NASA Technical Reports Server (NTRS)

Bly, J. M.; Kaforey, M. L.; Matthiesen, D. H.; Chait, A.

1997-01-01

Selenium-doped gallium arsenide, Se/GaAs, bulk crystals have been grown on earth using NASA's crystal growth furnace (CGF) in preparation for microgravity experimentation on the USML-2 spacelab mission. Peltier cooling pulses of 50 ms duration, 2040 A magnitude, and 0.0033 Hz frequency were used to successfully demark the melt-solid interface at known times during the crystal growth process. Post-growth characterization included interface shape measurement, growth rate calculation, and growth rate transient determinations. It was found that the interface shapes were always slightly concave into the solid. The curvature of the seeding interfaces was typically 1.5 mm for the 15 mm diameter samples. This was in agreement with the predicted interface shapes and positions relative to the furnace determined using a numerical model of the sample/ampoule/cartridge assembly (SACA).

Hot Stuff? Thermal Imaging Applied to Cryocrystallography

NASA Technical Reports Server (NTRS)

Snell, E. H.

2004-01-01

In the past we have used thermal imaging techniques to visualize the cryocooling processes of macromolecular crystals. From these images it was clear that a cold wave progresses through a crystal starting at the face closest to the origin of the cold stream and ending at the point furthest away. During these studies we used large volume crystals, which were clearly distinguished fiom the loop holding them. These large crystals, originally grown for neutron diffiaction studies, were chosen deliberately to enhance the imaging. As an extension to this work, we present used thermal imaging to study small crystals, held in a cryo-loop, in the presence of vitrified mother liquor. The different d a r e d transmission and reflectance properties of the crystal in comparison to the mother liquor surrounding it are thought to be the parameter that produces the contrast that makes the crystal visible. An application of this technology may be the determination of the exact location of small crystals in a cryo-loop. Data fkom initial tests in support of application development was recorded for lysozyme crystals and for bFGF/dna complex crystals, which were cryocooled and imaged in large loops, both with visible light mad with h i k e d rdi&tion. The crystals were clearly distinguished from the vitrified solution in the infiared spectrum, while in the case of the bFGF/dna complex the illumination had to be carefully manipulated to make the crystal visible in the visible spectrum. These results suggest that the thermal imaging may be more sensitive than visual imaging for automated location of small crystals. However, further work on small crystals robotically mounted at SSRL did not clearly visualize those crystals. The depth of field of the camera proved to be limiting and a different cooling geometry was used, compared to the previous, successful experiments. Analysis to exploit multiple images to improve depth of field and experimental work to understand cooling geometry effects is ongoing. These results will be presented along with advantages and disadvantages of the technique and a discussion of how it might be applied.

Influence of Secondary Cooling Mode on Solidification Structure and Macro-segregation Behavior for High-carbon Continuous Casting Bloom

NASA Astrophysics Data System (ADS)

Dou, Kun; Yang, Zhenguo; Liu, Qing; Huang, Yunhua; Dong, Hongbiao

2017-07-01

A cellular automaton-finite element coupling model for high-carbon continuously cast bloom of GCr15 steel is established to simulate the solidification structure and to investigate the influence of different secondary cooling modes on characteristic parameters such as equiaxed crystal ratio, grain size and secondary dendrite arm spacing, in which the effect of phase transformation and electromagnetic stirring is taken into consideration. On this basis, evolution of carbon macro-segregation for GCr15 steel bloom is researched correspondingly via industrial tests. Based on above analysis, the relationship among secondary cooling modes, characteristic parameters for solidification structure as well as carbon macro-segregation is illustrated to obtain optimum secondary cooling strategy and alleviate carbon macro-segregation degree for GCr15 steel bloom in continuous casting process. The evaluating method for element macro-segregation is applicable in various steel types.

Scanning electron microscope view of iron crystal growing on pyroxene crystal

NASA Technical Reports Server (NTRS)

1972-01-01

A scanning electron microscope photograph of a four-micron size iron crystal growing on a pyroxene crystal (calcium-magnesium-iron silicate) from the Apollo 15 Hadley-Apennino lunar landing site. The well developed crystal faces indicate that the crystal was formed from a hot vapor as the rock was cooling.

Specific features of the structural and magnetic states of a Zn1 - x Ni x Se crystal ( x = 0.0025) at low temperatures

NASA Astrophysics Data System (ADS)

Dubinin, S. F.; Sokolov, V. I.; Parkhomenko, V. D.; Teploukhov, S. G.; Gruzdev, N. B.

2008-12-01

The magnetic state and the structure of a Zn1 - x Ni x Se ( x = 0.0025) bulk crystal were studied at low temperatures. It is revealed that the magnetic and crystal structures below T ≅ 15 K are dependent on the cooling rate of this dilute semiconductor. For example, on fast cooling to 4.2 K, about 10% hexagonal ferromagnetic phase is formed in the crystal. During heating, the phase disappears at T ≅ 15 K. The results obtained are discussed with allowance for the specific features of the Jahn-Teller distortions in this compound.

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

Sundaramurthi, Prakash; Patapoff, Thomas W.; Suryanarayanan, Raj

To study the crystallization of trehalose in frozen solutions and to understand the phase transitions during the entire freeze-drying cycle. Aqueous trehalose solution was cooled to -40 C in a custom-designed sample holder. The frozen solution was warmed to -18 C and annealed, and then dried in the sample chamber of the diffractometer. XRD patterns were continuously collected during cooling, annealing and drying. After cooling, hexagonal ice was the only crystalline phase observed. However, upon annealing, crystallization of trehalose dihydrate was evident. Seeding the frozen solution accelerated the solute crystallization. Thus, phase separation of the lyoprotectant was observed in frozenmore » solutions. During drying, dehydration of trehalose dihydrate yielded a substantially amorphous anhydrous trehalose. Crystallization of trehalose, as trehalose dihydrate, was observed in frozen solutions. The dehydration of the crystalline trehalose dihydrate to substantially amorphous anhydrate occurred during drying. Therefore, analyzing the final lyophile will not reveal crystallization of the lyoprotectant during freeze-drying. The lyoprotectant crystallization can only become evident by continuous monitoring of the system during the entire freeze-drying cycle. In light of the phase separation of trehalose in frozen solutions, its ability to serve as a lyoprotectant warrants further investigation.« less

The Effect Of Additional Detergent In Crude Palm Oil In The Process Of Separation Stearin

NASA Astrophysics Data System (ADS)

Rezekyah Hasibuan, Vina; aini, Nur; Febriyanti; Ayubi Pane, Salahudin Al

2018-03-01

This study aims to find out how much stearin is formed from the addition of detergent and to understand the process of separation of crude olein with crude stearin from raw material of crude palm oil (CPO). Using a detergent fractionation system, detergent fractionation is a continuous crystallization of oil with controlled cooling and the separation of fractions by weight or centrifuge after supplementing surfactant.

Hot Views on Cold Crystals: The Application of Thermal Imaging in Cryocrystallography

NASA Technical Reports Server (NTRS)

Snell, Eddie

2003-01-01

We have used thermal imaging techniques to visualize the cryocooling processes of macromolecular crystals. Cryocooling is a common technique used for structural data collection to reduce radiation damage in intense X-ray beams and decrease the thermal motion of the atoms. From the thermal images it was clear that during cryocooling a cold wave progresses through a crystal starting at the face closest to the origin of the cold stream and ending at the point furthest away. As an extension to this work, we used thermal imaging to study small crystals, held in a cryo-loop, in the presence of vitrified mother liquor. The different infrared transmission and reflectance properties of the crystal in comparison to the mother liquor surrounding it are thought to be the parameter that produces the contrast that makes the crystal visible. An application of this technology may be the determination of the exact location of small crystals in a cryo-loop for automated structural genomics studies. Data from initial tests in support of application development was recorded for lysozyme crystals and for bFGF/dna complex crystals, which were cryocooled and imaged in large loops, both with visible light and with infrared radiation. The crystals were clearly distinguished from the vitrified solution in the infrared spectrum, while in the case of the bFGF/dna complex the illumination had to be carefully manipulated to make the crystal visible in the visible spectrum. These results suggest that the thermal imaging may be more sensitive than visual imaging for automated location of small crystals. However, further work on small crystals robotically mounted at SSRL did not clearly visualize those crystals. The depth of field of the camera proved to be limiting and a different cooling geometry was used, compared to the previous, successful experiments. Analysis to exploit multiple images to improve depth of field and experimental work to understand cooling geometry effects is ongoing. These results will be presented along with advantages and disadvantages of the technique and a discussion of how it might be applied.

Numerical Simulation and Experimental Casting of Nickel-Based Single-Crystal Superalloys by HRS and LMC Directional Solidification Processes

NASA Astrophysics Data System (ADS)

Yan, Xuewei; Wang, Run'nan; Xu, Qingyan; Liu, Baicheng

2017-04-01

Mathematical models for dynamic heat radiation and convection boundary in directional solidification processes are established to simulate the temperature fields. Cellular automaton (CA) method and Kurz-Giovanola-Trivedi (KGT) growth model are used to describe nucleation and growth. Primary dendritic arm spacing (PDAS) and secondary dendritic arm spacing (SDAS) are calculated by the Ma-Sham (MS) and Furer-Wunderlin (FW) models respectively. The mushy zone shape is investigated based on the temperature fields, for both high-rate solidification (HRS) and liquid metal cooling (LMC) processes. The evolution of the microstructure and crystallographic orientation are analyzed by simulation and electron back-scattered diffraction (EBSD) technique, respectively. Comparison of the simulation results from PDAS and SDAS with experimental results reveals a good agreement with each other. The results show that LMC process can provide both dendritic refinement and superior performance for castings due to the increased cooling rate and thermal gradient.

Cation ordering in orthopyroxenes and cooling rates of meteorites: Low temperature cooling rates of Estherville, Bondoc and Shaw

NASA Technical Reports Server (NTRS)

Ganguly, J.; Yang, H.; Ghose, S.

1993-01-01

The cooling rates of meteorites provide important constraints on the size of their parent bodies, and their accretionary and evolutionary histories. However, the cooling rates obtained so far from the commonly used metallographic, radiometric and fission-track methods have been sometimes quite controversial, such as in the case of the mesosiderites and the meteorite Shaw. We have undertaken a systematic study of the cooling rates of meteorites using a different approach, which involves single crystal x-ray determination of Fe(2+)-Mg ordering in orthopyroxenes (OP(x)) in meteorites, subject to bulk compositional constraints, and numerical simulation of the evolution of the ordering state as a function of cooling rate, within the framework of the thermodynamic and kinetic principles governing cation ordering. We report the results obtained for OP(x) crystals from Shaw and two mesosiderites, Estherville and Bondoc.

Seeded growth of boron arsenide single crystals with high thermal conductivity

NASA Astrophysics Data System (ADS)

Tian, Fei; Song, Bai; Lv, Bing; Sun, Jingying; Huyan, Shuyuan; Wu, Qi; Mao, Jun; Ni, Yizhou; Ding, Zhiwei; Huberman, Samuel; Liu, Te-Huan; Chen, Gang; Chen, Shuo; Chu, Ching-Wu; Ren, Zhifeng

2018-01-01

Materials with high thermal conductivities are crucial to effectively cooling high-power-density electronic and optoelectronic devices. Recently, zinc-blende boron arsenide (BAs) has been predicted to have a very high thermal conductivity of over 2000 W m-1 K-1 at room temperature by first-principles calculations, rendering it a close competitor for diamond which holds the highest thermal conductivity among bulk materials. Experimental demonstration, however, has proved extremely challenging, especially in the preparation of large high quality single crystals. Although BAs crystals have been previously grown by chemical vapor transport (CVT), the growth process relies on spontaneous nucleation and results in small crystals with multiple grains and various defects. Here, we report a controllable CVT synthesis of large single BAs crystals (400-600 μm) by using carefully selected tiny BAs single crystals as seeds. We have obtained BAs single crystals with a thermal conductivity of 351 ± 21 W m-1 K-1 at room temperature, which is almost twice as conductive as previously reported BAs crystals. Further improvement along this direction is very likely.

Novel polypropylene/inorganic fullerene-like WS2 nanocomposites containing a β-nucleating agent: dynamic crystallization and melting behavior.

PubMed

Naffakh, Mohammed; Marco, Carlos; Ellis, Gary

2011-09-22

The dynamic crystallization and melting behavior of isotactic polypropylene-tungsten disulfide (iPP/IF-WS(2)) nanocomposites incorporating a β-nucleating agent is investigated by X-ray diffraction and differential scanning calorimetry. A conventional melt-processing strategy is employed to generate new materials that exhibit variable α and β polymorphism under the appropriate kinetic conditions. The results show that when the dual additive system is employed the nucleation ability on isotactic polypropylene not only depends on the nucleation efficiency (NE) and relative content of the individual α and β-nucleating agents, but also on the cooling rates employed. The nucleating behavior of the additives is explained by competitive nucleation, and the correlation between crystallization and melting temperatures and relative content of α and β-crystals of iPP in the nanocomposites is discussed.

Phase field model of the nanoscale evolution during the explosive crystallization phenomenon

NASA Astrophysics Data System (ADS)

Lombardo, S. F.; Boninelli, S.; Cristiano, F.; Deretzis, I.; Grimaldi, M. G.; Huet, K.; Napolitani, E.; La Magna, A.

2018-03-01

Explosive crystallization is a well known phenomenon occurring due to the thermodynamic instability of strongly under-cooled liquids, which is particularly relevant in pulsed laser annealing processes of amorphous semiconductor materials due to the globally exothermic amorphous-to-liquid-to-crystal transition pathway. In spite of the assessed understanding of this phenomenon, quantitative predictions of the material kinetics promoted by explosive crystallization are hardly achieved due to the lack of a consistent model able to simulate the concurrent kinetics of the amorphous-liquid and liquid-crystal interfaces. Here, we propose a multi-well phase-field model specifically suited for the simulation of explosive crystallization induced by pulsed laser irradiation in the nanosecond time scale. The numerical implementation of the model is robust despite the discontinuous jumps of the interface speed induced by the phenomenon. The predictive potential of the simulations is demonstrated by means of comparisons of the modelling predictions with experimental data in terms of in situ reflectivity measurements and ex-situ micro-structural and chemical characterization.

Enhancement radiative cooling performance of nanoparticle crystal via oxidation

NASA Astrophysics Data System (ADS)

Jia, Zi-Xun; Shuai, Yong; Li, Meng; Guo, Yanmin; Tan, He-ping

2018-03-01

Nanoparticle-crystal is a promising candidate for large scale metamaterial fabrication. However, in radiative cooling application, the maximum blackbody radiation wavelength locates far from metal's plasmon wavelength. In this paper, it will be shown if the metallic nanoparticle crystal can be properly oxidized, the absorption performance within room temperature blackbody radiation spectrum can be improved. Magnetic polariton and surface plasmon polariton have been explained for the mechanism of absorption improvement. Three different oxidation patterns have been investigated in this paper, and the results show they share a similar enhancing mechanism.

Structured laser gain-medium by new bonding for power micro-laser

NASA Astrophysics Data System (ADS)

Kausas, Arvydas; Zheng, Lihe; Taira, Takunori

2017-02-01

In this work, we have compared the Q-switched performance of single rod crystal to a newly developed distributed face cooling structure. This structure was made by surface activated bonding technology and allowed to combine transparent heatsink to a gain crystal at room temperature. The Sapphire and Nd3+:YAG crystal plates were combined in this fashion to produce eight crystal chip which was further used to obtain Q-switch pulses with Cr4+:YAG crystal as saturable absorber. Energy of 9 mJ and pulse duration of 815 ps were achieved. Although the energy obtained with single rod system was 10 mJ, the degradation of the beam prevents such crystal to be used in further applications. This is the first demonstration of distributed face cooling system outperformed conventionally single rod system.

Cooling and crystallization of rhyolite-obsidian lava: Insights from micron-scale projections on plagioclase microlites

NASA Astrophysics Data System (ADS)

Sano, Kyohei; Toramaru, Atsushi

2017-07-01

To reveal the cooling process of a rhyolite-obsidian flow, we studied the morphology of plagioclase microlites in the Tokachi-Ishizawa lava of Shirataki, northern Hokkaido, Japan, where the structure of the lava can be observed from obsidian at the base of the flow to the innermost rhyolite. Needle-like micron-scale textures, known as "projections", occur on the short side surfaces of the plagioclase microlites. Using FE-SEM we discovered a positive correlation between the lengths and spacings of these projections. On the basis of the instability theory of an interface between melt and crystal, and to understand the length and spacing data, we developed a model that explains the positive correlation and allows us to simultaneously estimate growth rates and growth times. Applying the model to our morphological data and the estimated growth rates and growth times, we suggest that the characteristics of the projections reflect the degree of undercooling, which in turn correlates with lava structure (the obsidian at the margin of the flow experienced a higher degree of undercooling than the interior rhyolite). The newly developed method provides insights into the degree of undercooling during the final stages of crystallization of a rhyolitic lava flow.

Crystallization phenomena in slags

NASA Astrophysics Data System (ADS)

Orrling, Carl Folke

2000-09-01

The crystallization of the mold slag affects both the heat transfer and the lubrication between the mold and the strand in continuous casting of steel. In order for mold slag design to become an engineering science rather than an empirical exercise, a fundamental understanding of the melting and solidification behavior of a slag must be developed. Thus it is necessary to be able to quantify the phenomena that occur under the thermal conditions that are found in the mold of a continuous caster. The double hot thermocouple technique (DHTT) and the Confocal Laser Scanning Microscope used in this study are two novel techniques for investigating melting and solidification phenomena of transparent slags. Results from these techniques are useful in defining the phenomena that occur when the slag film infiltrates between the mold and the shell of the casting. TTT diagrams were obtained for various slags and indicated that the onset of crystallization is a function of cooling rate and slag chemistry. Crystal morphology was found to be dependent upon the experimental temperature and four different morphologies were classified based upon the degree of melt undercooling. Continuous cooling experiments were carried out to develop CCT diagrams and it was found that the amount and appearance of the crystalline fraction greatly depends on the cooling conditions. The DHTT can also be used to mimic the cooling profile encountered by the slag in the mold of a continuous caster. In this differential cooling mode (DCT), it was found that the details of the cooling rate determine the actual response of the slag to a thermal gradient and small changes can lead to significantly different results. Crystal growth rates were measured and found to be in the range between 0.11 mum/s to 11.73 mum/s depending on temperature and slag chemistry. Alumina particles were found to be effective innoculants in oxide melts reducing the incubation time for the onset of crystallization and also extending the temperature range of observed crystallization. The effect of changing the gas atmosphere surrounding the sample has been studied. The presence of water vapor increased the nucleation rate and crystal growth rate significantly when compared to experiments carried out in a dry atmosphere. With an atmosphere of Argon and Argon-3% Hydrogen mixture, the incubation time for crystallization was increased with several minutes. The crystal growth rate in these atmospheres was also drastically reduced compared to an atmosphere of normal air. Significant numbers of bubbles were formed during the initial melting of mold slag samples and the melting rate of the slag was found to be related to the rate of bubble generation and to the rate of heat transport.

Screening and Characterization of Hydrate Forms of T-3256336, a Novel Inhibitor of Apoptosis (IAP) Protein Antagonist.

PubMed

Takeuchi, Shoko; Kojima, Takashi; Hashimoto, Kentaro; Saito, Bunnai; Sumi, Hiroyuki; Ishikawa, Tomoyasu; Ikeda, Yukihiro

2015-01-01

Different crystal packing of hydrates from anhydrate crystals leads to different physical properties, such as solubility and stability. Investigation of the potential of varied hydrate formation, and understanding the stability in an anhydrous/hydrate system, are crucial to prevent an undesired transition during the manufacturing process and storage. Only one anhydrous form of T-3256336, a novel inhibitor of apoptosis (IAP) protein antagonist, was discovered during synthesis, and no hydrate form has been identified. In this study, we conducted hydrate screening such as dynamic water vapor sorption/desorption (DVS), and the slurry experiment, and characterized the solid-state properties of anhydrous/hydrate forms to determine the most desirable crystalline form for development. New hydrate forms, both mono-hydrate and hemi-hydrate forms, were discovered as a result of this hydrate screening. The characterization of two new hydrate forms was conducted, and the anhydrous form was determined to be the most desirable development form of T-3256336 in terms of solid-state stability. In addition, the stability of the anhydrous form was investigated using the water content and temperature controlled slurry experiment to obtain the desirable crystal form in the crystallization process. The water content regions of the stable phase of the desired form, the anhydrous form, were identified for the cooling crystallization process.

Drift mobility of holes in phenanthrene single crystals

NASA Technical Reports Server (NTRS)

Sonnonstine, T. J.; Hermann, A. M.

1974-01-01

The temperature dependence of drift mobilities of holes in single crystals of phenanthrene was measured in the range from 203 to 353 K in three crystallographic directions. Below the anomaly temperature of 72 C, the mobility temperature dependences are consistent with the Munn and Siebrand slow-phonon hopping process in the b direction and the Munn and Siebrand slow-phonon coherent mode in the a and c prime directions. The drift mobility temperature dependences in crystals that have been cooled through the anomaly temperature in the presence of illumination and an electric field are consistent with the model of Spielberg et al. (1971), in which the hindered vibration of the 4,5 hydrogens introduces a new degree of freedom above 72 C.

Surface Alloying of SUS 321 Chromium-Nickel Steel by an Electron-Plasma Process

NASA Astrophysics Data System (ADS)

Ivanov, Yu. F.; Teresov, A. D.; Petrikova, E. A.; Krysina, O. V.; Ivanova, O. V.; Shugurov, V. V.; Moskvin, P. V.

2017-07-01

The mechanisms of forming nanostructured, nanophase layers are revealed and analyzed in austenitic steel subjected to surface alloying using an electron-plasma process. Nanostructured, nanophase layers up to 30 μm in thickness were formed by melting of the film/substrate system with an electron beam generated by a SOLO facility (Institute of High Current Electronics, SB RAS), Tomsk), which ensured crystallization and subsequent quenching at the cooling rates within the range 105-108 K/s. The surface was modified with structural stainless steel specimens (SUS 321 steel). The film/substrate system (film thickness 0.5 μm) was formed by a plasma-assisted vacuum-arc process by evaporating a cathode made from a sintered pseudoalloy of the following composition: Zr - 6 at.% Ti - 6 at.% Cu. The film deposition was performed in a QUINTA facility equipped with a PINK hot-cathode plasma source and DI-100 arc evaporators with accelerated cooling of the process cathode, which allowed reducing the size and fraction of the droplet phase in the deposited film. It is found that melting of the film/substrate system (Zr-Ti-Cu)/(SUS 321 steel) using a high-intensity pulsed electron beam followed by the high-rate crystallization is accompanied by the formation of α-iron cellular crystallization structure and precipitation of Cr2Zr, Cr3C2 and TiC particles on the cell boundaries, which as a whole allowed increasing microhardness by a factor of 1.3, Young's modulus - by a factor of 1.2, wear resistance - by a factor of 2.7, while achieving a three-fold reduction in the friction coefficient.

High-temperature crystallization of nanocrystals into three-dimensional superlattices.

PubMed

Wu, Liheng; Willis, Joshua J; McKay, Ian Salmon; Diroll, Benjamin T; Qin, Jian; Cargnello, Matteo; Tassone, Christopher J

2017-08-10

Crystallization of colloidal nanocrystals into superlattices represents a practical bottom-up process with which to create ordered metamaterials with emergent functionalities. With precise control over the size, shape and composition of individual nanocrystals, various single- and multi-component nanocrystal superlattices have been produced, the lattice structures and chemical compositions of which can be accurately engineered. Nanocrystal superlattices are typically prepared by carefully controlling the assembly process through solvent evaporation or destabilization or through DNA-guided crystallization. Slow solvent evaporation or cooling of nanocrystal solutions (over hours or days) is the key element for successful crystallization processes. Here we report the rapid growth (seconds) of micrometre-sized, face-centred-cubic, three-dimensional nanocrystal superlattices during colloidal synthesis at high temperatures (more than 230 degrees Celsius). Using in situ small-angle X-ray scattering, we observe continuous growth of individual nanocrystals within the lattices, which results in simultaneous lattice expansion and fine nanocrystal size control due to the superlattice templates. Thermodynamic models demonstrate that balanced attractive and repulsive interparticle interactions dictated by the ligand coverage on nanocrystal surfaces and nanocrystal core size are responsible for the crystallization process. The interparticle interactions can also be controlled to form different superlattice structures, such as hexagonal close-packed lattices. The rational assembly of various nanocrystal systems into novel materials is thus facilitated for both fundamental research and for practical applications in the fields of magnetics, electronics and catalysis.

High-temperature crystallization of nanocrystals into three-dimensional superlattices

NASA Astrophysics Data System (ADS)

Wu, Liheng; Willis, Joshua J.; McKay, Ian Salmon; Diroll, Benjamin T.; Qin, Jian; Cargnello, Matteo; Tassone, Christopher J.

2017-08-01

Crystallization of colloidal nanocrystals into superlattices represents a practical bottom-up process with which to create ordered metamaterials with emergent functionalities. With precise control over the size, shape and composition of individual nanocrystals, various single- and multi-component nanocrystal superlattices have been produced, the lattice structures and chemical compositions of which can be accurately engineered. Nanocrystal superlattices are typically prepared by carefully controlling the assembly process through solvent evaporation or destabilization or through DNA-guided crystallization. Slow solvent evaporation or cooling of nanocrystal solutions (over hours or days) is the key element for successful crystallization processes. Here we report the rapid growth (seconds) of micrometre-sized, face-centred-cubic, three-dimensional nanocrystal superlattices during colloidal synthesis at high temperatures (more than 230 degrees Celsius). Using in situ small-angle X-ray scattering, we observe continuous growth of individual nanocrystals within the lattices, which results in simultaneous lattice expansion and fine nanocrystal size control due to the superlattice templates. Thermodynamic models demonstrate that balanced attractive and repulsive interparticle interactions dictated by the ligand coverage on nanocrystal surfaces and nanocrystal core size are responsible for the crystallization process. The interparticle interactions can also be controlled to form different superlattice structures, such as hexagonal close-packed lattices. The rational assembly of various nanocrystal systems into novel materials is thus facilitated for both fundamental research and for practical applications in the fields of magnetics, electronics and catalysis.

Observations on the crystallization of spodumene from aqueous solutions in a hydrothermal diamond-anvil cell

USGS Publications Warehouse

Li, Jianking; Chou, I-Ming; Yuan, Shunda; Burruss, Robert A.

2013-01-01

Crystallization experiments were conducted in a new type of hydrothermal diamond-anvil cell (HDAC; type V) using LiAlSi2O6 (S) gel and H2O (W) as starting materials. A total of 21 experiments were performed at temperatures up to 950°C and pressures up to 788 MPa. In the samples with relatively low W/S ratios, many small crystals formed in the melt phase during cooling. In those with high W/S ratios, only a few crystals with smooth surfaces crystallized from the aqueous fluid in the presence of melt droplets, which were gradually consumed during crystal growth, indicating rapid transfer of material from the melt to the crystals through the aqueous fluid. The nucleation of crystals started at 710 (±70)°C and 520 (±80) MPa, and crystal growth ended at 570 (±40)°C and 320 (±90) MPa, with the cooling P-T path within the stability field of spodumene + quartz in the S-W system. The observed linear crystal growth rates in the aqueous phase, calculated by dividing the maximum length of a single crystal by the duration of the entire growth step, were 4.7 × 10−6 and 5.7 × 10−6 cm s−1 for the cooling rates of 0.5 and 1°C min−1, respectively. However, a rapid crystal growth rate of 3.6 × 10−5 cm s−1 in the aqueous fluid was observed when the components were supplied by nearby melt droplets. Our results show that when crystals nucleate in the aqueous fluid instead of the melt phase, there are fewer nuclei formed, and they grow much faster due to the low viscosity of the aqueous fluid, which accelerates diffusion of components for the growth of crystals. Therefore, the large crystals in granitic pegmatite can crystallize directly from aqueous fluids rather than hydrosilicate melt.

Sparsity-based image monitoring of crystal size distribution during crystallization

NASA Astrophysics Data System (ADS)

Liu, Tao; Huo, Yan; Ma, Cai Y.; Wang, Xue Z.

2017-07-01

To facilitate monitoring crystal size distribution (CSD) during a crystallization process by using an in-situ imaging system, a sparsity-based image analysis method is proposed for real-time implementation. To cope with image degradation arising from in-situ measurement subject to particle motion, solution turbulence, and uneven illumination background in the crystallizer, sparse representation of a real-time captured crystal image is developed based on using an in-situ image dictionary established in advance, such that the noise components in the captured image can be efficiently removed. Subsequently, the edges of a crystal shape in a captured image are determined in terms of the salience information defined from the denoised crystal images. These edges are used to derive a blur kernel for reconstruction of a denoised image. A non-blind deconvolution algorithm is given for the real-time reconstruction. Consequently, image segmentation can be easily performed for evaluation of CSD. The crystal image dictionary and blur kernels are timely updated in terms of the imaging conditions to improve the restoration efficiency. An experimental study on the cooling crystallization of α-type L-glutamic acid (LGA) is shown to demonstrate the effectiveness and merit of the proposed method.

Approaches to automated protein crystal harvesting

PubMed Central

Deller, Marc C.; Rupp, Bernhard

2014-01-01

The harvesting of protein crystals is almost always a necessary step in the determination of a protein structure using X-ray crystallographic techniques. However, protein crystals are usually fragile and susceptible to damage during the harvesting process. For this reason, protein crystal harvesting is the single step that remains entirely dependent on skilled human intervention. Automation has been implemented in the majority of other stages of the structure-determination pipeline, including cloning, expression, purification, crystallization and data collection. The gap in automation between crystallization and data collection results in a bottleneck in throughput and presents unfortunate opportunities for crystal damage. Several automated protein crystal harvesting systems have been developed, including systems utilizing microcapillaries, microtools, microgrippers, acoustic droplet ejection and optical traps. However, these systems have yet to be commonly deployed in the majority of crystallography laboratories owing to a variety of technical and cost-related issues. Automation of protein crystal harvesting remains essential for harnessing the full benefits of fourth-generation synchrotrons, free-electron lasers and microfocus beamlines. Furthermore, automation of protein crystal harvesting offers several benefits when compared with traditional manual approaches, including the ability to harvest microcrystals, improved flash-cooling procedures and increased throughput. PMID:24637746

Solid-state microrefrigerator

DOEpatents

Ullom, Joel N.

2003-06-24

A normal-insulator-superconductor (NIS) microrefrigerator in which a superconducting single crystal is both the substrate and the superconducting electrode of the NIS junction. The refrigerator consists of a large ultra-pure superconducting single crystal and a normal metal layer on top of the superconducting crystal, separated by a thin insulating layer. The superconducting crystal can be either cut from bulk material or grown as a thick epitaxial film. The large single superconducting crystal allows quasiparticles created in the superconducting crystal to easily diffuse away from the NIS junction through the lattice structure of the crystal to normal metal traps to prevent the quasiparticles from returning across the NIS junction. In comparison to thin film NIS refrigerators, the invention provides orders of magnitude larger cooling power than thin film microrefrigerators. The superconducting crystal can serve as the superconducting electrode for multiple NIS junctions to provide an array of microrefrigerators. The normal electrode can be extended and supported by microsupports to provide support and cooling of sensors or arrays of sensors.

Improved reproducibility of unit-cell parameters in macromolecular cryocrystallography by limiting dehydration during crystal mounting.

PubMed

Farley, Christopher; Burks, Geoffry; Siegert, Thomas; Juers, Douglas H

2014-08-01

In macromolecular cryocrystallography unit-cell parameters can have low reproducibility, limiting the effectiveness of combining data sets from multiple crystals and inhibiting the development of defined repeatable cooling protocols. Here, potential sources of unit-cell variation are investigated and crystal dehydration during loop-mounting is found to be an important factor. The amount of water lost by the unit cell depends on the crystal size, the loop size, the ambient relative humidity and the transfer distance to the cooling medium. To limit water loss during crystal mounting, a threefold strategy has been implemented. Firstly, crystal manipulations are performed in a humid environment similar to the humidity of the crystal-growth or soaking solution. Secondly, the looped crystal is transferred to a vial containing a small amount of the crystal soaking solution. Upon loop transfer, the vial is sealed, which allows transport of the crystal at its equilibrated humidity. Thirdly, the crystal loop is directly mounted from the vial into the cold gas stream. This strategy minimizes the exposure of the crystal to relatively low humidity ambient air, improves the reproducibility of low-temperature unit-cell parameters and offers some new approaches to crystal handling and cryoprotection.

Improved reproducibility of unit-cell parameters in macromolecular cryocrystallography by limiting dehydration during crystal mounting

PubMed Central

Farley, Christopher; Burks, Geoffry; Siegert, Thomas; Juers, Douglas H.

2014-01-01

In macromolecular cryocrystallography unit-cell parameters can have low reproducibility, limiting the effectiveness of combining data sets from multiple crystals and inhibiting the development of defined repeatable cooling protocols. Here, potential sources of unit-cell variation are investigated and crystal dehydration during loop-mounting is found to be an important factor. The amount of water lost by the unit cell depends on the crystal size, the loop size, the ambient relative humidity and the transfer distance to the cooling medium. To limit water loss during crystal mounting, a threefold strategy has been implemented. Firstly, crystal manipulations are performed in a humid environment similar to the humidity of the crystal-growth or soaking solution. Secondly, the looped crystal is transferred to a vial containing a small amount of the crystal soaking solution. Upon loop transfer, the vial is sealed, which allows transport of the crystal at its equilibrated humidity. Thirdly, the crystal loop is directly mounted from the vial into the cold gas stream. This strategy minimizes the exposure of the crystal to relatively low humidity ambient air, improves the reproducibility of low-temperature unit-cell parameters and offers some new approaches to crystal handling and cryoprotection. PMID:25084331

Petrographic Evidence for Rapid Heating and Cooling During Chrondrule Formation

NASA Technical Reports Server (NTRS)

Wasson, J. T.

2004-01-01

The chondrule cooling rates used in most chondrule-formation models appear to be too low. Recent petrographic evidence indicates that the amount of crystal (especially olivine) growth that occurred after the last melting event was about 30 smaller than the grain sizes simulated in order to estimate cooling rates. The smaller amount of growth leads to an upwards revision of cooling rates by about a factor of 1000. Most chondrules are porphyritic. They consist of large and small crystals of olivine and, less commonly, pyroxene immersed in a mesostasis having a plagioclase-rich composition. In the most primitive chondrites the mesostasis is often vitreous. Because the large majority of chondrules contain FeS, it is clear that the nebula had cooled below the FeS condensation temperature (ca. 650 K) before chondrule formation occurred. The high FeO/(FeO+MgO) ratios of some chondrules require still lower nebular temperatures (less than 500 K). The traditional view has been that porphyritic chondrules formed in a single heating/cooling event and many laboratory experiments have been carried out in various kinds of kinds of furnaces to try to simulate the formation of chondrules textures in a single heating/cooling cycle. These furnace experiments have been used to infer the cooling rates of chondrules during the temperature range at which olivine crystallized from the melt. Most of these inferred values are in the range 0.01-1 K per second. These low cooling rates are problematical because there is no long-term nebular environment that yields such values. In transparent regions chondrules would cool at rates orders of magnitude higher, whereas in an opaque nebular disk the cooling rates would be many orders of magnitude lower. And these latter conditions are not suitable locations for chondrule formation because such high temperatures would cause the complete evaporation of chondrules (which have melting temperatures about 600 K higher than their evaporation temperatures). During the last several years several kinds of petrographic evidence indicating rapid chondrule cooling have been recognized. These include thin overgrowths on relict grains, clusters of small crystals that grew following the most recent melting event, and fragments preserving shardlike shapes that would have been hidden had several tens of micrometers of new growth occurred following the last melting event. And there are other indications of rapid cooling including the preservation of volatiles such as FeS and one case where the modeling of O-isotopic and FeO/(FeO+MgO) gradients indicated a high cooling rate.

Cooling of a magmatic system under thermal chaotic mixing

NASA Astrophysics Data System (ADS)

Petrelli, Maurizio; El Omari, Kamal; Le Guer, Yves; Perugini, Diego

2015-04-01

The cooling of a melt undergoing chaotic advection is studied numerically for a magma with a temperature-dependent viscosity in a 2D cavity with moving boundary. Different statistical mixing and energy indicators are used to characterize the efficiency of cooling by thermal chaotic mixing. We show that different cooling rates can be obtained during the thermal mixing even of a single basaltic magmatic batch undergoing chaotic advection. This process can induce complex temperature patterns inside the magma chamber. The emergence of chaotic dynamics strongly affects the temperature field during time and greatly increases the cooling rates. This mechanism has implications for the lifetime of a magmatic body and may favor the appearance of chemical heterogeneities in igneous systems as a result of different crystallization rates. Results from this study also highlight that even a single magma batch can develop, under chaotic thermal advection, complex thermal and therefore compositional patterns resulting from different cooling rates, which can account for some natural features that, to date, have received unsatisfactory explanations. Among them, the production of magmatic enclaves showing completely different cooling histories compared with the host magma, compositional zoning in mineral phases, and the generation of large-scale compositionally zoning observed in many plutons worldwide.

The Effect of Post-heat Treatment on the Microstructures of Single Crystal DD6 Superalloy

NASA Astrophysics Data System (ADS)

Li, Dongfan; Gao, Hangshan; Wen, Zhixun; Li, Zhenwei; Yue, Zhufeng

2016-09-01

Various thermal cycles at the end of solution heat treatment and their influences on microstructure of single crystal superalloy DD6 were studied by experiments. During various thermal cycles, the qualitative and quantitative microstructure of samples quenched of the transformations is microscopically characterized. This completely includes the large changes in volume fraction, size distribution and morphology of gamma prime precipitate experienced in the upper temperature transformation. Noticeable deviation from the equilibrium volume fraction of γ' phase is detected in both the dissolution and precipitation processes above 1,120°C for both moderate cooling and heating rate; differences were mainly attributed to the unsteady nature of the turbulent flow. The growth and alignment of the γ' precipitates are deeply influenced by several factors, e.g. ageing time, cooling rate and quenching temperature. In addition, interesting findings such as "labyrinth" and "cluster" morphologies were observed by scanning electron microscope. During precipitation processes, the complicated microstructure evolution is illustrated by considering the consecutive equilibrium shapes of a coherent precipitate, which grows under the interaction with its neighbors and the coherency of the precipitates improves their potential to resist dissolution.

LD side-pumped Nd:YAG Q-switched laser without water cooling

NASA Astrophysics Data System (ADS)

Ling, Ming; Jin, Guang-yong; Tan, Xue-chun; Wu, Zhi-chao; Liang, Zhu

2009-07-01

A novel LD side-pumped Nd:YAG Q-switched solid-state laser, which made use of the special pumping strcture with conductive cooling instead of water cooling, was investigated.After selecting an appropriate length and diameter of Nd:YAG laser crystal rod and using three groups of laser diode centimeter bar which was composed by 12 laser diodes and uniformly arranged according to the angle of 120°,side-pumping structure of laser was accomplished.Adopting plano-concave resonator ,mending double end face of laser crystal and designing heat-stability resonator made the resonator steadily oscillate.Laser crystal rod which was tight fastened by copper net was conductively cooled and radiation block was furnished on the external of copper net for increasing the radiation capacity.High reflection gold film was plated on the cooling wall in the opposite way of pumping light, so that the laser crystal was uniformly pumped and the laser with low order mode output.Making the use of pillar lens focus and ray trace computing, reasonable parameters were caculated to couple pumping light to laser with high-efficiency.It was the electrooptic Q-switched which was made to be micro-integration eliminating voltage by KD*P crystal that improved the ratio between acting and unacting.Inner heat radiated from laser in good time with TE cooler and the laser ran at constant temperature with water cooling when the big external heat sink emanated a steady heat to periphery. Experiments revealed that the syetem pumping efficiency riseed by 18% and the laser threshold energy was 192 mJ under the condition of this novel pumping structure. The low mode output of 10-12ns pulse width and the maximum output energy of 98 mJ was achieved with an incident pump energy of 720 mJ in 1064nm.The optical-to-optical conversion efficiency was up to 13. 6 %,and the power instability in 24 h was better than +/-1. 7 %.

The application of interference fits for overcoming limitations in clamping methodologies for cryo-cooling first crystal configurations in x-ray monochromators

NASA Astrophysics Data System (ADS)

Stimson, J.; Docker, P.; Ward, M.; Kay, J.; Chapon, L.; Diaz-Moreno, S.

2017-12-01

The work detailed here describes how a novel approach has been applied to overcome the challenging task of cryo-cooling the first monochromator crystals of many of the world’s synchrotrons’ more challenging beam lines. The beam line configuration investigated in this work requires the crystal to diffract 15 Watts of 4-34 keV X-ray wavelength and dissipate the additional 485 watts of redundant X-ray power without significant deformation of the crystal surface. In this case the beam foot print is 25 mm by 25 mm on a crystal surface measuring 38 mm by 25 mm and maintain a radius of curvature of more than 50 km. Currently the crystal is clamped between two copper heat exchangers which have LN2 flowing through them. There are two conditions that must be met simultaneously in this scenario: the crystal needs to be clamped strongly enough to prevent the thermal deformation developing whilst being loose enough not to mechanically deform the diffracting surface. An additional source of error also occurs as the configuration is assembled by hand, leading to human error in the assembly procedure. This new approach explores making the first crystal cylindrical with a sleeve heat exchanger. By manufacturing the copper sleeve to be slightly larger than the silicon crystal at room temperature the sleeve can be slid over the silicon and when cooled will form an interference fit. This has the additional advantage that the crystal and its heat exchanger become a single entity and will always perform the same way each time it is used, eliminating error due to assembly. Various fits have been explored to investigate the associated crystal surface deformations under such a regime

Heat transfer analytical models for the rapid determination of cooling time in crystalline thermoplastic injection molding and experimental validation

NASA Astrophysics Data System (ADS)

Didier, Delaunay; Baptiste, Pignon; Nicolas, Boyard; Vincent, Sobotka

2018-05-01

Heat transfer during the cooling of a thermoplastic injected part directly affects the solidification of the polymer and consequently the quality of the part in term of mechanical properties, geometric tolerance and surface aspect. This paper proposes to mold designers a methodology based on analytical models to provide quickly the time to reach the ejection temperature depending of the temperature and the position of cooling channels. The obtained cooling time is the first step of the thermal conception of the mold. The presented methodology is dedicated to the determination of solidification time of a semi-crystalline polymer slab. It allows the calculation of the crystallization time of the part and is based on the analytical solution of the Stefan problem in a semi-infinite medium. The crystallization is then considered as a phase change with an effective crystallization temperature, which is obtained from Fast Scanning Calorimetry (FSC) results. The crystallization time is then corrected to take the finite thickness of the part into account. To check the accuracy of such approach, the solidification time is calculated by solving the heat conduction equation coupled to the crystallization kinetics of the polymer. The impact of the nature of the contact between the polymer and the mold is evaluated. The thermal contact resistance (TCR) appears as significant parameter that needs to be taken into account in the cooling time calculation. The results of the simplified model including or not TCR are compared in the case of a polypropylene (PP) with experiments carried out with an instrumented mold. Then, the methodology is applied for a part made with PolyEtherEtherKetone (PEEK).

Effect of hydrogen on deformation structure and properties of CMSX-2 nickel-base single-crystal superalloy

NASA Technical Reports Server (NTRS)

Dollar, M.; Bernstein, I. M.; Walston, S.; Prinz, F.; Domnanovich, A.

1987-01-01

Material used in this study was a heat of the alloy CMSX-2. This nickel-based superalloy was provided in the form of oriented single crystals, solutionized for 3 hrs at 1315 C. It was then usually heat treated as follows: 1050 C/16h/air cool + 850 C/48h/air cool. The resulting microstructure is dominated by cuboidal, ordered gamma precipitates with a volume fraction of about 75% and an average size of 0.5 microns. In brief, the most compelling hydrogen induced-changes in deformation structure are: (1) enhanced dislocation accumulation in the gamma matrix; and (2) more extensive cross-slip of superdislocations in the gamma precipitates. The enhanced dislocation density in gamma acts to decrease the mean free path of a superdislocation, while easier cross slip hinders superdislocation movement by providing pinning points in the form of sessile jobs. Both processes contribute to the increase of flow stress and the notable work hardening that occurs prior to fracture.

Inhomogeneities and superconductivity in poly-phase Fe-Se-Te systems

NASA Astrophysics Data System (ADS)

Hartwig, S.; Schäfer, N.; Schulze, M.; Landsgesell, S.; Abou-Ras, D.; Blum, Ch. G. F.; Wurmehl, S.; Sokolowski, A.; Büchner, B.; Prokeš, K.

2018-02-01

The impact of synthesis conditions, post-preparation heating procedure, aging and influence of pressure on the superconducting properties of FeSe0.4Te0.6 crystals is reported. Two FeSe0.4Te0.6 single crystals were used in the study, prepared from stoichiometric melt but cooled down with very different cooling rates, and investigated using magnetic bulk and electrical-resistivity methods. The fast-cooled crystal contains large inclusions of Fe3Se2.1Te1.8 and exhibits bulk superconductivity in its as-prepared state, while the other is homogeneous and shows only traces of superconductivity. AC susceptibility measurements under hydrostatic pressure show that the superconducting transition temperature of the inhomogeneous crystal increases from 12.3 K at ambient pressure to Tsc = 17.9 K at 9 kbar. On the other hand, neither pressure nor mechanically-induced stress is sufficient to induce superconductivity in the homogeneous crystal. However, an additional heat treatment at 673 K followed by fast cooling down and/or long-term aging at ambient conditions leads to the appearance of bulk superconductivity also in the latter sample. This sample remains homogeneous on a scale down to few μm but shows an additional magnetic phase transition around 130 K suggesting that it must be inhomogeneous. For comparison also Fe3Se2.1Te1.8 polycrystals have been prepared and their magnetic properties have been studied. It appears that this phase is not superconducting by itself. It is concluded that nano-scale inhomogeneities that appear in the FeSexTe1-x system due to a spinodal decomposition in the solid state are necessary for bulk superconductivity, possibly due to minor changes in the crystal structure and microstructure. Macroscopic inclusions quenched by fast cooling from high temperatures lead obviously to strain and hence variations in the lattice constants, an effect that is further supported by application of pressure/stress.

Crystallization-driven one-dimensional self-assembly of polyethylene-b-poly(tert-butylacrylate) diblock copolymers in DMF: effects of crystallization temperature and the corona-forming block.

PubMed

Fan, Bin; Liu, Lei; Li, Jun-Huan; Ke, Xi-Xian; Xu, Jun-Ting; Du, Bin-Yang; Fan, Zhi-Qiang

2016-01-07

Crystallization-driven self-assembly of polyethylene-b-poly(tert-butylacrylate) (PE-b-PtBA) block copolymers (BCPs) in N,N-dimethyl formamide (DMF) was studied. It is found that all three PE-b-PtBA BCPs used in this work can self-assemble into one-dimensional crystalline cylindrical micelles. When the BCP solution is cooled to crystallization temperature (Tc) from 130 °C, the seed micelles may be produced via two competitive processes in the initial period: stepwise micellization/crystallization and simultaneous crystallization/micellization. Subsequently, the seed micelles can undergo growth driven by the epitaxial crystallization of the unimers. The lengths of both the seed micelles and the grown micelles are longer for the BCP with a longer PtBA block at a higher Tc. Quasi-living growth of the PE-b-PtBA crystalline cylindrical micelles is achieved at a higher Tc. A longer PtBA block evidently retards the attachment of unimers to the crystalline micelles, leading to a slower growth rate.

Structure, dielectric and electric properties of diisobutylammonium hydrogen sulfate crystal

NASA Astrophysics Data System (ADS)

Bednarchuk, Tamara J.; Kinzhybalo, Vasyl; Markiewicz, Ewa; Hilczer, Bożena; Pietraszko, Adam

2018-02-01

Diisobutylammonium hydrogen sulfate, a new organic-inorganic hybrid compound, was successfully synthesized and three structural phases in 298-433 K temperature range were revealed by differential scanning calorimetry and X-ray powder diffraction studies. Single crystal X-ray diffraction data were used to describe the crystal structures in each particular case. In phase III (below 336/319 K on heating/cooling) the crystal arrangement appears to be within the triclinic symmetry with P-1 space group. During heating in the 336-339 K region (and 319-337 K on cooling) the crystal exists in the phase II, characterized by monoclinic symmetry with P21/c space group. Consequently, above 339 K (during heating, and 337 K during cooling temperature sequences), i.e. in phase I the crystal exhibits orthorhombic symmetry (Cmce space group). Ferroelastic domain structure was observed in phase III. These phase boundaries (III→II and II→I) were accompanied by the presence of small anomalies, apparent in the dielectric permittivity and electric conductivity experimental data. Fast proton transport with activation energy of 0.23 eV was observed in the high temperature phase I and related to phonon assisted proton diffusion conditioned by disorder of diisobutylammonium (diba) cations, as well as by high thermal displacements of oxygen and sulfur atoms of hydrogen sulfate anion (hs).

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.

Silica and Pyroxene in IVA Irons; Possible Formation of the IVA Magma by Impact Melting and Reduction of L-LL-Chondrite Materials Followed by Crystallization and Cooling

NASA Technical Reports Server (NTRS)

Wasson, John T.; Matsunami, Yoshiyuki; Rubin, Alan E.

2006-01-01

Group IVA is a large magmatic group of iron meteorites. The mean DELTA O-17 (= delta O-17 - 0.52(raised dot) delta O-18) of the silicates is approx. plus or minus 1.2%o, similar to the highest values in L chondrites and the lowest values in LL chondrites; delta O-18 values are also in the L/LL range. This strongly suggests that IVA irons formed by melting L-LL parental material, but the mean Ni content of IVA irons (83 mg/g) is much lower than that of a presumed L-LL parent (approx. 170 mg/g) and the low-Ca pyroxene present in two IVA meteorites is Fs13, much lower than the Fs20-29 values in L and LL chondrites. Thus, formation from L-LL precursors requires extensive addition of metallic Fe, probably produced by reduction of FeS and FeO. Group IVA also has S/Ni, Ga/Ni, and Ge/Ni ratios that are much lower than those in L-LL chondrites or any chondrite group that preserves nebular compositions, implying loss of these volatile elements during asteroidal processing. We suggest that these reduction and loss processes occurred near the surface of the asteroid during impact heating, and resulted partly from reduction by C, and partly from the thermal dissociation of FeS and FeO with loss of O and S. The hot (approx. 1770 K) low-viscosity melt quickly moved through channels in the porous asteroid to form a core. Two members of the IVA group, Sao Joao Nepomuceno (hereafter, SJN) and Steinbach, contain moderate amounts of orthopyroxene and silica, and minor amounts of low-Ca clinopyroxene. Even though SJN formed after approx. 26% crystallization and Steinbach formed after approx. 77% Crystallization of the IVA core, both could have originated within several tens of meters of the core-mantle interface if 99% of the crystallization occurred from the center outwards. Two other members of the group (Gibeon and Bishop Canyon) contain tabular tridymite, which we infer to have initially formed as veins deposited from a cooling SiO-rich vapor. The silicates were clearly introduced into IVA irons after the initial magma crystallized. Because the y-iron crystals in SJN are typically about 5 cm across, an order of magnitude smaller than in IVA irons that do not contain massive silicates, we infer that the metal was in the gamma-iron field when the silicates were injected. The SJN and Steinbach silicate compositions are near the low-Ca-pyroxene/silica eutectic compositions. We suggest that a tectonic event produced a eutectic-like liquid and injected it together with unmelted pyroxene grains into fissures in the solid metal core. Published estimates of IVA metallographic cooling rates range from 20 to 3000 K/Ma, leading to a hypothesized breakup of the core during a major impact followed by scrambling of the core and mantle debris [Haack, H., Scott, E.R.D., Love, S.G., Brearley, A. 1996. Thermal histories of IVA stony-iron and iron meteorites: evidence for asteroid fragmentation and reaccretion. Geochim. Cosmochim. Acta 60, 3103-3113]. This scrambling model is physically implausible and cannot explain the strong correlation of estimated cooling rates with metal composition. Previous workers concluded that the low-Ca clinopyroxene in SJN and Steinbach formed from protopyroxene by quenching at a cooling rate of 10(sup 12) K/Ma, and suggested that this also supported an impact-scrambling model. This implausible spike in cooling rate by a factor of 10(sup 10) can be avoided if the low-Ca clinopyroxene were formed by a late shock event that converted orthopyroxene to clinopyroxene followed by minimal growth in the clinopyroxene field, probably because melt was also produced. We suggest that metallographic cooling-rate estimates (e.g., based on island taenite) giving similar values throughout the metal compositional range are more plausible, and that the IVA parent asteroid can be modeled by monotonic cooling followed by a high-temperature impact event that introduced silicates into the metal and a low-temperature impact event that partially converted thopyroxene into low-Ca clinopyroxene.

Generation of ionizing radiation from lithium niobate crystals

NASA Astrophysics Data System (ADS)

Orlikov, L. N.; Orlikov, N. L.; Arestov, S. I.; Mambetova, K. M.; Shandarov, S. M.

2017-01-01

The work done experimentally explores generation of electron and x-ray radiation in the process of heating and cooling monolithic and iron-doped crystals of lithium niobate. Iron doping to the concentrations in the range of 1023 m3 was carried out by adding ferric oxide into the melt during the process of crystal growth. The research into radiation generation was performed at 1-10 Pa. The speed of heating from -10 to 1070 C was 10-20 degrees a minute. Current pulses appeared at 17, 38, 56, 94, 98, 100, 105, 106, 1070 C with the interval of 1-3 minutes. The obtained electron current increased in direct proportion to the crystal surface area. The maximum current was 3mA at the design voltage 11 kV on the crystal with 14,5x10,5x10 mm3 surface area. The article describes the possibility to control the start of generation by introducing priming pulse. The results achieved are explained by the domain repolarization while heating the crystal and the appearance of electric field local strength. Bias and overcharge currents contribute to the appearance of electric strength, which stimulates breakdown and plasma formation. X-ray radiation appears both at the stage of discharge formation and during electron deceleration on gas and target material.

Direct flow crystal growth system

DOEpatents

Montgomery, Kenneth E.; Milanovich, Fred P.

1992-01-01

A crystal is grown in a constantly filtered solution which is flowed directly into the growing face of a crystal. In a continuous flow system, solution at its saturation temperature is removed from a crystal growth tank, heated above its saturation temperature, filtered, cooled back to its saturation temperature, and returned to the tank.

Control of the conformations of ion Coulomb crystals in a Penning trap

PubMed Central

Mavadia, Sandeep; Goodwin, Joseph F.; Stutter, Graham; Bharadia, Shailen; Crick, Daniel R.; Segal, Daniel M.; Thompson, Richard C.

2013-01-01

Laser-cooled atomic ions form ordered structures in radiofrequency ion traps and in Penning traps. Here we demonstrate in a Penning trap the creation and manipulation of a wide variety of ion Coulomb crystals formed from small numbers of ions. The configuration can be changed from a linear string, through intermediate geometries, to a planar structure. The transition from a linear string to a zigzag geometry is observed for the first time in a Penning trap. The conformations of the crystals are set by the applied trap potential and the laser parameters, and agree with simulations. These simulations indicate that the rotation frequency of a small crystal is mainly determined by the laser parameters, independent of the number of ions and the axial confinement strength. This system has potential applications for quantum simulation, quantum information processing and tests of fundamental physics models from quantum field theory to cosmology. PMID:24096901

Zircon age-temperature-compositional spectra in plutonic rocks

DOE PAGES

Samperton, Kyle M.; Bell, Elizabeth A.; Barboni, Mélanie; ...

2017-08-23

We present that geochronology can resolve dispersed zircon dates in plutonic rocks when magma cooling time scales exceed the temporal precision of individual U-Pb analyses; such age heterogeneity may indicate protracted crystallization between the temperatures of zircon saturation (T sat) and rock solidification (T solid). Diffusive growth models predict asymmetric distributions of zircon dates and crystallization temperatures in a cooling magma, with volumetrically abundant old, hot crystallization at T sat decreasing continuously to volumetrically minor young, cold crystallization at T solid. We present integrated geochronological and geochemical data from Bergell Intrusion tonalites (Central Alps, Europe) that document zircon compositional changemore » over hundreds of thousands of years at the hand-sample scale, indicating melt compositional evolution during solidification. Ti-in-zircon thermometry, crystallization simulation using MELTS software, and U-Pb dates produce zircon mass-temperature-time distributions that are in excellent agreement with zircon growth models. In conclusion, these findings provide the first quantitative validation of longstanding expectations from zircon saturation theory by direct geochronological investigation, underscoring zircon’s capacity to quantify supersolidus cooling rates in magmas and resolve dynamic differentiation histories in the plutonic rock record.« less

Zircon age-temperature-compositional spectra in plutonic rocks

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

Samperton, Kyle M.; Bell, Elizabeth A.; Barboni, Mélanie

We present that geochronology can resolve dispersed zircon dates in plutonic rocks when magma cooling time scales exceed the temporal precision of individual U-Pb analyses; such age heterogeneity may indicate protracted crystallization between the temperatures of zircon saturation (T sat) and rock solidification (T solid). Diffusive growth models predict asymmetric distributions of zircon dates and crystallization temperatures in a cooling magma, with volumetrically abundant old, hot crystallization at T sat decreasing continuously to volumetrically minor young, cold crystallization at T solid. We present integrated geochronological and geochemical data from Bergell Intrusion tonalites (Central Alps, Europe) that document zircon compositional changemore » over hundreds of thousands of years at the hand-sample scale, indicating melt compositional evolution during solidification. Ti-in-zircon thermometry, crystallization simulation using MELTS software, and U-Pb dates produce zircon mass-temperature-time distributions that are in excellent agreement with zircon growth models. In conclusion, these findings provide the first quantitative validation of longstanding expectations from zircon saturation theory by direct geochronological investigation, underscoring zircon’s capacity to quantify supersolidus cooling rates in magmas and resolve dynamic differentiation histories in the plutonic rock record.« less

Thermal and structural behavior of anhydrous milk fat. 3. Influence of cooling rate.

PubMed

Lopez, C; Lesieur, P; Bourgaux, C; Ollivon, M

2005-02-01

The crystallization behavior of anhydrous milk fat has been examined with a new instrument coupling time-resolved synchrotron x-ray diffraction as a function of temperature (XRDT) at both small and wide angles and high-sensitivity differential scanning calorimetry. Crystallizations were monitored at cooling rates of 3 and 1 degrees C/ min from 60 to -10 degrees C to determine the triacylglycerol organizations formed. Simultaneous thermal analysis permitted the correlation of the formation/melting of the different crystalline species monitored by XRDT to the thermal events recorded by differential scanning calorimetry. At intermediate cooling rates, milk fat triacylglycerols sequentially crystallize in 3 different lamellar structures with double-chain length of 46 and 38.5 A and a triple-chain length of 72 A stackings of alpha type, which are correlated to 2 exothermic peaks at 17.2 and 13.7 degrees C, respectively. A time-dependent slow sub-alpha <--> alpha reversible transition is observed at -10 degrees C. Subsequent heating at 2 degrees C/min has shown numerous structural rearrangements of the alpha varieties into a single beta' form before final melting. This polymorphic evolution on heating, as well as the final melting point observed (approximately 39 degrees C), confirmed that cooling at 3 degrees C/min leads to the formation of crystalline varieties that are not at equilibrium. An overall comparison of the thermal and structural properties of the crystalline species formed as a function of the cooling rate and stabilization time is presented. The influence on crystal size of the cooling rates applied in situ using temperature-controlled polarized microscopy is also determined for comparison.

Modification of defects and potential fluctuations in slow-cooled and quenched Cu2ZnSnSe4 single crystals

NASA Astrophysics Data System (ADS)

Bishop, Douglas M.; McCandless, Brian; Gershon, Talia; Lloyd, Michael A.; Haight, Richard; Birkmire, Robert

2017-02-01

Recent literature reports have shown the ability to manipulate Cu-Zn cation ordering for Cu2ZnSnSe4 (CZTSe) via low temperature treatments. Theoretical arguments suggest that one of the major roadblocks to higher VOC—significant band tailing—could be improved with increased cation order; however, few direct measurements have been reported and significant device improvements have not yet been realized. This report investigates electrical properties, defects, and devices from quenched and slow-cooled single crystals of CZTSe. The extent of disorder was characterized by Raman spectroscopy as well as x-ray diffraction, where the change in Cu-Zn order can be detected by a changing c/a ratio. Quenched samples show higher acceptor concentrations, lower hole mobilities, and a lower-energy photoluminescence (PL) peak than crystals cooled at slower rates, consistent with a reduction in the bandgap. In addition, samples quenched at the highest temperatures showed lower PL yield consistent with higher quantities of deep defects. Devices fabricated using slow-cooled CZTSe single crystals showed improved efficiencies, most notably with increased VOC; however, low temperature intensity-dependent photoluminescence measurements continue to indicate the existence of potential fluctuations. We discuss the possibility that potential fluctuations in slow-cooled samples may be related to the inability to achieve a long range order of the Cu-Zn sub-lattice resulting in local regions of high and low levels of cation order, and consequent local variations in the bandgap. The presence of significant potential fluctuations, even after the slow-cooling step, suggests the difficulty in eliminating band-tailing in this system, and thus, additional approaches may be needed for significant reduction of the VOC deficit.

Inhibition of calcium carbonate crystal growth by organic additives using the constant composition method in conditions of recirculating cooling circuits

NASA Astrophysics Data System (ADS)

Chhim, Norinda; Kharbachi, Chams; Neveux, Thibaut; Bouteleux, Céline; Teychené, Sébastien; Biscans, Béatrice

2017-08-01

The cooling circuits used in power plants are subject to mineral crystallization which can cause scaling on the surfaces of equipment and construction materials reducing their heat exchange efficiency. Precipitated calcium carbonate is the predominant mineral scale commonly observed in cooling systems. Supersaturation is the key parameter controlling the nucleation and growth of calcite in these systems. The present work focuses on the precipitation of calcite using the constant composition method at constant supersaturation, through controlled addition of reactants to a semi-batch crystallizer, in order to maintain constant solution pH. The determination of the thermodynamic driving force (supersaturation) was based on the relevant chemical equilibria, total alkalinity and calculation of the activity coefficients. Calcite crystallization rates were derived from the experiments performed at supersaturation levels similar to those found in industrial station cooling circuits. Several types of seeds particles were added into the aqueous solution to mimic natural river water conditions in terms of suspended particulate matters content, typically: calcite, silica or illite particles. The effect of citric and copolycarboxylic additive inhibitors added to the aqueous solution was studied. The calcium carbonate growth rate was reduced by 38.6% in the presence of the citric additive and a reduction of 92.7% was observed when the copolycarboxylic additive was used under identical experimental conditions. These results are explained by the location of the adsorbed inhibitor at the crystal surface and by the degree of chemical bonding to the surface.

Melt extraction during heating and cooling of felsic crystal mushes in shallow volcanic systems: An experimental study

NASA Astrophysics Data System (ADS)

Pistone, M.; Baumgartner, L. P.; Sisson, T. W.; Bloch, E. M.

2017-12-01

The dynamics and kinetics of melt extraction in near-solidus, rheologically stalled, felsic crystal mushes (> 50 vol.% crystals) are essential to feeding many volcanic eruptions. At shallow depths (< 15 km), most felsic crystal mushes would be volatile-saturated and may be thermally stable for long time periods (104-107 years). In absence of deformation, residual melt can segregate from the mush's crystalline framework stimulated by: 1) gas injecting from hot mafic magmas into felsic mushes (heating / partial melting scenario), and 2) gas exsolving from the crystallizing mush (cooling / crystallizing scenario). The conditions and efficiency of melt extraction from a mush in the two scenarios are not well understood. Thus, we conducted high-temperature (700 to 850 °C) and -pressure (1.1 kbar) cold seal experiments (8-day duration) on synthetic felsic mushes, composed of water-saturated (4.2 wt.%) rhyodacite melt bearing different proportions of added quartz crystals (60, 70, and 80 vol%; 68 mm average particle size). High-spatial resolution X-ray tomography of run products show: 1) in the heating scenario (> 750 °C) melt has not segregated due to coalescence of vesicles (≤ 23 vol%) and large melt connectivity (> 7 vol% glass) / low pressure gradient for melt movement up to 80 vol% crystals; 2) in the cooling scenario (≤ 750 °C) vesicle (< 11 vol%) coalescence is limited or absent and limited amount of melt (3 to 11 vol%) segregated from sample center to its outer periphery (30 to 100 mm melt-rich lenses), testifying to the efficiency of melt extraction dictated by increasing crystallinity. These results suggest that silicic melt hosted within a crystal-rich mush can accumulate rapidly due to the buildup of modest gas pressures during crystallization at temperatures near the solidus.

Characteristic Time Scales of Characteristic Magmatic Processes and Systems

NASA Astrophysics Data System (ADS)

Marsh, B. D.

2004-05-01

Every specific magmatic process, regardless of spatial scale, has an associated characteristic time scale. Time scales associated with crystals alone are rates of growth, dissolution, settling, aggregation, annealing, and nucleation, among others. At the other extreme are the time scales associated with the dynamics of the entire magmatic system. These can be separated into two groups: those associated with system genetics (e.g., the production and transport of magma, establishment of the magmatic system) and those due to physical characteristics of the established system (e.g., wall rock failure, solidification front propagation and instability, porous flow). The detailed geometry of a specific magmatic system is particularly important to appreciate; although generic systems are useful, care must be taken to make model systems as absolutely realistic as possible. Fuzzy models produce fuzzy science. Knowledge of specific time scales is not necessarily useful or meaningful unless the hierarchical context of the time scales for a realistic magmatic system is appreciated. The age of a specific phenocryst or ensemble of phenocrysts, as determined from isotopic or CSD studies, is not meaningful unless something can be ascertained of the provenance of the crystals. For example, crystal size multiplied by growth rate gives a meaningful crystal age only if it is from a part of the system that has experienced semi-monotonic cooling prior to chilling; crystals entrained from a long-standing cumulate bed that were mechanically sorted in ascending magma may not reveal this history. Ragged old crystals rolling about in the system for untold numbers of flushing times record specious process times, telling more about the noise in the system than the life of typical, first generation crystallization processes. The most helpful process-related time scales are those that are known well and that bound or define the temporal style of the system. Perhaps the most valuable of these times comes from the observed durations and rates of volcanism. There can be little doubt that the temporal styles of volcanism are the same as those of magmatism in general. Volcano repose times, periodicity, eruptive fluxes, acoustic emission structures, lava volumes, longevity, etc. must also be characteristic of pluton-dominated systems. We must therefore give up some classical concepts (e.g., instantaneous injection of crystal-free magma as an initial condition) for any plutonic/chambered system and move towards an integrated concept of magmatism. Among the host of process-related time scales, probably the three most fundamental of any magmatic system are (1) the time scale associated with crystal nucleation (J) and growth (G) (tx}=C{1(G3 J)-{1}/4; Zieg & Marsh, J. Pet. 02') along with the associated scales for mean crystal size (L) and population (N), (2) the time scale associated with conductive cooling controlled by a local length scale (d) (tc}=C{2 d2/K; K is thermal diffusivity), and (3) the time scale associated with intra-crystal diffusion (td}=C{3 L2/D; D is chemical diffusivity). It is the subtle, clever, and insightful application of time scales, dovetailed with realistic system geometry and attention paid to the analogous time scales of volcanism, that promises to reveal the true dynamic integration of magmatic systems.

Crystallization Conditions at Cascade and Other Arc Volcanoes: The Role of Recharge, and Ultimate, Proximal and Immediate Causes of Eruption

NASA Astrophysics Data System (ADS)

Putirka, K. D.

2016-12-01

A number of hypotheses have been offered to explain why volcanoes erupt. These include magma mixing, mafic recharge, or partial crystallization, any of which can drive parts or all of a system to vapor saturation, and so add to a magma's buoyancy. Age dates indicate long pre-eruption storage times for felsic magmas erupted at arcs, indicating that mafic recharge magmas, which can reinvigorate such systems, is a possible eruption trigger. However, plutonic systems reveal numerous recharge events that have no obvious ties to eruption (Coint et al. 2013; Putirka et al. 2014). And crystallization conditions at some arc systems support the implicit view, that recharge might be a necessary, but not a sufficient condition for eruption. At several Cascade volcanoes, Cpx and Amp crystals record coolings of 100-300oC. The Cpx grains derive exclusively from mafic enclaves, while Amp grains derive from both host and enclave materials. These considerable coolings call for a time lag following recharge, and indicate that vapor saturation is a proximal, although not necessarily an immediate cause of eruption. But we cannot discount recharge altogether. At the Cascades and at other arcs, Cpx crystalizes throughout the middle and upper crust, mostly from the surface down to 15 km. And high Fo olivine grains provide evidence for very hot magmas that intrude the upper mantle and lower crust, and possibly the middle crust, if hydrous. Volcanic pathways thus clearly extend into the middle crust, and at times, well below the Moho. It is unclear to what extent these deep pathways are hydraulically connected to the surface, or the role of deep-seated processes in initiating or sustaining eruptions. Progress in understanding these pathways, and triggering mechanisms, requires our differentiating "ultimate", "proximal" and "immediate" causes, and determining which of various magmatic processes provide necessary or sufficient conditions for eruption.

Microgravity

NASA Image and Video Library

1995-09-15

Large Isothermal Furnace (LIF) was flown on a mission in cooperation with the National Space Development Agency (NASDA) of Japan. LIF is a vacuum-heating furnace designed to heat large samples uniformly. The furnace consists of a sample container and heating element surrounded by a vacuum chamber. A crewmemeber will insert a sample cartridge into the furnace. The furnace will be activated and operations will be controlled automatically by a computer in response to an experiment number entered on the control panel. At the end of operations, helium will be discharged into the furnace, allowing cooling to start. Cooling will occur through the use of a water jacket while rapid cooling of samples can be accomplished through a controlled flow of helium. Data from experiments will help scientists better understand this important process which is vital to the production of high-quality semiconductor crystals.

PRODUCTION OF PURIFIED URANIUM

DOEpatents

Burris, L. Jr.; Knighton, J.B.; Feder, H.M.

1960-01-26

A pyrometallurgical method for processing nuclear reactor fuel elements containing uranium and fission products and for reducing uranium compound; to metallic uranium is reported. If the material proccssed is essentially metallic uranium, it is dissolved in zinc, the sulution is cooled to crystallize UZn/sub 9/ , and the UZn/sub 9/ is distilled to obtain uranium free of fission products. If the material processed is a uranium compound, the sollvent is an alloy of zinc and magnesium and the remaining steps are the same.

Interplay between Long-Range Crystal Order and Short-Range Molecular Interactions Tunes Carrier Mobility in Liquid Crystal Dyes

PubMed Central

2017-01-01

We investigated the influence of molecular packing on the optical and electrical properties of the liquid crystalline dye 4,7-bis[5-(2-fluoro-4-pentyl-phenyl)-2-thienyl]-2,1,3-benzothiadiazole (FPPTB). FPPTB is crystalline at room temperature, exhibits a nematic phase at temperatures above 149 °C and is in an isotropic melt at temperatures above 230 °C. Solution processed FPPTB films were subject to thermal annealing through these phase transition temperatures and characterized with X-ray diffraction and polarized optical microscopy. Cooling FPPTB films from the nematic and isotropic phases increased crystal domain size, but also induced local structural variations in the molecular packing of crystalline FPPTB. The decrease in long-range order was correlated with an increase in short-range π–π interactions, leading to changes in molecular aggregation which persisted even when the FPPTB films were cooled to room temperature. Annealing-induced changes in molecular aggregation were confirmed with optical spectroscopy. The carrier mobility in FPPTB films increased over 2 orders of magnitude from (2.2 ± 0.4) × 10–5 cm2 V–1 s–1 in as-spun films to μ = (5.0 ± 0.8) × 10–3 cm2 V–1 s–1 in films cooled from the isotropic melt. We discuss the relationship between thermal stability and high carrier mobility values in terms of the interplay between long-range molecular order and increased π–π interactions between molecular pairs in the FPPTB film. PMID:28139915

Direct observation of mineral–organic composite formation reveals occlusion mechanism

DOE PAGES

Cho, Kang Rae; Kim, Yi -Yeoun; Yang, Pengcheng; ...

2016-01-06

Manipulation of inorganic materials with organic macromolecules enables organisms to create biominerals such as bones and seashells, where occlusion of biomacromolecules within individual crystals generates superior mechanical properties. Current understanding of this process largely comes from studying the entrapment of micron-size particles in cooling melts. Here, by investigating micelle incorporation in calcite with atomic force microscopy and micromechanical simulations, we show that different mechanisms govern nanoscale occlusion. By simultaneously visualizing the micelles and propagating step edges, we demonstrate that the micelles experience significant compression during occlusion, which is accompanied by cavity formation. This generates local lattice strain, leading to enhancedmore » mechanical properties. Furthermore, these results give new insight into the formation of occlusions in natural and synthetic crystals, and will facilitate the synthesis of multifunctional nanocomposite crystals.« less

Anisotropy in the Ratchet Growth of PBX 9502

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

Schwarz, Ricardo Blum; Liu, Cheng; Thompson, Darla Graff

2015-03-12

TATB-based compactions and composites are known to undergo “ratchet growth”, an irreversible volume increase that occurs upon heating or cooling of a specimen. Ratchet growth likely arises because the coefficient of thermal expansion of the TATB crystals is strongly anisotropic, but the exact mechanism is not well-understood. TATB crystals in solid, plastic-bonded, explosive PBX 9502 parts can have a preferred crystallographic orientation (texture) caused by the compaction process. As a result, the irreversible strain associated with PBX 9502 ratchet growth is anisotropic. The present paper relates the magnitude of ratchet growth to the crystalline anisotropy of the TATB crystals. Themore » crystalline anisotropy is measured by x-ray diffraction and the ratchet growth is measured by a digital image-correlation technique.« less

Challenges for Synchrotron X-Ray Optics

NASA Astrophysics Data System (ADS)

Freund, Andreas K.

2002-12-01

It is the task of x-ray optics to adapt the raw beam generated by modern sources such as synchrotron storage rings to a great variety of experimental requirements in terms of intensity, spot size, polarization and other parameters. The very high quality of synchrotron radiation (source size of a few microns and beam divergence of a few micro-radians) and the extreme x-ray flux (power of several hundred Watts in a few square mm) make this task quite difficult. In particular the heat load aspect is very important in the conditioning process of the brute x-ray power to make it suitable for being used on the experimental stations. Cryogenically cooled silicon crystals and water-cooled diamond crystals can presently fulfill this task, but limits will soon be reached and new schemes and materials must be envisioned. A major tendency of instrument improvement has always been to concentrate more photons into a smaller spot utilizing a whole variety of focusing devices such as Fresnel zone plates, refractive lenses and systems based on bent surfaces, for example, Kirkpatrick-Baez systems. Apart from the resistance of the sample, the ultimate limits are determined by the source size and strength on one side, by materials properties, cooling, mounting and bending schemes on the other side, and fundamentally by the diffraction process. There is also the important aspect of coherence that can be both a nuisance and a blessing for the experiments, in particular for imaging techniques. Its conservation puts additional constraints on the quality of the optical elements. The overview of the present challenges includes the properties of present and also mentions aspects of future x-ray sources such as the "ultimate" storage ring and free electron lasers. These challenges range from the thermal performances of monochromators to the surface quality of mirrors, from coherence preservation of modern multilayers to short pulse preservation by crystals, and from micro- and nano-focusing techniques to the accuracy and stability of mechanical supports.

Modeling the Bergeron-Findeisen Process Using PDF Methods With an Explicit Representation of Mixing

NASA Astrophysics Data System (ADS)

Jeffery, C.; Reisner, J.

2005-12-01

Currently, the accurate prediction of cloud droplet and ice crystal number concentration in cloud resolving, numerical weather prediction and climate models is a formidable challenge. The Bergeron-Findeisen process in which ice crystals grow by vapor deposition at the expense of super-cooled droplets is expected to be inhomogeneous in nature--some droplets will evaporate completely in centimeter-scale filaments of sub-saturated air during turbulent mixing while others remain unchanged [Baker et al., QJRMS, 1980]--and is unresolved at even cloud-resolving scales. Despite the large body of observational evidence in support of the inhomogeneous mixing process affecting cloud droplet number [most recently, Brenguier et al., JAS, 2000], it is poorly understood and has yet to be parameterized and incorporated into a numerical model. In this talk, we investigate the Bergeron-Findeisen process using a new approach based on simulations of the probability density function (PDF) of relative humidity during turbulent mixing. PDF methods offer a key advantage over Eulerian (spatial) models of cloud mixing and evaporation: the low probability (cm-scale) filaments of entrained air are explicitly resolved (in probability space) during the mixing event even though their spatial shape, size and location remain unknown. Our PDF approach reveals the following features of the inhomogeneous mixing process during the isobaric turbulent mixing of two parcels containing super-cooled water and ice, respectively: (1) The scavenging of super-cooled droplets is inhomogeneous in nature; some droplets evaporate completely at early times while others remain unchanged. (2) The degree of total droplet evaporation during the initial mixing period depends linearly on the mixing fractions of the two parcels and logarithmically on Damköhler number (Da)---the ratio of turbulent to evaporative time-scales. (3) Our simulations predict that the PDF of Lagrangian (time-integrated) subsaturation (S) goes as S-1 at high Da. This behavior results from a Gaussian mixing closure and requires observational validation.

Kinetics of Nucleation and Crystal Growth in Glass Forming Melts in Microgravity

NASA Technical Reports Server (NTRS)

Day, Delbert E.; Ray, Chandra S.

2001-01-01

This flight definition project has the specific objective of investigating the kinetics of nucleation and crystal growth in high temperature inorganic oxide, glass forming melts in microgravity. It is related to one of our previous NASA projects that was concerned with glass formation for high temperature containerless melts in microgravity. The previous work culminated in two experiments which were conducted aboard the space shuttle in 1983 and 1985 and which consisted of melting (at 1500 C) and cooling levitated 6 to 8 mm diameter spherical samples in a Single Axis Acoustic Levitator (SAAL) furnace. Compared to other types of materials, there have been relatively few experiments, 6 to 8, conducted on inorganic glasses in space. These experiments have been concerned with mass transport (alkali diffusion), containerless melting, critical cooling rate for glass formation, chemical homogeneity, fiber pulling, and crystallization of glass forming melts. One of the most important and consistent findings in all of these experiments has been that the glasses prepared in microgravity are more resistant to crystallization (better glass former) and more chemically homogeneous than equivalent glasses made on Earth (1 g). The chemical composition of the melt appears relatively unimportant since the same general results have been reported for oxide, fluoride and chalcogenide melts. These results for space-processed glasses have important implications, since glasses with a higher resistance to crystallization or higher chemical homogeneity than those attainable on Earth can significantly advance applications in areas such as fiber optics communications, high power laser glasses, and other photonic devices where glasses are the key functional materials.

Transient Self-assembly of Edible Lipids During Crystallization

NASA Astrophysics Data System (ADS)

Mazzanti, Gianfranco; Marangoni, Alejandro; Idziak, Stefan

2002-03-01

The effects of cooling rate and shear on the structure and crystallization behavior of two natural triglyceride melts were studied using rheology and light scattering. A transparent Couette Cell with 1 mm gap was used to perform light scattering measurements. A rheometer with concentric cylinders with 1 mm gap was used for the rheological tests. Experiments were carried out at cooling rates of 3 and 0.5 C/min from the 45 C melt down to temperatures between 17.5 C and 30 C. The shear rates imposed were 90 and 1440 s-1. Results show that the effect of shear on the onset of crystallization is especially evident at slow cooling rates. The effect of shear on crystalline phase growth is more pronounced at higher temperatures and slow cooling rates. Quasi-stationary studies were carried out in the rheometer operated in a controlled stress oscillatory mode, and strain amplitudes were less than 2experiments were performed in a petroleum analyzer and in a glass capillary. The onset of light scattering coincides with an unexpected transient increase in the amplitude of the oscillatory response.

A metallurgical route to solar-grade silicon

NASA Technical Reports Server (NTRS)

Schei, A.

1986-01-01

The aim of the process is to produce silicon for crystallization into ingots that can be sliced to wafers for processing into photovoltaic cells. If the potential purity can be realized, the silicon will also be applicable for ribbon pulling techniques where the purification during crystallization is negligible. The process consists of several steps: selection and purification of raw materials, carbothermic reduction of silica, ladle treatment, casting, crushing, leaching, and melting. The leaching step is crucial for high purity, and the obtainable purity is determined by the solidification before leaching. The most difficult specifications to fulfill are the low contents of boron, phosphorus, and carbon. Boron and phosphorus can be excluded from the raw materials, but the carbothermic reduction will unavoidably saturate the silicon with carbon at high temperature. During cooling carbon will precipitate as silicon carbide crystals, which will be harmful in solar cells. The cost of this solar silicon will depend strongly on the scale of production. It is as yet premature to give exact figures, but with a scale of some thousand tons per year, the cost will only be a few times the cost of ordinary metallurgical silicon.

Insights into crystal growth rates from a study of orbicular granitoids from western Australia

NASA Astrophysics Data System (ADS)

Zhang, J.; Lee, C. T.

2017-12-01

The purpose of this study is to develop new tools for constraining crystal growth rate in geologic systems. Of interest is the growth of crystals in magmatic systems because crystallization changes the rheology of a magma as well as provides surfaces on which bubbles can nucleate. To explore crystal growth in more detail, we conducted a case study of orbicular granitoids from western Australia. The orbicules occur as spheroids dispersed in a granitic matrix. Most orbicules have at least two to three concentric bands, composed of elongate and radially oriented hornblende surrounded by interstitial plagioclase. We show that mineral modes and hence bulk composition at the scale of the band is homogeneous from rim to core. Crystal number density decreases and crystal size increases from rim to core. These observations suggest that the orbicules crystallized rapidly from rim to core. We hypothesize that the orbicules are blobs of hot dioritic liquid injected into a cold granitic magma and subsequently cooled and solidified. Crystals stop growing when the mass transport rate tends to zero due to the low temperature. We estimated cooling timescales based on conductive cooling models, constraining crystal growth rates to be 10-6 to 10-5 m/s. We also show that the oscillatory banding is controlled by disequilibrium crystallization, wherein hornblende preferentially crystallizes, resulting in the diffusive growth of a chemical boundary layer enriched in plagioclase component, which in turns results in crystallization of plagioclase. We show that the correlation between the width of each crystallization couplet (band) with distance from orbicule rim is linear, with the slope corresponding to the square root of the ratio between chemical diffusivity in the growth medium and thermal diffusivity. We estimate chemical diffusivity of 2*10-7 m2/s, which is remarkably fast for silicate liquids but reasonable for diffusion in hot aqueous fluids, suggesting that crystallization occurred during water-saturated conditions. Combined with the estimate of the boundary layer thickness, we use the diffusivity to estimate the diffusive flux, arriving at crystal growth rates similar to that constrained by thermal modeling. In the presence of fluids, we show that crystal growth rates in magmatic systems may be under-estimated.

Cu-Zn slags from Røros (Norway): a case study of rapid cooling and crystal nucleation

NASA Astrophysics Data System (ADS)

Warchulski, Rafał; Szopa, Krzysztof

2014-09-01

The mining town of Røros located in central Norway was established in 1644 and it is known of historical mining industry related to copper. Røros was designated as an UNESCO World Heritage Site in 1980 on the base of mining culture represented by, e.g., unique wooden architecture. Slag pieces are composed of three parts differing in glass to crystallites ratio. Røros slags are composed of olivine- and pyroxene- group minerals accompanied by sulphides, with glass in the interstices. Temperature gradient and volatiles content were determined as the main factor influencing crystallization process in this material

Cu-Zn Slags from R⊘ros (Norway): A Case Study of Rapid Cooling and Crystal Nucleation

NASA Astrophysics Data System (ADS)

Warchulski, Rafał; Szopa, Krzysztof

2014-09-01

The mining town of R⊘ros located in central Norway was established in 1644 and it is known of historical mining industry related to copper. R⊘ros was designated as an UNESCO World Heritage Site in 1980 on the base of mining culture represented by, e.g., unique wooden architecture. Slag pieces are composed of three parts differing in glass to crystallites ratio. R⊘ros slags are composed of olivine- and pyroxene- group minerals accompanied by sulphides, with glass in the interstices. Temperature gradient and volatiles content were determined as the main factor influencing crystallization process in this material.

In-situ Crystallization of Highly Volatile Commercial Mold Flux Using an Isolated Observation System in the Confocal Laser Scanning Microscope

NASA Astrophysics Data System (ADS)

Park, Jun-Yong; Ryu, Jae Wook; Sohn, Il

2014-08-01

The in situ crystallization behavior of highly volatile commercial mold fluxes for medium carbon steels was investigated using the confocal laser scanning microscope (CLSM) equipped with an optimized isolated observation system. The highly volatile compounds of the mold flux were suppressed during heating allowing direct observation in the CLSM. Cooling rates of 25, 50, 100, 400, and 800 K/min were incorporated and continuous cooling transformation (CCT) diagrams of 4 different commercial mold fluxes for medium carbon steels were developed. Identification of the crystalline phase was conducted with XRD and SEM-EDS analysis. A cuspidine crystalline was observed in all samples at various cooling rates. With higher basicity, CaF2, and NaF, the crystallization of the fluxes was enhanced according to the CCT diagram. As the slag structure becomes depolymerized, the diffusion rate of the cathodic ions seems to increase.

Cryopreservation: Vitrification and Controlled Rate Cooling.

PubMed

Hunt, Charles J

2017-01-01

Cryopreservation is the application of low temperatures to preserve the structural and functional integrity of cells and tissues. Conventional cooling protocols allow ice to form and solute concentrations to rise during the cryopreservation process. The damage caused by the rise in solute concentration can be mitigated by the use of compounds known as cryoprotectants. Such compounds protect cells from the consequences of slow cooling injury, allowing them to be cooled at cooling rates which avoid the lethal effects of intracellular ice. An alternative to conventional cooling is vitrification. Vitrification methods incorporate cryoprotectants at sufficiently high concentrations to prevent ice crystallization so that the system forms an amorphous glass thus avoiding the damaging effects caused by conventional slow cooling. However, vitrification too can impose damaging consequences on cells as the cryoprotectant concentrations required to vitrify cells at lower cooling rates are potentially, and often, harmful. While these concentrations can be lowered to nontoxic levels, if the cells are ultra-rapidly cooled, the resulting metastable system can lead to damage through devitrification and growth of ice during subsequent storage and rewarming if not appropriately handled.The commercial and clinical application of stem cells requires robust and reproducible cryopreservation protocols and appropriate long-term, low-temperature storage conditions to provide reliable master and working cell banks. Though current Good Manufacturing Practice (cGMP) compliant methods for the derivation and banking of clinical grade pluripotent stem cells exist and stem cell lines suitable for clinical applications are available, current cryopreservation protocols, whether for vitrification or conventional slow freezing, remain suboptimal. Apart from the resultant loss of valuable product that suboptimal cryopreservation engenders, there is a danger that such processes will impose a selective pressure on the cells selecting out a nonrepresentative, freeze-resistant subpopulation. Optimizing this process requires knowledge of the fundamental processes that occur during the freezing of cellular systems, the mechanisms of damage and methods for avoiding them. This chapter draws together the knowledge of cryopreservation gained in other systems with the current state-of-the-art for embryonic and induced pluripotent stem cell preservation in an attempt to provide the background for future attempts to optimize cryopreservation protocols.

High-temperature crystallization of nanocrystals into three-dimensional superlattices

DOE PAGES

Wu, Liheng; Willis, Joshua J.; McKay, Ian Salmon; ...

2017-07-31

Crystallization of colloidal nanocrystals into superlattices represents a practical bottom-up process with which to create ordered metamaterials with emergent functionalities. With precise control over the size, shape and composition of individual nanocrystals, various single-and multi-component nanocrystal superlattices have been produced, the lattice structures and chemical compositions of which can be accurately engineered. Nanocrystal superlattices are typically prepared by carefully controlling the assembly process through solvent evaporation or destabilization or through DNA-guided crystallization. Slow solvent evaporation or cooling of nanocrystal solutions (over hours or days) is the key element for successful crystallization processes. Here we report the rapid growth (seconds) ofmore » micrometre-sized, face-centred-cubic, three-dimensional nanocrystal superlattices during colloidal synthesis at high temperatures (more than 230 degrees Celsius). Using in situ small-angle X-ray scattering, we observe continuous growth of individual nanocrystals within the lattices, which results in simultaneous lattice expansion and fine nanocrystal size control due to the superlattice templates. Thermodynamic models demonstrate that balanced attractive and repulsive interparticle interactions dictated by the ligand coverage on nanocrystal surfaces and nanocrystal core size are responsible for the crystallization process. The interparticle interactions can also be controlled to form different superlattice structures, such as hexagonal close-packed lattices. In conclusion, the rational assembly of various nanocrystal systems into novel materials is thus facilitated for both fundamental research and for practical applications in the fields of magnetics, electronics and catalysis.« less

Ejection of Coulomb Crystals from a Linear Paul Ion Trap for Ion-Molecule Reaction Studies.

PubMed

Meyer, K A E; Pollum, L L; Petralia, L S; Tauschinsky, A; Rennick, C J; Softley, T P; Heazlewood, B R

2015-12-17

Coulomb crystals are being increasingly employed as a highly localized source of cold ions for the study of ion-molecule chemical reactions. To extend the scope of reactions that can be studied in Coulomb crystals-from simple reactions involving laser-cooled atomic ions, to more complex systems where molecular reactants give rise to multiple product channels-sensitive product detection methodologies are required. The use of a digital ion trap (DIT) and a new damped cosine trap (DCT) are described, which facilitate the ejection of Coulomb-crystallized ions onto an external detector for the recording of time-of-flight (TOF) mass spectra. This enables the examination of reaction dynamics and kinetics between Coulomb-crystallized ions and neutral molecules: ionic products are typically cotrapped, thus ejecting the crystal onto an external detector reveals the masses, identities, and quantities of all ionic species at a selected point in the reaction. Two reaction systems are examined: the reaction of Ca(+) with deuterated isotopologues of water, and the charge exchange between cotrapped Xe(+) with deuterated isotopologues of ammonia. These reactions are examples of two distinct types of experiment, the first involving direct reaction of the laser-cooled ions, and the second involving reaction of sympathetically-cooled heavy ions to form a mixture of light product ions. Extensive simulations are conducted to interpret experimental results and calculate optimal operating parameters, facilitating a comparison between the DIT and DCT approaches. The simulations also demonstrate a correlation between crystal shape and image shape on the detector, suggesting a possible means for determining crystal geometry for nonfluorescing ions.

Defect chemistry and characterization of Hg(1-x)Cd(x)Te

NASA Technical Reports Server (NTRS)

Vydyanath, H. R.

1981-01-01

Undoped mercury cadmium telluride crystals were subjected to high temperature equilibration at temperatures ranging from 400 C to 655 C in various Hg atmospheres. Hall effect and mobility measurements were carried out on the crystals quenched to room temperature subsequent to the high temperature equilibration. The variation of the hole concentration in the cooled crystals at 77 K as a function of the partial pressure of Hg at the equlibration temperatures, together with a comparison of the hole mobility in the undoped samples with that in the copper and phosphorous doped samples yielded a defect model for the undoped crystals, according to which, the undoped crystals are essentially intrinsic at the equilibration temperatures and the native acceptor defects are doubly ionized. Native donor defects appear to be negligible in concentration, implying that the p to n conversion in these alloys is mainly due to residual foreign donor impurities. The thermodynamic constants for the intrinsic excitation process as well as for the incorporation of the doubly ionized native acceptor defects in the undoped crystals were obtained.

Micro- and nano-porous surface patterns prepared by surface-confined directional melt crystallization of solvent

NASA Astrophysics Data System (ADS)

Kim, Byoung Soo; Kim, Hyun Jin; An, Suyeong; Chi, Sangwon; Kim, Junseok; Lee, Jonghwi

2017-07-01

Recently, numerous attempts have been made to engineer micro- and nano-porous surface patterns or to develop convenient preparation methods for the practical applications of self-cleaning surfaces, water-repellent surfaces, novel textures, etc. Herein, we introduce a simple, cheap, and repeatable crystallization-based method to produce porous surface structures, on any surface of already fabricated polymeric materials. Contact of the solvent phase with cooled polymer surfaces enabled the limited dissolution of the surfaces and the subsequent extremely fast melt crystallization of the solvent. After removing the crystals, various micro- and nano-porous patterns were obtained, whose pore sizes ranged over three orders of magnitude. Pore depth was linearly dependent on the dissolution time. Crystal growth was mainly directed normal to the surfaces, but it was also controlled in-plane, resulting in cylindrical or lamellar structures. Superhydrophobic surfaces were successfully prepared on both polystyrene and polycarbonate. This process offers a novel surface engineering tool for a variety of polymer surfaces, whose topology can be conveniently controlled over a wide range by crystal engineering.

Growth and properties of transparent conducting CuAlO2 single crystals by a flux self-removal method

NASA Astrophysics Data System (ADS)

Yoon, J. S.; Nam, Y. S.; Baek, K. S.; Park, C. W.; Ju, H. L.; Chang, S. K.

2013-03-01

We investigated the growth and properties of CuAlO2 single crystals grown by a flux self-removal method. In this method, the flux crept up the wall of an alumina crucible completely during the slow cooling process, leaving flux-free CuAlO2 crystals on the bottom of the crucible. The resulting CuAlO2 crystals had typical dimensions of 0.5-5 mm in the ab-plane and 10-300 μm along the c-axis. The crystals had a hexagonal structure with a=b=2.857(1) Å and c=16.939(2) Å. Their resistivity was anisotropic with a c-axis resistivity (ρc) about ˜17 times higher than the ab-plane resistivity (ρab). However, both ρab and ρc showed thermally activated behavior with the same activation energy of ˜0.6 eV. The CuAlO2 crystals had direct and indirect bandgaps of 3.40 eV and 2.22 eV, respectively.

Fabrication of graded index single crystal in glass

PubMed Central

Veenhuizen, Keith; McAnany, Sean; Nolan, Daniel; Aitken, Bruce; Dierolf, Volkmar; Jain, Himanshu

2017-01-01

Lithium niobate crystals were grown in 3D through localized heating by femtosecond laser irradiation deep inside 35Li2O-35Nb2O5-30SiO2 glass. Laser scanning speed and power density were systematically varied to control the crystal growth process and determine the optimal conditions for the formation of single crystal lines. EBSD measurements showed that, in principle, single crystals can be grown to unlimited lengths using optimal parameters. We successfully tuned the parameters to a growth mode where nucleation and growth occur upon heating and ahead of the scanning laser focus. This growth mode eliminates the problem reported in previous works of non-uniform polycrystallinity because of a separate growth mode where crystallization occurs during cooling behind the scanning laser focus. To our knowledge, this is the first report of such a growth mode using a fs laser. The crystal cross-sections possessed a symmetric, smooth lattice misorientation with respect to the c-axis orientation in the center of the crystal. Calculations indicate the observed misorientation leads to a decrease in the refractive index of the crystal line from the center moving outwards, opening the possibility to produce within glass a graded refractive index single crystal (GRISC) optically active waveguide. PMID:28287174

High-Temperature Formation Phases and Crystal Structure of Hot-Pressed Thermoelectric CuGaTe2 with Chalcopyrite-Type Structure

NASA Astrophysics Data System (ADS)

Fujii, Yosuke; Kosuga, Atsuko

2017-11-01

Polycrystalline CuGaTe2 with a chalcopyrite-type structure consolidated by hot-pressing is a potential candidate as a medium-temperature thermoelectric (TE) material. However, its high-temperature formation phases have rarely been reported to date. Here, we investigated the temperature-dependent formation phases and crystal structure at 300-800 K of hot-pressed CuGaTe2. From synchrotron x-ray diffraction data and crystal structure analysis of the heating and cooling processes, it was clarified that a certain amount of impurity phases, such as Te and CuTe, precipitated from the CuGaTe2 matrix when the temperature was increased (to 500-650 K). This is the temperature range where CuGaTe2 has been reported to show high TE performance. After CuGaTe2 was heated to 800 K, such impurity phases remained, even when cooled to room temperature. They also affected the tetragonal distortion and the x-coordinate of Te in the CuGaTe2 matrix, probably due to deficiencies of Cu and Te in the matrix. Our results reveal detailed information on the formation phases of CuGaTe2 at high temperature and thus provide insight for evaluation of its high-temperature stability and transport properties.

High-Temperature Formation Phases and Crystal Structure of Hot-Pressed Thermoelectric CuGaTe2 with Chalcopyrite-Type Structure

NASA Astrophysics Data System (ADS)

Fujii, Yosuke; Kosuga, Atsuko

2018-06-01

Polycrystalline CuGaTe2 with a chalcopyrite-type structure consolidated by hot-pressing is a potential candidate as a medium-temperature thermoelectric (TE) material. However, its high-temperature formation phases have rarely been reported to date. Here, we investigated the temperature-dependent formation phases and crystal structure at 300-800 K of hot-pressed CuGaTe2. From synchrotron x-ray diffraction data and crystal structure analysis of the heating and cooling processes, it was clarified that a certain amount of impurity phases, such as Te and CuTe, precipitated from the CuGaTe2 matrix when the temperature was increased (to 500-650 K). This is the temperature range where CuGaTe2 has been reported to show high TE performance. After CuGaTe2 was heated to 800 K, such impurity phases remained, even when cooled to room temperature. They also affected the tetragonal distortion and the x-coordinate of Te in the CuGaTe2 matrix, probably due to deficiencies of Cu and Te in the matrix. Our results reveal detailed information on the formation phases of CuGaTe2 at high temperature and thus provide insight for evaluation of its high-temperature stability and transport properties.

On the Lower Limit of Chondrule Cooling Rates: The Significance of Iron Loss in Dynamic Crystallization Experiments

NASA Technical Reports Server (NTRS)

Paque, Julie M.; Connolly, Harold C., Jr.; Lofgren, Gary E.

1998-01-01

It is unlikely that the presence of chondrules, and thus their formation, within the protoplanetary nebula would be predicted if it were not for their ubiquitous presence in most chondritic meteorites. The study of these enigmatic, igneous objects has a direct influence on how meteoritic and solar system researchers model the processes operating and the materials present within our protoplanetary nebula. Key to understanding chondrule formation is a determination of constraints on their thermal histories. The three important variables in this history are their peak melting temperatures, the duration of their melting at peak temperatures, and the rate at which these object cool. Although these three variables are interdependent, it is cooling rate that provides the most powerful constraint. Cooling rate has a direct affect on the development of both crystal morphology and the elemental distributions within these grains. To date, experiments have indicated that chondrule cooling rates are in the range of 10's to 100's of degrees per hour for porphyritic chondrules (the most abundant type). The cooling rate for radial and barred chondrules is thought to be more rapid. To generate these cooling rates (rapid relative to the cooling of the nebula as a whole, but slow compared to simple black body radiation) the environment of chondrule formation must have been localized, and the abundance of solid materials must have been greatly enhanced above a gas of solar composition. Thus accurate determinations of chondrule cooling rates is critical in understanding both their formation and the nebular environment in which they formed. In a quest to more accurately determine the lower limit on cooling rates and to determine in more detail the effects of Fe loss from a molten sample to Pt wire loops, Weinbruch et al. have explored this issue experimentally and reevaluated the findings of Radomsky and Hewins in light of their new results. The basic conclusions of their paper are an important contribution to our understanding of how experimental techniques can affect established constraints on chondrule formation and are thus of interest to a wide audience. We do believe, however, that their methodology produces results that provide inappropriate impressions of the applicability of their study to chondrule formation and nebular processes. Furthermore, the extensive body of previous experimental work on chondrule bulk compositions cannot be invalidated, as they suggest, by the results of Weinbruch et al. It is for these reasons that within this comment we address to applicability of the results presented by Weinbruch et al. to previous studies, and illustrate how the experimental conditions chosen for their series of experiments introduced a significant bias in their results.

Study on the structural transition of CoNi nanoclusters using molecular dynamics simulations

NASA Astrophysics Data System (ADS)

Xia, J. H.; Gao, Xue-Mei

2018-04-01

In this work, the segregation and structural transitions of CoNi clusters, between 1500 and 300 K, have been investigated using molecular dynamics simulations with the embedded atom method potential. The radial distribution function was used to analyze the segregation during the cooling processes. It is found that Co atoms segregate to the inside and Ni atoms preferably to the surface during the cooling processes, the Co147Ni414 cluster becomes a core-shell structure. We discuss the structural transition according to the pair-correction function and pair-analysis technique, and finally the liquid Co147Ni414 crystallizes into the coexistence of hcp and fcc structure at 300 K. At the same time, it is found that the frozen structure of CoNi cluster is strongly related to the Co concentration.

Modeling and Validation of a Three-Stage Solidification Model for Sprays

NASA Astrophysics Data System (ADS)

Tanner, Franz X.; Feigl, Kathleen; Windhab, Erich J.

2010-09-01

A three-stage freezing model and its validation are presented. In the first stage, the cooling of the droplet down to the freezing temperature is described as a convective heat transfer process in turbulent flow. In the second stage, when the droplet has reached the freezing temperature, the solidification process is initiated via nucleation and crystal growth. The latent heat release is related to the amount of heat convected away from the droplet and the rate of solidification is expressed with a freezing progress variable. After completion of the solidification process, in stage three, the cooling of the solidified droplet (particle) is described again by a convective heat transfer process until the particle approaches the temperature of the gaseous environment. The model has been validated by experimental data of a single cocoa butter droplet suspended in air. The subsequent spray validations have been performed with data obtained from a cocoa butter melt in an experimental spray tower using the open-source computational fluid dynamics code KIVA-3.

The Si ribbon crystal for the solar battery using the horizontal pull method

NASA Technical Reports Server (NTRS)

Norifuji, H.; Matsuo, M.; Maki, T.

1979-01-01

A method utilizing a device to spray noble gases to cool the site of silicon crystal growth is described. The salient points are: (1) soft and uniform cooling was possible, (2) the length of the boundary surface of growth along the growth direction was made long over a wide width compared to the thickness, and (3) this made it possible to effectively remove the heat produced from solification. By using forced gas spraying on the solution surface in contact with the points of crystal growth, growth at the points of growth is enhanced and the rate of growth is speeded up.

Rheology and thermal budget of lunar basalts: an experimental study and its implications for rille formation of non-Newtonian lavas on the Moon

NASA Astrophysics Data System (ADS)

Sehlke, A.; Whittington, A. G.

2015-12-01

Sinuous lava channels are a characteristic feature observed on the Moon. Their formation is assumed to be due to a combination of mechanical and thermal erosion of the lava into the substrate during emplacement as surface channels, or due to collapsed subsurface lava tubes after the lava has evacuated. The viscosity (η) of the lava plays an important role, because it controls the volume flux of the emplaced lava that governs the mechanical and thermal erosion potential of the lava flow. Thermal properties, such as heat capacity (Cp) and latent heat of crystallization (ΔHcryst) are important parameters in order for the substrate to melt and causing thermal buffering during crystallization of the flowing lava. We experimentally studied the rheological evolution of analog lavas representing the KREEP terrain and high-Ti mare basalts during cooling and crystallization. We find that the two lavas behave very differently. High-Ti mare lava begins to crystallize around 1300 ºC with a viscosity of 8.6±0.6 Pa s and crystal content around 2 vol%. On cooling to 1169 ºC, the effective viscosity of the crystal-melt suspension is increased to only 538±33 Pa s (at a strain rate of 1 s-1) due to crystallization of 14±1 vol% blocky magnetite and acicular ulvöspinel-rich magnetite. The flow behavior of these suspensions depends on the strain rate, where flow curves below strain rates of 10 s-1show shear-thinning character, but resemble Bingham behavior at greater strain rates. In contrast, the KREEP lava crystallizes rapidly over a narrow temperature interval of ~ 30 degrees. The first crystals detected were ulvospinel-rich magnetites at 1204 ºC with ~2 vol% and a viscosity of 90±2 Pa s. On cooling to 1178 ºC, anorthite and enstatite appears, so that the crystal-melt suspension has become strongly pseudoplastic at a crystal content of 22±2 vol% with a flow index (n) of 0.63 and an effective viscosity of 1600±222 Pa s at a strain rate of 1 s-1. We are currently measuring the heat capacity of crystal-bearing glasses (representing erodible solid substrate) and the heat released during lava crystallization at different cooling rates measured by differential scanning calorimetry (DSC). The rheological and thermal properties will then be integrated into thermo-mechanical models of rille formation in non-Newtonian lavas on the lunar surface.

Cooling of a Magmatic System Under Thermal Chaotic Mixing

NASA Astrophysics Data System (ADS)

El Omari, Kamal; Le Guer, Yves; Perugini, Diego; Petrelli, Maurizio

2015-07-01

The cooling of a basaltic melt undergoing chaotic advection is studied numerically for a magma with a temperature-dependent viscosity in a two-dimensional (2D) cavity with moving boundary. Different statistical mixing and energy indicators are used to characterize the efficiency of cooling by thermal chaotic mixing. We show that different cooling rates can be obtained during the thermal mixing of a single basaltic magmatic batch undergoing chaotic advection. This process can induce complex temperature patterns inside the magma chamber. The emergence of chaotic dynamics strongly modulates the temperature fields over time and greatly increases the cooling rates. This mechanism has implications for the thermal lifetime of the magmatic body and may favor the appearance of chemical heterogeneities in the igneous system as a result of different crystallization rates. Results from this study also highlight that even a single magma batch can develop, under chaotic thermal advection, complex thermal and therefore compositional patterns resulting from different cooling rates, which can account for some natural features that, to date, have received unsatisfactory explanations, including the production of magmatic enclaves showing completely different cooling histories compared with the host magma, compositional zoning in mineral phases, and the generation of large-scale compositional zoning observed in many plutons worldwide.

Congruent melting of gallium nitride at 6 GPa and its application to single-crystal growth.

PubMed

Utsumi, Wataru; Saitoh, Hiroyuki; Kaneko, Hiroshi; Watanuki, Tetsu; Aoki, Katsutoshi; Shimomura, Osamu

2003-11-01

The synthesis of large single crystals of GaN (gallium nitride) is a matter of great importance in optoelectronic devices for blue-light-emitting diodes and lasers. Although high-quality bulk single crystals of GaN suitable for substrates are desired, the standard method of cooling its stoichiometric melt has been unsuccessful for GaN because it decomposes into Ga and N(2) at high temperatures before its melting point. Here we report that applying high pressure completely prevents the decomposition and allows the stoichiometric melting of GaN. At pressures above 6.0 GPa, congruent melting of GaN occurred at about 2,220 degrees C, and decreasing the temperature allowed the GaN melt to crystallize to the original structure, which was confirmed by in situ X-ray diffraction. Single crystals of GaN were formed by cooling the melt slowly under high pressures and were recovered at ambient conditions.

Recent progress in X-ray optics at the ESRF

NASA Astrophysics Data System (ADS)

Freund, A.

2003-03-01

It is the task of x-ray optics to adapt the raw beam generated by modern sources such as synchrotron storage rings to a great variety of experimental requirements in terms of intensity, spot size, polarization and other parameters. The very high quality of synchrotron radiation (source size of a few microns and beam divergence of a few micro-radians) and the extreme x-ray flux (power of several hundred Watts in a few square mm) make this task quite difficult. In particular the heat load aspect is very important in the conditioning process of the brute x-ray power. Cryogenically cooled silicon crystals and water-cooled diamond crystals can presently fulfil this task, but limits will soon be reached and new schemes and materials must be envisioned. A major tendency of instrument improvement has a ways been to concentrate more photons into a smaller spot utilizing a whole variety of focusing devices such as Fresnel zone plates, refractive lenses and Systems based on bent surfaces, for example Kirkpatrick-Baez Systems. Apart from the resistance of the sample, the ultimate limits are determined by the source size and strength on one side, by materials properties, cooling, mounting and bending schemes on the other side, and fundamentally by the diffraction process. There is also the important aspect of coherence that can be both a nuisance and a blessing for the experiments, in particular for imaging techniques. Its conservation puts additional constraints on the quality of the optical elements. A review of recent progress in this field is given.

An Undergraduate Laboratory Exercise for Studying Kinetics of Batch Crystallization

ERIC Educational Resources Information Center

Louhi­-Kultanen, Marjatta; Han, Bing; Nurkka, Annikka; Hatakka, Henry

2015-01-01

The present work describes an undergraduate laboratory exercise for improving understanding of fundamental phenomena in cooling crystallization. The exercise of nucleation and crystal growth kinetics supports learning of theories and models presented in lectures and calculation exercises. The teaching methodology incorporates precepts the…

Experiments on microjets of undercooled liquid hydrogen

NASA Astrophysics Data System (ADS)

Fernández, José M.; Kühnel, Matthias; Tejeda, Guzmán; Kalinin, Anton; Grisenti, Robert E.; Montero, Salvador

2012-11-01

Novel experiments on liquid microjets (filaments) of hydrogen and deuterium, carried out at the Laboratory of Molecular Fluid Dynamics of the IEM, are reported. These filaments, less than 10 microns in diameter, are an ideal medium to produce highly undercooled liquid samples and to investigate the homogeneous solidification process, free from wall effects. The filaments exit from cryogenic capillary nozzles into a vacuum chamber, to cool down very fast by surface evaporation. Finite size radius leads to a temperature gradient across the filament, determined by thermal conductivity, and, possibly, to a velocity gradient as well. The filaments are monitored by laser shadowgraphy, and analyzed by means of high performance Raman spectroscopy. Real-time measurements in the rotational and vibrational spectral regions reveal the structure and temperature along the filaments, allowing to track the crystal growth process. The high spatial resolution of Raman spectroscopy allows observing in situ the structural changes of the liquid microjets, with a time resolution of ˜ 10 ns. The filaments of pure para-H2 can be cooled down to 9 K (65% of its melting point at 13.8 K), while staying liquid, before eventually solidifying into a metastable polymorph. Crystallization kinetics revealed a growth rate of 33 cm/s, much higher than expected for a thermally activated process. The time and spatial control attained in these experiments offers new opportunities for investigating the processes of nonequilibrium phase transformations in undercooled fluids, as well as the propagation of liquid jets into a rarefied gas media.

Effects of micro electric current load during cooling of plant tissues on intracellular ice crystal formation behavior and pH.

PubMed

Ninagawa, Takako; Kawamura, Yukio; Konishi, Tadashi; Narumi, Akira

2016-08-01

Cryopreservation techniques are expected to evolve further to preserve biomaterials and foods in a fresh state for extended periods of time. Long-term cryopreservation of living materials such as food and biological tissue is generally achieved by freezing; thus, intracellular freezing occurs. Intracellular freezing injures the cells and leads to cell death. Therefore, a dream cryopreservation technique would preserve the living materials without internal ice crystal formation at a temperature low enough to prevent bacterial activity. This study was performed to investigate the effect of micro electrical current loading during cooling as a new cryopreservation technique. The behavior of intracellular ice crystal formation in plant tissues with or without an electric current load was evaluated using the degree of supercooling, degree of cell deformation, and grain size and growing rate of intracellular ice crystal. Moreover, the transition of intracellular pH during plant tissue cooling with or without electric current loading was also examined using the fluorescence intensity ratio to comprehend cell activity at lower temperatures. The results indicated that micro electric current load did not only decrease the degree of cell deformation and grain size of intracellular ice crystal but also reduced the decline in intracellular pH due to temperature lowering, compared with tissues subjected to the same cooling rate without an electric current load. Thus, the effect of electric current load on cryopreservation and the potential of a new cryopreservation technique using electric current load were discussed based on these results. Copyright © 2016 Elsevier Inc. All rights reserved.

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.

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

Dong, Xiaohao, E-mail: xiaohao.dong@xfel.eu; Sinn, Harald, E-mail: harald.sinn@xfel.eu; Shu, Deming, E-mail: shu@aps.anl.gov

An artificial channel-cut crystal monochromator for the hard X-Ray beamlines of SASE 1&2, cryogenically cooled by the so-called pulse tube cooler (cryorefrigerator), is currently under development at the European XFEL ( http://www.xfel.eu/ ). The fabrication is on-going. We present here the crystal optical consideration and the novel cooling configuration, according to the X-Ray FEL pulses proprieties. The mechanical design improvements are pointed out as well to implement such kind of monochromator based on the previous similar design.

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

Dong, Xiaohao; Shu, Deming; Sinn, Harald

An artificial channel-cut crystal monochromator for the hard X-Ray beamlines of SASE 1&2, cryogenically cooled by the so-called pulse tube cooler (cryorefrigerator), is currently under development at the European XFEL (http://www.xfel.eu/). The fabrication is on-going. We present here the crystal optical consideration and the novel cooling configuration, according to the X-Ray FEL pulses proprieties. The mechanical design improvements are pointed out as well to implement such kind of monochromator based on the previous similar design.

Crystal Phases Formed in a CaO-Fe2O3 System Under a High Cooling Rate in Air

NASA Astrophysics Data System (ADS)

Kashiwaya, Yoshiaki

2017-12-01

A CaO-Fe2O3 system is a fundamental binary system for the iron ore sintering process. Although the basic reactions have been investigated since the 1960s, melting and solidification caused by the combustion of coke results in an unstable state owing to extreme temperature variations. In this study, using a hot thermocouple method, samples of 10 pct CaO-90 pct Fe2O3 and 20 pct CaO-80 pct Fe2O3 were melted on a thermocouple and quenched with several techniques. The obtained samples were precisely examined by XRD. It was found that the sample containing 10 pct CaO-90 pct Fe2O3 changed to 10 pct CaO-13 pct FeO-77 pct Fe2O3 under an oxygen partial pressure ( P_{{{O}2 }} ) of 0.21 during melting. For the 10 pct CaO sample, the crystal phases found at a low cooling rate (509 K/s) were WFss, C4WF8 (C: CaO, W: FeO, F: Fe2O3), and C2W4F9. When the sample composition was 20 pct CaO, the precipitated crystal phases were C4WF4, C4F7, and C4WF8. On the other hand, the crystal phases for high cooling rates (1590 and 7900 K/s) with 10 pct CaO were WFss (solid solution of WF and F), F, and C2W4F9. The formation of the equilibrium phases WFss, F, C4WF4, and C4WF8 can be understood by examining the isothermal section of the phase diagrams, while the unstable phases C2W4F9 and C4F7 are discussed on the basis of the reactions under an equilibrium state.

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

Marra, James; Kim, Dong -Sang; Maio, Vincent

A number of waste components in US defense high level radioactive wastes (HLW) have proven challenging for current Joule heated ceramic melter (JHCM) operations and have limited the ability to increase waste loadings beyond already realized levels. Many of these “troublesome" waste species cause crystallization in the glass melt that can negatively impact product quality or have a deleterious effect on melter processing. Recent efforts at US Department of Energy laboratories have focused on understanding crystallization behavior within HLW glass melts and investigating approaches to mitigate the impacts of crystallization so that increases in waste loading can be realized. Advancedmore » glass formulations have been developed to highlight the unique benefits of next-generation melter technologies such as the Cold Crucible Induction Melter (CCIM). Crystal-tolerant HLW glasses have been investigated to allow sparingly soluble components such as chromium to crystallize in the melter but pass out of the melter before accumulating.The Hanford site AZ-101 tank waste composition represents a waste group that is waste loading limited primarily due to high concentrations of Fe 2O 3 (also with high Al 2O 3 concentrations). Systematic glass formulation development utilizing slightly higher process temperatures and higher tolerance to spinel crystals demonstrated that an increase in waste loading of more than 20% could be achieved for this waste composition, and by extension higher loadings for wastes in the same group. An extended duration CCIM melter test was conducted on an AZ-101 waste simulant using the CCIM platform at the Idaho National Laboratory (INL). The melter was continually operated for approximately 80 hours demonstrating that the AZ-101 high waste loading glass composition could be readily processed using the CCIM technology. The resulting glass was close to the targeted composition and exhibited excellent durability in both the as poured state and after being slowly cooled according to the canister centerline cooling (CCC) profile. Glass formulation development was also completed on other Hanford tank wastes that were identified to further challenge waste loading due to the presence of appreciable quantities (>750 g) of plutonium in the waste tanks. In addition to containing appreciable Pu quantities, the C-102 waste tank and the 244-TX waste tank contain high concentrations of aluminum and iron, respectively that will further challenge vitrification processing. Glass formulation testing also demonstrated that high waste loadings could be achieved with these tank compositions using the attributes afforded by the CCIM technology.« less

The Fe2(+)-Mg interdiffusion in orthopyroxene: Constraints from cation ordering and structural data and implications for cooling rates of meteorites

NASA Technical Reports Server (NTRS)

Ganguly, J.; Tazzoli, V.

1993-01-01

Orthopyroxene crystals in a number of meteorites exhibit compositional zoning of Fe and Mg, which provide important constraint on their cooling rates. However, attempts to model cooling rate of these crystals from Fe-Mg zoning profiles suffer from the lack of any measured or theoretically well constrained Fe-Mg interdiffusion data in OP(x) It has been assumed that Fe-Mg interdiffusion in OP(x) only slightly slower than that in olivine. The purpose of this paper is to (1) calculate the Fe-Mg fractionation, and (2) provide analytical formulation relating cooling rate to the length of the diffusion zone across the interface of the overgrowth of a mineral on itself with application to Mg diffusion profile across OP(x) growth on OP(x) in certain mesosiderites.

Frazil-ice growth rate and dynamics in mixed layers and sub-ice-shelf plumes

NASA Astrophysics Data System (ADS)

Rees Jones, David W.; Wells, Andrew J.

2018-01-01

The growth of frazil or granular ice is an important mode of ice formation in the cryosphere. Recent advances have improved our understanding of the microphysical processes that control the rate of ice-crystal growth when water is cooled beneath its freezing temperature. These advances suggest that crystals grow much faster than previously thought. In this paper, we consider models of a population of ice crystals with different sizes to provide insight into the treatment of frazil ice in large-scale models. We consider the role of crystal growth alongside the other physical processes that determine the dynamics of frazil ice. We apply our model to a simple mixed layer (such as at the surface of the ocean) and to a buoyant plume under a floating ice shelf. We provide numerical calculations and scaling arguments to predict the occurrence of frazil-ice explosions, which we show are controlled by crystal growth, nucleation, and gravitational removal. Faster crystal growth, higher secondary nucleation, and slower gravitational removal make frazil-ice explosions more likely. We identify steady-state crystal size distributions, which are largely insensitive to crystal growth rate but are affected by the relative importance of secondary nucleation to gravitational removal. Finally, we show that the fate of plumes underneath ice shelves is dramatically affected by frazil-ice dynamics. Differences in the parameterization of crystal growth and nucleation give rise to radically different predictions of basal accretion and plume dynamics, and can even impact whether a plume reaches the end of the ice shelf or intrudes at depth.

High temperature in-situ synchrotron-based XRD study on the crystal structure evolution of C/C composite impregnated by FLiNaK molten salt.

PubMed

Feng, Shanglei; Yang, Yingguo; Li, Li; Zhang, Dongsheng; Yang, Xinmei; Xia, Huihao; Yan, Long; Tsang, Derek K L; Huai, Ping; Zhou, Xingtai

2017-09-06

An in-situ real-time synchrotron-based grazing incidence X-ray diffraction was systematically used to investigate the crystal structural evolution of carbon fiber reinforced carbon matrix (C/C) composite impregnated with FLiNaK molten salt during the heat-treatment process. It was found that the crystallographic thermal expansion and contraction rate of interlayer spacing d 002 in C/C composite with FLiNaK salt impregnation is smaller than that in the virgin sample, indicating the suppression on interlayer spacing from FLiNaK salt impregnated. Meanwhile the crystallite size L C002 of C/C composite with FLiNaK salt impregnation is larger than the virgin one after whole heat treatment process, indicating that FLiNaK salt impregnation could facilitate the crystallization of C/C composite after heat treatment process. This improved crystallization in C/C composite with FLiNaK salt impregnation suggests the synthetic action of the salt squeeze effect on crooked carbon layer and the release of internal residual stress after heating-cooling process. Thus, the present study not only contribute to reveal the interaction mechanism between C/C composite and FLiNaK salt in high temperature environment, but also promote the design of safer and more reliable C/C composite materials for the next generation molten salt reactor.

Large single crystal quaternary alloys of IB-IIIA-Se/sub 2/ and methods of synthesizing the same

DOEpatents

Ciszek, T.F.

1986-07-15

New alloys of Cu/sub x/Ag/sub (1-x)/InSe/sub 2/ (where x ranges between 0 and 1 and preferably has a value of about 0.75) and CuIn/sub y/Ga/sub (1-y)/Se/sub 2/ (where y ranges between 0 and 1 and preferably has a value of about 0.90) in the form of single crystals with enhanced structure perfection, which crystals are substantially free of fissures, are disclosed. Processes are disclosed for preparing the new alloys of Cu/sub x/Ag/sub (1-x)/InSe/sub 2/. The process includes placing stoichiometric quantities of a Cu, Ag, In, and Se reaction mixture or stoichiometric quantities of a Cu, In, Ga, and Se reaction mixture in a refractory crucible in such a manner that the reaction mixture is surrounded by B/sub 2/O/sub 3/, placing the thus loaded crucible in a chamber under a high pressure atmosphere of inert gas to confine the volatile Se to the crucible, and heating the reaction mixture to its melting point. The melt can then be cooled slowly to form, by direct solidification, a single crystal with enhanced structure perfection, which crystal is substantially free of fissures.

Crystallization in high-level waste glass: A review of glass theory and noteworthy literature

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

Christian, J. H.

2015-08-01

There is a fundamental need to continue research aimed at understanding nepheline and spinel crystal formation in high-level waste (HLW) glass. Specifically, the formation of nepheline solids (K/NaAlSiO₄) during slow cooling of HLW glass can reduce the chemical durability of the glass, which can cause a decrease in the overall durability of the glass waste form. The accumulation of spinel solids ((Fe, Ni, Mn, Zn)(Fe,Cr)₂O₄), while not detrimental to glass durability, can cause an array of processing problems inside of HLW glass melters. In this review, the fundamental differences between glass and solid-crystals are explained using kinetic, thermodynamic, and viscositymore » arguments, and several highlights of glass-crystallization research, as it pertains to high-level waste vitrification, are described. In terms of mitigating spinel in the melter and both spinel and nepheline formation in the canister, the complexity of HLW glass and the intricate interplay between thermal, chemical, and kinetic factors further complicates this understanding. However, new experiments seeking to elucidate the contributing factors of crystal nucleation and growth in waste glass, and the compilation of data from older experiments, may go a long way towards helping to achieve higher waste loadings while developing more efficient processing strategies.« less

Large single crystal quaternary alloys of IB-IIIA-SE.sub.2 and methods of synthesizing the same

DOEpatents

Ciszek, Theodore F.

1988-01-01

New alloys of Cu.sub.x Ag.sub.(1-x) InSe.sub.2 (where x ranges between 0 and 1 and preferably has a value of about 0.75) and CuIn.sub.y Ga.sub.(1-y) Se.sub.2 (where y ranges between 0 and 1 and preferably has a value of about 0.90) in the form of single crystals with enhanced structure perfection, which crystals are substantially free of fissures are disclosed. Processes are disclosed for preparing the new alloys of Cu.sub.x Ag.sub.(1-x) InSe.sub.2. The process includes placing stoichiometric quantities of a Cu, Ag, In, and Se reaction mixture or stoichiometric quantities of a Cu, In, Ga, and Se reaction mixture in a refractory crucible in such a manner that the reaction mixture is surrounded by B.sub.2 O.sub.3, placing the thus loaded crucible in a chamber under a high pressure atmosphere of inert gas to confine the volatile Se to the crucible, and heating the reaction mixture to its melting point. The melt can then be cooled slowly to form, by direct solidification, a single crystal with enhanced structure perfection, which crystal is substantially free of fissures.

Real-time observation of the isothermal crystallization kinetics in a deeply supercooled liquid

NASA Astrophysics Data System (ADS)

Zanatta, M.; Cormier, L.; Hennet, L.; Petrillo, C.; Sacchetti, F.

2017-03-01

Below the melting temperature Tm, crystals are the stable phase of typical elemental or molecular systems. However, cooling down a liquid below Tm, crystallization is anything but inevitable. The liquid can be supercooled, eventually forming a glass below the glass transition temperature Tg. Despite their long lifetimes and the presence of strong barriers that produces an apparent stability, supercooled liquids and glasses remain intrinsically a metastable state and thermodynamically unstable towards the crystal. Here we investigated the isothermal crystallization kinetics of the prototypical strong glassformer GeO2 in the deep supercooled liquid at 1100 K, about half-way between Tm and Tg. The crystallization process has been observed through time-resolved neutron diffraction for about three days. Data show a continuous reorganization of the amorphous structure towards the alpha-quartz phase with the final material composed by crystalline domains plunged into a low-density, residual amorphous matrix. A quantitative analysis of the diffraction patterns allows determining the time evolution of the relative fractions of crystal and amorphous, that was interpreted through an empirical model for the crystallization kinetics. This approach provides a very good description of the experimental data and identifies a predator-prey-like mechanism between crystal and amorphous, where the density variation acts as a blocking barrier.

Fracture mechanics and geochemical factors influencing the emplacement mechanisms of the Stewart Lithia gem bearing granitic pegmatite, Pala District, San Diego County, California

NASA Astrophysics Data System (ADS)

Patterson, Jeffrey E.

The emplacement mechanisms and cooling characteristics of pegmatites are not well understood, yet little work has been done on this subject. Historically, it is the pegmatite mineralogy and zonation that has been the focus of attention because of fascination with giant sized crystals, diversity of mineralization, and abundance of minerals containing important strategic elements, (Li, Be, Ta, Nb, and others). In this thesis the subject of the emplacement mechanisms is a synergistic approach from geophysical and engineering viewpoints, using the principals of fracture mechanics to determine the properties related to emplacement. From this, the cooling characteristics are considered to explain the zonation of a pegmatite based upon the temperature of crystallization of each mineral. This provides a model to image the position of each mineral according to the temperature profiles over time. Finally, the mineral growth characteristics are considered in light of the boundary conditions placed upon them by the cooling period. To test these hypothetical conditions in the real world, the Stewart Lithia Pegmatite, Pala, California, has been evaluated both physically and geochemically. The structure of the pegmatite was examined along strike and along dip, as exposed in underground workings. The analyses of these data show that there are 5 discreet divisions along strike. The analyses of the geochemical data for precisely located tourmalines shows that these divisions are composed of approximately 10 discreet pulses, with the economically important "Chimney Division" containing all 10. The importance of this work is that it demonstrates the following. A complex pegmatite is more likely to consist of multiple pulses of different melt composition than a single pulse with un-explainable mineralogy and zonation; Giant crystals are more likely due to rapid polymerization of a few mineral species where the cooling rate and crystallization rate are nearly equal; The range of mineral sizes to eleven orders of magnitude is due to the minimal rate of cooling, with the smallest crystals nucleating and not growing because there is no thermal differential driving force; and gem crystals generally only occur in fluid filled miarolitic cavities.

Control of melt-crystal interface shape during sapphire crystal growth by heat exchanger method

NASA Astrophysics Data System (ADS)

Wu, Ming; Liu, Lijun; Ma, Wencheng

2017-09-01

We numerically investigate the melt-crystal interface shape during the early stage of the solidification process when the crystal diameter increases. The contact angle between the melt-crystal interface and the crucible bottom wall is found obtuse during this stage, which is unfavorable for the crystal quality. We found that the obtuse contact angle is caused by the thermal resistance difference between the sapphire crystal and melt as well as the insufficient cooling effect of the crucible bottom. Two approaches are proposed to suppress the obtuse contact angle. The first approach is to increase the emissivity of the outer surface of crucible bottom. The second approach is to install a heat shield near the crucible bottom. The reduction of the emissivity of the heat shield is also favorable for the suppression of the obtuse contact angle. Compared with the increase of the emissivity of the crucible bottom, the installation of a heat shield is a more effective approach to prevent the appearance of an obtuse contact angle for the sake of reliability since a molybdenum heat shield can be reused and will not induce other impurities.

Kinetics of Nucleation and Crystal Growth in Glass Forming Melts in Microgravity

NASA Technical Reports Server (NTRS)

Day, Delbert E.; Ray, Chandra S.

2003-01-01

This flight definition project has the specific objective of investigating the kinetics of nucleation and crystal growth in high temperature inorganic oxide, glass forming melts in microgravity. It is related to one1 of our previous NASA projects that was concerned with glass formation for high temperature containerless melts in microgravity. The previous work culminated in two experiments which were conducted aboard the space shuttle in 1983 and 1985 and which consisted of melting (at 1500 C) and cooling levitated 6 to 8 mm diameter spherical samples in a Single Axis Acoustic Levitator (SAAL) furnace. Compared to other types of materials, there have been relatively few experiments, 6 to 8, conducted on inorganic glasses in space. These experiments have been concerned with mass transport (alkali diffusion), containerless melting, critical cooling rate for glass formation, chemical homogeneity, fiber pulling, and crystallization of glass forming melts. One of the most important and consistent findings in all of these experiments has been that the glasses prepared in microgravity are more resistant to crystallization (better glass former) and more chemically homogeneous than equivalent glasses made on earth (1g). The chemical composition of the melt appears relatively unimportant since the same general results have been reported for oxide, fluoride and chalcogenide melts. These results for space-processed glasses have important implications, since glasses with a higher resistance to crystallization or higher chemical homogeneity than those attainable on earth can significantly advance applications in areas such as fiber optics communications, high power laser glasses, and other photonic devices where glasses are the key functional materials. The classical theories for nucleation and crystal growth for a glass or melt do not contain any parameter that is directly dependent upon the g-value, so it is not readily apparent why glasses prepared in microgravity should be more resistant to crystallization than equivalent glasses prepared on earth. Similarly, the gravity-driven convection in a fluid melt is believed to be the primary force field that is responsible for melt homogenization on earth. Thus, it is not obvious why a glass prepared in space, where gravity-driven convection is ideally absent, would be more chemically homogeneous than a glass identically prepared on earth. The primary objective of the present research is to obtain experimental data for the nucleation rate and crystal growth rate for a well characterized silicate melt (lithium disilicate) processed entirely in space (low gravity) and compare these rates with the nucleation and crystal growth rates for a similar glass prepared identically on earth (1g).

Scanning electron microscope view of iron crystal

NASA Technical Reports Server (NTRS)

1972-01-01

A scanning electron microscope photograph of iron crystals which grow in a small vug or cavity in a recrystallized breccia (fragmented rock) from the Apollo 15 Hadley-Apennino lunar landing site. The largest crystal is three microns across. Perfectly developed crystals such as these indicate slow formation from a hot vapor as the rock was cooling. The crystals are resting on an interlocking lattice of pyroxene (calsium-magnesium-iron silicate).

Scanning electron microscope view of iron crystal

NASA Image and Video Library

1972-11-10

A scanning electron microscope photograph of iron crystals which grow in a small vug or cavity in a recrystallized breccia (fragmented rock) from the Apollo 15 Hadley-Apennino lunar landing site. The largest crystal is three microns across. Perfectly developed crystals such as these indicate slow formation from a hot vapor as the rock was cooling. The crystals are resting on an interlocking lattice of pyroxene (calsium-magnesium-iron silicate).

Low-Temperature Biodiesel Research Reveals Potential Key to Successful Blend Performance (Fact Sheet)

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

Not Available

Relatively low-cost solutions could improve reliability while making biodiesel blends an affordable option. While biodiesel has very low production costs and the potential to displace up to 10% of petroleum diesel, until now, issues with cold weather performance have prevented biodiesel blends from being widely adopted. Some biodiesel blends have exhibited unexplained low-temperature performance problems even at blend levels as low as 2% by volume. The most common low-temperature performance issue is vehicle stalling caused by fuel filter clogging, which prevents fuel from reaching the engine. Research at the National Renewable Energy Laboratory (NREL) reveals the properties responsible for thesemore » problems, clearing a path for the development of solutions and expanded use of energy-conserving and low-emissions alternative fuel. NREL researchers set out to study the unpredictable nature of biodiesel crystallization, the condition that impedes the flow of fuel in cold weather. Their research revealed for the first time that saturated monoglyceride impurities common to the biodiesel manufacturing process create crystals that can cause fuel filter clogging and other problems when cooling at slow rates. Biodiesel low-temperature operational problems are commonly referred to as 'precipitates above the cloud point (CP).' NREL's Advanced Biofuels team spiked distilled soy and animal fat-derived B100, as well as B20, B10, and B5 biodiesel blends with three saturated monoglycerides (SMGs) at concentration levels comparable to those of real-world fuels. Above a threshold or eutectic concentration, the SMGs (monomyristin, monopalmitin, and monostearin) were shown to significantly raise the biodiesel CP, and had an even greater impact on the final melting temperature. Researchers discovered that upon cooling, monoglyceride initially precipitates as a metastable crystal, but it transforms over time or upon slight heating into a more stable crystal with a much lower solubility and higher melting temperature - and with increased potential to cause vehicle performance issues. This explains why fuel-filter clogging typically occurs over the course of long, repeated diurnal cooling cycles. The elevated final melting points mean that restarting vehicles with clogged filters can be difficult even after ambient temperatures have warmed to well above CP. By examining how biodiesel impurities affect filtration and crystallization during warming and cooling cycles, NREL researchers uncovered an explanation for poor biodiesel performance at low temperatures. The observation of a eutectic point, or a concentration below which SMGs have no effect, indicates that SMGs do not have to be completely removed from biodiesel to solve low-temperature performance problems.« less

SBIR Grant:No-Vibration Agile Cryogenic Optical Refrigerator

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

Epstein, Richard

2013-04-09

Optical refrigeration is currently the only all-solid-state cryocooling technology that has been demonstrated. Optical cryocoolers are devices that use laser light to cool small crystal or glass cooling elements. The cooling element absorbs the laser light and reradiates it at higher energy, an example of anti-Stokes fluorescence. The dif-ference between the energy of the outgoing and incoming light comes from the thermal energy of the cooling element, which in turn becomes colder. Entitled No-Vibration Agile Cryocoolers using Optical Refrigeration, this Phase I proposal directly addressed the continued development of the optical refrigerator components necessary to transition this scientific breakthrough intomore » National Nu-clear Security Administration (NNSA) sensor applications in line with the objectives of topic 50b. ThermoDynamic Films LLC (TDF), in collaboration with the University of New Mexico (UNM), cooled an optical-refrigerator cooling element comprised of an ytterbium-doped yttrium lithium fluoride (Yb:YLF) crystal from room tempera-ture to 123 K with about 2% efficiency. This is the world record in optical refrigera-tion and an important step toward revolutionizing cryogenic systems for sensor ap-plications. During this period, they also designed and analyzed the crucial elements of a prototype optical refrigerator including the thermal link that connects the cool-ing element with the load.« less

The effect of oxygen fugacity on the rheological evolution of crystallizing basaltic melts

NASA Astrophysics Data System (ADS)

Kolzenburg, S.; Di Genova, D.; Giordano, D.; Hess, K. U.; Dingwell, D. B.

2018-04-01

Storage and transport of silicate melts in the Earth's crust and their emplacement on the planet's surface occur almost exclusively at sub-liquidus temperatures. At these conditions, the melts undergo crystallization under a wide range of cooling-rates, deformation-rates, and oxygen fugacities (fO2). Oxygen fugacity is known to influence the thermodynamics and kinetics of crystallization in magmas and lavas. Yet, its influence on sub-liquidus rheology remains largely uncharted. We present the first rheological characterization of crystallizing lavas along natural cooling paths and deformation-rates and at varying fO2. Specifically, we report on apparent viscosity measurements for two crystallizing magmatic suspensions 1) at log ⁡ fO2 of -9.15 (quartz-fayalite-magnetite buffer, QFM, -2.1) and 2) in air. These fugacities span a range of reduced to oxidized conditions pertinent to magma migration and lava emplacement. We find that: 1) crystallization at constant cooling-rates results in a quasi-exponential increase in the apparent viscosity of the magmatic suspensions until they achieve their rheological cut off temperature (Tcutoff), where the melt effectively solidifies 2) the rheological departure and Tcutoff increase with increasing fO2 and 3) increasing fO2 results in decreased crystallization-rates. Based on the experimental results and by comparison with previous rheological isothermal studies we propose a generalisation of the effect of fO2 on the dynamic rheological evolution of natural magmatic and volcanic suspensions. We further discuss the implications for magmatic transport in plumbing and storage systems (e.g. conduits, dikes and magma chambers) and during lava flow emplacement.

Advantages of a Special Post-Growth THM Program for the Reduction of Inclusions in CdTe Crystals

NASA Astrophysics Data System (ADS)

Fochuk, P.; Zakharuk, Z.; Nykonyuk, Ye.; Rarenko, A.; Kolesnik, M.; Bolotnikov, A. E.; Yang, G.; James, R. B.

2016-06-01

CdTe crystals are used widely for manufacturing gamma-ray radiation sensors, and we can improve their properties if we eliminate as many as possible of their Te inclusions. In this paper, we describe our two modes of removing them; first, we used the traveling heater method for growing them, and then we applied post-growth cooling, for which we used a special slow-cooling program. Here, we placed the CdTe ingot, containing inclusions, into a quartz container, and moved a narrow heater zone along it. The molten inclusions moved together with the hot zone, and, at end of the process, they were concentrated heavily at the ingot's surface. Consequently, very few inclusions were observed in much of the CdTe ingot. Hall effect measurements showed that after such annealing the value of the carrier mobility was increased significantly, and the concentration of ionized centers was reduced. One major advantage of this treatment, compared to thermal annealing alone, is that both the inclusions and impurities are eliminated simultaneously.

Cation–Eutectic Transition via Sublattice Melting in CuInP 2S 6/In 4/3P 2S 6 van der Waals Layered Crystals

DOE PAGES

Susner, Michael A.; Chyasnavichyus, Marius; Puretzky, Alexander A.; ...

2017-07-07

Single crystals of the van der Waals layered ferrielectric material CuInP 2S 6 spontaneously phase separate when synthesized with Cu deficiency. In this paper, we identify a route to form and tune intralayer heterostructures between the corresponding ferrielectric (CuInP 2S 6) and paraelectric (In 4/3P 2S 6) phases through control of chemical phase separation. We conclusively demonstrate that Cu-deficient Cu 1–xIn 1+x/3P 2S 6 forms a single phase at high temperature. We also identify the mechanism by which the phase separation proceeds upon cooling. Above 500 K both Cu + and In 3+ become mobile, while P 2S 6 4–more » anions maintain their structure. We therefore propose that this transition can be understood as eutectic melting on the cation sublattice. Such a model suggests that the transition temperature for the melting process is relatively low because it requires only a partial reorganization of the crystal lattice. As a result, varying the cooling rate through the phase transition controls the lateral extent of chemical domains over several decades in size. At the fastest cooling rate, the dimensional confinement of the ferrielectric CuInP 2S 6 phase to nanoscale dimensions suppresses ferrielectric ordering due to the intrinsic ferroelectric size effect. Finally, intralayer heterostructures can be formed, destroyed, and re-formed by thermal cycling, thus enabling the possibility of finely tuned ferroic structures that can potentially be optimized for specific device architectures.« less

Cation–Eutectic Transition via Sublattice Melting in CuInP 2S 6/In 4/3P 2S 6 van der Waals Layered Crystals

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

Susner, Michael A.; Chyasnavichyus, Marius; Puretzky, Alexander A.

Single crystals of the van der Waals layered ferrielectric material CuInP 2S 6 spontaneously phase separate when synthesized with Cu deficiency. In this paper, we identify a route to form and tune intralayer heterostructures between the corresponding ferrielectric (CuInP 2S 6) and paraelectric (In 4/3P 2S 6) phases through control of chemical phase separation. We conclusively demonstrate that Cu-deficient Cu 1–xIn 1+x/3P 2S 6 forms a single phase at high temperature. We also identify the mechanism by which the phase separation proceeds upon cooling. Above 500 K both Cu + and In 3+ become mobile, while P 2S 6 4–more » anions maintain their structure. We therefore propose that this transition can be understood as eutectic melting on the cation sublattice. Such a model suggests that the transition temperature for the melting process is relatively low because it requires only a partial reorganization of the crystal lattice. As a result, varying the cooling rate through the phase transition controls the lateral extent of chemical domains over several decades in size. At the fastest cooling rate, the dimensional confinement of the ferrielectric CuInP 2S 6 phase to nanoscale dimensions suppresses ferrielectric ordering due to the intrinsic ferroelectric size effect. Finally, intralayer heterostructures can be formed, destroyed, and re-formed by thermal cycling, thus enabling the possibility of finely tuned ferroic structures that can potentially be optimized for specific device architectures.« less

TRANSVERSE MODE ELECTRO-OPTIC MATERIALS.

DTIC Science & Technology

electro - optic modulators presently used are crystals such as KDP which exhibit a longitudinal electro - optic effect. It has been demonstrated that a more efficient modulator can be produced when a crystal having a transverse electro - optic effect is employed. Generally these crystals are produced either from the melt or from fluxes. Since melt grown crystals must be cooled through several hundred degrees and often must undergo phase transitions, these crystals are generally highly strained. Flux grown crystals are also

Crystal Nucleation Using Surface-Energy-Modified Glass Substrates.

PubMed

Nordquist, Kyle A; Schaab, Kevin M; Sha, Jierui; Bond, Andrew H

2017-08-02

Systematic surface energy modifications to glass substrates can induce nucleation and improve crystallization outcomes for small molecule active pharmaceutical ingredients (APIs) and proteins. A comparatively broad probe for function is presented in which various APIs, proteins, organic solvents, aqueous media, surface energy motifs, crystallization methods, form factors, and flat and convex surface energy modifications were examined. Replicate studies ( n ≥ 6) have demonstrated an average reduction in crystallization onset times of 52(4)% (alternatively 52 ± 4%) for acetylsalicylic acid from 91% isopropyl alcohol using two very different techniques: bulk cooling to 0 °C using flat surface energy modifications or microdomain cooling to 4 °C from the interior of a glass capillary having convex surface energy modifications that were immersed in the solution. For thaumatin and bovine pancreatic trypsin, a 32(2)% reduction in crystallization onset times was demonstrated in vapor diffusion experiments ( n ≥ 15). Nucleation site arrays have been engineered onto form factors frequently used in crystallization screening, including microscope slides, vials, and 96- and 384-well high-throughput screening plates. Nucleation using surface energy modifications on the vessels that contain the solutes to be crystallized adds a layer of useful variables to crystallization studies without requiring significant changes to workflows or instrumentation.

Crystalline nucleation in undercooled liquids: a Bayesian data-analysis approach for a nonhomogeneous Poisson process.

PubMed

Filipponi, A; Di Cicco, A; Principi, E

2012-12-01

A Bayesian data-analysis approach to data sets of maximum undercooling temperatures recorded in repeated melting-cooling cycles of high-purity samples is proposed. The crystallization phenomenon is described in terms of a nonhomogeneous Poisson process driven by a temperature-dependent sample nucleation rate J(T). The method was extensively tested by computer simulations and applied to real data for undercooled liquid Ge. It proved to be particularly useful in the case of scarce data sets where the usage of binned data would degrade the available experimental information.

Linking Plagioclase Zoning Patterns to Active Magma Processes

NASA Astrophysics Data System (ADS)

Izbekov, P. E.; Nicolaysen, K. P.; Neill, O. K.; Shcherbakov, V.; Plechov, P.; Eichelberger, J. C.

2015-12-01

Plagioclase, one of the most common and abundant mineral phases in volcanic products, will vary in composition in response to changes in temperature, pressure, composition of the ambient silicate melt, and melt H2O concentration. Changes in these parameters may cause dissolution or growth of plagioclase crystals, forming characteristic textural and compositional variations (zoning patterns), the complete core-to-rim sequence of which describes events experienced by an individual crystal from its nucleation to the last moments of its growth. Plagioclase crystals in a typical volcanic rock may look drastically dissimilar despite their spatial proximity and the fact that they have erupted together. Although they shared last moments of their growth during magma ascent and eruption, their prior experiences could be very different, as plagioclase crystals often come from different domains of the same magma system. Distinguishing similar zoning patterns, correlating them across the entire population of plagioclase crystals, and linking these patterns to specific perturbations in the magmatic system may provide additional perspective on the variety, extent, and timing of magma processes at active volcanic systems. Examples of magma processes, which may be distinguished based on plagioclase zoning patterns, include (1) cooling due to heat loss, (2) heating and/or pressure build up due to an input of new magmatic material, (3) pressure drop in response to magma system depressurization, and (4) crystal transfer between different magma domains/bodies. This review will include contrasting examples of zoning patters from recent eruptions of Karymsky, Bezymianny, and Tolbachik Volcanoes in Kamchatka, Augustine and Cleveland Volcanoes in Alaska, as well as from the drilling into an active magma body at Krafla, Iceland.

Features of changes in electrophysical properties of silicon under the influence of thermal treatment

NASA Astrophysics Data System (ADS)

Gaidar, G. P.; Baranskii, P. I.

2018-06-01

The influence of the annealing temperatures and cooling rates of n-silicon crystals, grown by the Czochralski method and doped with phosphorus impurity, on their electric and thermoelectric properties was studied. In the region of predominantly impurity scattering a more essential dependence of the charge carrier mobility on the cooling conditions of crystals was established in comparison with the dependence on the annealing temperature. The analysis of the measurement results of tensoresistance and tenso-thermo-emf was carried out, on the basis of which the dependence of the anisotropy parameter of drag thermo-emf on the cooling rate was obtained. The feature of the anisotropy parameter of thermo-emf M in the form of its maximal deviation from the linear dependence M = M(lg(υcl)) was revealed in the region of cooling rates from 8 to 15 K/min.

Diffusion-driven magnesium and iron isotope fractionation in Hawaiian olivine

USGS Publications Warehouse

Teng, F.-Z.; Dauphas, N.; Helz, R.T.; Gao, S.; Huang, S.

2011-01-01

Diffusion plays an important role in Earth sciences to estimate the timescales of geological processes such as erosion, sediment burial, and magma cooling. In igneous systems, these diffusive processes are recorded in the form of crystal zoning. However, meaningful interpretation of these signatures is often hampered by the fact that they cannot be unambiguously ascribed to a single process (e.g., magmatic fractionation, diffusion limited transport in the crystal or in the liquid). Here we show that Mg and Fe isotope fractionations in olivine crystals can be used to trace diffusive processes in magmatic systems. Over sixty olivine fragments from Hawaiian basalts show isotopically fractionated Mg and Fe relative to basalts worldwide, with up to 0.4??? variation in 26Mg/24Mg ratios and 1.6??? variation in 56Fe/54Fe ratios. The linearly and negatively correlated Mg and Fe isotopic compositions [i.e., ??56Fe=(??3.3??0.3)????26Mg], co-variations of Mg and Fe isotopic compositions with Fe/Mg ratios of olivine fragments, and modeling results based on Mg and Fe elemental profiles demonstrate the coupled Mg and Fe isotope fractionation to be a manifestation of Mg-Fe inter-diffusion in zoned olivines during magmatic differentiation. This characteristic can be used to constrain the nature of mineral zoning in igneous and metamorphic rocks, and hence determine the residence times of crystals in magmas, the composition of primary melts, and the duration of metamorphic events. With improvements in methodology, in situ isotope mapping will become an essential tool of petrology to identify diffusion in crystals. ?? 2011 Elsevier B.V.

Crystallization tendency of active pharmaceutical ingredients following rapid solvent evaporation--classification and comparison with crystallization tendency from undercooled melts.

PubMed

Van Eerdenbrugh, Bernard; Baird, Jared A; Taylor, Lynne S

2010-09-01

In this study, the crystallization behavior of a variety of compounds was studied following rapid solvent evaporation using spin coating. Initial screening to determine model compound suitability was performed using a structurally diverse set of 51 compounds in three different solvent systems [dichloromethane (DCM), a 1:1 (w/w) dichloromethane/ethanol mixture (MIX), and ethanol (EtOH)]. Of this starting set of 153 drug-solvent combinations, 93 (40 compounds) were selected for further evaluation based on solubility, chemical solution stability, and processability criteria. These systems were spin coated and their crystallization was monitored using polarized light microscopy (7 days, dry conditions). The crystallization behavior of the samples could be classified as rapid (Class I: 39 cases), intermediate (Class II: 23 cases), or slow (Class III: 31 cases). The solvent system employed influenced the classification outcome for only four of the compounds. The various compounds showed very diverse crystallization behavior. Upon comparison of classification results with those of a previous study, where cooling from the melt was used as a preparation technique, a good similarity was found whereby 68% of the cases were identically classified. Multivariate analysis was performed using a set of relevant physicochemical compound characteristics. It was found that a number of these parameters tended to differ between the different classes. These could be further interpreted in terms of the nature of the crystallization process. Additional multivariate analysis on the separate classes of compounds indicated some potential in predicting the crystallization tendency of a given compound.

Rapid hydrothermal cooling above the axial melt lens at fast-spreading mid-ocean ridge: Quantification through intra-plagioclase diffusion revealed by IODP Hole 1256D

NASA Astrophysics Data System (ADS)

Zhang, C.; Koepke, J.; Kirchner, C.; Götze, N.; Behrens, H.

2014-12-01

At fast-spreading mid-ocean ridges the axial melt lenses sandwiched between the lower oceanic crust and the sheeted dike sequences are assumed to be the major magma source of oceanic crust accretion. According to the widely discussed "gabbro glacier" model, the formation of the lower oceanic crust requires efficient cooling of the axial melt lens, resulting in partly crystallization and leading to crystal-melt mush which may subside down to form the lower crust. These processes are believed to be controlled dominantly by periodical magma supply and hydrothermal circulation above melt lens. Here we quantify the cooling rate above melt lens using chemical zoning of plagioclase from hornfelsic recrystallized sheeted dikes overlying the uppermost gabbros, which are part of the dike-gabbro transition zone drilled in Hole 1256D in the Eastern equatorial Pacific by the Integrated Ocean Drilling Program, where for the first time the dike-gabbro transition zone of an intact oceanic crust was penetrated and sampled. The measured zoning patterns are supposed to be a combined result of diffusion during both on-ridge and off-ridge cooling. We estimate the on-ridge cooling rate using a forward modelling approach based on CaAl-NaSi interdiffusion in plagioclase. The results show that the recrystallized sheeted dikes have been cooled from the peak thermal overprint at 1000-1050 °C to 600 °C within about 5-30 years as a result of hydrothermal circulation above a melt lens during a period of magma starvation, corresponding to a cooling rate of 30±15 °C/yr. Heat balance calculation also approves that in order to balance the heat output of a melt lens at a fast-spreading mid-ocean ridge similar to the case of IODP Hole 1256D, the cooling rate above the melt lens is required to be around 30 °C/yr. The estimated rapid hydrothermal cooling rate coincides with the observed annual to decal episodes of melt lens fluctuation and lava eruption, which favors the "gabbro glacier" model and explains how the effective heat extraction from melt lens is achieved at fast-spreading mid-ocean ridges.

Self-assembling process of Oxalamide compounds and their nucleation efficiency in bio-degradable Poly(hydroxyalkanoate)s

NASA Astrophysics Data System (ADS)

Ma, Piming; Deshmukh, Yogesh S.; Wilsens, Carolus H. R. M.; Ryan Hansen, Michael; Graf, Robert; Rastogi, Sanjay

2015-08-01

One of the key requirements in semi-crystalline polyesters, synthetic or bio-based, is the control on crystallization rate and crystallinity. One of the limiting factors in the commercialization of the bio-based polyesters, for example polyhydroxyalkanoates synthesized by bacteria for energy storage purposes, is the slow crystallization rate. In this study, we show that by tailoring the molecular structure of oxalamide compounds, it is possible to dissolve these compounds in molten poly(hydroxybutyrate) (PHB), having a hydroxyvalerate co-monomer content of less than 2 mol%. Upon cooling the polymer melt, the homogeneously dispersed oxalamide compound crystallizes just below the melting temperature of the polymer. The phase-separated compound reduces the nucleation barrier of the polymer, thus enhancing the crystallization rate, nucleation density and crystallinity. The findings reported in this study provide a generic route for the molecular design of oxalamide-based compounds that can be used for enhancing nucleation efficiency of semi-crystalline bio-based polyesters.

Seed crystals with improved properties for melt processing superconductors for practical applications

DOEpatents

Veal, Boyd W.; Paulikas, Arvydas; Balachandran, Uthamalingam; Zhong, Wei

1997-01-01

A method of fabricating bulk superconducting material including RBa.sub.2 Cu.sub.3 O.sub.7-.delta. comprising heating compressed powder oxides and/or carbonates of R and Ba and Cu present in mole ratios to form RBa.sub.2 Cu.sub.3 O.sub.7-.delta. in physical contact with an oxide single crystal seed to a temperature sufficient to form a liquid phase in the RBa.sub.2 Cu.sub.3 O.sub.7-.delta. while maintaining the single crystal seed solid to grow the superconducting material and thereafter cooling to provide a material including RBa.sub.2 Cu.sub.3 O.sub.7-.delta.. R is a rare earth or Y or La and the single crystal seed has a lattice mismatch with RBa.sub.2 Cu.sub.3 O.sub.7-.delta. of less than about 2% at the growth temperature. The starting material may be such that the final product contains a minor amount of R.sub.2 BaCuO.sub.5.

Separation and Precipitation of Nickel from Acidic Sulfate Leaching Solution of Molybdenum-Nickel Black Shale by Potassium Nickel Sulfate Hexahydrate Crystallization

NASA Astrophysics Data System (ADS)

Deng, Zhigan; Wei, Chang; Fan, Gang; Li, Xingbin; Li, Minting; Li, Cunxiong

2018-02-01

Nickel was separated and precipitated with potassium nickel sulfate hexahydrate [K2Ni(SO4)2·6H2O] from acidic sulfate solution, a leach solution from molybdenum-nickel black shale. The effects of the potassium sulfate (K2SO4) concentration, crystallization temperature, solution pH, and crystallization time on nickel(II) recovery and iron(III) precipitation were investigated, revealing that nickel and iron were separated effectively. The optimum parameters were K2SO4 concentration of 200 g/L, crystallization temperature of 10°C, solution pH of 0.5, and crystallization time of 24 h. Under these conditions, 97.6% nickel(II) was recovered as K2Ni(SO4)2·6H2O crystals while only 2.0% of the total iron(III) was precipitated. After recrystallization, 98.4% pure K2Ni(SO4)2·6H2O crystals were obtained in the solids. The mother liquor was purified by hydrolysis-precipitation followed by cooling, and more than 99.0% K2SO4 could be crystallized. A process flowsheet was developed to separate iron(III) and nickel(II) from acidic-sulfate solution.

Conductive properties of switchable photoluminescence thermosetting systems based on liquid crystals.

PubMed

Tercjak, Agnieszka; Gutierrez, Junkal; Ocando, Connie; Mondragon, Iñaki

2010-03-16

Conductive properties of different thermosetting materials modified with nematic 4'-(hexyl)-4-biphenyl-carbonitrile (HBC) liquid crystal and rutile TiO(2) nanoparticles were successfully studied by means of tunneling atomic force miscroscopy (TUNA). Taking into account the liquid crystal state of the HBC at room temperature, depending on both the HBC content and the presence of TiO(2) nanoparticles, designed materials showed different TUNA currents passed through the sample. The addition of TiO(2) nanoparticles into the systems multiply the detected current if compared to the thermosetting systems without TiO(2) nanoparticles and simultaneously stabilized the current passed through the sample, making the process reversible since the absolute current values were almost the same applying both negative and positive voltage. Moreover, thermosetting systems modified with liquid crystals with and without TiO(2) nanoparticles are photoluminescence switchable materials as a function of temperature gradient during repeatable heating/cooling cycle. Conductive properties of switchable photoluminescence thermosetting systems based on liquid crystals can allow them to find potential application in the field of photoresponsive devices, with a high contrast ratio between transparent and opaque states.

Influence of convection on free growth of dendrite crystals from solution

NASA Technical Reports Server (NTRS)

Hallett, J.; Wedum, E.

1979-01-01

The free growth of dendrites in a uniformly supercooled solution was examined using cine photography with a Schlieren optical system. Crystals were grown in the bulk of the solution from a centrally located capillary tube, nucleated at the interface with a liquid nitrogen cooled wire. Crystals propagated along the tube, the slower growing orientations eliminated, and emerged at the tip, usually growing parallel to the tube direction. For both sodium sulfate decahydrate from its solution and ice from sodium chloride solution, growth rate and fineness of dendrites increased with supercooling. In sodium sulfate, upward convection of the less dense depleted solution occurs; downward convection was observed for the rejected, more concentrated sodium chloride solution. In both cases, there was a spatial and temporal delay in the release of the convective plume from the moving dendrite tip. The role of this convection on the growth characteristics and the production of secondary crystals is examined. A proposed low-g experiment to examine differences in growth rate, crystal texture, and secondary nucleation in a reduced convective regime where molecular diffusion is the dominant transfer process is discussed.

Crystallization in high-level waste glass: A review of glass theory and noteworthy literature

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

Christian, J. H.

2015-08-18

There is a fundamental need to continue research aimed at understanding nepheline and spinel crystal formation in high-level waste (HLW) glass. Specifically, the formation of nepheline solids (K/NaAlSiO 4) during slow cooling of HLW glass can reduce the chemical durability of the glass, which can cause a decrease in the overall durability of the glass waste form. The accumulation of spinel solids ((Fe, Ni, Mn, Zn)(Fe, Cr) 2O 4), while not detrimental to glass durability, can cause an array of processing problems inside HLW glass melters. In this review, the fundamental differences between glass and solid-crystals are explained using kinetic,more » thermodynamic, and viscosity arguments, and several highlights of glass-crystallization research, as it pertains to high-level waste vitrification, are described. In terms of mitigating spinel in the melter and both spinel and nepheline formation in the canister, the complexity of HLW glass and the intricate interplay between thermal, chemical, and kinetic factors further complicates this understanding. However, new experiments seeking to elucidate the contributing factors of crystal nucleation and growth in waste glass, and the compilation of data from older experiments, may go a long way towards helping to achieve higher waste loadings while developing more efficient processing strategies. Higher waste loadings and more efficient processing strategies will reduce the overall HLW Hanford Tank Waste Treatment and Immobilization Plant (WTP) vitrification facilities mission life.« less

Initiating Growth Of Crystals Away From Container Walls

NASA Technical Reports Server (NTRS)

Kroes, Roger L.; Reiss, Donald A.; Lehoczky, Sandor L.

1991-01-01

Nucleation controlled to obtain better crystals. In technique proposed specifically for growing large protein crystals in microgravity (where no thermal convection), small region of high supersaturation created by injection of hot concentrated solution or by use of cold probe. Crystals nucleate preferably in this small region. Also conceivable technique applied on Earth to crystallizations in melts and solutions sufficiently viscous to suppress convection to extent necessary to prevent cooling-induced nucleation in undesired sites.

'Nose method' of calculating critical cooling rates for glass formation

NASA Technical Reports Server (NTRS)

Weinberg, Michael C.; Uhlmann, Donald R.; Zanotto, Edgar D.

1989-01-01

The use of the so-called 'nose method' for computing critical cooling rates for glass formation is examined and compared with other methods, presenting data for the glass-forming systems SiO2, GeO2, and P2O5. It is shown that, for homogeneous crystallization, the nose-method will give an overestimate of Rc, a conclusion which was drawn after assessing the enfluence of a range of values for the parameters which control crystal growth and nucleation. The paper also proposes an alternative simple procedure (termed the 'cutoff method') for computing critical cooling rates from T-T-T diagrams, which was shown in the SiO2 and GeO2 systems to be superior to the nose method.

Crystal Engineering for Low Defect Density and High Efficiency Hybrid Chemical Vapor Deposition Grown Perovskite Solar Cells.

PubMed

Ng, Annie; Ren, Zhiwei; Shen, Qian; Cheung, Sin Hang; Gokkaya, Huseyin Cem; So, Shu Kong; Djurišić, Aleksandra B; Wan, Yangyang; Wu, Xiaojun; Surya, Charles

2016-12-07

Synthesis of high quality perovskite absorber is a key factor in determining the performance of the solar cells. We demonstrate that hybrid chemical vapor deposition (HCVD) growth technique can provide high level of versatility and repeatability to ensure the optimal conditions for the growth of the perovskite films as well as potential for batch processing. It is found that the growth ambient and degree of crystallization of CH 3 NH 3 PbI 3 (MAPI) have strong impact on the defect density of MAPI. We demonstrate that HCVD process with slow postdeposition cooling rate can significantly reduce the density of shallow and deep traps in the MAPI due to enhanced material crystallization, while a mixed O 2 /N 2 carrier gas is effective in passivating both shallow and deep traps. By careful control of the perovskite growth process, a champion device with power conversion efficiency of 17.6% is achieved. Our work complements the existing theoretical studies on different types of trap states in MAPI and fills the gap on the theoretical analysis of the interaction between deep levels and oxygen. The experimental results are consistent with the theoretical predictions.

Solid state crystal physics at very low temperatures

NASA Technical Reports Server (NTRS)

Davis, W.; Krack, K.; Richard, J. P.; Weber, J.

1980-01-01

The properties of nearly perfect crystals was studied at cryogenic temperatures. A large Helium 3 and Helium 4 dilution refrigerator has been assembled, and is described. A cryostat suitable for cooling a 35 liter volume to .020 Kelvin was designed and constructed, together with instrumentation to observe the properties of nearly perfect crystals.

Defect-induced local variation of crystal phase transition temperature in metal-halide perovskites.

PubMed

Dobrovolsky, Alexander; Merdasa, Aboma; Unger, Eva L; Yartsev, Arkady; Scheblykin, Ivan G

2017-06-26

Solution-processed organometal halide perovskites are hybrid crystalline semiconductors highly interesting for low-cost and efficient optoelectronics. Their properties are dependent on the crystal structure. Literature shows a variety of crystal phase transition temperatures and often a spread of the transition over tens of degrees Kelvin. We explain this inconsistency by demonstrating that the temperature of the tetragonal-to-orthorhombic phase transition in methylammonium lead triiodide depends on the concentration and nature of local defects. Phase transition in individual nanowires was studied by photoluminescence microspectroscopy and super-resolution imaging. We propose that upon cooling from 160 to 140 K, domains of the crystal containing fewer defects stay in the tetragonal phase longer than highly defected domains that readily transform to the high bandgap orthorhombic phase at higher temperatures. The existence of relatively pure tetragonal domains during the phase transition leads to drastic photoluminescence enhancement, which is inhomogeneously distributed across perovskite microcrystals.Understanding crystal phase transition in materials is of fundamental importance. Using luminescence spectroscopy and super-resolution imaging, Dobrovolsky et al. study the transition from the tetragonal to orthorhombic crystal phase in methylammonium lead triiodide nanowires at low temperature.

Giant magnetocaloric effect and temperature induced magnetization jump in GdCrO{sub 3} single crystal

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

Yin, L. H.; Yang, J.; Kan, X. C.

2015-04-07

We report on a systematic study of the single-crystal GdCrO{sub 3}, which shows various novel magnetic features, such as temperature-induced magnetization reversal (TMR), temperature-induced magnetization jump (TMJ), spin reorientation, and giant magnetocaloric effect (MCE). In the field-cooled cooling process with modest magnetic field along the c axis, GdCrO{sub 3} first shows a TMR at T{sub comp}∼120−130 K and then an abrupt TMJ with a sign change of magnetization at T{sub jump}∼52−120 K, and finally a spin reorientation at T{sub SR}∼4−7 K. Interestingly, the remarkable TMJ behavior, which was not reported ever before, persists at higher fields up to 10 kOe even when TMRmore » disappears. In addition, giant MCE with the maximum value of magnetic entropy change reaching ∼31.6 J/kg K for a field change of 44 kOe was also observed in GdCrO{sub 3} single crystal, suggesting it could be a potential material for low-T magnetic refrigeration. A possible mechanism for these peculiar magnetic behaviors is discussed based on the various competing magnetic interactions between the 3d electrons of Cr{sup 3+} ions and 4f electrons of Gd{sup 3+} ions.« less

Experimental validation of analytical models for a rapid determination of cycle parameters in thermoplastic injection molding

NASA Astrophysics Data System (ADS)

Pignon, Baptiste; Sobotka, Vincent; Boyard, Nicolas; Delaunay, Didier

2017-10-01

Two different analytical models were presented to determine cycle parameters of thermoplastics injection process. The aim of these models was to provide quickly a first set of data for mold temperature and cooling time. The first model is specific to amorphous polymers and the second one is dedicated to semi-crystalline polymers taking the crystallization into account. In both cases, the nature of the contact between the polymer and the mold could be considered as perfect or not (thermal contact resistance was considered). Results from models are compared with experimental data obtained with an instrumented mold for an acrylonitrile butadiene styrene (ABS) and a polypropylene (PP). Good agreements were obtained for mold temperature variation and for heat flux. In the case of the PP, the analytical crystallization times were compared with those given by a coupled model between heat transfer and crystallization kinetics.

SKYLAB (SL)-4 - POST-FLIGHT (WASHINGTON, D.C.)

NASA Image and Video Library

1974-10-01

S74-34046 (October 1974) --- Dr. James C. Fletcher, left, NASA Administrator, explains the formation of the indium-antimonide crystal, manufactured in space, to President Gerald R. Ford at the White House. Standing at right is Harold Johnson, Chairman of the Massachusetts Institute of Technology. The segment of indium-antimonide is cut from a cylindrical single crystal that was partially melted and resolidified aboard the Skylab space station on Jan. 6, 1974, during the third and final manned flight. This segment is approximately one by one centimeters and about three millimeters thick. The sequence of heating and cooling was started and supervised by the members of the third Skylab crew, astronauts Gerald P. Carr, Edward G. Gibson and William R. Pogue. The crystal forming was accomplished in a special multipurpose furnace, known as the Materials Processing Facility (Skylab Technology Experiment M512). Photo credit: NASA

Solidification of undercooled liquids

NASA Technical Reports Server (NTRS)

Perepezko, J. H.; Shiohara, Y.; Paik, J. S.; Flemmings, M. C.

1982-01-01

During rapid solidification processing (RSP) the amount of liquid undercooling is an important factor in determining microstructural development by controlling phase selection during nucleation and morphological evolution during crystal growth. While undercooling is an inherent feature of many techniques of RSP, the deepest undercoolings and most controlled studies have been possible in carefully prepared fine droplet samples. From past work and recent advances in studies of nucleation kinetics it has become clear that the initiation of crystallization during RSP is governed usually by heterogeneous sites located at surfaces. With known nucleant sites, it has been possible to identify specific pathways of metastable phase formation and microstructural development in alloys. These advances have allowed for a clearer assessment of the interplay between undercooling, cooling rate and particle size statistics in structure formation. New approaches to the examination of growth processes have been developed to follow the thermal behavior and morphology in small samples in the period of rapid crystallization and recalescence. Based upon the new experimental information from these studies, useful models can be developed for the overall solidification process to include nucleation behavior, thermodynamic constraints, thermal history, growth kinetics, solute redistribution and resulting structures. From the refinement of knowledge concerning the underlying factors that govern RSP a basis is emerging for an effective alloy design and processing strategy.

Bulk formation of a metallic glass - Pd40Ni40P20

NASA Technical Reports Server (NTRS)

Drehman, A. J.; Greer, A. L.; Turnbull, D.

1982-01-01

Molten spheroids of Pd40Ni40P20, of up to 0.53-cm minor diameter, were slowly cooled (1.4 K/s) on a fused silica surface under 10 to the -6 torr vacuum to a form which was entirely glassy except for some superficial crystallinity comprising less than 0.5% of the volume. The occurrence of crystallization was eliminated by subjecting the specimens to surface etching followed by a succession of heating and cooling cycles. The absence of crystallization in bulk was confirmed by X-ray diffraction, transmission electron microscopy, and calorimetry. Using the last technique, the heat of crystallization of the glass was measured to be 5.3 + or - 0.3 kJ/g atom.

Studies of the Influence of Beam Profile and Cooling Conditions on the Laser Deposition of a Directionally-Solidified Superalloy.

PubMed

Yang, Shuo; Du, Dong; Chang, Baohua

2018-02-04

In the laser deposition of single crystal and directionally-solidified superalloys, it is desired to form laser deposits with high volume fractions of columnar grains by suppressing the columnar-to-equiaxed transition efficiently. In this paper, the influence of beam profile (circular and square shapes) and cooling conditions (natural cooling and forced cooling) on the geometric morphology and microstructure of deposits were experimentally studied in the laser deposition of a directionally-solidified superalloy, IC10, and the mechanisms of influence were revealed through a numerical simulation of the thermal processes during laser deposition. The results show that wider and thinner deposits were obtained with the square laser beam than those with the circular laser beam, regardless of whether natural or forced cooling conditions was used. The heights and contact angles of deposits were notably increased due to the reduced substrate temperatures by the application of forced cooling for both laser beam profiles. Under natural cooling conditions, columnar grains formed epitaxially at both the center and the edges of the deposits with the square laser beam, but only at the center of the deposits with the circular laser beam; under forced cooling conditions, columnar grains formed at both the center and the edges of deposits regardless of the laser beam profile. The high ratios of thermal gradient and solidification velocity in the height direction of the deposits were favorable to forming deposits with higher volume fractions of columnar grains.

Studies of the Influence of Beam Profile and Cooling Conditions on the Laser Deposition of a Directionally-Solidified Superalloy

PubMed Central

Yang, Shuo; Du, Dong

2018-01-01

In the laser deposition of single crystal and directionally-solidified superalloys, it is desired to form laser deposits with high volume fractions of columnar grains by suppressing the columnar-to-equiaxed transition efficiently. In this paper, the influence of beam profile (circular and square shapes) and cooling conditions (natural cooling and forced cooling) on the geometric morphology and microstructure of deposits were experimentally studied in the laser deposition of a directionally-solidified superalloy, IC10, and the mechanisms of influence were revealed through a numerical simulation of the thermal processes during laser deposition. The results show that wider and thinner deposits were obtained with the square laser beam than those with the circular laser beam, regardless of whether natural or forced cooling conditions was used. The heights and contact angles of deposits were notably increased due to the reduced substrate temperatures by the application of forced cooling for both laser beam profiles. Under natural cooling conditions, columnar grains formed epitaxially at both the center and the edges of the deposits with the square laser beam, but only at the center of the deposits with the circular laser beam; under forced cooling conditions, columnar grains formed at both the center and the edges of deposits regardless of the laser beam profile. The high ratios of thermal gradient and solidification velocity in the height direction of the deposits were favorable to forming deposits with higher volume fractions of columnar grains. PMID:29401715

On the possibility of laser cooling of Cr3+ ions doped crystals

NASA Astrophysics Data System (ADS)

Feofilov, S. P.; Kulinkin, A. B.

2018-01-01

The fluorescence of Cr3+ ions doped insulating crystals was studied under the excitation in the long-wavelength tail of the absorption spectrum ("laser cooling regime"). The 4T2 - 4A2 and 2E - 4A2 fluorescence spectra with a dominant anti-Stokes component were observed. Though no optical refrigeration was detected in the presented experiments, the spectroscopic results suggest that electron-phonon bands of Cr3+ ions are of interest for further investigations from the point of view of achieving optical refrigeration.

Why is intracellular ice lethal? A microscopical study showing evidence of programmed cell death in cryo-exposed embryonic axes of recalcitrant seeds of Acer saccharinum

PubMed Central

Wesley-Smith, James; Walters, Christina; Pammenter, N. W.

2015-01-01

Background and Aims Conservation of the genetic diversity afforded by recalcitrant seeds is achieved by cryopreservation, in which excised embryonic axes (or, where possible, embryos) are treated and stored at temperatures lower than −180 °C using liquid nitrogen. It has previously been shown that intracellular ice forms in rapidly cooled embryonic axes of Acer saccharinum (silver maple) but this is not necessarily lethal when ice crystals are small. This study seeks to understand the nature and extent of damage from intracellular ice, and the course of recovery and regrowth in surviving tissues. Methods Embryonic axes of A. saccharinum, not subjected to dehydration or cryoprotection treatments (water content was 1·9 g H2O g−1 dry mass), were cooled to liquid nitrogen temperatures using two methods: plunging into nitrogen slush to achieve a cooling rate of 97 °C s−1 or programmed cooling at 3·3 °C s−1. Samples were thawed rapidly (177 °C s−1) and cell structure was examined microscopically immediately, and at intervals up to 72 h in vitro. Survival was assessed after 4 weeks in vitro. Axes were processed conventionally for optical microscopy and ultrastructural examination. Key Results Immediately following thaw after cryogenic exposure, cells from axes did not show signs of damage at an ultrastructural level. Signs that cells had been damaged were apparent after several hours of in vitro culture and appeared as autophagic decomposition. In surviving tissues, dead cells were sloughed off and pockets of living cells were the origin of regrowth. In roots, regrowth occurred from the ground meristem and procambium, not the distal meristem, which became lethally damaged. Regrowth of shoots occurred from isolated pockets of surviving cells of peripheral and pith meristems. The size of these pockets may determine the possibility for, the extent of and the vigour of regrowth. Conclusions Autophagic degradation and ultimately autolysis of cells following cryo-exposure and formation of small (0·2–0·4 µm) intracellular ice crystals challenges current ideas that ice causes immediate physical damage to cells. Instead, freezing stress may induce a signal for programmed cell death (PCD). Cells that form more ice crystals during cooling have faster PCD responses. PMID:25808653

Well-ordered polymer nano-fibers with self-cleaning property by disturbing crystallization process.

PubMed

Yang, Qin; Luo, Zhuangzhu; Tan, Sheng; Luo, Yimin; Wang, Yunjiao; Zhang, Zhaozhu; Liu, Weimin

2014-01-01

Bionic self-cleaning surfaces with well-ordered polymer nano-fibers are firstly fabricated by disturbing crystallization during one-step coating-curing process. Orderly thin (100 nm) and long (5-10 μm) polymer nano-fibers with a certain direction are fabricated by external macroscopic force (F blow) interference introduced by H2 gas flow, leading to superior superhydrophobicity with a water contact angle (WCA) of 170° and a water sliding angle (WSA) of 0-1°. In contrast, nano-wires and nano-bridges (1-8 μm in length/10-80 nm in width) are generated by "spinning/stretching" under internal microscopic force (F T) interference due to significant temperature difference in the non-uniform cooling medium. The findings provide a novel theoretical basis for controllable polymer "bionic lotus" surface and will further promote practical application in many engineering fields such as drag-reduction and anti-icing.

Well-ordered polymer nano-fibers with self-cleaning property by disturbing crystallization process

NASA Astrophysics Data System (ADS)

Yang, Qin; Luo, Zhuangzhu; Tan, Sheng; Luo, Yimin; Wang, Yunjiao; Zhang, Zhaozhu; Liu, Weimin

2014-07-01

Bionic self-cleaning surfaces with well-ordered polymer nano-fibers are firstly fabricated by disturbing crystallization during one-step coating-curing process. Orderly thin (100 nm) and long (5-10 μm) polymer nano-fibers with a certain direction are fabricated by external macroscopic force ( F blow) interference introduced by H2 gas flow, leading to superior superhydrophobicity with a water contact angle (WCA) of 170° and a water sliding angle (WSA) of 0-1°. In contrast, nano-wires and nano-bridges (1-8 μm in length/10-80 nm in width) are generated by "spinning/stretching" under internal microscopic force ( F T) interference due to significant temperature difference in the non-uniform cooling medium. The findings provide a novel theoretical basis for controllable polymer "bionic lotus" surface and will further promote practical application in many engineering fields such as drag-reduction and anti-icing.

Computer Simulation To Assess The Feasibility Of Coring Magma

NASA Astrophysics Data System (ADS)

Su, J.; Eichelberger, J. C.

2017-12-01

Lava lakes on Kilauea Volcano, Hawaii have been successfully cored many times, often with nearly complete recovery and at temperatures exceeding 1100oC. Water exiting nozzles on the diamond core bit face quenches melt to glass just ahead of the advancing bit. The bit readily cuts a clean annulus and the core, fully quenched lava, passes smoothly into the core barrel. The core remains intact after recovery, even when there are comparable amounts of glass and crystals with different coefficients of thermal expansion. The unique resulting data reveal the rate and sequence of crystal growth in cooling basaltic lava and the continuous liquid line of descent as a function of temperature from basalt to rhyolite. Now that magma bodies, rather than lava pooled at the surface, have been penetrated by geothermal drilling, the question arises as to whether similar coring could be conducted at depth, providing fundamentally new insights into behavior of magma. This situation is considerably more complex because the coring would be conducted at depths exceeding 2 km and drilling fluid pressures of 20 MPa or more. Criteria that must be satisfied include: 1) melt is quenched ahead of the bit and the core itself must be quenched before it enters the barrel; 2) circulating drilling fluid must keep the temperature of the coring assembling cooled to within operational limits; 3) the drilling fluid column must nowhere exceed the local boiling point. A fluid flow simulation was conducted to estimate the process parameters necessary to maintain workable temperatures during the coring operation. SolidWorks Flow Simulation was used to estimate the effect of process parameters on the temperature distribution of the magma immediately surrounding the borehole and of drilling fluid within the bottom-hole assembly (BHA). A solid model of the BHA was created in SolidWorks to capture the flow behavior around the BHA components. Process parameters used in the model include the fluid properties and temperature of magma, coolant flow rate, rotation speed, and rate of penetration (ROP). The modeling results indicate that there are combinations of process parameters that will provide sufficient cooling to enable the desired coring process in magma.

Phase development in the Bi 2Sr 2CaCu 2O y system . Effects of oxygen pressure

NASA Astrophysics Data System (ADS)

List, F. A.; Hsu, H.; Cavin, O. B.; Porter, W. D.; Hubbard, C. R.; Kroeger, D. M.

1992-11-01

Studies have been undertaken using thermal analysis, in conjunction with high-temperature and room temperature X-ray diffraction, fraction, to elucidate phase relationships during thermal processing of thick films of initially phase pure Bi 2Sr 2CaCu 2O y (2212) on silver substrates in various oxygen-containing atmospheres (0.001 to 100% O 2). Exothermic events on cooling at 10°C/min from a partially liquid state vary with oxygen partial pressure and can be grouped into three sets (I-III). Set I is prominent for 0.001% and 0.1% O 2 in the range of 740-775°C and is believed to be associated with the crystallization of a Cu-free ∼ Bi 5Sr 3Ca 1 oxide phase. Set II results from the crystallization of 2212; it is observed for p(O 2)≥1.0% in the temperature range 800-870°C. Set III appears for 21% and 100% O 2 in the temperature range 880-910°C, and its origin is not clear from the results of this study. Subsequent room temperature X-ray diffraction from these samples suggests that in general high oxygen partial pressures (100% O 2) tend to favor the formation of Bi 2Sr 2CuO 6 (2201), whereas low oxygen partial pressures (0.001-0.1% O 2) lead to the formation of a Cu-free, Bi-Sr-Ca oxide phase. The 2212 phase forms at this cooling rate predominantly for intermediate oxygen partial pressures (7.6-21% O 2). High-temperature X-ray diffraction during cooling (2°C/h) from the partially liquid state shows a pronounced dependence of the order of evolution of crystalline 2212 and 2201 phases on p(O 2). For an oxygen partial pressure of 1.0% the formation of 2212 precedes that of 2201, whereas for 0.01% O 2 2201 crystallizes at a higher temperature than 2212. The implications of these results pertaining to thermal processing of thick 2212 films are discussed.

Predicting the crystallization propensity of carboxylic acid buffers in frozen systems--relevance to freeze-drying.

PubMed

Sundaramurthi, Prakash; Suryanarayanan, Raj

2011-04-01

Selective crystallization of buffer components in frozen solutions is known to cause pronounced pH shifts. Our objective was to study the crystallization behavior and the consequent pH shift in frozen aqueous carboxylic acid buffers. Aqueous carboxylic acid buffers were cooled to -25°C and the pH of the solution was measured as a function of temperature. The thermal behavior of solutions during freezing and thawing was investigated by differential scanning calorimetry. The crystallized phases in frozen solution were identified by X-ray diffractometry. The malate buffer system was robust with no evidence of buffer component crystallization and hence negligible pH shift. In the citrate and tartarate systems, at initial pH

FORTRAN 77 programs for conductive cooling of dikes with temperature-dependent thermal properties and heat of crystallization

USGS Publications Warehouse

Delaney, P.T.

1988-01-01

Temperature histories obtained from transient heat-conduction theory are applicable to most dikes despite potential complicating effects related to magma flow during emplacement, groundwater circulation, and metamorphic reaction during cooling. Here. machine-independent FORTRAN 77 programs are presented to calculate temperatures in and around dikes as they cool conductively. Analytical solutions can treat thermal-property contrasts between the dike and host rocks, but cannot address the release of magmatic heat of crystallization after the early stages of cooling or the appreciable temperature dependence of thermal conductivity and diffusivity displayed by most rock types. Numerical solutions can incorporate these additional factors. The heat of crystallization can raise the initial temperature at the dike contact, ??c1, about 100??C above that which would be estimated if it were neglected, and can decrease the rate at which the front of solidified magma moves to the dike center by a factor of as much as three. Thermal conductivity and diffusivity of rocks increase with decreasing temperature and, at low temperatures, these properties increase more if the rocks are saturated with water. Models that treat these temperature dependencies yield estimates of ??c1 that are as much as 75??C beneath those which would be predicted if they were neglected. ?? 1988.

Analyzing multistep homogeneous nucleation in vapor-to-solid transitions using molecular dynamics simulations

NASA Astrophysics Data System (ADS)

Tanaka, Kyoko K.; Diemand, Jürg; Tanaka, Hidekazu; Angélil, Raymond

2017-08-01

In this paper, we present multistep homogeneous nucleations in vapor-to-solid transitions as revealed by molecular dynamics simulations on Lennard-Jones molecules, where liquidlike clusters are created and crystallized. During a long, direct N V E (constant volume, energy, and number of molecules) involving the integration of (1.9 -15 )× 106 molecules in up to 200 million steps (=4.3 μ s ), crystallization in many large, supercooled nanoclusters is observed once the liquid clusters grow to a certain size (˜800 molecules for the case of T ≃0.5 ɛ /k ). In the simulations, we discovered an interesting process associated with crystallization: the solid clusters lost 2-5 % of their mass during crystallization at low temperatures below their melting temperatures. Although the crystallized clusters were heated by latent heat, they were stabilized by cooling due to evaporation. The clusters crystallized quickly and completely except at surface layers. However, they did not have stable crystal structures, rather they had metastable structures such as icosahedral, decahedral, face-centered-cubic-rich (fcc-rich), and hexagonal-close-packed-rich (hcp-rich). Several kinds of cluster structures coexisted in the same size range of ˜1000 -5000 molecules. Our results imply that multistep nucleation is a common first stage of condensation from vapor to solid.

Thin transparent conducting films of cadmium stannate

DOEpatents

Wu, Xuanzhi; Coutts, Timothy J.

2001-01-01

A process for preparing thin Cd.sub.2 SnO.sub.4 films. The process comprises the steps of RF sputter coating a Cd.sub.2 SnO.sub.4 layer onto a first substrate; coating a second substrate with a CdS layer; contacting the Cd.sub.2 SnO.sub.4 layer with the CdS layer in a water- and oxygen-free environment and heating the first and second substrates and the Cd.sub.2 SnO.sub.4 and CdS layers to a temperature sufficient to induce crystallization of the Cd.sub.2 SnO.sub.4 layer into a uniform single-phase spinel-type structure, for a time sufficient to allow full crystallization of the Cd.sub.2 SnO.sub.4 layer at that temperature; cooling the first and second substrates to room temperature; and separating the first and second substrates and layers from each other. The process can be conducted at temperatures less than 600.degree. C., allowing the use of inexpensive soda lime glass substrates.

A green preparation method of battery grade α-PbO based on Pb-O2 fuel cell

NASA Astrophysics Data System (ADS)

Wang, Pingyuan; Pan, Junqing; Gong, Shumin; Sun, Yanzhi

2017-08-01

In order to solve the problem of high pollution and high energy consumption of the current lead oxide (PbO) preparation processes, a new clean and energy saving preparation method for high purity α-PbO via discharge of a Pb-O2 fuel cell is reported. The fuel cell with metallic lead anode, oxygen cathode, and 30% NaOH electrolyte can provide a discharge voltage of 0.66-0.38 V corresponding to discharge current range of 5-50 mA cm-2. PbO is precipitated from the NaHPbO2-containing electrolyte through a cooling crystallization process after discharge process, and the XRD patterns indicate the structure is pure α-PbO. The mother liquid after crystallization can be recycled for the next batch. The obtained PbO mixed with 60% Shimadzu PbO is superior to the pure Shimadzu PbO in discharge capacity and cycle ability.

Viscosity measurements of crystallizing andesite from Tungurahua volcano (Ecuador).

PubMed

Chevrel, Magdalena Oryaëlle; Cimarelli, Corrado; deBiasi, Lea; Hanson, Jonathan B; Lavallée, Yan; Arzilli, Fabio; Dingwell, Donald B

2015-03-01

Viscosity has been determined during isothermal crystallization of an andesite from Tungurahua volcano (Ecuador). Viscosity was continuously recorded using the concentric cylinder method and employing a Pt-sheathed alumina spindle at 1 bar and from 1400°C to subliquidus temperatures to track rheological changes during crystallization. The disposable spindle was not extracted from the sample but rather left in the sample during quenching thus preserving an undisturbed textural configuration of the crystals. The inspection of products quenched during the crystallization process reveals evidence for heterogeneous crystal nucleation at the spindle and near the crucible wall, as well as crystal alignment in the flow field. At the end of the crystallization, defined when viscosity is constant, plagioclase is homogeneously distributed throughout the crucible (with the single exception of experiment performed at the lowest temperature). In this experiments, the crystallization kinetics appear to be strongly affected by the stirring conditions of the viscosity determinations. A TTT (Time-Temperature-Transformation) diagram illustrating the crystallization "nose" for this andesite under stirring conditions and at ambient pressure has been constructed. We further note that at a given crystal content and distribution, the high aspect ratio of the acicular plagioclase yields a shear-thinning rheology at crystal contents as low as 13 vol %, and that the relative viscosity is higher than predicted from existing viscosity models. These viscosity experiments hold the potential for delivering insights into the relative influences of the cooling path, undercooling, and deformation on crystallization kinetics and resultant crystal morphologies, as well as their impact on magmatic viscosity.

Viscosity measurements of crystallizing andesite from Tungurahua volcano (Ecuador)

PubMed Central

Cimarelli, Corrado; deBiasi, Lea; Hanson, Jonathan B.; Lavallée, Yan; Arzilli, Fabio; Dingwell, Donald B.

2015-01-01

Abstract Viscosity has been determined during isothermal crystallization of an andesite from Tungurahua volcano (Ecuador). Viscosity was continuously recorded using the concentric cylinder method and employing a Pt‐sheathed alumina spindle at 1 bar and from 1400°C to subliquidus temperatures to track rheological changes during crystallization. The disposable spindle was not extracted from the sample but rather left in the sample during quenching thus preserving an undisturbed textural configuration of the crystals. The inspection of products quenched during the crystallization process reveals evidence for heterogeneous crystal nucleation at the spindle and near the crucible wall, as well as crystal alignment in the flow field. At the end of the crystallization, defined when viscosity is constant, plagioclase is homogeneously distributed throughout the crucible (with the single exception of experiment performed at the lowest temperature). In this experiments, the crystallization kinetics appear to be strongly affected by the stirring conditions of the viscosity determinations. A TTT (Time‐Temperature‐Transformation) diagram illustrating the crystallization “nose” for this andesite under stirring conditions and at ambient pressure has been constructed. We further note that at a given crystal content and distribution, the high aspect ratio of the acicular plagioclase yields a shear‐thinning rheology at crystal contents as low as 13 vol %, and that the relative viscosity is higher than predicted from existing viscosity models. These viscosity experiments hold the potential for delivering insights into the relative influences of the cooling path, undercooling, and deformation on crystallization kinetics and resultant crystal morphologies, as well as their impact on magmatic viscosity. PMID:27656114

Methods for predicting properties and tailoring salt solutions for industrial processes

NASA Technical Reports Server (NTRS)

Ally, Moonis R.

1993-01-01

An algorithm developed at Oak Ridge National Laboratory accurately and quickly predicts thermodynamic properties of concentrated aqueous salt solutions. This algorithm is much simpler and much faster than other modeling schemes and is unique because it can predict solution behavior at very high concentrations and under varying conditions. Typical industrial applications of this algorithm would be in manufacture of inorganic chemicals by crystallization, thermal storage, refrigeration and cooling, extraction of metals, emissions controls, etc.

Methods of studying aging and stabilization of spray-congealed solid dispersions with carnauba wax. 1. Microcalorimetric investigation.

PubMed

Emås, M; Nyqvist, H

2000-03-20

Rapidly cooled materials are often unstable as a result of changes in their physical properties due to imperfect crystallization. In the process of spray-congealing, melted material is atomized into droplets which very quickly solidify. This increases the possibility of the material crystallizing in different metastable forms. In this study it is shown that isothermal microcalorimetry can be used to observe the change in the thermodynamic state of spray-congealed carnauba wax during storage. In order to accelerate the thermodynamic change in the spray-congealed wax, three annealing procedures have been developed and compared using isothermal microcalorimetry. By means of annealing, a spray-congealed product closer to a thermodynamically stable state has been achieved.

Linking Plagioclase Zoning Patterns to Active Magma Processes

NASA Astrophysics Data System (ADS)

Izbekov, P. E.; Nicolaysen, K. P.; Neill, O. K.; Shcherbakov, V.; Eichelberger, J. C.; Plechov, P.

2016-12-01

Plagioclase, one of the most common and abundant mineral phases in volcanic products, will vary in composition in response to changes in temperature, pressure, composition of the ambient silicate melt, and melt H2O concentration. Changes in these parameters may cause dissolution or growth of plagioclase crystals, forming characteristic textural and compositional variations (zoning patterns), the complete core-to-rim sequence of which describes events experienced by an individual crystal from its nucleation to the last moments of its growth. Plagioclase crystals in a typical volcanic rock may look drastically dissimilar despite their spatial proximity and the fact that they have erupted together. Although they shared last moments of their growth during magma ascent and eruption, their prior experiences could be very different, as plagioclase crystals often come from different domains of the same magma system. Distinguishing similar zoning patterns, correlating them across the entire population of plagioclase crystals, and linking these patterns to specific perturbations in the magmatic system may provide additional perspective on the variety, extent, and timing of magma processes at active volcanic systems. Examples of magma processes, which may be distinguished based on plagioclase zoning patterns, include (1) cooling due to heat loss, (2) heating and/or pressure build up due to an input of new magmatic material, (3) pressure drop in response to magma system depressurization, and (4) crystal transfer between different magma domains/bodies. This review will include contrasting examples of zoning patters from recent eruptions of Augustine and Cleveland Volcanoes in Alaska, Sakurajima Volcano in Japan, Karymsky, Bezymianny, and Tolbachik Volcanoes in Kamchatka, as well as from the drilling into an active magma body at Krafla, Iceland.

Magmatic structures in the Krkonoše Jizera Plutonic Complex, Bohemian Massif: evidence for localized multiphase flow and small-scale thermal mechanical instabilities in a granitic magma chamber

NASA Astrophysics Data System (ADS)

Žák, Jiří; Klomínský, Josef

2007-08-01

The present paper examines magmatic structures in the Jizera and Liberec granites of the Krkonoše-Jizera Plutonic Complex, Bohemian Massif. The magmatic structures are here interpreted to preserve direct field evidence for highly localized magma flow and other processes in crystal-rich mushes, and to capture the evolution of physical processes in an ancient granitic magma chamber. We propose that after chamber-wide mixing and hybridization, as suggested by recent petrological studies, laminar magma flow became highly localized to weaker channel-like domains within the higher-strength crystal framework. Mafic schlieren formed at flow rims, and their formation presumably involved gravitational settling and velocity gradient flow sorting coupled with interstitial melt escape. Local thermal or compositional convection may have resulted in the formation of vertical schlieren tubes and ladder dikes whereas subhorizontal tubes or channels formed during flow driven by lateral gradients in magma pressure. After the cessation or deceleration of channel flow, gravity-driven processes (settling of crystals and enclaves, gravitational differentiation, development of downward dripping instabilities), accompanied by compaction, filter pressing and melt segregation, dominated in the crystal mush within the flow channels. Subsequently, magmatic folds developed in schlieren layers and the magma chamber recorded complex, late magmatic strains at high magma crystallinities. Late-stage magma pulsing into localized submagmatic cracks represents the latest events of magmatic history of the chamber prior to its final crystallization. We emphasize that the most favorable environments for the formation and preservation of magmatic structures, such as those hosted in the Jizera and Liberec granites, are slowly cooling crystal-rich mushes. Therefore, where preserved in plutons, these structures may lend strong support for a "mush model" of magmatic systems.

3D printed glass: surface finish and bulk properties as a function of the printing process

NASA Astrophysics Data System (ADS)

Klein, Susanne; Avery, Michael P.; Richardson, Robert; Bartlett, Paul; Frei, Regina; Simske, Steven

2015-03-01

It is impossible to print glass directly from a melt, layer by layer. Glass is not only very sensitive to temperature gradients between different layers but also to the cooling process. To achieve a glass state the melt, has to be cooled rapidly to avoid crystallization of the material and then annealed to remove cooling induced stress. In 3D-printing of glass the objects are shaped at room temperature and then fired. The material properties of the final objects are crucially dependent on the frit size of the glass powder used during shaping, the chemical formula of the binder and the firing procedure. For frit sizes below 250 μm, we seem to find a constant volume of pores of less than 5%. Decreasing frit size leads to an increase in the number of pores which then leads to an increase of opacity. The two different binders, 2- hydroxyethyl cellulose and carboxymethylcellulose sodium salt, generate very different porosities. The porosity of samples with 2-hydroxyethyl cellulose is similar to frit-only samples, whereas carboxymethylcellulose sodium salt creates a glass foam. The surface finish is determined by the material the glass comes into contact with during firing.

Polymer composites and porous materials prepared by thermally induced phase separation and polymer-metal hybrid methods

NASA Astrophysics Data System (ADS)

Yoon, Joonsung

The primary objective of this research is to investigate the morphological and mechanical properties of composite materials and porous materials prepared by thermally induced phase separation. High melting crystallizable diluents were mixed with polymers so that the phase separation would be induced by the solidification of the diluents upon cooling. Theoretical phase diagrams were calculated using Flory-Huggins solution thermodynamics which show good agreement with the experimental results. Porous materials were prepared by the extraction of the crystallized diluents after cooling the mixtures (hexamethylbenzene/polyethylene and pyrene/polyethylene). Anisotropic structures show strong dependence on the identity of the diluents and the composition of the mixtures. Anisotropic crystal growth of the diluents was studied in terms of thermodynamics and kinetics using DSC, optical microscopy and SEM. Microstructures of the porous materials were explained in terms of supercooling and dendritic solidification. Dual functionality of the crystallizable diluents for composite materials was evaluated using isotactic polypropylene (iPP) and compatible diluents that crystallize upon cooling. The selected diluents form homogeneous mixtures with iPP at high temperature and lower the viscosity (improved processability), which undergo phase separation upon cooling to form solid particles that function as a toughening agent at room temperature. Tensile properties and morphology of the composites showed that organic crystalline particles have the similar effect as rigid particles to increase toughness; de-wetting between the particle and iPP matrix occurs at the early stage of deformation, followed by unhindered plastic flow that consumes significant amount of fracture energy. The effect of the diluents, however, strongly depends on the identity of the diluents that interact with the iPP during solidification step, which was demonstrated by comparing tetrabromobisphenol-A and phthalic anhydride. A simple method to prepare composite surfaces that can change the wettability in response to the temperature change was proposed and evaluated. Composite surfaces prepared by nanoporous alumina templates filled with polymers showed surface morphology and wettability that depend on temperature. This effect is attributed to the significant difference in thermal conductivity and the thermal expansion coefficient between the alumina and the polymers. The reversibility in thermal response depends on the properties of the polymers.

Enhanced cooling of Yb:YLF using astigmatic Herriott cell (Conference Presentation)

NASA Astrophysics Data System (ADS)

Gragossian, Aram; Meng, Junwei; Ghasemkhani, Mohammadreza; Albrecht, Alexander R.; Tonelli, Mauro; Sheik-Bahae, Mansoor

2017-02-01

Optical refrigeration of solids requires crystals with exceptional qualities. Crystals with external quantum efficiencies (EQE) larger than 99% and background absorptions of 4×10-4cm-1 have been cooled to cryogenic temperatures using non resonant cavities. Estimating the cooling efficiency requires accurate measurements of the above mentioned quantities. Here we discuss measurements of EQE and background absorption for two high quality Yb:YLF samples. For any given sample, to reach minimum achievable temperatures heat generated by fluorescence must be removed from the surrounding clamshell and more importantly, absorption of the laser light must be maximized. Since the absorption coefficient drops at lower temperatures the only option is to confine laser light in a cavity until almost 100% of the light is absorbed. This can be achieved by placing the crystal between a cylindrical and spherical mirror to form an astigmatic Herriott cell. In this geometry light enters through a hole in the middle of the spherical mirror and if the entrance angle is correct, it can make as many round trips as required to absorb all the light. At 120 K 60 passes and 150 passes at 100K ensures more than 95% absorption of the laser light. 5 and 10% Yb:YLF crystals placed in such a cell cool to sub 90K temperatures. Non-contact temperature measurements are more challenging for such a geometry. Reabsorption of fluorescence for each pass must be taken into account for accurate temperature measurements by differential luminescence thermometry (DLT). Alternatively, we used part of the spectrum that is not affected by reabsorption.

Sidewall crystallization and saturation front formation in silicic magma chambers

NASA Astrophysics Data System (ADS)

Lake, E. T.

2012-12-01

The cooling and crystallization style of silicic magma bodies in the upper crust falls on a continuum between whole-chamber processes of convection, crystal settling, and cumulate formation and interface driven processes of conduction and crystallization front migration. In the former case, volatile saturation occurs uniformly chamber wide, in the latter volatile saturation occurs along an inward propagating front. Ambient thermal gradient primarily controls the propagation rate; warm (> 30 °C / km) geothermal gradients promote 1000m+ thick crystal mush zones but slow crystallization front propagation. Cold geothermal gradients support the opposite. Magma chamber geometry plays a second order role in controlling propagation rates; bodies with high surface to magma ratio and large Earth's surface parallel faces exhibit more rapid propagation and smaller mush zones. Crystallization front propagation occurs at speeds of up to 6 cm/year (rhyolitic magma, thin sill geometry, 10 °C / km geotherm), far faster than diffusion of volatiles in magma and faster than bubbles can nucleate and ascend under certain conditions. Saturation front propagation is fixed by pressure and magma crystal content; above certain modest initial water contents (4.4 wt% in a dacite) mobile magma above 10 km depth always contains a saturation front. Saturation fronts propagate down from the magma chamber roof at lower water contents (3.3 wt% in a dacite at 5 km depth), creating an upper saturated interface for most common (4 - 6 wt%) magma water contents. This upper interface promotes the production of a fluid pocket underneath the apex of the magma chamber. Magma de-densification by bubble nucleation promotes convection and homogenization in dacitic systems. If the fluid pocket grew rapidly without draining, hydro-fracturing and eruption would result. The combination of fluid escape pathways and metal scavenging would generate economic vein or porphyry deposits.

Liquid Crystal Mediated Nano-assembled Gold Micro-shells

NASA Astrophysics Data System (ADS)

Quint, Makiko; Sarang, Som; Quint, David; Huang, Kerwyn; Gopinathan, Ajay; Hirst, Linda; Ghosh, Sayantani

We have created 3D nano-assenbled micro-shell by using thermotropic liquid crystal (LC), 4-Cyano-4'-pentylbiphenyl (5CB), doped with mesogen-functionalized gold nanoparticles (AuNPs). The assembly process is driven by the isotropic-nematic phase transition dynamics. We uniformly disperse the functionalized AuNPs into isotropic liquid crystal matrix and the mixture is cooled from the isotropic to the nematic phase. During the phase transition, the separation of LC-AuNP rich isotropic and ordered 5CB rich domains cause the functionalized AuNPs to move into the shrinking isotropic regions. The mesogenic ligands are locally crystalized during this process, which leads to the formation of a spherical shell with a densely packed wall of AuNPs. These micro-shells are capable of encapsulating fluorescence dye without visible leakages for several months. Additionally, they demonstrate strong localized surface plasmon resonance, which leads to localized heating on optical excitation. This photothermal effect disrupts the structure, releasing contents within seconds. Our results exhibiting the capture and optically regulated release of encapsulated substances is a novel platform that combines drug-delivery and photothermal therapy in one versatile and multifunctional unit. This work is supported by the NSF Grants No. DMR-1056860, ECC-1227034, and a University of California Merced Faculty Mentor Fellowship.

The onset of planet formation in brown dwarf disks.

PubMed

Apai, Dániel; Pascucci, Ilaria; Bouwman, Jeroen; Natta, Antonella; Henning, Thomas; Dullemond, Cornelis P

2005-11-04

The onset of planet formation in protoplanetary disks is marked by the growth and crystallization of sub-micrometer-sized dust grains accompanied by dust settling toward the disk mid-plane. Here, we present infrared spectra of disks around brown dwarfs and brown dwarf candidates. We show that all three processes occur in such cool disks in a way similar or identical to that in disks around low- and intermediate-mass stars. These results indicate that the onset of planet formation extends to disks around brown dwarfs, suggesting that planet formation is a robust process occurring in most young circumstellar disks.

Optimization and characterization of bulk hexagonal boron nitride single crystals grown by the nickel-chromium flux method

NASA Astrophysics Data System (ADS)

Hoffman, Tim

Hexagonal boron nitride (hBN) is a wide bandgap III-V semiconductor that has seen new interest due to the development of other III-V LED devices and the advent of graphene and other 2-D materials. For device applications, high quality, low defect density materials are needed. Several applications for hBN crystals are being investigated, including as a neutron detector and interference-less infrared-absorbing material. Isotopically enriched crystals were utilized for enhanced propagation of phonon modes. These applications exploit the unique physical, electronic and nanophotonics applications for bulk hBN crystals. In this study, bulk hBN crystals were grown by the flux method using a molten Ni-Cr solvent at high temperatures (1500°C) and atmospheric pressures. The effects of growth parameters, source materials, and gas environment on the crystals size, morphology and purity were established and controlled, and the reliability of the process was greatly improved. Single-crystal domains exceeding 1mm in width and 200microm in thickness were produced and transferred to handle substrates for analysis. Grain size dependence with respect to dwell temperature, cooling rate and cooling temperature were analyzed and modeled using response surface morphology. Most significantly, crystal grain width was predicted to increase linearly with dwell temperature, with single-crystal domains exceeding 2mm in at 1700°C. Isotopically enriched 10B and 11B hBN crystal were produced using a Ni-Cr-B flux method, and their properties investigated. 10B concentration was evaluated using SIMS and correlated to the shift in the Raman peak of the E2g mode. Crystals with enrichment of 99% 10B and >99% 11B were achieved, with corresponding Raman shift peaks at 1392.0 cm-1 and 1356.6 cm-1, respectively. Peak FWHM also decreased as isotopic enrichment approached 100%, with widths as low as 3.5 cm-1 achieved, compared to 8.0 cm-1 for natural abundance samples. Defect selective etching was performed using a molten NaOH-KOH etchant at 425°C-525°C, to quantify the quality of the crystals. Three etch pit shapes were identified and etch pit width was investigated as a function of temperature. Etch pit density and etch pit activation energy was estimated at 5x107 cm-2 and 60 kJ/mol, respectively. Screw and mixed-type dislocations were identified using diffraction-contrast TEM imaging.

Effect of cooling rate on magnetic domain structure and magnetic properties of Tb0.27Dy0.73Fe1.95 alloys solidified in high magnetic field

NASA Astrophysics Data System (ADS)

Liu, Tie; Dong, Meng; Gao, Pengfei; Xiao, Yubao; Yuan, Yi; Wang, Qiang

2018-05-01

In this work, Tb0.27Dy0.73Fe1.95 alloys were solidified in a high magnetic field of 4.4 T at various cooling rates. Changes in the magnetostriction, crystal orientation, magnetization, and magnetic domain of the solidified alloys were investigated. The application of the magnetic field can induce <111> orientation of (Tb, Dy)Fe2 phase. However, the effect of the magnetic field is strongly dependent on the cooling rate. The alloy solidified at 5 °C/min shows the highest magnetostriction, strongest <111> orientation, best contrast of light and dark in the domain image, and fastest magnetization, and followed in descending order by the alloys solidified at 1.5 °C/min and 60 °C/min. The change in the magnetostriction of the alloys can be attributed to the changes in crystal orientation and magnetic domain structure caused by both the magnetic field and cooling rate.

Crystallization and Cooling of a Deep Silicate Magma Ocean

NASA Astrophysics Data System (ADS)

Bower, Dan; Wolf, Aaron

2016-04-01

Impact and accretion simulations of terrestrial planet formation suggest that giant impacts are both common and expected to produce extensive melting. The moon-forming impact, for example, likely melted the majority of Earth's mantle to produce a global magma ocean that subsequently cooled and crystallised. Understanding the cooling process is critical to determining magma ocean lifetimes and recognising possible remnant signatures of the magma ocean in present-day mantle heterogeneities. Modelling this evolution is challenging, however, due to the vastly different timescales and lengthscales associated with turbulent convection (magma ocean) and viscous creep (present-day mantle), in addition to uncertainties in material properties and chemical partitioning. We consider a simplified spherically-symmetric (1-D) magma ocean to investigate both its evolving structure and cooling timescale. Extending the work of Abe (1993), mixing-length theory is employed to determine convective heat transport, producing a high resolution model that parameterises the ultra-thin boundary layer (few cms) at the surface of the magma ocean. The thermodynamics of mantle melting are represented using a pseudo-one-component model, which retains the simplicity of a standard one-component model while introducing a finite temperature interval for melting. This model is used to determine the cooling timescale for a variety of plausible thermodynamic models, with special emphasis on comparing the center-outwards vs bottom-up cooling scenarios that arise from the assumed EOS.

Effect of Fe2O3 on the crystallization behavior of glass-ceramics produced from naturally cooled yellow phosphorus furnace slag

NASA Astrophysics Data System (ADS)

Liu, Hong-pan; Huang, Xiao-feng; Ma, Li-ping; Chen, Dan-li; Shang, Zhi-biao; Jiang, Ming

2017-03-01

CaO-Al2O3-SiO2 (CAS) glass-ceramics were prepared via a melting method using naturally cooled yellow phosphorus furnace slag as the main raw material. The effects of the addition of Fe2O3 on the crystallization behavior and properties of the prepared glass-ceramics were studied by differential thermal analysis, X-ray diffraction, and scanning electron microscopy. The crystallization activation energy was calculated using the modified Johnson-Mehl-Avrami equation. The results show that the intrinsic nucleating agent in the yellow phosphorus furnace slag could effectively promote the crystallization of CAS. The crystallization activation energy first increased and then decreased with increasing amount of added Fe2O3. At 4wt% of added Fe2O3, the crystallization activation energy reached a maximum of 676.374 kJ·mol-1. The type of the main crystalline phase did not change with the amount of added Fe2O3. The primary and secondary crystalline phases were identified as wollastonite (CaSiO3) and hedenbergite (CaFe(Si2O6)), respectively.

Effect of natural phenolics on the thermal and processing behaviour of poly(3-hydroxybutyrate)

NASA Astrophysics Data System (ADS)

Auriemma, Maria; Piscitelli, Amodio; Pasquino, Rossana; Cerruti, Pierfrancesco; Angelini, Stefania; Scarinzi, Gennaro; Malinconico, Mario; Grizzuti, Nino

2015-12-01

Poly(3-hydroxybutyrate) (PHB) is a biodegradable polymer, whose applicability is limited by its relatively poor mechanical properties and narrow processing window. In this paper, different natural phenol-based additives, including tannic acid (TA), grape bagasse extract (EP), and a lignocellulosic biomass (LC) were used as thermal and processing stabilizers for PHB. The thermal stability of both neat and doped PHB samples was studied by rheology and calorimetry. The experimental results showed that neat PHB massively degrades and that the addition of phenol additives enhances the thermal stability of PHB, preserving the polymer molecular weight after processing. This finding was in agreement with the slower decay in viscosity observed through rheological tests. Physical and chemical interactions between polymer and additive were considered as key factors to interpret the experimental data. LC affected the melt crystallization kinetics of PHB enhancing crystallization upon cooling. This finding suggests that LC was a heterogeneous nucleating agent, potentially able to control the physical aging of PHB. The described results are of interest for the development of sustainable alternatives to synthetic polymer additives, by increasing the applicability of bio-based materials.

On the Principles of Building a Layered Intrusion

NASA Astrophysics Data System (ADS)

Marsh, B. D.

2009-12-01

An accurate and realistic understanding of all magmatic processes involves knowing the combined physical and chemical fundamentals governing the overall process. Magmatic processes involve such a vast array of sub-processes (e.g., heat and mass transfer, crystal growth, slurry transport and sorting, annealing, resorbtion, etc.) that rarely is there any single feature or measurement that can be safely inverted to solve the problem. And each event as in the formation of an intrusion must at some level for heuristic purposes be defined as an isolated event. This is commonly done without much forethought, as is the absolutely critical assumption of the initial conditions defining the beginning of the event. Almost without exception, it is the initial conditions that determine the outcome of the entire process in all physical and biological systems. Automobile factories produce motorized vehicles not water melons or chimpanzees. Nucleosynthesis of H and He always gives the same set of elements. The initial conditions of the magma giving rise to the end product for mafic layered systems are especially difficult to discern and must be bounded by observing simpler, real time magmatic and volcanic processes. Initial conditions come from posing a series of questions: What was the style and duration of filling? What was the rate of influx and final volume of each delivery of magma? What was the compositional variation and phenocryst content of the individual magmatic deliveries? If phenocrysts are present, were they sorted prior to injection during ascension? What was the original and ongoing shape of the magmatic reservoir? A failure to appreciate or answer such basic questions leads to vastly untenable evolutionary scenarios. Unrealistic initial conditions necessarily lead to unrealistic magmatic scenarios. There are certain safe starting points. Eruptive and emplacement fluxes are limited. The larger an intrusion is the longer it took to build and the longer to build the more varied are the deliveries in time, volume, and constitution. Instantaneous emplacement of crystal free magma are unlikely initial conditions for a large intrusion. The most realistic initial conditions are that intrusions are made of a combination of crystal poor and crystal-rich inputs. Examples abound of the outcomes of systems with clearly known initial conditions. The huge Sudbury magma was produced in 5 minutes at a temperature of 1700C. Clearly crystal free, it produced no layering whatsoever. Sills worldwide, regardless of size, approaching these initial conditions are similarly featureless. At the other extreme are the lava outputs of large volcanic systems like Kilauea. The ensuing lava lakes produced over months are filled with magma containing varied amounts of phenocrysts/xenocrysts and ultramafic layers are produced. Intrusions abound of all sizes that show the same characteristics. Ponding in crystal-laden sills forms layered systems with many of the features of large bodies. Rapid cooling preserves diagnostic textural relations lost to annealing in large bodies. Slow cooling promotes annealing to sharpen and accentuate the initial modal and cryptic layering. Initial conditions are fundamental to understanding the final product. Physical processes buttressed by chemistry mainly dominate magmatic systems.

Analysis of mercerization process based on the intensity change of deconvoluted resonances of (13)C CP/MAS NMR: Cellulose mercerized under cooling and non-cooling conditions.

PubMed

Miura, Kento; Nakano, Takato

2015-08-01

The area intensity change of C1, C4, and C6 in spectrum obtained by (13)C CP/MAS NMR and the mutual relationship between their changes were examined for cellulose samples treated with various concentrations of aqueous NaOH solutions under non-cooling and cooling conditions. The area intensity of C1-up and C6-down changed cooperatively with that of C4-down which corresponds to the crystallinity of samples: "-up" and "-down" are the up- and down- field component in a splitting peak of NMR spectrum, respectively. The intensity change of C1-up starts to decrease with decreasing in that of C4-down after that of C6-down is almost complete. These changes were more clearly observed for samples treated under cooling condition. It can be suggested that their characteristic change relates closely to the change in conformation of cellulose chains by induced decrystallization and the subsequent crystallization of cellulose II, and presumed that their changes at microscopic level relate to the macroscopic morphological changes such as contraction along the length of cellulose chains and recovery along the length. Copyright © 2015 Elsevier B.V. All rights reserved.

Growth of 2 Inch Eu-doped SrI2 single crystals for scintillator applications

NASA Astrophysics Data System (ADS)

Yoshikawa, Akira; Shoji, Yasuhiro; Yokota, Yuui; Kurosawa, Shunsuke; Hayasaka, Shoki; Chani, Valery I.; Ito, Tomoki; Kamada, Kei; Ohashi, Yuji; Kochurikhin, Vladimir

2016-10-01

A vertical Bridgman (VB) crystal growth process was established using modified micro-pulling-down (μ-PD) crystal growth system with a removable chamber that was developed for the growth of deliquescent halide single crystals because conventional μ-PD method does not allow growth of large bulk single crystals. Eu:SrI2 crystals were grown from the melt of (Sr0.98Eu0.02)I2 composition using carbon crucibles. Undoped μ-PD SrI2 crystals were used as seeds that were affixed to the bottom of the crucible. All the preparations preceding the growths and the hot zone assembling were performed in a glove box with Ar gas. Then the removable chamber was taken out of the glove box, attached to the μ-PD system, connected with a Turbo Molecular pump, and evacuated down to 10-4 Pa at 300 °C. After the baking procedure, high purity Ar gas (6N) was injected into the chamber. The crucible was heated by a high frequency induction coil up to the melting point of Eu:SrI2. After melting the starting materials, the crucible was displaced in downward direction for the crystal growth and then cooled down to room temperature. Thus, 2 in. and crack-free Eu:SrI2 bulk crystals were produced. The crystals had high transparency and did not contain any visible inclusions. The crystals were cut and polished in the glove box and then sealed in an aluminum container with an optical window for characterization. The details of the crystal growth are discussed.

Improvement in Stability of SPring-8 Standard X-Ray Monochromators with Water-Cooled Crystals

NASA Astrophysics Data System (ADS)

Yamazaki, Hiroshi; Shimizu, Yasuhiro; Miura, Takanori; Tanaka, Masayuki; Kishimoto, Hikaru; Matsuzaki, Yasuhisa; Shimizu, Nobtaka; Kawano, Yoshiaki; Kumasaka, Takashi; Yamamoto, Masaki; Koganezawa, Tomoyuki; Sato, Masugu; Hirosawa, Ichiro; Senba, Yasunori; Ohashi, Haruhiko; Goto, Shunji; Ishikawa, Tetsuya

2010-06-01

SPring-8 standard double-crystal monochromators containing water-cooled crystals were stabilized to a sufficient level to function as a part of optics components to supply stable microfocused x-ray beams, by determining causes of the instability and then removing them. The instability was caused by two factors—thermal deformation of fine stepper stages in the monochromator, which resulted in reduction in beam intensity with time, and vibrations of coolant supply units and vacuum pumps, which resulted in fluctuation in beam intensity. We remodeled the crystal holders to maintain the stage temperatures constant with water, attached x-ray and electron shields to the stages in order to prevent their warming up, introduced accumulators in the water circuits to absorb pressure pulsation, used polyurethane tubes to stabilize water flow, and placed rubber cushions un der scroll vacuum pumps. As a result, the intensity reduction rate of the beam decreased from 26% to 1% per hour and the intensity fluctuation from 13% to 1%. The monochromators were also modified to prevent radiation damage to the crystals, materials used as a water seal, and motor cables.

Growth, structural, thermal, dielectric and optical studies on HBST crystal: A potential THz emitter

NASA Astrophysics Data System (ADS)

Ma, Yuzhe; Teng, Bing; Cao, Lifeng; Zhong, Degao; Ji, Shaohua; Teng, Fei; Liu, Jiaojiao; Yao, Yuan; Tang, Jie; Tong, Jiaming

2018-02-01

The efficient organic nonlinear optical material 4-hydroxy benzaldehyde-N-methyl 4-stilbazolium tosylate (HBST) was grown from methanol by slope nucleation method combined with slow cooling (SNM-SC) for the first time. The optimum growth conditions based on the cooling rate was further investigated. The single crystal X-ray diffraction (XRD) revealed that the chromophores of HBST crystal make an angle of about 33° with respect to the a-axis, which is close to the optimum of Terahertz (THz)-wave generation and electro-optics applications. NMR and FT-IR spectral studies have been performed to ascertain various functional groups present in the sample. Futhermore, the thermal stability and decomposition stages were analyzed through TG-DTA and DSC techniques. The dielectric constant and dielectric loss of HBST crystal have been studied. Critical optical properties like the absorption coefficient, refractive index, cut-off wavelength and band gap energy were calculated. Photoluminescence (PL) exication studies indicated green emission occured at 507 nm. All the results of HBST crystal make it a promising candidate in the fields of optoelectronic and the generation of THz.

Manufacturing unique glasses in space

NASA Technical Reports Server (NTRS)

Happe, R. P.

1976-01-01

An air suspension melting technique is described for making glasses from substances which to date have been observed only in the crystalline condition. A laminar flow vertical wind tunnel was constructed for suspending oxide melts that were melted using the energy from a carbon dioxide laser beam. By this method it is possible to melt many high-melting-point materials without interaction between the melt and crucible material. In addition, space melting permits cooling to suppress crystal growth. If a sufficient amount of under cooling is accompanied by a sufficient increase in viscosity, crystallization will be avoided entirely and glass will result.

Sterilization by Cooling in Isochoric Conditions: The Case of Escherichia coli

PubMed Central

Salinas-Almaguer, Samuel; Angulo-Sherman, Abril; Sierra-Valdez, Francisco Javier; Mercado-Uribe, Hilda

2015-01-01

High hydrostatic pressure (HHP) affects the structure, metabolism and survival of micro-organisms including bacteria. For this reason HHP is a promising treatment in the food industry. The aim of this work is to evaluate the effect of high pressure, under isochoric cooling conditions, on Escherichia coli, where such high pressure develops due to the fact water cannot expand. We combine survival curves obtained by spectrophotometry and images of atomic force microscopy in this study. Our results show that cooling at -20 and -30°C leads to a partial destruction of a Escherichia coli population. However, cooling at -15°C causes a total extermination of bacteria. This intriguing result is explained by the phase diagram of water. In the first case, the simultaneous formation of ice III and ice Ih crystals provides a safe environment for bacteria. In the second case (-15°C) Escherichia coli remains in a metastable and amorphous free-of-crystals liquid subjected to high pressure. Our work is the first experimental study carried out to inactivate Escherichia coli under isochoric cooling conditions. Unlike HHP, which is based on the application of an external load to augment the pressure, this technique only requires cooling. The method could be used for annihilation of other Escherichia coli strains and perhaps other micro-organisms. PMID:26480032

Effects of Melt Processing on Evolution of Structure in PEEK

NASA Technical Reports Server (NTRS)

Georgiev, Georgi; Dai, Patrick Shuanghua; Oyebode, Elizabeth; Cebe, Peggy; Capel, Malcolm

1999-01-01

We report on the effects of melt processing temperature on structure formation in Poly(ether-ether-ketone), PEEK. Real time Small Angle X-ray Scattering, SAXS, and thermal analysis are used to follow the melting behavior after various stages of processing. Assignment of peaks to structural entities within the material, the relative perfection of the crystals, and the possibility of their reorganization, are all influenced by the melt processing history. With the advent of high intensity synchrotron sources of X-radiation, polymer scientists gain a research tool which, when used along with thermal analysis, provides additional structural information about the crystals during growth and subsequent melting. PEEK is an engineering thermoplastic polymer with a very high glass transition temperature (145 C) and crystal melting point (337 C). PEEK has been the subject of recent studies by X-ray scattering in which melt and cold crystallization were followed in real-time. X-ray scattering and thermal studies have been used to address the formation of dual endothermic response which has been variously ascribed to lamellar insertion, dual crystal populations, or melting followed by re-crystallization. Another important issue is whether all of the amorphous phase is located in interlamellar regions, or alternatively whether some is located in "pockets" away from the crystalline lamellar stacks. The interpretation of scattering from lamellar stacks varies depending upon whether such amorphous pockets are formed. Some groups believe all of the amorphous phase is interlamellar. This leads to selection of a smaller thickness for the crystals. Other groups suggest that most amorphous phase is not interlamellar, and this leads to the suggestion that the crystal thickness is larger than the amorphous layer within the stacks. To investigate these ideas, we used SAXS and Differential Scanning Calorimetry to compare results of single and dual stage melt crystallization of PEEK using a treatment scheme involving annealing/crystallization at T(sub a1) followed by annealing at T(sub a2) where either T(sub a1) < T(sub a2) or T(sub a1) > T(sub a2). We proposed a model to explain multiple melting endotherms in PPS, treated according to one or two-stage melt or cold crystallization. Key features of this model are that multiple endotherms: (1) are due to reorganization/recrystallization after cold crystallization; and, (2) are dominated by crystal morphology after melt crystallization at high T. In other words, multiple distinct crystal populations are formed by the latter treatment, leading to observation of multiple melting. PEEK 45OG pellets (ICI Americas) were the starting material for this study. Films were compression molded at 400 C, then quenched to ice water. Samples were heated to 375 C in a Mettler FP80 hot stage and held for three min. to erase crystal seeds before cooling them to T(sub a1) = 280 C . Samples were held at T(sub a2) for a period of time, then immediately heated to 360 C. In the second treatment samples were held at T(sub a1) = 31 C for different crystallization times t(sub c) then cooled to 295 C and held 15 min. In situ (SAXS) experiments were performed at the Brookhaven National Synchrotron Light Source with the sample located inside the Mettler hot stage. The system was equipped with a two-dimensional position sensitive detector. The sample to detector distance was 172.7 cm and the X-ray wavelength was 1.54 Angstroms. SAXS data were taken continuously during the isothermal periods and during the heating to 360 C at 5 C/min. Each SAXS scan was collected for 30 sec. Since the samples were isotropic, circular integration was used to increase the signal to noise ratio. After dual stage melt crystallization with T(sub a1) < T(sub a2) the lower melting endotherm arises from holding at T(sub a1). During cooling a broad distribution of crystals forms, and the low-melting tail is perfected during T(sub al). Heating to T(sub a2) melts these imperfect crystals and allows others with greater average long spacing to form in their place. After dual stage crystallization with T(sub a1) > T(sub a2), the amount of space remaining for additional growth at T(sub a2) depends upon the holding time at T(sub a1). The long period of crystals formed at T(sub a2) is smaller than that formed at T(sub a1) due to growth in a now-restricted geometry. Perfection of crystals is seen as an increase of the intensity of the population scattering at higher s, while the intensity of the population scattering at lower s stays constant. During heating from below to above the minor endotherm, we see rapid decrease of the intensity of the X-ray scattering corresponding to the population of crystals scattering in the shoulder. Another important observation is that after the sample is annealed at 295 C, the shoulder intensity is restored once again. The population scattering at higher s remains longer before it disappears in the sample treated to the second stage of melt crystallization, compared to the sample crystallized with a single stage. This could be interpreted as an effect of continued perfection of the less perfect population, which is also reflected in the increased melting temperature of the smaller endotherm as the holding time at 295 C increases. In the corresponding DSC scans we see a shift in the area and the peak temperature of the lower melting endotherm with an increase of the annealing time.

A cross correlation method for chemical profiles in minerals, with an application to zircons of the Kilgore Tuff (USA)

NASA Astrophysics Data System (ADS)

Probst, L. C.; Sheldrake, T. E.; Gander, M. J.; Wallace, G.; Simpson, G.; Caricchi, L.

2018-03-01

Magmatic crystals are characterised by chemical zonation patterns that reflect the thermal and chemical conditions within magma reservoirs in which they grew. Crystals that exhibit similar patterns of zonation are often interpreted to have experienced similar conditions of growth. These patterns of zonation may represent continuous processes such as cooling, or more instantaneous events such as magma injection, and provide an insight into the structure and evolution of a magmatic system, both temporally and spatially. We have developed an algorithm that is objectively able to quantify the similarity within and between suites of magmatic crystals from different samples. Significantly, the algorithm is able to identify correlation that occurs between the interiors of two crystals, but does not extend to the rim, which provides an opportunity to understand the long-term evolution of magmatic systems. We develop and explain the mathematical basis for our algorithm and introduce its application using cathodoluminescence images of zircons from the Kilgore Tuff (USA). The results allow us to correlate samples from two different outcrops that are found over 80 km apart.

Seed crystals with improved properties for melt processing superconductors for practical applications

DOEpatents

Veal, B.W.; Paulikas, A.; Balachandran, U.; Zhong, W.

1997-03-18

A method of fabricating bulk superconducting material is disclosed including RBa{sub 2}Cu{sub 3}O{sub 7{minus}{delta}} comprising heating compressed powder oxides and/or carbonates of R and Ba and Cu present in mole ratios to form RBa{sub 2}Cu{sub 3}O{sub 7{minus}{delta}} in physical contact with an oxide single crystal seed to a temperature sufficient to form a liquid phase in the RBa{sub 2}Cu{sub 3}O{sub 7{minus}{delta}} while maintaining the single crystal seed solid to grow the superconducting material and thereafter cooling to provide a material including RBa{sub 2}Cu{sub 3}O{sub 7{minus}{delta}}. R is a rare earth or Y or La and the single crystal seed has a lattice mismatch with RBa{sub 2}Cu{sub 3}O{sub 7{minus}{delta}} of less than about 2% at the growth temperature. The starting material may be such that the final product contains a minor amount of R{sub 2}BaCuO{sub 5}.

Amorphization and Directional Crystallization of Metals Confined in Carbon Nanotubes Investigated by in Situ Transmission Electron Microscopy.

PubMed

Tang, Dai-Ming; Ren, Cui-Lan; Lv, Ruitao; Yu, Wan-Jing; Hou, Peng-Xiang; Wang, Ming-Sheng; Wei, Xianlong; Xu, Zhi; Kawamoto, Naoyuki; Bando, Yoshio; Mitome, Masanori; Liu, Chang; Cheng, Hui-Ming; Golberg, Dmitri

2015-08-12

The hollow core of a carbon nanotube (CNT) provides a unique opportunity to explore the physics, chemistry, biology, and metallurgy of different materials confined in such nanospace. Here, we investigate the nonequilibrium metallurgical processes taking place inside CNTs by in situ transmission electron microscopy using CNTs as nanoscale resistively heated crucibles having encapsulated metal nanowires/crystals in their channels. Because of nanometer size of the system and intimate contact between the CNTs and confined metals, an efficient heat transfer and high cooling rates (∼10(13) K/s) were achieved as a result of a flash bias pulse followed by system natural quenching, leading to the formation of disordered amorphous-like structures in iron, cobalt, and gold. An intermediate state between crystalline and amorphous phases was discovered, revealing a memory effect of local short-to-medium range order during these phase transitions. Furthermore, subsequent directional crystallization of an amorphous iron nanowire formed by this method was realized under controlled Joule heating. High-density crystalline defects were generated during crystallization due to a confinement effect from the CNT and severe plastic deformation involved.

Silicate Crystal Formation in the Disk of an Erupting Star Artist Concept

NASA Image and Video Library

2009-05-13

This artist's concept illustrates how silicate crystals like those found in comets can be created by an outburst from a growing star. The image shows a young sun-like star encircled by its planet-forming disk of gas and dust. The silicate that makes up most of the dust would have begun as non-crystallized, amorphous particles. Streams of material are seen spiraling from the disk onto the star increasing its mass and causing the star to brighten and heat up dramatically. The outburst causes temperatures to rise in the star's surrounding disk. The animation (figure 1) zooms into the disk to show close-ups of silicate particles. When the disk warms from the star's outburst, the amorphous particles of silicate melt. As they cool off, they transform into forsterite (figure 2), a type of silicate crystal often found in comets in our solar system. In April 2008, NASA's Spitzer Space Telescope detected evidence of this process taking place on the disk of a young sun-like star called EX Lupi. http://photojournal.jpl.nasa.gov/catalog/PIA12008

Barium Transport Process in Impregnated Dispenser Cathodes.

DTIC Science & Technology

1982-01-25

experiments were carried out on pure tungsten. The tung- sten was either in the form of thin foils (6 mm on a side) or single crystal disks (6 mm in...temperature reveal the presence of car- bon, silicon , calcium, and nitrogen impurities, with only trace amounts (ɚ%) of calcium and nitrogen. Carbon is not...expected to be present at diffusion temperatures but forms as an overlayer only upon cooling [6]. We hope to re- duce silicon impurity levels by use of

Fast Cooling and Vitrification of Aqueous Solutions for Cryopreservation

NASA Astrophysics Data System (ADS)

Warkentin, Matt; Husseini, Naji; Berejnov, Viatcheslav; Thorne, Robert

2006-03-01

In many applications, a small volume of aqueous solution must be cooled at a rate sufficient to produce amorphous solid water. Two prominent examples include flash-freezing of protein crystals for X-ray data collection and freezing of cells (i.e. spermatozoa) for cryopreservation. The cooling rate required to vitrify pure water (˜10^6 K/s) is unattainable for volumes that might contain cells or protein crystals, but the required rate can be reduced by adding cryoprotectants. We report the first measurements of the critical concentration required to produce a vitrified sample as a function of the sample's volume, the cryogen into which the sample is plunged, and the temperature of the cryogen, for a wide range of cryoprotectants. These experiments have broad practical consequences for cryopreservation, and provide insight into the physics of glass formation in aqueous systems.

The Effect of Solution Thermal History on Chicken Egg White Lysozyme Nucleation

NASA Technical Reports Server (NTRS)

Burke, Michael W.; Judge, Russell A.; Pusey, Marc L.

2001-01-01

Proteins are highly flexible molecules and often exhibit defined conformational changes in response to changes in the ambient temperature. Chicken egg white lysozyme has been previously shown to undergo an apparent structural change when warmed above the tetragonal/orthorhombic phase transition temperature. This is reflected by a change in the habit of the tetragonal and orthorhombic crystals so formed. In this study, we show that possible conformational changes induced by heating are stable and apparently non-reversible by simple cooling. Exposure of protein solutions to temperatures above the phase change transition temperature, before combining with precipitant solution to begin crystallization, reduces final crystal numbers. Protein that is briefly warmed to 37 C, then cooled shows no sign of reversal to the unheated nucleation behavior even after storage for four weeks at 4 C. The change in nucleation behavior of tetragonal lysozyme crystals, attributed to a structural shift, occurs faster the greater the exposure to temperature above the equi-solubility point for the two phases. Heating for 2 hours at 48 C reduces crystal numbers by 20 fold in comparison to the same solution heated for the same time at 30 C. Thermal treatment of solutions is therefore a possible tool to reduce crystal numbers and increase crystal size. The effects of a protein's previous thermal history are now shown to be a potentially critical factor in subsequent macromolecule crystal nucleation and growth studies.

The Effect of Solution Thermal History on Chicken Egg White Lysozyme Nucleation

NASA Technical Reports Server (NTRS)

Burke, Michael W.; Judge, Russell A.; Pusey, Marc L.; Rose, M. Franklin (Technical Monitor)

2000-01-01

Proteins are highly flexible molecules and often exhibit defined conformational changes in response to changes in the ambient temperature. Chicken egg white lysozyme has been previously shown to undergo an apparent structural change when warmed above the tetragonal/orthorhombic phase transition temperature. This is reflected by a change in the habit of the tetragonal and orthorhombic crystals so formed. In this study we show that possible conformational changes induced by heating are stable and apparently non- reversible by simple cooling. Exposure of protein solutions to temperatures above the phase change transition temperature, before combining with precipitant solution to begin crystallization, reduces final crystal numbers. Protein that is briefly warmed to 37 C, then cooled shows no sign of reversal to the unheated nucleation behavior even after storage for 4 weeks at 4 C. The change in nucleation behavior of tetragonal lysozyme crystals, attributed to a structural shift, occurs faster the greater the exposure to temperature above the equi-solubility point for the two phases. Heating for 2 h at 48 C reduces crystal numbers by 20 fold in comparison to the same solution heated for the same time at 30 C. Thermal treatment of solutions is therefore a possible tool to reduce crystal numbers and increase crystal size. The effects of a protein's previous thermal history are now shown to be a potentially critical factor in subsequent macromolecule crystal nucleation and growth studies.

-Based Slag System

NASA Astrophysics Data System (ADS)

Jiang, Binbin; Wang, Wanlin; Sohn, Il; Wei, Juan; Zhou, Lejun; Lu, Boxun

2014-06-01

The crystallization behavior of a CaO-Al2O3-based slag system with various ZrO2 content (from 1 to 5 wt pct) and CaO/Al2O3 (C/A) ratio (from 0.8 to 1.2) has been studied by using single hot thermocouple technology (SHTT) in this article. The continuous-cooling-transformation (CCT) diagrams and time-temperature-transformation (TTT) diagrams of the above slag system were constructed for the analysis of the varying crystallization behaviors. The results suggested that Al2O3 tended to enhance the slag samples crystallization when the C/A ratio ranged from 0.8 to 1.2, and the critical cooling rate and crystallization temperature increased with the decrease of C/A ratio; meanwhile, the incubation time was also getting shorter with the reduction of C/A ratio. The addition of ZrO2 would enhance the crystallization of slag samples because of the induced heterogeneous nucleation of molten slag. However, the general crystallization was determined by the balance between molten slag viscosity and heterogeneous nucleation, such that Sample 3 (C/A = 1.0, ZrO2 = 3 pct, B2O3 = 10 pct, Li2O = 3 pct [in wt pct]) would demonstrate the strongest crystallization kinetics in a high-temperature zone. The different crystals formed during the tests were also analyzed by scanning electron microscopy (SEM) and X-ray diffraction (XRD).

Three-dimensional bioactive glass implants fabricated by rapid prototyping based on CO(2) laser cladding.

PubMed

Comesaña, R; Lusquiños, F; Del Val, J; López-Álvarez, M; Quintero, F; Riveiro, A; Boutinguiza, M; de Carlos, A; Jones, J R; Hill, R G; Pou, J

2011-09-01

Three-dimensional bioactive glass implants were produced by rapid prototyping based on laser cladding without using moulds. CO(2) laser radiation was employed to melt 45S5 and S520 bioactive glass particles and to deposit the material layer by layer following a desired geometry. Controlled thermal input and cooling rate by fine tuning of the processing parameters allowed the production of crack-free fully dense implants. Microstructural characterization revealed chemical composition stability, but crystallization during processing was extensive when 45S5 bioactive glass was used. Improved results were obtained using the S520 bioactive glass, which showed limited surface crystallization due to an expanded sintering window (the difference between the glass transition temperature and crystallization onset temperature). Ion release from the S520 implants in Tris buffer was similar to that of amorphous 45S5 bioactive glass prepared by casting in graphite moulds. Laser processed S520 scaffolds were not cytotoxic in vitro when osteoblast-like MC3T3-E1 cells were cultured with the dissolution products of the glasses; and the MC3T3-E1 cells attached and spread well when cultured on the surface of the materials. Copyright © 2011 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Membrane-Based Technologies in the Pharmaceutical Industry and Continuous Production of Polymer-Coated Crystals/Particles.

PubMed

Chen, Dengyue; Sirkar, Kamalesh K; Jin, Chi; Singh, Dhananjay; Pfeffer, Robert

2017-01-01

Membrane technologies are of increasing importance in a variety of separation and purification applications involving liquid phases and gaseous mixtures. Although the most widely used applications at this time are in water treatment including desalination, there are many applications in chemical, food, healthcare, paper and petrochemical industries. This brief review is concerned with existing and emerging applications of various membrane technologies in the pharmaceutical and biopharmaceutical industry. The goal of this review article is to identify important membrane processes and techniques which are being used or proposed to be used in the pharmaceutical and biopharmaceutical operations. How novel membrane processes can be useful for delivery of crystalline/particulate drugs is also of interest. Membrane separation technologies are extensively used in downstream processes for bio-pharmaceutical separation and purification operations via microfiltration, ultrafiltration and diafiltration. Also the new technique of membrane chromatography allows efficient purification of monoclonal antibodies. Membrane filtration techniques of reverse osmosis and nanofiltration are being combined with bioreactors and advanced oxidation processes to treat wastewaters from pharmaceutical plants. Nanofiltration with organic solvent-stable membranes can implement solvent exchange and catalyst recovery during organic solvent-based drug synthesis of pharmaceutical compounds/intermediates. Membranes in the form of hollow fibers can be conveniently used to implement crystallization of pharmaceutical compounds. The novel crystallization methods of solid hollow fiber cooling crystallizer (SHFCC) and porous hollow fiber anti-solvent crystallization (PHFAC) are being developed to provide efficient methods for continuous production of polymer-coated drug crystals in the area of drug delivery. This brief review provides a general introduction to various applications of membrane technologies in the pharmaceutical/biopharmaceutical industry with special emphasis on novel membrane techniques for pharmaceutical applications. The method of coating a drug particle with a polymer using the SHFCC method is stable and ready for scale-up for operation over an extended period. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

Velocity of the high-spin low-spin interface inside the thermal hysteresis loop of a spin-crossover crystal, via photothermal control of the interface motion.

PubMed

Slimani, Ahmed; Varret, François; Boukheddaden, Kamel; Garrot, Damien; Oubouchou, Hassane; Kaizaki, Sumio

2013-02-22

We investigated by optical microscopy the thermal transition of the spin-crossover dinuclear iron(II) compound [(Fe(NCSe)(py)(2))(2)(m-bpypz)]. In a high-quality crystal the high-spin (HS) low-spin (LS) thermal transition took place with a sizable hysteresis, at ~108 K and ~116 K on cooling and heating, respectively, through the growth of a single macroscopic domain with a straight LS and HS interface. The interface orientation was almost constant and its propagation velocity was close to ~6 and 26 μ m s(-1) for the on-cooling and on-heating processes, respectively. We found that the motion of the interface was sensitive to the intensity of the irradiation beam of the microscope, through a photothermal effect. By fine-tuning the intensity we could stop and even reverse the interface motion. This way we stabilized a biphasic state of the crystal, and we followed the spontaneous motion of the interface at different temperatures inside the thermal hysteresis loop. This experiment gives access for the first time to an accurate determination of the equilibrium temperature in the case of thermal hysteresis--which was not accessible by the usual quasistatic investigations. The temperature dependence of the propagation velocity inside the hysteretic interval was revealed to be highly nonlinear, and it was quantitatively reproduced by a dynamical mean-field theory, which made possible an estimate of the macroscopic energy barrier.

Numerical modeling perspectives on zircon crystallization and magma reservoir growth at the Laguna del Maule volcanic field, central Chile

NASA Astrophysics Data System (ADS)

Andersen, N. L.; Dufek, J.; Singer, B. S.

2017-12-01

Magma reservoirs in the middle to upper crust are though to accumulate incrementally over 104 -105 years. Coupled crystallization ages and compositions of zircon are a potentially powerful tracer of reservoir growth and magma evolution. However, complex age distributions and disequilibrium trace element partitioning complicate the interpretation of the zircon record in terms of magmatic processes. In order to make quantitative predictions of the effects of magmatic processes that contribute reservoir growth and evolution—such as cooling and crystallization, magma recharge and mixing, and rejuvenation and remelting of cumulate-rich reservoir margins—we develop a model of zircon saturation and growth within a numerical framework of coupled thermal transfer, phase equilibrium, and magma dynamics. We apply this model to the Laguna del Maule volcanic field (LdM), located in central Chile. LdM has erupted at least 40 km3 of rhyolite from 36 vents distributed within a 250 km2 lake basin. Ongoing unrest demonstrates the large, silicic magma system beneath LdM remains active to this day. Zircon from rhyolite erupted between c. 23 and 1.8 ka produce a continuous distribution of 230Th-238U ages ranging from eruption to 40 ka, as well as less common crystal domains up to 165 ka and rare xenocrysts. Zircon trace element compositions fingerprint compositionally distinct reservoirs that grew within the larger magma system. Despite the dominantly continuous distributions of ages, many crystals are characterized by volumetrically substantial, trace element enriched domains consistent with rapid crystal growth. We utilize numerical simulations to assess the magmatic conditions required to catalyze these "blooms" of crystallization and the magma dynamics that contributed to the assembly of the LdM magma system.

Petrology and Physics of Magma Ocean Crystallization

NASA Technical Reports Server (NTRS)

Elkins-Tanton, Linda T.; Parmentier, E. M.; Hess, P. C.

2003-01-01

Early Mars is thought to have been melted significantly by the conversion of kinetic energy to heat during accretion of planetesimals. The processes of solidification of a magma ocean determine initial planetary compositional differentiation and the stability of the resulting mantle density profile. The stability and compositional heterogeneity of the mantle have significance for magmatic source regions, convective instability, and magnetic field generation. Significant progress on the dynamical problem of magma ocean crystallization has been made by a number of workers. The work done under the 2003 MFRP grant further explored the implications of early physical processes on compositional heterogeneity in Mars. Our goals were to connect early physical processes in Mars evolution with the present planet's most ancient observable characteristics, including the early, strong magnetic field, the crustal dichotomy, and the compositional characteristics of the SNC meteorite's source regions as well as their formation as isotopically distinct compositions early in Mars's evolution. We had already established a possible relationship between the major element compositions of SNC meteorite sources and processes of Martian magma ocean crystallization and overturn, and under this grant extended the analysis to the crucial trace element and isotopic SNC signatures. This study then demonstrated the ability to create and end the magnetic field through magma ocean cumulate overturn and subsequent cooling, as well as the feasibility of creating a compositionally- and volumetrically-consistent crustal dichotomy through mode-1 overturn and simultaneous adiabatic melting.

Intracellular ice and cell survival in cryo-exposed embryonic axes of recalcitrant seeds of Acer saccharinum: an ultrastructural study of factors affecting cell and ice structures

PubMed Central

Wesley-Smith, James; Berjak, Patricia; Pammenter, N. W.; Walters, Christina

2014-01-01

Background and Aims Cryopreservation is the only long-term conservation strategy available for germplasm of recalcitrant-seeded species. Efforts to cryopreserve this form of germplasm are hampered by potentially lethal intracellular freezing events; thus, it is important to understand the relationships among cryo-exposure techniques, water content, structure and survival. Methods Undried embryonic axes of Acer saccharinum and those rapidly dried to two different water contents were cooled at three rates and re-warmed at two rates. Ultrastructural observations were carried out on radicle and shoot tips prepared by freeze-fracture and freeze-substitution to assess immediate (i.e. pre-thaw) responses to cooling treatments. Survival of axes was assessed in vitro. Key Results Intracellular ice formation was not necessarily lethal. Embryo cells survived when crystal diameter was between 0·2 and 0·4 µm and fewer than 20 crystals were distributed per μm2 in the cytoplasm. Ice was not uniformly distributed within the cells. In fully hydrated axes cooled at an intermediate rate, the interiors of many organelles were apparently ice-free; this may have prevented the disruption of vital intracellular machinery. Intracytoplasmic ice formation did not apparently impact the integrity of the plasmalemma. The maximum number of ice crystals was far greater in shoot apices, which were more sensitive than radicles to cryo-exposure. Conclusions The findings challenge the accepted paradigm that intracellular ice formation is always lethal, as the results show that cells can survive intracellular ice if crystals are small and localized in the cytoplasm. Further understanding of the interactions among water content, cooling rate, cell structure and ice structure is required to optimize cryopreservation treatments without undue reliance on empirical approaches. PMID:24368198

Intracellular ice and cell survival in cryo-exposed embryonic axes of recalcitrant seeds of Acer saccharinum: an ultrastructural study of factors affecting cell and ice structures.

PubMed

Wesley-Smith, James; Berjak, Patricia; Pammenter, N W; Walters, Christina

2014-03-01

Cryopreservation is the only long-term conservation strategy available for germplasm of recalcitrant-seeded species. Efforts to cryopreserve this form of germplasm are hampered by potentially lethal intracellular freezing events; thus, it is important to understand the relationships among cryo-exposure techniques, water content, structure and survival. Undried embryonic axes of Acer saccharinum and those rapidly dried to two different water contents were cooled at three rates and re-warmed at two rates. Ultrastructural observations were carried out on radicle and shoot tips prepared by freeze-fracture and freeze-substitution to assess immediate (i.e. pre-thaw) responses to cooling treatments. Survival of axes was assessed in vitro. Intracellular ice formation was not necessarily lethal. Embryo cells survived when crystal diameter was between 0·2 and 0·4 µm and fewer than 20 crystals were distributed per μm(2) in the cytoplasm. Ice was not uniformly distributed within the cells. In fully hydrated axes cooled at an intermediate rate, the interiors of many organelles were apparently ice-free; this may have prevented the disruption of vital intracellular machinery. Intracytoplasmic ice formation did not apparently impact the integrity of the plasmalemma. The maximum number of ice crystals was far greater in shoot apices, which were more sensitive than radicles to cryo-exposure. The findings challenge the accepted paradigm that intracellular ice formation is always lethal, as the results show that cells can survive intracellular ice if crystals are small and localized in the cytoplasm. Further understanding of the interactions among water content, cooling rate, cell structure and ice structure is required to optimize cryopreservation treatments without undue reliance on empirical approaches.

Immersion Freezing of Aluminas: The Effect of Crystallographic Properties on Ice Nucleation

NASA Astrophysics Data System (ADS)

King, M.; Chong, E.; Freedman, M. A.

2017-12-01

Atmospheric aerosol particles serve as the nuclei for heterogeneous ice nucleation, a process that allows for ice to form at higher temperatures and lower supersaturations with respect to ice. This process is essential to the formation of ice in cirrus clouds. Heterogeneous ice nucleation is affected by many factors including the composition, crystal structure, porosity, and surface area of the particles. However, these factors are not well understood and, as such, are difficult to account for in climate models. To test the effects of crystal structure on ice nucleation, a system of transition aluminas (Al2O3) that differ only in their crystal structure, despite being compositionally similar, were tested using immersion freezing. Particles were immersed in water and placed into a temperature controlled chamber. Freezing events were then recorded as the chamber was cooled to negative 30 °. Alpha-alumina, which is a member of the hexagonal crystal system, showed a significantly higher temperature at which all particles froze in comparison to other samples. This supports the hypothesis that, since a hexagonal crystal structure is the lowest energy state for ice, hexagonal surface structures would best facilitate ice nucleation. However, a similar sample of hexagonal chi-alumina did not show the same results. Further analysis of the samples will be done to characterize surface structures and composition. These conflicting data sets raise interesting questions about the effect of other surface features, such as surface area and porosity, on ice nucleation.

Synthesis of highly uniform Cu2O spheres by a two-step approach and their assembly to form photonic crystals with a brilliant color.

PubMed

Su, Xin; Chang, Jie; Wu, Suli; Tang, Bingtao; Zhang, Shufen

2016-03-21

Monodisperse semiconductor colloidal spheres with a high refractive index hold great potential for building photonic crystals with a strong band gap, but the difficulty in separating the nucleation and growth processes makes it challenging to prepare highly uniform semiconductor colloidal spheres. Herein, real monodisperse Cu2O spheres were prepared via a hot-injection & heating-up two-step method using diethylene glycol as a milder reducing agent. The diameter of the as prepared Cu2O spheres can be tuned from 90 nm to 190 nm precisely. The SEM images reveal that the obtained Cu2O spheres have a narrow size distribution, which permits their self-assembly to form photonic crystals. The effects of precursor concentration and heating rates on the size and morphology of the Cu2O spheres were investigated in detail. The results indicate that the key points of the method include the burst nucleation to form seeds at a high temperature followed by rapid cooling to prevent agglomeration, and appropriate precursor concentration as well as a moderate growth rate during the further growth process. Importantly, photonic crystal films exhibiting a brilliant structural color were fabricated with the obtained monodisperse Cu2O spheres as building blocks, proving the possibility of making photonic crystals with a strong band gap. The developed method was also successfully applied to prepare monodisperse CdS spheres with diameters in the range from 110 nm to 210 nm.

A study on cooling characteristics of clathrate compound as low temperature latent heat storage material

NASA Astrophysics Data System (ADS)

Kim, Chang Oh; Kim, Jin Heung; Chung, Nak Kyu

2007-07-01

Materials that can store low temperature latent heat are organic/inorganic chemicals, eutectic salt system and clathrate compound. Clathrate compound is the material that host compound in hydrogen bond forms cage and guest compound is included into it and combined. Crystallization of hydrate is generated at higher temperature than that of ice from pure water. And physical properties according to temperature are stable and congruent melting phenomenon is occurred without phase separation and it has relatively high latent heat. But clathrate compound still has supercooling problem occurred in the course of phase change and supercooling should be minimized because it affects efficiency of equipment very much. Therefore, various studies on additives to restrain this or heat storage methods are needed. Supercooling is the phenomenon that low temperature thermal storage material is not crystallized and existed as liquid for some time under phase change temperature. Because phase change into solid is delayed and it is existed as liquid due to this, heat transfer from low temperature thermal storage material is lowered. Therefore it is not crystallized at original phase change temperature and crystallized after cooled as much as supercooling degree and operation time of refrigerator is increased. In this study was investigated the cooling characteristics of the clathrate compound as a low temperature latent heat storage material. And additive was added to clathrate compound and its supercooling restrain effect was studied experimentally.

Crystallization Behavior and Heat Transfer of Fluorine-Free Mold Fluxes with Different Na2O Concentration

NASA Astrophysics Data System (ADS)

Yang, Jian; Zhang, Jianqiang; Sasaki, Yasushi; Ostrovski, Oleg; Zhang, Chen; Cai, Dexiang; Kashiwaya, Yoshiaki

2016-08-01

In this study, the crystallization behavior and heat transfer of CaO-SiO2-Na2O-B2O3-TiO2-Al2O3-MgO-Li2O fluorine-free mold fluxes with different Na2O contents (5 to 11 mass pct) were studied using single/double hot thermocouple technique (SHTT/DHTT) and infrared emitter technique (IET), respectively. Continuous cooling transformation (CCT) and time-temperature transformation (TTT) diagrams constructed using SHTT showed that crystallization temperature increased and incubation time shortened with the increase of Na2O concentration, indicating an enhanced crystallization tendency. The crystallization process of mold fluxes in the temperature field simulating the casting condition was also investigated using DHTT. X-ray diffraction (XRD) analysis of the quenched mold fluxes showed that the dominant phase changed from CaSiO3 to Ca11Si4B2O22 with the increasing concentration of Na2O. The heat transfer examined by IET showed that the increase of Na2O concentration reduced the responding heat flux when Na2O was lower than 9 mass pct but the further increase of Na2O to 11 mass pct enhanced the heat flux. The correlation between crystallinity and heat transfer was discussed in terms of crystallization tendency and crystal morphology.

Effect of crystals and fibrous network polymer additives on cellular morphology of microcellular foams

NASA Astrophysics Data System (ADS)

Miyamoto, Ryoma; Utano, Tatsumi; Yasuhara, Shunya; Ishihara, Shota; Ohshima, Masahiro

2015-05-01

In this study, the core-back foam injection molding was used for preparing microcelluar polypropylene (PP) foam with either a 1,3:2,4 bis-O-(4-methylbenzylidene)-D-sorbitol gelling agent (Gel-all MD) or a fibros network polymer additive (Metablen 3000). Both agent and addiive could effectively control the celluar morphology in foams but somehow different ways. In course of cooling the polymer with Gel-all MD in the mold caity, the agent enhanced the crystal nucleation and resulted in the large number of small crystals. The crystals acted as effective bubble nucleation agent in foaming process. Thus, the agent reduced the cell size and increased the cell density, drastically. Furthermore, the small crystals provided an inhomogenuity to the expanding cell wall and produced the high open cell content with nano-scale fibril structure. Gell-all as well as Metablene 3000 formed a gel-like fibrous network in melt. The network increased the elongational viscosity and tended to prevent the cell wall from breaking up. The foaming temperature window was widened by the presence of the network. Especially, the temperature window where the macro-fibrous structure was formed was expanded to the higher temperature. The effects of crystal nucleating agent and PTFE on crystals' size and number, viscoelsticity, rheological propreties of PP and cellular morphology were compared and thorougly investigated.

Crustal accretion at fast spreading ridges and implications for hydrothermal circulation

NASA Astrophysics Data System (ADS)

Theissen-Krah, S.; Rupke, L.; Hasenclever, J.

2015-12-01

Oceanic crust is continuously created at mid-ocean ridges, but the location of lower crust crystallization continues to be debated since the proposal of the gabbro glacier and many sills end-member models. Geophysical and geochemical studies find evidence for either of the models. The crust is cooled by a combination of heat diffusion and advection, and hydrothermal circulation is thought to play a key role in distinguishing between both models. We use our numerical model for joint modeling of crustal accretion and hydrothermal circulation1 to test different accretion and hydrothermal cooling scenarios. The results match the seismic and structural observations from the East Pacific Rise2 and the Oman Ophiolite3, with a shallow melt lens at the correct location overlaying a narrow volume of partially molten rocks. Our results show that no more than 25-50% of the lower crust crystallizes in situ and that deep circulation is likely to occur at fast and intermediate spreading ridges. The occurrence of deep hydrothermal cooling however does not rule out that a major portion of the lower crust is formed in the shallow melt lens; our simulations rather suggest that it is necessary independent of where in the lower crust crystallization takes place. 1 Theissen-Krah, S., Iyer, K., Rupke, L. H. & Morgan, J. P. Coupled mechanical and hydrothermal modeling of crustal accretion at intermediate to fast spreading ridges. Earth and Planetary Science Letters 311, 275-286, doi:10.1016/j.epsl.2011.09.018 (2011). 2 Dunn, R. A., Toomey, D. R. & Solomon, S. C. Three-dimensional seismic structure and physical properties of the crust and shallow mantle beneath the East Pacific Rise at 9 degrees 30'N. Journal of Geophysical Research-Solid Earth 105, 23537-23555 (2000). 3 Nicolas, A. & Boudier, F. Structural contribution from the Oman ophiolite to processes of crustal accretion at the East Pacific Rise. Terra Nova 27, 77-96, doi:10.1111/ter.12137 (2015).

(U-Th-Sm)/He thermochronological age distribution in a slowly cooled plutonic complex (Ploumanac'h intrusion, France): insights into helium diffusion processes.

NASA Astrophysics Data System (ADS)

Recanati, A. C.; Gautheron, C.; Barbarand, J.; Tassan-Got, L.; Missenard, Y.; Pinna-Jamme, R.

2015-12-01

(U-Th-Sm)/He thermochronology is widely used to determine the thermal histories of mountain ranges and sedimentary basins. Apatite crystals retain helium at low temperatures, thus giving an insight into upper crustal evolution (e.g. exhumation, subsidence, erosion). Advanced models predict He production and diffusion rates in apatite crystals, thereby allowing determination of helium dates by integration over time/temperature paths (e.g. Gautheron et al., 2009). However, scattered dates and discordance between predicted and measured dates suggest that other parameters than time or temperature may also influence helium contents in apatite. The present study determines the variables that affect He diffusion in apatite over long timescales. We report the (U-Th-Sm)/He date distribution within a slowly cooled intrusion, along with AFT data, as well as extensive petrological and chemical characterization. The Ploumanac'h site (Brittany, France) was chosen because it includes small-scale spatial variations in petrology and chemistry (6-9106 tracks/cm2). GAUTHERON C., TASSAN-GOT L., BARBARAND J., PAGEL M., 2009. Effect of alpha-damage annealing on apatite (U-Th)/He thermochronology. Chem. Geol. 266, 166-179.

Cholesterol-Based Grafted Polymer Brushes as Alignment Coating with Temperature-Tuned Anchoring for Nematic Liquid Crystals.

PubMed

Stetsyshyn, Yurij; Raczkowska, Joanna; Budkowski, Andrzej; Awsiuk, Kamil; Kostruba, Andriy; Nastyshyn, Svyatoslav; Harhay, Khrystyna; Lychkovskyy, Edward; Ohar, Halyna; Nastishin, Yuriy

2016-10-11

Novel alignment coating with temperature-tuned anchoring for nematic liquid crystals (NLCs) was successfully fabricated in three step process, involving polymerization of poly(cholesteryl methacrylate) (PChMa) from oligoproxide grafted to the glass surface premodified with 3-aminopropyltriethoxysilane. Molecular composition, thickness, wettability of the PChMa coating and its alignment action for a NLC were examined with time of flight-secondary ion mass spectrometry, ellipsometry, contact angle measurements, polarization optical microscopy and commercially produced PolScope technique allowing for mapping of the optic axis and optical retardance within the microscope field view. We find that the PChMa coating provides a specific monotonous increase (decrease) in the tilt angle of the NLC director with respect to the substrates normal upon heating (cooling) referred to as anchoring tuning.

Plans and Preliminary Results of Fundamental Studies of Ice Crystal Icing Physics in the NASA Propulsion Systems Laboratory

NASA Technical Reports Server (NTRS)

Struk, Peter; Tsao, Jen-Ching; Bartkus, Tadas

2017-01-01

This paper describes plans and preliminary results for using the NASA Propulsion Systems Lab (PSL) to experimentally study the fundamental physics of ice-crystal ice accretion. NASA is evaluating whether this facility, in addition to full-engine and motor-driven-rig tests, can be used for more fundamental ice-accretion studies that simulate the different mixed-phase icing conditions along the core flow passage of a turbo-fan engine compressor. The data from such fundamental accretion tests will be used to help develop and validate models of the accretion process. This paper presents data from some preliminary testing performed in May 2015 which examined how a mixed-phase cloud could be generated at PSL using evaporative cooling in a warmer-than-freezing environment.

Plans and Preliminary Results of Fundamental Studies of Ice Crystal Icing Physics in the NASA Propulsion Systems Laboratory

NASA Technical Reports Server (NTRS)

Struk, Peter; Tsao, Jen-Ching; Bartkus, Tadas

2016-01-01

This presentation accompanies the paper titled Plans and Preliminary Results of Fundamental Studies of Ice Crystal Icing Physics in the NASA Propulsion Systems Laboratory. NASA is evaluating whether PSL, in addition to full-engine and motor-driven-rig tests, can be used for more fundamental ice-accretion studies that simulate the different mixed-phase icing conditions along the core flow passage of a turbo-fan engine compressor. The data from such fundamental accretion tests will be used to help develop and validate models of the accretion process. This presentation (and accompanying paper) presents data from some preliminary testing performed in May 2015 which examined how a mixed-phase cloud could be generated at PSL using evaporative cooling in a warmer-than-freezing environment.

Thermo-optical dynamics in an optically pumped Photonic Crystal nano-cavity.

PubMed

Brunstein, M; Braive, R; Hostein, R; Beveratos, A; Rober-Philip, I; Sagnes, I; Karle, T J; Yacomotti, A M; Levenson, J A; Moreau, V; Tessier, G; De Wilde, Y

2009-09-14

Linear and non-linear thermo-optical dynamical regimes were investigated in a photonic crystal cavity. First, we have measured the thermal relaxation time in an InP-based nano-cavity with quantum dots in the presence of optical pumping. The experimental method presented here allows one to obtain the dynamics of temperature in a nanocavity based on reflectivity measurements of a cw probe beam coupled through an adiabatically tapered fiber. Characteristic times of 1.0+/-0.2 micros and 0.9+/-0.2 micros for the heating and the cooling processes were obtained. Finally, thermal dynamics were also investigated in a thermo-optical bistable regime. Switch-on/off times of 2 micros and 4 micros respectively were measured, which could be explained in terms of a simple non-linear dynamical representation.

The Crystals Cave in a test tube

NASA Astrophysics Data System (ADS)

Puig, C.; Romero, M. L.

2012-04-01

It's quite easy to understand formation of crystals in Nature by evaporation of the solutions that contain minerals, but many times we have realised that our pupils hardly understand that precipitation is a process mostly caused by changing parameters in a solution, like pH, temperature, etc. and not necessarily depending on evaporation. We propose a hands-on activity using the context of the Cave of the Crystals in Naica's mine, Mexico. The Crystals Cave is a wonderful place where giant crystals of selenite (gypsum) have grown feeding from a supersaturated anhydrite solution1. Miners discovered the cave filled with hot water, and drained it to explore the gallery. The cave is now a giant laboratory where scientists are looking for the keys to understand geological processes. Teaching sequence (for students 15 years old) is as follows: DISCOVERING A MARVELLOUS PLACE: We showed our pupils several images and a short video of the Cave of the Crystals and ask them about the process that may have caused the phenomenon. Whole-class discussion. PRESENTING A CHALLENGE TO OUR STUDENTS: "COULD WE CREATE A CRYSTALS CAVE IN A TEST TUBE?" EXPERIMENTING TO IMITATE NATURE: Students tried to grow crystals simulating the same conditions as those in Naica's mine. We have chosen KNO3, a salt more soluble than gypsum. We added 85 g of salt to 200 ml of water (solubility of KNO3 at 25°C is 36 g per 100 gr of water) and heated it until it is dissolved. Afterwards, we poured the solution into some test tubes and other recipients and let them cool at room temperature. And they got a beautiful crystals cave!! THINKING A LITTLE MORE: we asked pupils some questions to make them think about the process and to predict what would happen in different situations. For example: a) What would happen with crystals if we heated the tubes again? or b) What would happen if we took the remaining solution from the tubes and keep it in the fridge? PROVING A NEW HYPOTHESIS: Pupils collected the remaining solutions from all the containers, poured them in a Petri dish and let them inside the fridge for a day: New crystals grew at the bottom of the Petri dishes!!! LOOKING FOR THE SCIENTIFIC EXPLANATIONS: We made them work in pairs in order to find an explanation about giant crystals in Naica's mine, by using short videos2, a scientific article or any information they can find on line. THINKING OF FUTURE: Should we close Naica's mine in order to preserve it? Whole-class discussion

The Thermal and Radiation Exposure History of Lunar Meteorites

NASA Technical Reports Server (NTRS)

Benoit, Paul H.; Sears, Derek W. G.; Symes, Steven J. K.

1996-01-01

We have measured the natural and induced thermoluminescence (TL) of seven lunar meteorites in order to examine their crystallization, irradiation, and recent thermal histories. Lunar meteorites have induced TL properties similar to Apollo samples of the same provenance (highland or mare), indicating similar crystallization and metamorphic histories. MacAlplne Hills 88104/5 has experienced the greatest degree of impact/regolith processing among the highland-dominated meteorites. The basaltic breccia QUE 94281 is dominated by mare component but may also contain a significant highland component. For the mare-dominated meteorites, EET 87521 may have a significant highland impact-melt component, while Asuka 881757 and Y-793169 have been heavily shocked. The thermal history of Y-793169 included slow cooling, either during impact processing or during its initial crystallization. Our natural TL data indicate that most lunar meteorites have apparently been irradiated in space a few thousand years, with most less than 15,000 a. Elephant Moraine 87521 has the lowest irradiation exposure time, being less than 1,000 a. Either the natural TL of ALHA81005, Asuka 881757 and Y-82192 was only partially reset by lunar ejection or these meteorites were in small perihelia orbits (less than or equal to 0.7 AU).

Programming scale-free optics in disordered ferroelectrics.

PubMed

Parravicini, Jacopo; Conti, Claudio; Agranat, Aharon J; DelRe, Eugenio

2012-06-15

Using the history dependence of a dipolar glass hosted in a compositionally disordered lithium-enriched potassium tantalate niobate (KTN:Li) crystal, we demonstrate scale-free optical propagation at tunable temperatures. The operating equilibration temperature is determined by previous crystal spiralling in the temperature/cooling-rate phase space.

Concomitant Ordering and Symmetry Lowering

ERIC Educational Resources Information Center

Boo, William O. J.; Mattern, Daniell L.

2008-01-01

Examples of concomitant ordering include magnetic ordering, Jahn-Teller cooperative ordering, electronic ordering, ionic ordering, and ordering of partially-filled sites. Concomitant ordering sets in when a crystal is cooled and always lowers the degree of symmetry of the crystal. Concomitant ordering concepts can also be productively applied to…

Development of a cryopreservation protocol for testicular interstitial cells with the account of temperature intervals for controlled cooling below -60°С.

PubMed

Gurina, T M; Pakhomov, A V; Kyryliuk, A L; Bozhok, G A

2011-04-01

A long course of anticancer therapy may lead to testicular steroidogenesis destruction. Cryopreservation of testicular interstitial cells (TIC) would be a strategy to protect hormonal and fertile potential of pre-pubertal boys treated with chemo - or radiotherapy. The aim of this research was to optimize protocols for freezing of TIC. Essential physical processes associated with the presence of dimethyl sulphoxide (Me(2)SO) in the cryoprotectant solution take place at the temperatures below -60°С. These processes are the eutectic crystallization at the stage of freezing and the recrystallization before the melting of the eutectic mixture at the stage of heating. Both of the processes affect the viability of the cells subjected to cryopreservation. Temperature intervals when these processes take place were determined by the method of thermoplastic deformation for 10% Me(2)SO selected for cryopreservation of TIC. Rat TIC were cryopreserved using five different protocols which varied in cooling rates within the chosen temperature intervals. Post-thaw cell viability and metabolic activity were evaluated by Trypan Blue and 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) staining assays. Leydig cell recovery after cryopreservation was measured by 3-beta-hydroxysteroid dehydrogenase reaction. Based on the obtained results, the authors developed a cryopreservation protocol for TIC which makes it possible to achieve great cell viability due to using controlled cooling rates within the temperature intervals below -60°С. Copyright © 2011 Elsevier Inc. All rights reserved.

Crystallization, flow and thermal histories of lunar and terrestrial compositions

NASA Technical Reports Server (NTRS)

Uhlmann, D. R.

1979-01-01

Contents: a kinetic treatment of glass formation; effects of nucleating heterogeneities on glass formation; glass formation under continuous cooling conditions; crystallization statistics; kinetics of crystal nucleation; diffusion controlled crystal growth; crystallization of lunar compositions; crystallization between solidus and liquidus; crystallization on reheating a glass; temperature distributions during crystallization; crystallization of anorthite and anorthite-albite compositions; effect of oxidation state on viscosity; diffusive creep and viscous flow; high temperature flow behavior of glass-forming liquids, a free volume interpretation; viscous flow behavior of lunar compositions; thermal history of orange soil material; breccias formation by viscous sintering; viscous sintering; thermal histories of breccias; solute partitioning and thermal history of lunar rocks; heat flow in impact melts; and thermal histories of olivines.

In situ visualization of domain structure evolution during field cooling in 0.67PMN-0.33PT single crystal

NASA Astrophysics Data System (ADS)

Ushakov, A. D.; Esin, A. A.; Chezganov, D. S.; Turygin, A. P.; Akhmatkhanov, A. R.; Hu, Q.; Sun, L.; Wei, X.; Shur, V. Ya

2017-10-01

The evolution of the domain structure during in-field cooling was in situ studied in [001]-cut single crystals of relaxor ferroelectric (1-x)Pb(Mg1/3Nb2/3)O3-xPbTiO3 (PMN-PT) with x = 0.33 with maximum of dielectric permittivity at 150°C. The main stages of domain evolution have been separated. The visualization of the static as-grown and polarized domain structures with high spatial resolution by piezoresponse force microscopy and scanning electron microscopy allowed measuring the characteristic features of maze and needle-like domain structures.

On the behaviour and origin of the major deep level (EL2) in GaAs

NASA Technical Reports Server (NTRS)

Lagowski, J.; Parsey, J. M.; Kaminska, M.; Wada, K.; Gatos, H. C.

1982-01-01

In an extensive crystal growth and characterization study of Bridgman-grown GaAs it was established that the following factors affect the concentration of the EL2 level: (1) the As pressure during growth; (2) the partial pressure of Ga2O; (3) the concentration of shallow donors and acceptors; and (4) the post-growth cooling cycle. The role of these factors is qualitatively and quantitatively explained by attributing the 0.82 eV donor state to the antisite defect As-sub-Ga formed as a result of Ga-vacancy migration during the post-growth cooling of the crystals.

Crystallization and transformation of polymorphic forms of trioleoyl glycerol and 1,2-dioleoyl-3-rac-linoleoyl glycerol.

PubMed

Bayés-García, Laura; Calvet, Teresa; Cuevas-Diarte, Miquel Àngel; Ueno, Satoru; Sato, Kiyotaka

2013-08-08

This study examined the influence of different thermal treatments on the crystallization and transformation of trioleoyl glycerol (OOO) and 1,2-dioleoyl-3-rac-linoleoyl glycerol (OOL). Two triacylglycerol (TAG) samples were cooled at 0.5-15 °C·min(-1) and heated at 2 and 15 °C·min(-1). The polymorphic characteristics of the two TAGs were analyzed in situ using differential scanning calorimetry, Raman spectroscopy, and synchrotron radiation X-ray diffraction. Multiple polymorphic forms were identified in OOO (α, β'2, β'1, β2, and β1) and OOL (α, β'2, and β'1). Larger quantities of more stable forms (e.g., β2 and β1 of OOO and β'1 of OOL) were obtained when the samples were slowly cooled and heated. In contrast, less stable polymorphs were obtained with increased cooling and heating rates. Polymorphic transformations occurred in either solid-state or melt-mediation and were influenced by heating rates. The results were analyzed by considering the activation energies for crystallization and transformation of stable and less stable polymorphic forms in comparison with previous studies on 1,3-dipalmitoyl-2-oleoyl-glycerol and 1, 3-dioleoyl-2-palmitoyl-glycerol.

Crystals and Crystals: On the Mythology of Magmatic Processes

NASA Astrophysics Data System (ADS)

Marsh, B.

2008-12-01

The intimate records of the deep functioning of magmatic systems reside in the temporal and spatial records of magma flux, composition and crystal load. The records for a single system are piecemeal: Plutons show good spatial records, but poor temporal records. Volcanoes give through lava sequences good temporal records, but no spatial context. Because of this dichotomy, two, almost mutually exclusive, branches of magmatology have developed, whereas in Nature there is only a single process. The processes envisioned in these schools necessary to deliver the end rock record are distinct. It is our tools and historic perspectives that have steered the science, not the subject itself. Due to this approach an almost mythical conception of how magmas function has become commonplace. The circumvention of this dilemma rests in carefully evaluating the records on hand in the light of a broad understanding of the fundamental mechanics of how magma lives and dies. It is these basic principles that promise to unify plutonic and volcanic evidence to reveal the full nature of magmatism on all scales. The two most basic features of all magmatic processes are the universal presence of solidification fronts and the presence or absence of a crystal cargo. Almost without exception (e.g., shallow pressure quenching) all first generation crystals grow in marginal solidification fronts (SFs) bordering all magmas. The package of isotherms bounded by the liquidus and solidus define SFs, which propagate in response to the rate of cooling. All physical and chemical processes occurring within SFs compete with the advancement or retreat of solidification. SFs are governed by crystallinity regimes: Suspension Zone (<25 % xtals), Capture Front (~25 %), Mush Zone (25-55%), Rigidity Front (~55%; Critical Crystallinity), and Rigid Crust Zone (>55% xtals). Magmas are laced with nuclei that multiply and grow when overtaken. Crystal growth rates are bounded; tiny crystals reside at the front of SFs and big crystals at the rear. It is unlikely that crystals can ever escape SFs once beyond the Capture Front, and crystals that do fall (singly or in plumes) from the leading edge of SFs may suffer resorbtion upon transit through deeper, hotter magma. Above all, differentiation is severely limited as there is no crystallization in the central, hottest part of the body, and the crystals that are available for separation are tiny and have little effect on melt composition. Recall, ~50% loss of olivine enhances silica by 5%, but this places this magma at Critical Crystallinity. Phenocrysts come from disrupted SFs and are essential to read as such; they may come from a wide range of P's and T's. Ragged old crystals rolling about for untold numbers of flushing times record specious process times; telling more about transport and crystal-chemical noise in the system than the life of typical, first generation crystallization processes. Yet, noise is a system characteristic as is exemplified by the disharmonious isotope heritage of neighbor phenocrysts. Differentiation mainly comes from the sudden loss of a dynamically entrained load of crystals of diverse heritage equilibrating with the 'carrier' magma. Big crystals carrying fluid inclusions, for example, come from deep within SFs where residual melt is low and enriched and not from the central, early, primitive magma. All systems show these characteristics. They are exceedingly important to recognize and to put in the context of the power, longevity, and geometry of the system. Not recognizing them for what they are and what they are not recording only builds mythological magmatic systems.

Why is intracellular ice lethal? A microscopical study showing evidence of programmed cell death in cryo-exposed embryonic axes of recalcitrant seeds of Acer saccharinum.

PubMed

Wesley-Smith, James; Walters, Christina; Pammenter, N W; Berjak, Patricia

2015-05-01

Conservation of the genetic diversity afforded by recalcitrant seeds is achieved by cryopreservation, in which excised embryonic axes (or, where possible, embryos) are treated and stored at temperatures lower than -180 °C using liquid nitrogen. It has previously been shown that intracellular ice forms in rapidly cooled embryonic axes of Acer saccharinum (silver maple) but this is not necessarily lethal when ice crystals are small. This study seeks to understand the nature and extent of damage from intracellular ice, and the course of recovery and regrowth in surviving tissues. Embryonic axes of A. saccharinum, not subjected to dehydration or cryoprotection treatments (water content was 1·9 g H2O g(-1) dry mass), were cooled to liquid nitrogen temperatures using two methods: plunging into nitrogen slush to achieve a cooling rate of 97 °C s(-1) or programmed cooling at 3·3 °C s(-1). Samples were thawed rapidly (177 °C s(-1)) and cell structure was examined microscopically immediately, and at intervals up to 72 h in vitro. Survival was assessed after 4 weeks in vitro. Axes were processed conventionally for optical microscopy and ultrastructural examination. Immediately following thaw after cryogenic exposure, cells from axes did not show signs of damage at an ultrastructural level. Signs that cells had been damaged were apparent after several hours of in vitro culture and appeared as autophagic decomposition. In surviving tissues, dead cells were sloughed off and pockets of living cells were the origin of regrowth. In roots, regrowth occurred from the ground meristem and procambium, not the distal meristem, which became lethally damaged. Regrowth of shoots occurred from isolated pockets of surviving cells of peripheral and pith meristems. The size of these pockets may determine the possibility for, the extent of and the vigour of regrowth. Autophagic degradation and ultimately autolysis of cells following cryo-exposure and formation of small (0·2-0·4 µm) intracellular ice crystals challenges current ideas that ice causes immediate physical damage to cells. Instead, freezing stress may induce a signal for programmed cell death (PCD). Cells that form more ice crystals during cooling have faster PCD responses. Published by Oxford University Press on behalf of the Annals of Botany Company 2015. This work is written by (a) US Government employee(s) and is in the public domain in the US.

Phase transformations, anisotropic pyroelectric energy harvesting and electrocaloric properties of (Pb,La)(Zr,Sn,Ti)O3 single crystals.

PubMed

Zhuo, Fangping; Li, Qiang; Gao, Jinghan; Yan, Qingfeng; Zhang, Yiling; Xi, Xiaoqing; Chu, Xiangcheng

2017-05-31

(Pb,La)(Zr,Sn,Ti)O 3 (PLZST) single crystals with their chemical composition located at the tetragonal antiferroelectric region are grown via the flux method in a PbO-PbF 2 -B 2 O 3 mixture. Segregation of the Ti 4+ component in the as-grown crystals is observed due to the strong affinity between the oxygen anion and Ti 4+ ions. The critical electric field of the antiferroelectric to ferroelectric phase transition is determined to be about 0.5 kV mm -1 . The electric field induced ferroelectric phase transforms back into the antiferroelectric phase at a depolarization temperature of 125 °C. Anisotropy of the harvested energy density and electrocaloric behaviors are achieved for the [100], [110] and [111]-oriented PLZST crystals. Based on the thermodynamic theory approach, all the abovementioned behaviors originate from the anisotropic total entropy change. Enhanced electrocaloric strength (0.3 K mm kV -1 ) and the harvested energy density of 0.62 J cm -3 are obtained in the [111]-oriented PLZST crystals. Our results demonstrate the competence of PLZST single crystals for cooling devices and pyroelectric energy harvesting and provide new opportunities to improve energy harvesting density and electrocaloric properties via the anisotropic structural layout, which make the PLZST crystals attractive for solid state cooling devices and energy conversion technologies.

The effects of crystallization and residual glass on the chemical durability of iron phosphate waste forms containing 40 wt% of a high MoO3 Collins-CLT waste

NASA Astrophysics Data System (ADS)

Hsu, Jen-Hsien; Bai, Jincheng; Kim, Cheol-Woon; Brow, Richard K.; Szabo, Joe; Zervos, Adam

2018-03-01

The effects of cooling rate on the chemical durability of iron phosphate waste forms containing up to 40 wt% of a high MoO3 Collins-CLT waste simulant were determined at 90 °C using the product consistency test (PCT). The waste form, designated 40wt%-5, meets appropriate Department of Energy (DOE) standards when rapidly quenched from the melt (as-cast) and after slow cooling following the CCC (canister centerline cooling)-protocol, although the quenched glass is more durable. The analysis of samples from the vapor hydration test (VHT) and the aqueous corrosion test (differential recession test) reveals that rare earth orthophosphate (monazite) and Zr-pyrophosphate crystals that form on cooling are more durable than the residual glass in the 40wt%-5 waste form. The residual glass in the CCC-treated samples has a greater average phosphate chain length and a lower Fe/P ratio, and those contribute to its faster corrosion kinetics.

Unsteady High Turbulence Effects on Turbine Blade Film Cooling Heat Transfer Performance Using a Transient Liquid Crystal Technique

NASA Technical Reports Server (NTRS)

Han, J. C.; Ekkad, S. V.; Du, H.; Teng, S.

2000-01-01

Unsteady wake effect, with and without trailing edge ejection, on detailed heat transfer coefficient and film cooling effectiveness distributions is presented for a downstream film-cooled gas turbine blade. Tests were performed on a five-blade linear cascade at an exit Reynolds number of 5.3 x 10(exp 5). Upstream unsteady wakes were simulated using a spoke-wheel type wake generator. Coolant blowing ratio was varied from 0.4 to 1.2; air and CO2 were used as coolants to simulate different density ratios. Surface heat transfer and film effectiveness distributions were obtained using a transient liquid crystal technique; coolant temperature profiles were determined with a cold wire technique. Results show that Nusselt numbers for a film cooled blade are much higher compared to a blade without film injection. Unsteady wake slightly enhances Nusselt numbers but significantly reduces film effectiveness versus no wake cases. Nusselt numbers increase only slic,htly but film cooling, effectiveness increases significantly with increasing, blowing ratio. Higher density coolant (CO2) provides higher effectiveness at higher blowing ratios (M = 1.2) whereas lower density coolant (Air) provides higher 0 effectiveness at lower blowing ratios (M = 0.8). Trailing edge ejection generally has more effect on film effectiveness than on the heat transfer, typically reducing film effectiveness and enhancing heat transfer. Similar data is also presented for a film cooled cylindrical leading edge model.

A thermodynamics model for morphology prediction of aluminum nano crystals fabricated by the inert gas condensation method

NASA Astrophysics Data System (ADS)

Wen, Yu; Xia, Dehong

2018-03-01

The purpose of this study is to provide scientific guidance for the morphological control of nanoparticle synthesis using the gas phase method. A universal thermodynamics model is developed to predict the morphology of nanoparticles fabricated using the inert gas condensation method. By using this model, the morphologies of aluminum nanocrystals are predicted under various preparation conditions. There are two types of energy that jointly determine the formation of nanoparticle morphology—Gibbs free energy for nanoparticles and energy variation during the process. The results show that energy variation dominates morphology formation when the cooling rate is less than 2 × 1011 K s-1 in the aluminum nanocrystal production process. At the beginning of the nanoparticle growth, the most stable morphology is predicted to be spherical, but the energetically preferred morphology becomes cubic as the particle grows. The turning point in the particle size at which spherical morphology is no longer the most stable morphology is exhibited as a function of pressure in a condensation chamber for different cooling rates. In this paper, we focus on the need for morphology prediction based on preparation conditions. It is concluded that nanoparticles with various morphologies could be obtained by adjusting the cooling rate and pressure in the condensation chamber.

Texturing by cooling a metallic melt in a magnetic field.

PubMed

Tournier, Robert F; Beaugnon, Eric

2009-02-01

Processing in a magnetic field leads to the texturing of materials along an easy-magnetization axis when a minimum anisotropy energy exists at the processing temperature; the magnetic field can be applied to a particle assembly embedded into a liquid, or to a solid at a high diffusion temperature close to the melting temperature or between the liquidus and the solidus temperatures in a region of partial melting. It has been shown in many experiments that texturing is easy to achieve in congruent and noncongruent compounds by applying the field above the melting temperature T m or above the liquidus temperature of alloys. Texturing from a melt is successful when the overheating temperature is just a few degrees above T m and fails when the processing time above T m is too long or when the overheating temperature is too high; these observations indicate the presence of unmelted crystals above T m with a size depending on these two variables that act as growth nuclei. A recent model that predicts the existence of unmelted crystals above the melting temperature is used to calculate their radius in a bismuth melt.

Recycling of Ammonia Wastewater During Vanadium Extraction from Shale

NASA Astrophysics Data System (ADS)

Shi, Qihua; Zhang, Yimin; Liu, Tao; Huang, Jing

2018-03-01

In the vanadium metallurgical industry, massive amounts of ammonia hydroxide or ammonia salt are added during the precipitation process to obtain V2O5; therefore, wastewater containing a high level of NH4 + is generated, which poses a serious threat to environmental and hydrologic safety. In this article, a novel process was developed to recycle ammonia wastewater based on a combination of ammonia wastewater leaching and crystallization during vanadium extraction from shale. The effects of the NH4 + concentration, temperature, time and liquid-to-solid ratio on the leaching efficiencies of vanadium, aluminum and potassium were investigated, and the results showed that 93.2% of vanadium, 86.3% of aluminum and 96.8% of potassium can be leached from sulfation-roasted shale. Subsequently, 80.6% of NH4 + was separated from the leaching solution via cooling crystallization. Vanadium was recovered via a combined method of solvent extraction, precipitation and calcination. Therefore, ammonia wastewater was successfully recycled during vanadium extraction from shale.

Survival of plant tissue at super-low temperatures v. An electron microscope study of ice in cortical cells cooled rapidly.

PubMed

Sakai, A; Otsuka, K

1967-12-01

Experiments were carried out with cortical cells in twig bark of mulberry trees in winter in order to clarify the mechanism of survival at super-low temperatures with rapid cooling and rewarming. Attention was given to the relation between the existence of intracellular ice crystals and survival.Cortical cells were cooled rapidly by direct immersion into liquid nitrogen or isopentane cooled at various temperatures. After immersion, they were freeze-substituted with absolute ethanol at -78 degrees . They were then embedded, sectioned and examined under the electron microscope for the presence and distribution of cavities left after ice removal.Cells were found to remain alive and contain no ice cavities when immersed rapidly into isopentane baths kept below -60 degrees . Those cells at intermediate temperatures from -20 degrees to -45 degrees , were almost all destroyed. It was also observed that many ice cavities were contained in the cells immersed rapidly into isopentane baths at -30 degrees . The data seem to indicate that no ice crystals were formed when cooled rapidly by direct immersion into isopentane baths below -60 degrees or into liquid nitrogen.The tissue sections immersed in liquid nitrogen were rapidly transferred to isopentane baths at temperatures ranging from -70 degrees to -10 degrees before rapid rewarming. There was little damage when samples were held at temperatures below -50 degrees for 10 minutes or below -60 degrees for 16 hours. No cavities were found in these cells. Above -45 degrees , and especially at -30 degrees , however, all cells were completely destroyed even when exposed only for 1 minute. Many ice cavities were observed throughout these cells. The results obtained may be explained in terms of the growth rate of intracellular ice crystals.

Fragile morphotropic phase boundary and phase stability in the near-surface region of the relaxor ferroelectric (1 -x ) Pb (Z n1 /3N b2 /3) O3-x PbTi O3 : [001] field-cooled phase diagrams

NASA Astrophysics Data System (ADS)

Wang, Yaojin; Wang, Ding; Yuan, Guoliang; Ma, He; Xu, Feng; Li, Jiefang; Viehland, D.; Gehring, Peter M.

2016-11-01

We have examined the effects of field cooling on the phase diagram of the relaxor system (1 -x ) Pb (Z n1 /3N b2 /3) O3-x PbTi O3 (PZN-x PT ) for compositions near the morphotropic phase boundary (MPB). High-resolution diffraction measurements using Cu Kα x rays, which probe ≈3 μ m below the crystal surface, were made on field-cooled (FC) single-crystal specimens of PZN-4.5 %PT and PZN-6.5 %PT under electric fields of 1 and 2 kV/cm applied along [001] and combined with previous neutron diffraction data, which probe the entire crystal volume, for FC PZN-8 %PT [Ohwada et al., Phys. Rev. B 67, 094111 (2003), 10.1103/PhysRevB.67.094111]. A comparison to the zero-field-cooled (ZFC) PZN-x PT phase diagram reveals several interesting features: (1) The short-range monoclinic phase observed in the ZFC state on the low-PT side of the MPB is replaced by a monoclinic MA phase; (2) field cooling extends the tetragonal phase to higher temperatures and lower-PT concentrations; (3) the orthorhombic phase near the MPB is replaced by a monoclinic MC phase; (4) the vertical MPB in the ZFC phase diagram bends significantly towards the low-PT side in the FC state. These results demonstrate that both the phase stability and the nature of the MPB in PZN-PT within the near-surface regions are fragile in the presence of electric fields.

Improvement in Stability of SPring-8 Standard X-Ray Monochromators with Water-Cooled Crystals

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

Yamazaki, Hiroshi; Shimizu, Nobtaka; Kumasaka, Takashi

2010-06-23

SPring-8 standard double-crystal monochromators containing water-cooled crystals were stabilized to a sufficient level to function as a part of optics components to supply stable microfocused x-ray beams, by determining causes of the instability and then removing them. The instability was caused by two factors--thermal deformation of fine stepper stages in the monochromator, which resulted in reduction in beam intensity with time, and vibrations of coolant supply units and vacuum pumps, which resulted in fluctuation in beam intensity. We remodeled the crystal holders to maintain the stage temperatures constant with water, attached x-ray and electron shields to the stages in ordermore » to prevent their warming up, introduced accumulators in the water circuits to absorb pressure pulsation, used polyurethane tubes to stabilize water flow, and placed rubber cushions under scroll vacuum pumps. As a result, the intensity reduction rate of the beam decreased from 26% to 1% per hour and the intensity fluctuation from 13% to 1%. The monochromators were also modified to prevent radiation damage to the crystals, materials used as a water seal, and motor cables.« less

Growth, structural, thermal, dielectric and optical studies on HBST crystal: A potential THz emitter.

PubMed

Ma, Yuzhe; Teng, Bing; Cao, Lifeng; Zhong, Degao; Ji, Shaohua; Teng, Fei; Liu, Jiaojiao; Yao, Yuan; Tang, Jie; Tong, Jiaming

2018-02-05

The efficient organic nonlinear optical material 4-hydroxy benzaldehyde-N-methyl 4-stilbazolium tosylate (HBST) was grown from methanol by slope nucleation method combined with slow cooling (SNM-SC) for the first time. The optimum growth conditions based on the cooling rate was further investigated. The single crystal X-ray diffraction (XRD) revealed that the chromophores of HBST crystal make an angle of about 33° with respect to the a-axis, which is close to the optimum of Terahertz (THz)-wave generation and electro-optics applications. NMR and FT-IR spectral studies have been performed to ascertain various functional groups present in the sample. Futhermore, the thermal stability and decomposition stages were analyzed through TG-DTA and DSC techniques. The dielectric constant and dielectric loss of HBST crystal have been studied. Critical optical properties like the absorption coefficient, refractive index, cut-off wavelength and band gap energy were calculated. Photoluminescence (PL) exication studies indicated green emission occured at 507nm. All the results of HBST crystal make it a promising candidate in the fields of optoelectronic and the generation of THz. Copyright © 2017 Elsevier B.V. All rights reserved.

Samples for estimating primary volatiles in Martian magmas and ancient atmospheric pressures on Mars

NASA Technical Reports Server (NTRS)

Anderson, A. T., Jr.

1988-01-01

Inclusions of glass are likely to be present in phenocrysts in volcanic rocks from Mars, because these occur in volcanic rocks from both Earth and Moon. The usefulness of the inclusions depends upon their size and composition. The compositions of tiny inclusions may be modified by diffusion during growth of the enclosing crystal, the modifications increasing with melt viscosity (silica). Slow cooling results in crystallization and possible redistribution of volatiles, the effects increasing with decreasing silica. Primary volatile concentrations are best sought in inclusions larger than about 50 micrometer diameter in olivine or chromite crystals from quickly cooled basaltic scoria. Such crystals may be present in sands, but it would be preferable to extract them from individual rocks which could be dated and compositionally characterized. This would allow eventual understanding of the role of time and place in outgassing and volcanism on Mars. Analyses of volatiles in inclusions of more siliceous glass in non-basaltic rocks will reveal whether deep outgassing occurs and whether surface volatiles are recycled. Most volcanic crystals contain inclusions, but large inclusions can be uncommon. In the case of terrestrial basalts sample masses of several hundred grams are generally sufficient.

Photonic crystal wave guide for non-cryogenic cooled carbon nanotube based middle wave infrared sensors

NASA Astrophysics Data System (ADS)

Fung, Carmen Kar Man; Xi, Ning; Lou, Jianyong; Lai, King Wai Chiu; Chen, Hongzhi

2010-10-01

We report high sensitivity carbon nanotube (CNT) based middle wave infrared (MWIR) sensors with a two-dimensional photonic crystal waveguide. MWIR sensors are of great importance in a variety of current military applications including ballistic missile defense, surveillance and target detection. Unlike other existing MWIR sensing materials, CNTs exhibit low noise level and can be used as new nano sensing materials for MWIR detection where cryogenic cooling is not required. However, the quantum efficiency of the CNT based infrared sensor is still limited by the small sensing area and low incoming electric field. Here, a photonic nanostructure is used as a resonant cavity for boosting the electric field intensity at the position of the CNT sensing element. A two-dimensional photonic crystal with periodic holes in a polymer thin film is fabricated and a resonant cavity is formed by removing holes from the array of the photonic crystal. Based on the design of the photonic crystal topologies, we theoretically study the electric field distribution to predict the resonant behavior of the structure. Numerical simulations reveal the field is enhanced and almost fully confined to the defect region of the photonic crystal. To verify the electric field enhancement effect, experiments are also performed to measure the photocurrent response of the sensor with and without the photonic crystal resonant cavity. Experimental results show that the photocurrent increases ~3 times after adding the photonic crystal resonant cavity.

Solid-state characterization of mefenamic acid.

PubMed

Panchagnula, Ramesh; Sundaramurthy, Prakash; Pillai, Omathanu; Agrawal, Shrutidevi; Raj, Yasvanth Ashok

2004-04-01

The purpose of this study was to characterize mefenamic acid (MA) from commercial samples and samples crystallized from different solvents. Various techniques used for characterization included microscopy (hot stage microscopy, scanning electron microscopy), intrinsic dissolution rate, differential scanning calorimetry (DSC), Fourier transform infrared (FTIR) spectroscopy and powder X-ray diffractometry (pXRD). The commercial samples varied in their crystal habit, thermal behavior, and intrinsic dissolution rate. It was found that the commercial samples were polymorphic Form I, which converted to Form II on heating in a DSC pan. Similarly, compression in an intrinsic dissolution rate (IDR) press resulted in the conversion of Form I to Form II. On the other hand, the samples recrystallized from different solvents under varying conditions yielded different crystal habits. Stirring and degree of supersaturation significantly influenced the crystal habit in all the solvents used in the study. Samples crystallized from ethanol and tetrahydrofuran yielded Form I, which behaved similarly to the commercial samples (M1 and M3). Recrystallization from ethyl acetate at a fast cooling rate yielded Form I, which on melting crystallized to Form II. The form I crystallized from ethyl acetate by fast cooling converted partially to form II on storing at ambient conditions. Forms I and II of MA were enantiotropically related. The results demonstrate the variable material characteristics of the commercial samples of MA and the influence of the crystallizing conditions on the formation of the polymorphs. Copyright 2004 Wiley-Liss, Inc. and the American Pharmacists Association.

Growth, structural, optical, thermal and mechanical properties of ammonium pentaborate single crystal.

PubMed

Balakrishnan, T; Bhagavannarayana, G; Ramamurthi, K

2008-11-15

Nonlinear optical single crystals of ammonium pentaborate (APB) were grown by the slow cooling method from aqueous solution. Grown crystal was characterized by powder X-ray diffraction (PXRD) and FT-IR spectral analysis. Perfection of the grown crystal was evaluated by high-resolution X-ray diffractometry (HRXRD). The effect of nylon threading on the perfection of the grown bigger crystal was also studied by HRXRD. The range and percentage of optical transmission was ascertained by recording UV-vis-NIR spectrum. Thermal properties were investigated by TG-DTA and DSC analyses. Its mechanical hardness was estimated by Vickers microhardness tester.

Phononic crystal devices

DOEpatents

El-Kady, Ihab F [Albuquerque, NM; Olsson, Roy H [Albuquerque, NM

2012-01-10

Phononic crystals that have the ability to modify and control the thermal black body phonon distribution and the phonon component of heat transport in a solid. In particular, the thermal conductivity and heat capacity can be modified by altering the phonon density of states in a phononic crystal. The present invention is directed to phononic crystal devices and materials such as radio frequency (RF) tags powered from ambient heat, dielectrics with extremely low thermal conductivity, thermoelectric materials with a higher ratio of electrical-to-thermal conductivity, materials with phononically engineered heat capacity, phononic crystal waveguides that enable accelerated cooling, and a variety of low temperature application devices.

Survival of mouse oocytes after being cooled in a vitrification solution to −196°C at 95° to 70,000°C/min and warmed at 610° to 118,000°C/min: A new paradigm for cryopreservation by vitrification☆

PubMed Central

Mazur, Peter; Seki, Shinsuke

2011-01-01

There is great interest in achieving reproducibly high survivals of mammalian oocytes (especially human) after cryopreservation, but the results to date have not matched the interest. A prime cause of cell death is the formation of more than trace amounts of intracellular ice, and one strategy to avoid it is vitrification. In vitrification procedures, cells are loaded with high concentrations of glass-inducing solutes and cooled to −196°C at rates high enough to presumably induce the glassy state. In the last decade, several devices have been developed to achieve very high cooling rates. Nearly all in the field have assumed that the cooling rate is the critical factor. The purpose of our study was to test that assumption by examining the consequences of cooling mouse oocytes in a vitrification solution at four rates ranging from 95°C/min to 69,250°C/min to −196°C and for each cooling rate, subjecting them to five warming rates back above 0°C at rates ranging from 610°C/min to 118,000°C/min. In samples warmed at the highest rate (118,000°C/min), survivals were 70 to 85% regardless of the prior cooling rate. In samples warmed at the lowest rate (610°C/min), survivals were low regardless of the prior cooling rate, but decreased from 25% to 0% as the cooling rate was increased from 95°C/min to 69,000°C/min. Intermediate cooling and warming rates gave intermediate survivals. The especially high sensitivity of survival to warming rate suggests that either the crystallization of intracellular glass during warming or the growth by recrystallization of small intracellular ice crystals formed during cooling are responsible for the lethality of slow warming. PMID:21055397

Survival of mouse oocytes after being cooled in a vitrification solution to -196°C at 95° to 70,000°C/min and warmed at 610° to 118,000°C/min: A new paradigm for cryopreservation by vitrification.

PubMed

Mazur, Peter; Seki, Shinsuke

2011-02-01

There is great interest in achieving reproducibly high survivals of mammalian oocytes (especially human) after cryopreservation, but the results to date have not matched the interest. A prime cause of cell death is the formation of more than trace amounts of intracellular ice, and one strategy to avoid it is vitrification. In vitrification procedures, cells are loaded with high concentrations of glass-inducing solutes and cooled to -196°C at rates high enough to presumably induce the glassy state. In the last decade, several devices have been developed to achieve very high cooling rates. Nearly all in the field have assumed that the cooling rate is the critical factor. The purpose of our study was to test that assumption by examining the consequences of cooling mouse oocytes in a vitrification solution at four rates ranging from 95 to 69,250°C/min to -196°C and for each cooling rate, subjecting them to five warming rates back above 0°C at rates ranging from 610 to 118,000°C/min. In samples warmed at the highest rate (118,000°C/min), survivals were 70% to 85% regardless of the prior cooling rate. In samples warmed at the lowest rate (610°C/min), survivals were low regardless of the prior cooling rate, but decreased from 25% to 0% as the cooling rate was increased from 95 to 69,000°C/min. Intermediate cooling and warming rates gave intermediate survivals. The especially high sensitivity of survival to warming rate suggests that either the crystallization of intracellular glass during warming or the growth by recrystallization of small intracellular ice crystals formed during cooling are responsible for the lethality of slow warming. Copyright © 2010 Elsevier Inc. All rights reserved.

Contribution of early impact events to metal-silicate separation, thermal annealing, and volatile redistribution: Evidence in the Pułtusk H chondrite

NASA Astrophysics Data System (ADS)

Krzesińska, Agata M.

2017-11-01

Three-dimensional X-ray tomographic reconstructions and petrologic studies reveal voluminous accumulations of metal in Pułtusk H chondrite. At the contact of these accumulations, the chondritic rock is enriched in troilite. The rock contains plagioclase-rich bands, with textures suggesting crystallization from melt. Unusually large phosphates are associated with the plagioclase and consist of assemblages of merrillite, and fluorapatite and chlorapatite. The metal accumulations were formed by impact melting, rapid segregation of metal-sulfide melt and the incorporation of this melt into the fractured crater basement. The impact most likely occurred in the early evolution of the H chondrite parent body, when post-impact heat overlapped with radiogenic heat. This enabled slow cooling and separation of the metallic melt into metal-rich and sulfide-rich fractions. This led to recrystallization of chondritic rock in contact with the metal accumulations and the crystallization of shock melts. Phosphorus was liberated from the metal and subsumed by the silicate shock melt, owing to oxidative conditions upon slow cooling. The melt was also a host for volatiles. Upon further cooling, phosphorus reacted with silicates leading to the formation of merrillite, while volatiles partitioned into the residual halogen-rich, dry fluid. In the late stages, the fluid altered merrillite to patchy Cl/F-apatite. The above sequence of alterations demonstrates that impact during the early evolution of chondritic parent bodies might have contributed to local metal segregation and silicate melting. In addition, postshock conditions supported secondary processes: compositional/textural equilibration, redistribution of volatiles, and fluid alterations.

On melt solutions for the growth of CaTiO3 crystals

NASA Astrophysics Data System (ADS)

Klimm, Detlef; Schmidt, Max; Wolff, Nora; Guguschev, Christo; Ganschow, Steffen

2018-03-01

When calcium titanate crystals are grown from stoichiometric melts, they crystallize in the cubic perovskite structure. Upon cooling to room temperature they undergo subsequent phase transitions to tetragonal and orthorhombic modifications. These phase transitions are disruptive and result in severely damaged crystals. This paper presents differential thermal analysis data for several prospective solvents, with the aim to identify a system offering the possibility to perform crystal growth of undistorted CaTiO3 crystals by crystallizing them significantly below the melting point directly in the low temperature modification. From mixtures CaF2:TiO2:CaTiO3 = 3:1:1 (molar ratio) the growth of undistorted, at least millimeter-sized CaTiO3 crystals is possible.

Study of recrystallization and devitrification of lunar glass

NASA Technical Reports Server (NTRS)

Ulrich, D. R.

1974-01-01

The technique of differential thermal analysis (DTA) was applied to the study of the Apollo 17 orange soil (74220,63) and the Apollo 16 glass coated anorthite (64455,21). These glasses show accentuated exotherms of strain relief in the annealing range which is indicative of rapid cooling. These are amenable to interpretation by comparison to the known history of synthetic glasses. Synthetic glasses were prepared whose similarity in behavior between the lunar glasses and their synthetic analogs is striking. Approximate rates of cooling of the lunar glasses were determined from comparative DTA of lunar and synthetic glasses and from the determination of the relation of strain relief in the annealing range to quench rate. At higher temperatures the glasses show exotherms of crystallization. The crystallization products associated with the exothermic reactions have been identified by X-ray diffraction and the surface morphologies developed by strain relief and crystallization have been characterized with scanning electron microscopy.

Influence of additive L-phenylalanine on stabilization of metastable α-form of L-glutamic acid in cooling crystallization

NASA Astrophysics Data System (ADS)

Quang, Khuu Chau; Nhan, Le Thi Hong; Huyen, Trinh Thi Thanh; Tuan, Nguyen Anh

2017-09-01

The influence of additive amino acid L-phenylalanine on stabilization of metastable α-form of L-glutamic acid was investigated in cooling crystallization. The present study found that the additive L-phenylalanine could be used to stabilize the pure metastable α-form in L-glutamic acid crystallization, where the additive concentration of 0.05-0.1 (g/L) was sufficient to stabilize the 100% wt metastable α-form in solid product at L-glutamic acid concentration of 30-45 (g/L). Additionally, the present results indicated that the adsorption of additive L-phenylalanine on the (001) surface of α-form was more favorable than that of the β-form molecular, so the nucleation sites of stable β-form was occupied by additive molecular, which resulted in inhibition of nucleation and growth of β-form, allowing stabilization of metastable α-form.

Direct Measurement of Water States in Cryopreserved Cells Reveals Tolerance toward Ice Crystallization

PubMed Central

Huebinger, Jan; Han, Hong-Mei; Hofnagel, Oliver; Vetter, Ingrid R.; Bastiaens, Philippe I.H.; Grabenbauer, Markus

2016-01-01

Complex living systems such as mammalian cells can be arrested in a solid phase by ultrarapid cooling. This allows for precise observation of cellular structures as well as cryopreservation of cells. The state of water, the main constituent of biological samples, is crucial for the success of cryogenic applications. Water exhibits many different solid states. If it is cooled extremely rapidly, liquid water turns into amorphous ice, also called vitreous water, a glassy and amorphous solid. For cryo-preservation, the vitrification of cells is believed to be mandatory for cell survival after freezing. Intracellular ice crystallization is assumed to be lethal, but experimental data on the state of water during cryopreservation are lacking. To better understand the water conditions in cells subjected to freezing protocols, we chose to directly analyze their subcellular water states by cryo-electron microscopy and tomography, cryoelectron diffraction, and x-ray diffraction both in the cryofixed state and after warming to different temperatures. By correlating the survival rates of cells with their respective water states during cryopreservation, we found that survival is less dependent on ice-crystal formation than expected. Using high-resolution cryo-imaging, we were able to directly show that cells tolerate crystallization of extra- and intracellular water. However, if warming is too slow, many small ice crystals will recrystallize into fewer but bigger crystals, which is lethal. The applied cryoprotective agents determine which crystal size is tolerable. This suggests that cryoprotectants can act by inhibiting crystallization or recrystallization, but they also increase the tolerance toward ice-crystal growth. PMID:26541066

Online monitoring of thermo-cycles and its correlation with microstructure in laser cladding of nickel based super alloy

NASA Astrophysics Data System (ADS)

Muvvala, Gopinath; Patra Karmakar, Debapriya; Nath, Ashish Kumar

2017-01-01

Laser cladding, basically a weld deposition technique, is finding applications in many areas including surface coatings, refurbishment of worn out components and generation of functionally graded components owing to its various advantages over conventional methods like TIG, PTA etc. One of the essential requirements to adopt this technique in industrial manufacturing is to fulfil the increasing demand on product quality which could be controlled through online process monitoring and correlating the signals with the mechanical and metallurgical properties. Rapid thermo-cycle i.e. the fast heating and cooling rates involved in this process affect above properties of the deposited layer to a great extent. Therefore, the current study aims to monitor the thermo-cycles online, understand its variation with process parameters and its effect on different quality aspects of the clad layer, like microstructure, elemental segregations and mechanical properties. The effect of process parameters on clad track geometry is also studied which helps in their judicious selection to deposit a predefined thickness of coating. In this study Inconel 718, a nickel based super alloy is used as a clad material and AISI 304 austenitic steel as a substrate material. The thermo-cycles during the cladding process were recorded using a single spot monochromatic pyrometer. The heating and cooling rates were estimated from the recorded thermo-cycles and its effects on microstructures were characterised using SEM and XRD analyses. Slow thermo-cycles resulted in severe elemental segregations favouring Laves phase formation and increased γ matrix size which is found to be detrimental to the mechanical properties. Slow cooling also resulted in termination of epitaxial growth, forming equiaxed grains near the surface, which is not preferred for single crystal growth. Heat treatment is carried out and the effect of slow cooling and the increased γ matrix size on dissolution of segregated elements in metal matrix is studied.

Tunneling-thermally activated vacancy diffusion mechanism in quantum crystals

NASA Astrophysics Data System (ADS)

Natsik, V. D.; Smirnov, S. N.

2017-10-01

We consider a quasiparticle model of a vacancy in a quantum crystal, with metastable quantum states localized at the lattice sites in potential wells of the crystal field. It is assumed that the quantum dynamics of such vacancies can be described in the semi-classical approximation, where its spectrum consists of a broad band with several split-off levels. The diffusive movement of the vacancy in the crystal volume is reduced to a sequence of tunneling and thermally activated hops between the lattice cites. The temperature dependence of the vacancy diffusion coefficient shows a monotonic decrease during cooling with a sharp transition from an exponential dependence that is characteristic of a high-temperature thermally activated diffusion, to a non-thermal tunneling process in the region of extremely low temperatures. Similar trends have been recently observed in an experimental study of mass-transfer in the 4He and 3He crystals [V. A. Zhuchkov et al., Low Temp. Phys. 41, 169 (2015); Low Temp. Phys. 42, 1075 (2016)]. This mechanism of vacancy diffusion and its analysis complement the concept of a diffusional flow of a defection-quasiparticle quantum gas with a band energy spectrum proposed by Andreev and Lifshitz [JETP 29, 1107 (1969)] and Andreev [Sov. Phys. Usp. 19, 137 (1976)].

Water softening by induced crystallization in fluidized bed.

PubMed

Chen, Yuefang; Fan, Rong; An, Danfeng; Cheng, Yujie; Tan, Hazel

2016-12-01

Fluidized bed and induced crystallization technology were combined to design a new type of induced crystallization fluidized bed reactor. The added particulate matter served as crystal nucleus to induce crystallization so that the insoluble material, which was in a saturated state, could precipitate on its surface. In this study, by filling the fluidized bed with quartz sand and by adjusting water pH, precipitation of calcium carbonate was induced on the surface of quartz sand, and the removal of water hardness was achieved. With a reactor influent flow of 60L/hr, a fixed-bed height of 0.5m, pH value of 9.5, quartz sand nuclear diameter of 0.2-0.4mm, and a reflux ratio of 60%, the effluent concentration of calcium hardness was reduced to 60mg/L and 86.6% removal efficiency was achieved. The resulting effluent reached the quality standard set for circulating cooling water. Majority of the material on the surface of quartz sand was calculated to be calcium carbonate based on energy spectrum analysis and moisture content was around 15.994%. With the low moisture content, dewatering treatment is no longer required and this results to cost savings on total water treatment process. Copyright © 2016. Published by Elsevier B.V.

Uranyl nitrate hexahydrate solubility in nitric acid and its crystallization selectivity in the presence of nitrate salts

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

Burns, Jonathan D.; Moyer, Bruce A.

The solubility of uranyl nitrate hexahydrate was determined as a function of nitric acid concentration and temperature, and the crystallization yield was calculated. Results showed an increase in crystal formation at lower initial nitric acid concentrations upon cooling a saturated solution of U(VI) from 50 °C to 2 °C, with over 70% recovery of U(VI) mass at all nitric acid concentrations and nearly quantitative recovery starting at 4 M HNO 3. A direct correlation between the change in mother liquor volume percent and U mass removal percent was observed. By reducing the cooling rate from roughly 4.0 °C/min to 0.22more » °C/min, the separation factor was increased from 3.88 to 15.7 to greater than 81 for the separation of U(VI) from Sr, Cs, and Nd. At the slower cooling rate, the separation factors were measured as a function of acidity for 2.0–4.3 M HNO 3, showing a decrease in selectivity with a decrease in the acidity. There was also no indication that tetravalent metal double-salt precipitation occurred with either Zr 4+ or Ce 4+. Here, these results indicate that a high-yield, high purity hexavalent actinide crystallization scheme may offer attractive benefits for nuclear-fuel recycle in that only a single very simple and well-understood technology is employed, and the use of organic compounds and solvents is avoided.« less

Raman scattering evidence of hydrohalite formation on frozen yeast cells.

PubMed

Okotrub, K A; Surovtsev, N V

2013-02-01

We studied yeast cells in physiological solution during freezing by Raman microspectroscopy technique. The purpose was to find out the origin of a sharp peak near ∼3430cm(-1) in Raman spectrum of frozen mammalian cells, observed earlier (J. Dong et al., Biophys. J. 99 (2010) 2453), which presumably could be used as an indicator of intracellar ice appearance. We have shown that this line (actually doublet of 3408 and 3425cm(-1)) corresponds to Raman spectrum of hydrohalite (NaCl⋅2H(2)O), which is formed as the result of the eutectic crystallization of the liquid solution around the cells. We also show that the spatial distribution of hydrohalite in the sample significantly depends on the cooling rate. At lower cooling rate (1°C/min), products of eutectic crystallization form layer on the cell surface which thickness varies for different cells and can reach ∼1μm in thickness. At higher cooling rate (20°C/min), the hydrohalite distribution appears more homogeneous, in the sample, and the eutectic crystallization layer around the cells was estimated to be less than ∼20nm. These experimental results are consistent with scenarios predicted by the two-factor hypothesis for freezing induced cell injury. This work demonstrates a potential of Raman microspectroscopy to study peculiarities of the eutectic crystallization around single cells in vivo with the high spatial resolution. Copyright © 2012 Elsevier Inc. All rights reserved.

Uranyl nitrate hexahydrate solubility in nitric acid and its crystallization selectivity in the presence of nitrate salts

DOE PAGES

Burns, Jonathan D.; Moyer, Bruce A.

2017-10-23

The solubility of uranyl nitrate hexahydrate was determined as a function of nitric acid concentration and temperature, and the crystallization yield was calculated. Results showed an increase in crystal formation at lower initial nitric acid concentrations upon cooling a saturated solution of U(VI) from 50 °C to 2 °C, with over 70% recovery of U(VI) mass at all nitric acid concentrations and nearly quantitative recovery starting at 4 M HNO 3. A direct correlation between the change in mother liquor volume percent and U mass removal percent was observed. By reducing the cooling rate from roughly 4.0 °C/min to 0.22more » °C/min, the separation factor was increased from 3.88 to 15.7 to greater than 81 for the separation of U(VI) from Sr, Cs, and Nd. At the slower cooling rate, the separation factors were measured as a function of acidity for 2.0–4.3 M HNO 3, showing a decrease in selectivity with a decrease in the acidity. There was also no indication that tetravalent metal double-salt precipitation occurred with either Zr 4+ or Ce 4+. Here, these results indicate that a high-yield, high purity hexavalent actinide crystallization scheme may offer attractive benefits for nuclear-fuel recycle in that only a single very simple and well-understood technology is employed, and the use of organic compounds and solvents is avoided.« less

Origin of ultramafic xenoliths containing exsolved pyroxenes from Hualalai Volcano, Hawaii

USGS Publications Warehouse

Bohrson, W.A.; Clague, D.A.

1988-01-01

Hualalai Volcano, Hawaii, is best known for the abundant and varied xenoliths included in the historic 1800 Kaupulehu alkalic basalt flow. Xenoliths, which range in composition from dunite to anorthosite, are concentrated at 915-m elevation in the flow. Rare cumulate ultramafic xenoliths, which include websterite, olivine websterite, wehrlite, and clinopyroxenite, display complex pyroxene exsolution textures that indicate slow cooling. Websterite, olivine websterite, and one wehrlite are spinel-bearing orthopyroxene +olivine cumulates with intercumulus clinopyroxene +plagioclase. Two wehrlite samples and clinopyroxenite are spinel-bearing olivine cumulates with intercumulus clinopyroxene+orthopyroxene + plagioclase. Two-pyroxene geothermometry calculations, based on reconstructed pyroxene compositions, indicate that crystallization temperatures range from 1225?? to 1350?? C. Migration or unmixing of clinopyroxene and orthopyroxene stopped between 1045?? and 1090?? C. Comparisons of the abundance of K2O in plagioclase and the abundances of TiO2 and Fe2O3in spinel of xenoliths and mid-ocean ridge basalt, and a single 87Sr/ 86Sr determination, indicate that these Hualalai xenoliths are unrelated to mid-ocean ridge basalt. Similarity between the crystallization sequence of these xenoliths and the experimental crystallization sequence of a Hawaiian olivine tholeiite suggest that the parental magma of the xenoliths is Hualalai tholeiitic basalt. Xenoliths probably crystallized between about 4.5 and 9 kb. The 155??-230?? C of cooling which took place over about 120 ka - the age of the youngest Hualalai tholeiitic basalt - yield maximum cooling rates of 1.3??10-3-1.91??10-3 ??C/yr. Hualalai ultramafic xenoliths with exsolved pyroxenes crystallized from Hualalai tholeiitic basalt and accumulated in a magma reservoir located between 13 and 28 km below sealevel. We suspect that this reservoir occurs just below the base of the oceanic crust at about 19 km below sealevel. ?? 1988 Springer-Verlag.

Thermal History and Crystallinity of Sheet Intrusions

NASA Astrophysics Data System (ADS)

Whittington, A. G.; Nabelek, P. I.; Hofmeister, A.

2011-12-01

Magma emplaced in a sheet intrusion has two potential fates: to crystallize, or quench to glass. Rapidly chilled sheet margins are typically glassy or microcrystalline, while interiors are coarser-grained. The actual textures result from a combination of thermal history and crystallization kinetics, which are related by various feedback mechanisms. The thermal history of cooling sheet intrusions is often approximated using the analytical solution for a semi-infinite half-space, which uses constant thermal properties such as heat capacity (CP), thermal diffusivity (D) and thermal conductivity (k = DρCP), where ρ is density. In reality, both CP and D are strongly T-dependent for glasses and crystals, and melts have higher CP and lower D than crystals or glasses. Another first-order feature ignored in the analytical solution is latent heat of crystallization (ΔHxt), which can be implemented numerically as extra heat capacity over the crystallization interval. For rhyolite melts, D is ~0.5 mm2s-1 and k is ~1.5 Wm-1K-1, which are similar to those of major crustal rock types and granitic protoliths at magmatic temperatures, suggesting that changes in thermal properties accompanying partial melting of the crust should be relatively minor. Numerical models of hot (~920°C liquidus for 0.5 wt.% H2O) shallow rhyolite intrusions indicate that the key difference in thermal history between bodies that quench to obsidian, and those that crystallize, results from the release of latent heat of crystallization, which enables bodies that crystallize to remain at high temperatures for much longer times. The time to solidification is similar in both cases, however, because solidification requires cooling through the glass transition (Tg ~620°C) in the first case, and cooling only to the solidus (~770°C) in the second. For basaltic melts, D is ~0.3 mm2s-1 and k is ~1.0 Wm-1K-1, compared to ~0.6 mm2s-1 and 2.5 Wm-1K-1 for crystalline basalt or peridotite at magmatic temperatures, suggesting that changes in thermal properties accompanying partial melting of the mantle or crystallization of basalt may be important. Numerical models of basaltic sheet intrusions indicate that they will almost always crystallize, even at sheet margins, because their emplacement temperature (~1220°C) is sufficiently high that the country rock adjacent to the sheet will be raised above the Tg of the melt (~650°C). The long period of time spent above Tg, combined with the rapid crystallization kinetics of basaltic melts, ensures that crystallization is near-complete, even if the crystal size is small, except where unusually rapid chilling occurs due to efficient convective or radiative losses (for example subaerial, subaqeous or subglacial lava flows).

A zero-liquid-discharge scheme for vanadium extraction process by electrodialysis-based technology.

PubMed

Wang, Meng; Xing, Hong-Bo; Jia, Yu-Xiang; Ren, Qing-Chun

2015-12-30

The sharp increase of demand for vanadium makes the treatment of the wastewater generated from its extraction process become an urgent problem. In this study, a hybrid process coupling the electrodialysis with the cooling crystallization is put forward for upgrading the conventional vanadium extraction process to zero discharge. Accordingly, the objective of this work lies in evaluating the feasibility of the proposed scheme on the basis of a systematic study on the influences of membrane types and operating parameters on the electrodialysis performance. The results indicate that the relative importance of osmosis and electro-osmosis to overall water transport is closely related to the applied current density. The increase in the applied current density and the decrease in the mole ratio of water and salt flux will contribute to the concentration degree. Moreover, it is worth noting that a relatively large concentration ratio can result in the remarkable decrease of current efficiency and increase of energy consumption. In general, the reclamation scheme can easily achieve the recovered water with relatively low salt content and the highly concentrated Na2SO4 solution (e.g., 300 g/L) for producing high-purity sodium sulphate crystals. Copyright © 2015. Published by Elsevier B.V.

NE-CAT Upgrade of the Bending Magnet Beamline 8BM at the ALS

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

Wang Jun; Ogata, Craig; Yang Xiaochun

2007-01-19

NE-CAT, North East Collaborative Access Team, bending magnet beamline (8BM) is a beamline for protein crystallography. Recently, the beamline has undergone upgrades of its x-ray optics, control system, and the addition of a robot automounter. The first crystal of the double crystal monochromator was replaced by a new design offered by Oxford Danfysik with a micro-finned, direct water-cooled crystal assembly that would provide better cooling and reduced thermal distortion, pressure induced bulge, and residual strain. Gear reduced motors were added to enhance the torque of the bender and obtain better control. For measuring displacement of the bender directly, two linearmore » variable differential transformers (LVDT) were installed to the second crystal assembly. Early optics characterization and analysis has been carried out. Besides the upgrade of the optical components, the Blu-Ice control system originally developed at SSRL has been implemented. The installation of an automated robotic sample mounting system, from the ALS, was carried out in collaboration with the engineering group at LBNL. Preliminary results are presented.« less

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

Vu-khanh, T.; Denault, J.

The effects of the conditions of the processing of PEEK/carbon prepregs and comingled fabric on the microstructure and mechanical characteristics of the resulting composites were investigated. Results showed that, in the comingled fabric system, the fiber/matrix adhesion depends on the molding temperature, the residence time at the melt temperature, and the cooling rate. Too high molding temperature resulted in degradation of the PEEK matrix, which affected the crystallization behavior of the composites, the fiber/matrix adhesion, and the matrix properties. This effect was most important in the case of comingled systems containing sized carbon fibers. 17 refs.

A complex magma mixing origin for rocks erupted in 1915, Lassen Peak, California

USGS Publications Warehouse

Clynne, M.A.

1999-01-01

The eruption of Lassen Peak in May 1915 produced four volcanic rock types within 3 days, and in the following order: (1) hybrid black dacite lava containing (2) undercooled andesitic inclusions, (3) compositionally banded pumice with dark andesite and light dacite bands, and (4) unbanded light dacite. All types represent stages of a complex mixing process between basaltic andesite and dacite that was interrupted by the eruption. They contain disequilibrium phenocryst assemblages characterized by the co-existence of magnesian olivine and quartz and by reacted and unreacted phenocrysts derived from the dacite. The petrography and crystal chemistry of the phenocrysts and the variation in rock compositions indicate that basaltic andesite intruded dacite magma and partially hybridized with it. Phenocrysts from the dacite magma were reacted. Cooling, cyrstallization, and vesiculation of the hybrid andesite magma converted it to a layer of mafic foam. The decreased density of the andesite magma destabilized and disrupted the foam. Blobs of foam rose into and were further cooled by the overlying dacite magma, forming the andesitic inclusions. Disaggregation of andesitic inclusions in the host dacite produced the black dacite and light dacite magmas. Formation of foam was a dynamic process. Removal of foam propagated the foam layer downward into the hybrid andesite magma. Eventually the thermal and compositional contrasts between the hybrid andesite and black dacite magmas were reduced. Then, they mixed directly, forming the dark andesite magma. About 40-50% andesitic inclusions were disaggregated into the host dacite to produce the hybrid black dacite. Thus, disaggregation of inclusions into small fragments and individual crystals can be an efficient magma-mixing process. Disaggregation of undercooled inclusions carrying reacted host-magma phenocrysts produces co-existing reacted and unreacted phenocrysts populations.

Efficiency and Accuracy in Thermal Simulation of Powder Bed Fusion of Bulk Metallic Glass

NASA Astrophysics Data System (ADS)

Lindwall, J.; Malmelöv, A.; Lundbäck, A.; Lindgren, L.-E.

2018-05-01

Additive manufacturing by powder bed fusion processes can be utilized to create bulk metallic glass as the process yields considerably high cooling rates. However, there is a risk that reheated material set in layers may become devitrified, i.e., crystallize. Therefore, it is advantageous to simulate the process to fully comprehend it and design it to avoid the aforementioned risk. However, a detailed simulation is computationally demanding. It is necessary to increase the computational speed while maintaining accuracy of the computed temperature field in critical regions. The current study evaluates a few approaches based on temporal reduction to achieve this. It is found that the evaluated approaches save a lot of time and accurately predict the temperature history.

Trondhjemitic melts produced by in-situ differentiation of a tholeiitic lava flow, Reykjanes Peninsula, Iceland.

NASA Astrophysics Data System (ADS)

Martin, E.; Sigmarsson, O.

2006-12-01

How the continental crust began to form early in Earth's history is unconstrained. However, it is reasonable to presume that higher heat flow in the past, resulted in more frequent interaction of mantle plumes and mid- oceanic ridges. If true, then Iceland could be a good analogue for processes occurring on Earth at its youth stage. This is supported by the relatively high abundance of silicic rocks in Iceland but their rarity on other oceanic hot spots. The origin of Icelandic silicic rocks has been a subject of a lively debate but has been shown to be principally formed by partial melting of hydrothermally altered basaltic crust. However, in rare cases, their origin by fractional crystallization from mantle derived basalts is suggested. Segregation veins in lava flows frequently contain interstitial glasses of silicic compositions. Moreover, they allow an exceptional overview of the fractional crystallization mechanism. These veins form by gas filter pressing during cooling and degassing of solidifying lava flows, after approximately 50% fractional crystallization of anhydrous minerals. Pairs of samples, host lava and associated segregation veins, from Reykjanes Peninsula (Iceland), Lanzarote (Canary Island) and Masaya's volcano (Nicaragua), allow the assessment of a near-complete fractional crystallization of olivine tholeiitic basalt at pressure close to one atmosphere. Interstitial glass patches in segregation veins represent the final product of this process (80 97 % of fractional crystallization). These ultimate liquids are of granitic composition in the case of Lanzarote and Masaya but overwhelmingly trondhjemitic at Reykjanes. It appears that the initial K2O/Na2O of the basaltic liquid controls the evolution path of the residual liquid composition produced at pressure close to 0.1 MPa (1 bar). Granitic liquids are generated from basalts of high initial K2O/Na2O whereas low initial K2O/Na2O leads to trondhjemitic compositions. The trondhjemitic composition of glass patches from the segregation vein at Reykjanes Peninsula differs from Icelandic silicic magmas but is close to those of the Archaean TTG (trondhjemite-tonalite-granodiorite) suite. Taken at face value, this may imply that fractional crystallisation of olivine tholeiites (low K2O/Na2O) could have played a significant role during the formation of the early continental crust. At higher pressure, where garnet is on liquidus, fractional crystallisation can generate the observed trace element patterns observed in TTG. The progressive cooling, crystallization and degassing of basaltic magma ocean, thought to have been prevailing during the Hadean, could have led to high degree of fractional crystallization producing significant volume of trondhjemitic melts that because of its buoyancy contributed to the formation of the earliest continental crust.

Quantification of the intrusion process at Kīlauea volcano, Hawai'i

NASA Astrophysics Data System (ADS)

Wright, Thomas L.; Marsh, Bruce

2016-12-01

The characteristic size of two types of intrusions identified beneath Kīlauea's East Rift zone are uniquely estimated by combining time constraints from fractional crystallization and the rates of magma solidification during cooling. Some intrusions were rapidly emplaced as dikes, but stalled before reaching the surface, and cooled and crystallized to feed later fractionated eruptions. More specifically, using the observed time interval between initial emplacement and eruption of fractionated lava, whose degree of fractionation is estimated from petrologic mixing calculations, the extent of solidification or cooling needed to produce this amount of fractionation can be directly inferred. And from the known erupted volumes the spatial extent or size of this fractionated volume can be analytically related to the full size of the source body itself. Two examples yield dike widths of 82 and 68 m. Other intrusions remain close to the east rift magma transport path and are observed to last for decades or longer as viable magma bodies that may participate in feeding later eruptions. The thickness of semi-permanent reservoirs near the East Rift Zone magma transport path can be estimated by assuming a resupply rate that is sufficiently frequent to restrict cooling to < 10 °C. It is inferred that both types of intrusions likely began as dike offshoots from the East Rift Zone magma transport path, but the frequently resupplied bodies may have later been converted to sills or laccoliths of heights estimated at 43-62 m. Our modeled intrusions contrast with models of rapidly emplaced thinner dikes feeding shallow intrusions, which are accompanied by intense rift earthquake swarms and are often associated with eruptions. These calculations show that long-term heating of the wallrock of the magma transport paths serves to slow conduit cooling, which may be partly responsible for sustaining long East Rift Zone eruptions. Adjacent to the vertical transport path beneath Kīlauea's summit, the combined effects of heating and ever-increasing magma supply rate may have forced a commensurate enlarging of the conduit, perhaps explaining the occurrence of a temporary burst of deep (5-15 km) long-period earthquake swarms between 1987 and 1992.

Auger electron spectroscopy analysis for growth interface of cubic boron nitride single crystals synthesized under high pressure and high temperature

NASA Astrophysics Data System (ADS)

Lv, Meizhe; Xu, Bin; Cai, Lichao; Guo, Xiaofei; Yuan, Xingdong

2018-05-01

After rapid cooling, cubic boron nitride (c-BN) single crystals synthesized under high pressure and high temperature (HPHT) are wrapped in the white film powders which are defined as growth interface. In order to make clear that the transition mechanism of c-BN single crystals, the variation of B and N atomic hybrid states in the growth interface is analyzed with the help of auger electron spectroscopy in the Li-based system. It is found that the sp2 fractions of B and N atoms decreases, and their sp3 fractions increases from the outer to the inner in the growth interface. In addition, Lithium nitride (Li3N) are not found in the growth interface by X-ray diffraction (XRD) experiment. It is suggested that lithium boron nitride (Li3BN2) is produced by the reaction of hexagonal boron nitride (h-BN) and Li3N at the first step, and then B and N atoms transform from sp2 into sp3 state with the catalysis of Li3BN2 in c-BN single crystals synthesis process.

Evaluation of a method for heat transfer measurements and thermal visualization using a composite of a heater element and liquid crystals. [thermal performance of turbine blade cooling configurations

NASA Technical Reports Server (NTRS)

Hippensteele, S. A.; Russell, L. M.; Stepka, F. S.

1981-01-01

Commercially available elements of a composite consisting of a plastic sheet coated with liquid crystal, another sheet with a thin layer of a conducting material (gold or carbon), and copper bus bar strips were evaluated and found to provide a simple, convenient, accurate, and low-cost measuring device for use in heat transfer research. The particular feature of the composite is its ability to obtain local heat transfer coefficients and isotherm patterns that provide visual evaluation of the thermal performances of turbine blade cooling configurations. Examples of the use of the composite are presented.

Multicomponent Diffusion in Experimentally Cooled Melt Inclusions

NASA Astrophysics Data System (ADS)

Saper, L.; Stolper, E.

2017-12-01

Glassy olivine-hosted melt inclusions are compositionally zoned, characterized by a boundary layer depleted in olivine-compatible components that extends into the melt inclusion from its wall. The boundary layer forms in response to crystallization of olivine and relaxes with time due to diffusive exchange with the interior of the inclusion. At magmatic temperatures, the time scale for homogenization of inclusions is minutes to hours. Preservation of compositional gradients in natural inclusions results from rapid cooling upon eruption. A model of MgO concentration profiles that couples crystal growth and diffusive relaxation of a boundary layer can be used to solve for eruptive cooling rates [1]. Controlled cooling-rate experiments were conducted to test the accuracy of the model. Mauna Loa olivine containing >80 µm melt inclusions were equilibrated at 1225°C in a 1-atm furnace for 24 hours, followed by linear cooling at rates of 102 - 105 °C/hr. High-resolution concentration profiles of 40 inclusions were obtained using an electron microprobe. The model of [1] fits the experimental data with low residuals and the best-fit cooling rates are within 30% of experimental values. The initial temperature of 1225 °C is underestimated by 65°C. The model was modified using (i) MELTS to calculate the interface melt composition as a function of temperature, and (ii) a concentration-dependent MgO diffusion coefficient using the functional form of [2]. With this calibration the best-fit starting temperatures are within 5°C of the experimental values and the best-fit cooling rates are within 20% of experimental rates. The evolution of the CaO profile during cooling is evidence for strong diffusive coupling between melt components. Because CaO is incompatible in olivine, CaO concentrations are expected to be elevated in the boundary layer adjacent to the growing olivine. Although this is observed at short time scales, as the profile evolves the CaO concentration near the crystal interface becomes increasingly depleted. The drawdown in CaO can be explained by non-ideal mixing that leads to increases in the CaO activity coefficient in the melt. A regular solution model [3] can be used to describe the evolution of the CaO profiles. [1]Newcombe et al (2014) CMP 168 [2] Zhang (2010) RevMineralGeochem 72 [3] Ghiorso & Sack (1995) CMP 119

Microphysical modeling of cirrus. 2: Sensitivity studies

NASA Technical Reports Server (NTRS)

Jensen, Eric J.; Toon, Owen B.; Westphal, Douglas L.; Kinne, Stefan; Heymsfield, Andrew J.

1994-01-01

The one-dimensional cirrus model described in part 1 of this issue has been used to study the sensitivity of simulated cirrus microphysical and radiative properties to poorly known model parameters, poorly understood physical processes, and environmental conditions. Model parameters and physical processes investigated include nucleation rate, mode of nucleation (e.g., homogeneous freezing of aerosols and liquid droplets or heterogeneous deposition), ice crystal shape, and coagulation. These studies suggest that the leading sources of uncertainty in the model are the phase change (liquid-solid) energy barrier and the ice-water surface energy which dominate the homogeneous freezing nucleation rate and the coagulation sticking efficiency at low temperatures which controls the production of large ice crystals (radii greater than 100 mcirons). Environmental conditions considered in sensitivity tests were CN size distribution, vertical wind speed, and cloud height. We found that (unlike stratus clouds) variations in the total number of condensation nuclei (NC) have little effect on cirrus microphysical and radiative properties, since nucleation occurs only on the largest CN at the tail of the size distribution. The total number of ice crystals which nucleate has little or no relationship to the number of CN present and depends primarily on the temperature and the cooling rate. Stronger updrafts (more rapid cooling) generate higher ice number densities, ice water content, cloud optical depth, and net radiative forcing. Increasing the height of the clouds in the model leads to an increase in ice number density, a decrease in effective radius, and a decrease in ice water content. The most prominent effect of increasing cloud height was a rapid increase in the net cloud radiative forcing which can be attributed to the change in cloud temperature as well as change in cloud ice size distributions. It has long been recognized that changes in cloud height or cloud area have the greatest potential for causing feedbacks on climate change. Our results suggest that variations in vertical velocity or cloud microphysical changes associatd with cloud height changes may also be important.

Adsorption of saturated fatty acid in urea complexation: Kinetics and equilibrium studies

NASA Astrophysics Data System (ADS)

Setyawardhani, Dwi Ardiana; Sulistyo, Hary; Sediawan, Wahyudi Budi; Fahrurrozi, Mohammad

2018-02-01

Urea complexation is fractionation process for concentrating poly-unsaturated fatty acids (PUFAs) from vegetable oil or animal fats. For process design and optimization in commercial industries, it is necessary to provide kinetics and equilibrium data. Urea inclusion compounds (UICs) as the product is a unique complex form which one molecule (guest) is enclosed within another molecule (host). In urea complexation, the guest-host bonding exists between saturated fatty acids (SFAs) and crystalline urea. This research studied the complexation is analogous to an adsorption process. The Batch adsorption process was developed to obtain the experimental data. The ethanolic urea solution was mixed with SFA in certain compositions and adsorption times. The mixture was heated until it formed homogenous and clear solution, then it cooled very slowly until the first numerous crystal appeared. Adsorption times for the kinetic data were determined since the crystal formed. The temperature was maintained constant at room temperature. Experimental sets of data were observed with adsorption kinetics and equilibrium models. High concentration of saturated fatty acid (SFA) was used to represent adsorption kinetics and equilibrium parameters. Kinetic data were examined with pseudo first-order, pseudo second-order and intra particle diffusion models. Linier, Freundlich and Langmuir isotherm were used to study the equilibrium model of this adsorption. The experimental data showed that SFA adsorption in urea crystal followed pseudo second-order model. The compatibility of the data with Langmuir isotherm showed that urea complexation was a monolayer adsorption.

Magma Chambers, Thermal Energy, and the Unsuccessful Search for a Magma Chamber Thermostat

NASA Astrophysics Data System (ADS)

Glazner, A. F.

2015-12-01

Although the traditional concept that plutons are the frozen corpses of huge, highly liquid magma chambers ("big red blobs") is losing favor, the related notion that magma bodies can spend long periods of time (~106years) in a mushy, highly crystalline state is widely accepted. However, analysis of the thermal balance of magmatic systems indicates that it is difficult to maintain a significant portion in a simmering, mushy state, whether or not the system is eutectic-like. Magma bodies cool primarily by loss of heat to the Earth's surface. The balance between cooling via energy loss to the surface and heating via magma accretion can be denoted as M = ρLa/q, where ρ is magma density, L is latent heat of crystallization, a is the vertical rate of magma accretion, and q is surface heat flux. If M>1, then magma accretion outpaces cooling and a magma chamber forms. For reasonable values of ρ, L, and q, the rate of accretion amust be > ~15 mm/yr to form a persistent volume above the solidus. This rate is extremely high, an order of magnitude faster than estimated pluton-filling rates, and would produce a body 10 km thick in 700 ka, an order of magnitude faster than geochronology indicates. Regardless of the rate of magma supply, the proportion of crystals in the system must vary dramatically with depth at any given time owing to transfer of heat. Mechanical stirring (e.g., by convection) could serve to homogenize crystal content in a magma body, but this is unachievable in crystal-rich, locked-up magma. Without convection the lower part of the magma body becomes much hotter than the top—a process familiar to anyone who has scorched a pot of oatmeal. Thermal models that succeed in producing persistent, large bodies of magma rely on scenarios that are unrealistic (e.g., omitting heat loss to the planet's surface), self-fulfilling prophecies (e.g., setting unnaturally high temperatures as fixed boundary conditions), or physically unreasonable (e.g., magma is intruded faster than geodetic and geophysical observations allow). Magma addition and conductive heat loss rates that are consistent with observation invariably lead to the conclusion that large, long-lived magma bodies, mushy or not, are thermally unsustainable.

COMSOL Multiphysics Model for HLW Canister Filling

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

Kesterson, M. R.

2016-04-11

The U.S. Department of Energy (DOE) is building a Tank Waste Treatment and Immobilization Plant (WTP) at the Hanford Site in Washington to remediate 55 million gallons of radioactive waste that is being temporarily stored in 177 underground tanks. Efforts are being made to increase the loading of Hanford tank wastes in glass while meeting melter lifetime expectancies and process, regulatory, and product quality requirements. Wastes containing high concentrations of Al 2O 3 and Na 2O can contribute to nepheline (generally NaAlSiO 4) crystallization, which can sharply reduce the chemical durability of high level waste (HLW) glass. Nepheline crystallization canmore » occur during slow cooling of the glass within the stainless steel canister. The purpose of this work was to develop a model that can be used to predict temperatures of the glass in a WTP HLW canister during filling and cooling. The intent of the model is to support scoping work in the laboratory. It is not intended to provide precise predictions of temperature profiles, but rather to provide a simplified representation of glass cooling profiles within a full scale, WTP HLW canister under various glass pouring rates. These data will be used to support laboratory studies for an improved understanding of the mechanisms of nepheline crystallization. The model was created using COMSOL Multiphysics, a commercially available software. The model results were compared to available experimental data, TRR-PLT-080, and were found to yield sufficient results for the scoping nature of the study. The simulated temperatures were within 60 ºC for the centerline, 0.0762m (3 inch) from centerline, and 0.2286m (9 inch) from centerline thermocouples once the thermocouples were covered with glass. The temperature difference between the experimental and simulated values reduced to 40 ºC, 4 hours after the thermocouple was covered, and down to 20 ºC, 6 hours after the thermocouple was covered. This level of precision is considered acceptable for the scoping nature of the model and the subsequent laboratory glass studies Using the model, two additional glass pouring cycles were conducted. Representative thermocouple data were plotted to show the variations between the two cycles. This provides preliminary data that will be used in laboratory experiments to determine the potential for controlling nepheline crystallization in glass by varying the glass pouring conditions.« less

A step towards long-wavelength protein crystallography: subjecting protein crystals to a vacuum

PubMed Central

Panjikar, Santosh; Thomsen, Lars; O’Donnell, Kane Michael; Riboldi-Tunnicliffe, Alan

2015-01-01

Using the UHV experimental endstation on the soft X-ray beamline at the Australian Synchrotron, lysozyme and proteinase K crystals have been exposed to a vacuum of 10−5 mbar, prior to flash-cooling in a bath of liquid nitrogen. Subsequent data collection on the MX2 beamline at the Australian Synchrotron demonstrated that, for lysozyme and proteinase K, it is possible to subject these mounted crystals to a vacuum pressure of 10−5 mbar without destroying the crystal lattice. Despite the lower data quality of the vacuum-pumped crystals compared with control crystals, it is demonstrated that the protein crystals can survive in a vacuum under suitable conditions. PMID:26089765

Cupric oxide inclusions in cuprous oxide crystals grown by the floating zone method

NASA Astrophysics Data System (ADS)

Frazer, Laszlo; Chang, Kelvin B.; Poeppelmeier, Kenneth R.; Ketterson, John B.

2015-06-01

Phase-pure cuprous oxide (Cu2O) crystals are difficult to grow since cupric oxide can form within the crystal as the crystal is cooled to ambient conditions. Vacancies are the solute which causes precipitation of macroscopic defects. Therefore, even when a mostly phase-pure single crystal is used as a feed rod, cupric oxide inclusions persist in the recrystallized solid. Control of the thermal profile during crystal growth, however, can improve phase-purity; a slow counter-rotation rate of the feed and seed rods results in fewer inclusions. Cupric oxide can be removed by annealing, which produces a factor of 540 ± 70 increase in phase-purity.

Cupric oxide inclusions in cuprous oxide crystals grown by the floating zone method

PubMed Central

Frazer, Laszlo; Chang, Kelvin B; Poeppelmeier, Kenneth R; Ketterson, John B

2015-01-01

Phase-pure cuprous oxide (Cu2O) crystals are difficult to grow since cupric oxide can form within the crystal as the crystal is cooled to ambient conditions. Vacancies are the solute which causes precipitation of macroscopic defects. Therefore, even when a mostly phase-pure single crystal is used as a feed rod, cupric oxide inclusions persist in the recrystallized solid. Control of the thermal profile during crystal growth, however, can improve phase-purity; a slow counter-rotation rate of the feed and seed rods results in fewer inclusions. Cupric oxide can be removed by annealing, which produces a factor of 540 ± 70 increase in phase-purity. PMID:27877798

Crystal nucleation in metallic alloys using x-ray radiography and machine learning

PubMed Central

Arteta, Carlos; Lempitsky, Victor

2018-01-01

The crystallization of solidifying Al-Cu alloys over a wide range of conditions was studied in situ by synchrotron x-ray radiography, and the data were analyzed using a computer vision algorithm trained using machine learning. The effect of cooling rate and solute concentration on nucleation undercooling, crystal formation rate, and crystal growth rate was measured automatically for thousands of separate crystals, which was impossible to achieve manually. Nucleation undercooling distributions confirmed the efficiency of extrinsic grain refiners and gave support to the widely assumed free growth model of heterogeneous nucleation. We show that crystallization occurred in temporal and spatial bursts associated with a solute-suppressed nucleation zone. PMID:29662954

High-Throughput Non-Contact Vitrification of Cell-Laden Droplets Based on Cell Printing

NASA Astrophysics Data System (ADS)

Shi, Meng; Ling, Kai; Yong, Kar Wey; Li, Yuhui; Feng, Shangsheng; Zhang, Xiaohui; Pingguan-Murphy, Belinda; Lu, Tian Jian; Xu, Feng

2015-12-01

Cryopreservation is the most promising way for long-term storage of biological samples e.g., single cells and cellular structures. Among various cryopreservation methods, vitrification is advantageous by employing high cooling rate to avoid the formation of harmful ice crystals in cells. Most existing vitrification methods adopt direct contact of cells with liquid nitrogen to obtain high cooling rates, which however causes the potential contamination and difficult cell collection. To address these limitations, we developed a non-contact vitrification device based on an ultra-thin freezing film to achieve high cooling/warming rate and avoid direct contact between cells and liquid nitrogen. A high-throughput cell printer was employed to rapidly generate uniform cell-laden microdroplets into the device, where the microdroplets were hung on one side of the film and then vitrified by pouring the liquid nitrogen onto the other side via boiling heat transfer. Through theoretical and experimental studies on vitrification processes, we demonstrated that our device offers a high cooling/warming rate for vitrification of the NIH 3T3 cells and human adipose-derived stem cells (hASCs) with maintained cell viability and differentiation potential. This non-contact vitrification device provides a novel and effective way to cryopreserve cells at high throughput and avoid the contamination and collection problems.

High-Throughput Non-Contact Vitrification of Cell-Laden Droplets Based on Cell Printing

PubMed Central

Shi, Meng; Ling, Kai; Yong, Kar Wey; Li, Yuhui; Feng, Shangsheng; Zhang, Xiaohui; Pingguan-Murphy, Belinda; Lu, Tian Jian; Xu, Feng

2015-01-01

Cryopreservation is the most promising way for long-term storage of biological samples e.g., single cells and cellular structures. Among various cryopreservation methods, vitrification is advantageous by employing high cooling rate to avoid the formation of harmful ice crystals in cells. Most existing vitrification methods adopt direct contact of cells with liquid nitrogen to obtain high cooling rates, which however causes the potential contamination and difficult cell collection. To address these limitations, we developed a non-contact vitrification device based on an ultra-thin freezing film to achieve high cooling/warming rate and avoid direct contact between cells and liquid nitrogen. A high-throughput cell printer was employed to rapidly generate uniform cell-laden microdroplets into the device, where the microdroplets were hung on one side of the film and then vitrified by pouring the liquid nitrogen onto the other side via boiling heat transfer. Through theoretical and experimental studies on vitrification processes, we demonstrated that our device offers a high cooling/warming rate for vitrification of the NIH 3T3 cells and human adipose-derived stem cells (hASCs) with maintained cell viability and differentiation potential. This non-contact vitrification device provides a novel and effective way to cryopreserve cells at high throughput and avoid the contamination and collection problems. PMID:26655688

Study of the growth and pyroelectric properties of TGS crystals doped with aniline-family dipolar molecules

NASA Astrophysics Data System (ADS)

Zhang, Kecong; Song, Jiancheng; Wang, Min; Fang, Changshui; Lu, Mengkai

1987-04-01

TGS crystals doped with aniline-family dipolar molecules (aniline, 2-aminobenzoic acid, 3-aminobenzoic acid, 3-aminobenzene-sulphonic acid, 4-aminobenzenesulphonic acid and 4-nitroraniline) have been grown by the slow-cooling solution method. The influence of these dopants on the growth habits, crystal morphology pyroelectric properties, and structure parameters of TGS crystals has been systematically investigated. The effects of the domain structure of the seed crystal on the pyroelectric properties of the doped crystals have been studied. It is found that the spontaneous polarization (P), pyroelectric coefficient (lambda), and internal bias field of the doped crystals are slightly higher than those of the pure TGS, and the larger the dipole moment of the dopant molecule, the higher the P and lambda of the doped TGS crystal.

Is EG 50 a White or Strange Dwarf?

NASA Astrophysics Data System (ADS)

Hajyan, G. S.; Vartanyan, Yu. L.

2017-12-01

The time dependences of the luminosity of a white dwarf and four strange dwarfs with masses of 0.5 M (the mass of the white dwarf EG 50 with a surface temperature of 2.1·104 K) are determined taking neutrino energy losses into account. It was assumed that these configurations radiate only at the expense of thermal energy reserves. It is shown that the sources of thermal energy owing to nonequilibrium b-processes and the phenomenon of crystallization of electron-nuclear matter are insignificant in determining the cooling time of white and strange dwarfs with masses of 0.5 M⨀. It is shown that in this approximation the time dependences of the luminosity of white and strange dwarfs with masses of 0.5 M⨀ differ significantly only for surface temperatures TR≥7·104 K, so it is impossible to determine whether EG 50 is a white or strange dwarf based on the cooling time.

Thermal stability of Pt nanoclusters interacting to carbon sublattice

NASA Astrophysics Data System (ADS)

Baidyshev, V. S.; Gafner, Yu. Ya.; Gafner, S. L.; Redel, L. V.

2017-12-01

The catalytic activity of Pt clusters is dependent not only on the nanoparticle size and its composition, but also on its internal structure. To determine the real structure of the nanoparticles used in catalysis, the boundaries of the thermal structure stability of Pt clusters to 8.0 nm in diameter interacting with carbon substrates of two types: a fixed α-graphite plane and a mobile substrate with the diamond structure. The effect of a substrate on the processes melting of Pt nanoclusters is estimated. The role of the cooling rate in the formation of the internal structure of Pt clusters during crystallization is studied. The regularities obtained in the case of "free" Pt clusters and Pt clusters on a substrate are compared. It is concluded that platinum nanoparticles with diameter D ≤ 4.0 nm disposed on a carbon substrate conserve the initial fcc structure during cooling.