ECL gate array with integrated PLL-based clock recovery and synthesis for high-speed data and telecom applications

NASA Astrophysics Data System (ADS)

Rosky, David S.; Coy, Bruce H.; Friedmann, Marc D.

1992-03-01

A 2500 gate mixed signal gate array has been developed that integrates custom PLL-based clock recovery and clock synthesis functions with 2500 gates of configurable logic cells to provide a single chip solution for 200 - 1244 MHz fiber based digital interface applications. By customizing the digital logic cells, any of the popular telecom and datacom standards may be implemented.

Nucleation of metastable aragonite CaCO3 in seawater.

PubMed

Sun, Wenhao; Jayaraman, Saivenkataraman; Chen, Wei; Persson, Kristin A; Ceder, Gerbrand

2015-03-17

Predicting the conditions in which a compound adopts a metastable structure when it crystallizes out of solution is an unsolved and fundamental problem in materials synthesis, and one which, if understood and harnessed, could enable the rational design of synthesis pathways toward or away from metastable structures. Crystallization of metastable phases is particularly accessible via low-temperature solution-based routes, such as chimie douce and hydrothermal synthesis, but although the chemistry of the solution plays a crucial role in governing which polymorph forms, how it does so is poorly understood. Here, we demonstrate an ab initio technique to quantify thermodynamic parameters of surfaces and bulks in equilibrium with an aqueous environment, enabling the calculation of nucleation barriers of competing polymorphs as a function of solution chemistry, thereby predicting the solution conditions governing polymorph selection. We apply this approach to resolve the long-standing "calcite-aragonite problem"--the observation that calcium carbonate precipitates as the metastable aragonite polymorph in marine environments, rather than the stable phase calcite--which is of tremendous relevance to biomineralization, carbon sequestration, paleogeochemistry, and the vulnerability of marine life to ocean acidification. We identify a direct relationship between the calcite surface energy and solution Mg:Ca [corrected] ion concentrations, showing that the calcite nucleation barrier surpasses that of metastable aragonite in solutions with Mg:Ca ratios consistent with modern seawater, allowing aragonite to dominate the kinetics of nucleation. Our ability to quantify how solution parameters distinguish between polymorphs marks an important step toward the ab initio prediction of materials synthesis pathways in solution.

Nucleation of metastable aragonite CaCO 3 in seawater

DOE PAGES

Sun, Wenhao; Jayaraman, Saivenkataraman; Chen, Wei; ...

2015-03-04

Predicting the conditions in which a compound adopts a metastable structure when it crystallizes out of solution is an unsolved and fundamental problem in materials synthesis, and one which, if understood and harnessed, could enable the rational design of synthesis pathways toward or away from metastable structures. Crystallization of metastable phases is particularly accessible via low-temperature solution-based routes, such as chimie douce and hydrothermal synthesis, but although the chemistry of the solution plays a crucial role in governing which polymorph forms, how it does so is poorly understood. Here, we demonstrate an ab initio technique to quantify thermodynamic parameters ofmore » surfaces and bulks in equilibrium with an aqueous environment, enabling the calculation of nucleation barriers of competing polymorphs as a function of solution chemistry, thereby predicting the solution conditions governing polymorph selection. We apply this approach to resolve the long-standing “calcite–aragonite problem”––the observation that calcium carbonate precipitates as the metastable aragonite polymorph in marine environments, rather than the stable phase calcite––which is of tremendous relevance to biomineralization, carbon sequestration, paleogeochemistry, and the vulnerability of marine life to ocean acidification. We identify a direct relationship between the calcite surface energy and solution Mg–Ca ion concentrations, showing that the calcite nucleation barrier surpasses that of metastable aragonite in solutions with Mg:Ca ratios consistent with modern seawater, allowing aragonite to dominate the kinetics of nucleation. The ability to quantify how solution parameters distinguish between polymorphs marks an important step toward the ab initio prediction of materials synthesis pathways in solution.« less

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

Sun, Wenhao; Jayaraman, Saivenkataraman; Chen, Wei

Predicting the conditions in which a compound adopts a metastable structure when it crystallizes out of solution is an unsolved and fundamental problem in materials synthesis, and one which, if understood and harnessed, could enable the rational design of synthesis pathways toward or away from metastable structures. Crystallization of metastable phases is particularly accessible via low-temperature solution-based routes, such as chimie douce and hydrothermal synthesis, but although the chemistry of the solution plays a crucial role in governing which polymorph forms, how it does so is poorly understood. Here, we demonstrate an ab initio technique to quantify thermodynamic parameters ofmore » surfaces and bulks in equilibrium with an aqueous environment, enabling the calculation of nucleation barriers of competing polymorphs as a function of solution chemistry, thereby predicting the solution conditions governing polymorph selection. We apply this approach to resolve the long-standing “calcite–aragonite problem”––the observation that calcium carbonate precipitates as the metastable aragonite polymorph in marine environments, rather than the stable phase calcite––which is of tremendous relevance to biomineralization, carbon sequestration, paleogeochemistry, and the vulnerability of marine life to ocean acidification. We identify a direct relationship between the calcite surface energy and solution Mg–Ca ion concentrations, showing that the calcite nucleation barrier surpasses that of metastable aragonite in solutions with Mg:Ca ratios consistent with modern seawater, allowing aragonite to dominate the kinetics of nucleation. The ability to quantify how solution parameters distinguish between polymorphs marks an important step toward the ab initio prediction of materials synthesis pathways in solution.« less

Total synthesis of TMG-chitotriomycin based on an automated electrochemical assembly of a disaccharide building block.

PubMed

Isoda, Yuta; Sasaki, Norihiko; Kitamura, Kei; Takahashi, Shuji; Manmode, Sujit; Takeda-Okuda, Naoko; Tamura, Jun-Ichi; Nokami, Toshiki; Itoh, Toshiyuki

2017-01-01

The total synthesis of TMG-chitotriomycin using an automated electrochemical synthesizer for the assembly of carbohydrate building blocks is demonstrated. We have successfully prepared a precursor of TMG-chitotriomycin, which is a structurally-pure tetrasaccharide with typical protecting groups, through the methodology of automated electrochemical solution-phase synthesis developed by us. The synthesis of structurally well-defined TMG-chitotriomycin has been accomplished in 10-steps from a disaccharide building block.

Total synthesis of TMG-chitotriomycin based on an automated electrochemical assembly of a disaccharide building block

PubMed Central

Isoda, Yuta; Sasaki, Norihiko; Kitamura, Kei; Takahashi, Shuji; Manmode, Sujit; Takeda-Okuda, Naoko; Tamura, Jun-ichi

2017-01-01

The total synthesis of TMG-chitotriomycin using an automated electrochemical synthesizer for the assembly of carbohydrate building blocks is demonstrated. We have successfully prepared a precursor of TMG-chitotriomycin, which is a structurally-pure tetrasaccharide with typical protecting groups, through the methodology of automated electrochemical solution-phase synthesis developed by us. The synthesis of structurally well-defined TMG-chitotriomycin has been accomplished in 10-steps from a disaccharide building block. PMID:28684973

n-Type Conductivity of Cu2O Thin Film Prepared in Basic Aqueous Solution Under Hydrothermal Conditions

NASA Astrophysics Data System (ADS)

Ursu, Daniel; Miclau, Nicolae; Miclau, Marinela

2018-03-01

We report for the first time in situ hydrothermal synthesis of n-type Cu2O thin film using strong alkaline solution. The use of copper foil as substrate and precursor material, low synthesis temperature and short reaction time represent the arguments of a new, simple, inexpensive and high field synthesis method for the preparation of n-type Cu2O thin film. The donor concentration of n-type Cu2O thin film obtained at 2 h of reaction time has increased two orders of magnitude than previous reported values. We have demonstrated n-type conduction in Cu2O thin film prepared in strong alkaline solution, in the contradiction with the previous works. Based on experimental results, the synthesis mechanism and the origin of n-type photo-responsive behavior of Cu2O thin film were discussed. We have proposed that the unexpected n-type character could be explained by H doping of Cu2O thin film in during of the hydrothermal synthesis that caused the p-to-n conductivity-type conversion. Also, this work raises new questions about the origin of n-type conduction in Cu2O thin film, the influence of the synthesis method on the nature of the intrinsic defects and the electrical conduction behavior.

Time- and energy-efficient solution combustion synthesis of binary metal tungstate nanoparticles with enhanced photocatalytic activity.

PubMed

Thomas, Abegayl; Janáky, Csaba; Samu, Gergely F; Huda, Muhammad N; Sarker, Pranab; Liu, J Ping; van Nguyen, Vuong; Wang, Evelyn H; Schug, Kevin A; Rajeshwar, Krishnan

2015-05-22

In the search for stable and efficient photocatalysts beyond TiO2 , the tungsten-based oxide semiconductors silver tungstate (Ag2 WO4 ), copper tungstate (CuWO4 ), and zinc tungstate (ZnWO4 ) were prepared using solution combustion synthesis (SCS). The tungsten precursor's influence on the product was of particular relevance to this study, and the most significant effects are highlighted. Each sample's photocatalytic activity towards methyl orange degradation was studied and benchmarked against their respective commercial oxide sample obtained by solid-state ceramic synthesis. Based on the results herein, we conclude that SCS is a time- and energy-efficient method to synthesize crystalline binary tungstate nanomaterials even without additional excessive heat treatment. As many of these photocatalysts possess excellent photocatalytic activity, the discussed synthetic strategy may open sustainable materials chemistry avenues to solar energy conversion and environmental remediation. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Implementation of the block-Krylov boundary flexibility method of component synthesis

NASA Technical Reports Server (NTRS)

Carney, Kelly S.; Abdallah, Ayman A.; Hucklebridge, Arthur A.

1993-01-01

A method of dynamic substructuring is presented which utilizes a set of static Ritz vectors as a replacement for normal eigenvectors in component mode synthesis. This set of Ritz vectors is generated in a recurrence relationship, which has the form of a block-Krylov subspace. The initial seed to the recurrence algorithm is based on the boundary flexibility vectors of the component. This algorithm is not load-dependent, is applicable to both fixed and free-interface boundary components, and results in a general component model appropriate for any type of dynamic analysis. This methodology was implemented in the MSC/NASTRAN normal modes solution sequence using DMAP. The accuracy is found to be comparable to that of component synthesis based upon normal modes. The block-Krylov recurrence algorithm is a series of static solutions and so requires significantly less computation than solving the normal eigenspace problem.

Control of crystallite and particle size in the synthesis of layered double hydroxides: Macromolecular insights and a complementary modeling tool.

PubMed

Galvão, Tiago L P; Neves, Cristina S; Caetano, Ana P F; Maia, Frederico; Mata, Diogo; Malheiro, Eliana; Ferreira, Maria J; Bastos, Alexandre C; Salak, Andrei N; Gomes, José R B; Tedim, João; Ferreira, Mário G S

2016-04-15

Zinc-aluminum layered double hydroxides with nitrate intercalated (Zn(n)Al-NO3, n=Zn/Al) is an intermediate material for the intercalation of different functional molecules used in a wide range of industrial applications. The synthesis of Zn(2)Al-NO3 was investigated considering the time and temperature of hydrothermal treatment. By examining the crystallite size in two different directions, hydrodynamic particle size, morphology, crystal structure and chemical species in solution, it was possible to understand the crystallization and dissolution processes involved in the mechanisms of crystallite and particle growth. In addition, hydrogeochemical modeling rendered insights on the speciation of different metal cations in solution. Therefore, this tool can be a promising solution to model and optimize the synthesis of layered double hydroxide-based materials for industrial applications. Copyright © 2016 Elsevier Inc. All rights reserved.

Solution phase synthesis of aluminum-doped silicon nanoparticles via room-temperature, solvent based chemical reduction of silicon tetrachloride

NASA Astrophysics Data System (ADS)

Mowbray, Andrew James

We present a method of wet chemical synthesis of aluminum-doped silicon nanoparticles (Al-doped Si NPs), encompassing the solution-phase co-reduction of silicon tetrachloride (SiCl4) and aluminum chloride (AlCl 3) by sodium naphthalide (Na[NAP]) in 1,2-dimethoxyethane (DME). The development of this method was inspired by the work of Baldwin et al. at the University of California, Davis, and was adapted for our research through some noteworthy procedural modifications. Centrifugation and solvent-based extraction techniques were used throughout various stages of the synthesis procedure to achieve efficient and well-controlled separation of the Si NP product from the reaction media. In addition, the development of a non-aqueous, formamide-based wash solution facilitated simultaneous removal of the NaCl byproduct and Si NP surface passivation via attachment of 1-octanol to the particle surface. As synthesized, the Si NPs were typically 3-15 nm in diameter, and were mainly amorphous, as opposed to crystalline, as concluded from SAED and XRD diffraction pattern analysis. Aluminum doping at various concentrations was accomplished via the inclusion of aluminum chloride (AlCl3); which was in small quantities dissolved into the synthesis solution to be reduced alongside the SiCl4 precursor. The introduction of Al into the chemically-reduced Si NP precipitate was not found to adversely affect the formation of the Si NPs, but was found to influence aspects such as particle stability and dispersibility throughout various stages of the procedure. Analytical techniques including transmission electron microscopy (TEM), FTIR spectroscopy, and ICP-optical emission spectroscopy were used to comprehensively characterize the product NPs. These methods confirm both the presence of Al and surface-bound 1-octanol in the newly formed Si NPs.

Synthesis and Evaluation of Cyclodextrin-based Polymers for Patulin Extraction from Aqueous Solutions

USDA-ARS?s Scientific Manuscript database

Patulin is a mycotoxin produced by fungi that contaminate fruits, juices, and other agricultural commodities. Sorption properties of polyurethane-beta-cyclodextrin polymers were evaluated for the ability to remove patulin from solutions, including apple juice. Freundlich isotherm analysis determin...

Nanofiber based triple layer hydro-philic/-phobic membrane - a solution for pore wetting in membrane distillation

PubMed Central

Prince, J. A.; Rana, D.; Matsuura, T.; Ayyanar, N.; Shanmugasundaram, T. S.; Singh, G.

2014-01-01

The innovative design and synthesis of nanofiber based hydro-philic/phobic membranes with a thin hydro-phobic nanofiber layer on the top and a thin hydrophilic nanofiber layer on the bottom of the conventional casted micro-porous layer which opens up a solution for membrane pore wetting and improves the pure water flux in membrane distillation. PMID:25377488

Remarkable lowering in the synthesis temperature of LiMn2O4via citrate solution-gel synthesis facilitated by ethanol.

PubMed

Maino, G; Carleer, R; Marchal, W; Bonneux, G; Hardy, A; Van Bael, M K

2017-11-07

LiMn 2 O 4 (LMO) is interesting from the viewpoint of its energy storage applications as it is a cathode in lithium ion batteries (LIB), which contains no rare, toxic or expansive elements, while it provides a high theoretical capacity (148 mA h g -1 ) at a reasonable voltage (4 V region) and a higher thermal stability compared to cobalt based cathodes and has a good rechargeability and cycling stability due to its spinel structure. Low temperature synthesis routes for cathode materials are currently gaining attention, in order to decrease the ecological footprint of the final LIB. Here, the crystallization temperature of LMO by a citrate based solution-gel synthesis was significantly lowered, to as low as 250 °C by the addition of ethanol to the precursor. The role of ethanol in this synthesis process was explored. It was found to lead to a considerable increase in the oxidation rate of the redox couple Mn 2+ /Mn 3+ , a lowering of the precursor decomposition temperature by 200 °C, besides a drastic decrease in the crystallization temperature (reaching 250 °C). Moreover, the main cause was identified to be an esterification reaction of ethanol with the carboxylic acid in the precursor complexes, taking place before the oxide formation. The insights obtained strengthen the knowledge regarding citrato-Mn 2+ /Mn 3+ complexes present in aqueous solution-gel synthesis routes and are relevant for the preparation of various manganese containing oxides. Moreover, the precursor developed opens up a new possibility for the low temperature synthesis of LMO powders and thin films for application in LIB. In the case of thin film batteries, the low temperature processing provides compatibility with other materials in the thin film battery stack, avoiding undesired oxidations or interfacial reactions.

Self-Supporting, Hydrophobic, Ionic Liquid-Based Reference Electrodes Prepared by Polymerization-Induced Microphase Separation.

PubMed

Chopade, Sujay A; Anderson, Evan L; Schmidt, Peter W; Lodge, Timothy P; Hillmyer, Marc A; Bühlmann, Philippe

2017-10-27

Interfaces of ionic liquids and aqueous solutions exhibit stable electrical potentials over a wide range of aqueous electrolyte concentrations. This makes ionic liquids suitable as bridge materials that separate in electroanalytical measurements the reference electrode from samples with low and/or unknown ionic strengths. However, methods for the preparation of ionic liquid-based reference electrodes have not been explored widely. We have designed a convenient and reliable synthesis of ionic liquid-based reference electrodes by polymerization-induced microphase separation. This technique allows for a facile, single-pot synthesis of ready-to-use reference electrodes that incorporate ion conducting nanochannels filled with either 1-octyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide or 1-dodecyl-3-methylimidazolium bis(trifluoromethyl sulfonyl)imide as ionic liquid, supported by a mechanically robust cross-linked polystyrene phase. This synthesis procedure allows for the straightforward design of various reference electrode geometries. These reference electrodes exhibit a low resistance as well as good reference potential stability and reproducibility when immersed into aqueous solutions varying from deionized, purified water to 100 mM KCl, while requiring no correction for liquid junction potentials.

Interactive program for analysis and design problems in advanced composites technology

NASA Technical Reports Server (NTRS)

Cruse, T. A.; Swedlow, J. L.

1971-01-01

During the past year an experimental program in the fracture of advanced fiber composites has been completed. The experimental program has given direction to additional experimental and theoretical work. A synthesis program for designing low weight multifastener joints in composites is proposed, based on extensive analytical background. A number of failed joints have been thoroughly analyzed to evaluate the failure hypothesis used in the synthesis procedure. Finally, a new solution is reported for isotropic and anisotropic laminates using the boundary-integral method. The solution method offers significant savings of computer core and time for important problems.

Solution-Based Synthesis of Crystalline Silicon from Liquid Silane through Laser and Chemical Annealing

DOE PAGES

Iyer, Ganjigunte R. S.; Hobbie, Erik K.; Guruvenket, Srinivasan; ...

2012-05-23

We report a solution process for the synthesis of crystalline silicon from the liquid silane precursor cyclohexasilane (Si 6H 12). Polysilane films were crystallized through thermal and laser annealing, with plasma hydrogenation at atmospheric pressure generating further structural changes in the films. The evolution from amorphous to microcrystalline is characterized using scanning electron microscopy (SEM), atomic force microscopy (AFM), Raman spectroscopy and impedance spectroscopy. A four-decade enhancement in the electrical conductivity is attributed to a disorder-order transition in a bonded Si network. Lastly, our results demonstrate a potentially attractive approach that employs a solution process coupled with ambient post-processing tomore » produce crystalline silicon thin films.« less

Atomistic Insights Into the Oriented Attachment of Tunnel-Based Oxide Nanostructures

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

Yuan, Yifei; Wood, Stephen M; He, Kun

Controlled synthesis of nanomaterials is one of the grand challenges facing materials scientists. In particular, how tunnel-based nanomaterials aggregate during synthesis while maintaining their well-aligned tunneled structure is not fully understood. Here, we describe the atomistic mechanism of oriented attachment (OA) during solution synthesis of tunneled α-MnO2 nanowires based on a combination of in situ liquid cell transmission electron microscopy (TEM), aberration-corrected scanning TEM with subangstrom spatial resolution, and first-principles calculations. It is found that primary tunnels (1 × 1 and 2 × 2) attach along their common {110} lateral surfaces to form interfaces corresponding to 2 × 3 tunnelsmore » that facilitate their short-range ordering. The OA growth of α-MnO2 nanowires is driven by the stability gained from elimination of {110} surfaces and saturation of Mn atoms at {110}-edges. During this process, extra [MnOx] radicals in solution link the two adjacent {110} surfaces and bond with the unsaturated Mn atoms from both surface edges to produce stable nanowire interfaces. Our results provide insights into the controlled synthesis and design of nanomaterials in which tunneled structures can be tailored for use in catalysis, ion exchange, and energy storage applications.« less

Eco-friendly synthesis of metal dichalcogenides nanosheets and their environmental remediation potential driven by visible light

PubMed Central

Mishra, Ashish Kumar; Lakshmi, K. V.; Huang, Liping

2015-01-01

Exfoliated transition metal dichalcogenides (TMDs) such as WS2 and MoS2 have shown exciting potential for energy storage, catalysis and optoelectronics. So far, solution based methods for scalable production of few-layer TMDs usually involve the use of organic solvents or dangerous chemicals. Here, we report an eco-friendly method for facile synthesis of few-layer WS2 and MoS2 nanosheets using dilute aqueous solution of household detergent. Short time sonication of varying amount of bulk samples in soapy water was used to scale up the production of nanosheets. Thermal stability, optical absorption and Raman spectra of as-synthesized WS2 and MoS2 nanosheets are in close agreement with those from other synthesis techniques. Efficient photocatalytic activity of TMDs nanosheets was demonstrated by decomposing Brilliant Green dye in aqueous solution under visible light irradiation. Our study shows the great potential of TMDs nanosheets for environmental remediation by degrading toxic industrial chemicals in wastewater using sunlight. PMID:26503125

Eco-friendly synthesis of metal dichalcogenides nanosheets and their environmental remediation potential driven by visible light

NASA Astrophysics Data System (ADS)

Mishra, Ashish Kumar; Lakshmi, K. V.; Huang, Liping

2015-10-01

Exfoliated transition metal dichalcogenides (TMDs) such as WS2 and MoS2 have shown exciting potential for energy storage, catalysis and optoelectronics. So far, solution based methods for scalable production of few-layer TMDs usually involve the use of organic solvents or dangerous chemicals. Here, we report an eco-friendly method for facile synthesis of few-layer WS2 and MoS2 nanosheets using dilute aqueous solution of household detergent. Short time sonication of varying amount of bulk samples in soapy water was used to scale up the production of nanosheets. Thermal stability, optical absorption and Raman spectra of as-synthesized WS2 and MoS2 nanosheets are in close agreement with those from other synthesis techniques. Efficient photocatalytic activity of TMDs nanosheets was demonstrated by decomposing Brilliant Green dye in aqueous solution under visible light irradiation. Our study shows the great potential of TMDs nanosheets for environmental remediation by degrading toxic industrial chemicals in wastewater using sunlight.

An improved synthesis of haloaceteamidine-based inactivators of protein arginine deiminase 4 (PAD4).

PubMed

Causey, Corey P; Thompson, Paul R

2008-07-07

Protein arginine deiminase 4 (PAD4) is an enzyme that hydrolyzes peptidyl arginine residues to form citrulline and ammonia. This enzyme has been implicated in several disease states, e.g. rheumatoid arthritis, and therefore represents a unique target for the development of a novel therapeutic. A solution-phase synthesis of Cl-amidine, the most potent PAD4 inactivator described to date, has been developed. This synthesis proceeds in 80% yield over 4 steps at a significantly (12-fold) lower cost.

Automated electrochemical assembly of the protected potential TMG-chitotriomycin precursor based on rational optimization of the carbohydrate building block.

PubMed

Nokami, Toshiki; Isoda, Yuta; Sasaki, Norihiko; Takaiso, Aki; Hayase, Shuichi; Itoh, Toshiyuki; Hayashi, Ryutaro; Shimizu, Akihiro; Yoshida, Jun-ichi

2015-03-20

The anomeric arylthio group and the hydroxyl-protecting groups of thioglycosides were optimized to construct carbohydrate building blocks for automated electrochemical solution-phase synthesis of oligoglucosamines having 1,4-β-glycosidic linkages. The optimization study included density functional theory calculations, measurements of the oxidation potentials, and the trial synthesis of the chitotriose trisaccharide. The automated synthesis of the protected potential N,N,N-trimethyl-d-glucosaminylchitotriomycin precursor was accomplished by using the optimized building block.

The prebiotic synthesis of oligonucleotides

NASA Technical Reports Server (NTRS)

Oro, J.; Stephen-Sherwood, E.

1974-01-01

This paper is primarily a review of recent developments in the abiotic synthesis of nucleotides, short chain oligonucleotides, and their mode of replication in solution. It also presents preliminary results from this laboratory on the prebiotic synthesis of thymidine oligodeoxynucleotides. A discussion, based on the physicochemical properties of RNA and DNA oligomers, relevant to the molecular evolution of these compounds leads to the tentative hypothesis that oligodeoxyribonucleotides of about 12 units may have been of sufficient length to initiate a self replicating coding system. Two models are suggested to account for the synthesis of high molecular weight oligomers using short chain templates and primers.

New Mexico's Academic Achievement Gaps: A Synthesis of Status, Causes, and Solutions. A White Paper

ERIC Educational Resources Information Center

Martinez, Joseph P.

2017-01-01

The Center for Positive Practices (CPP) conducted an analysis and synthesis of K-12 educational achievement gaps in New Mexico. The white paper was requested by the New Mexico based Coalition for the Majority, which includes various institutions, organizations and individuals supporting the New Mexico English Learner Teacher Preparation Act. The…

Multiscale Model for the Templated Synthesis of Mesoporous Silica: The Essential Role of Silica Oligomers

DOE PAGES

Perez-Sanchez, German; Chien, Szu -Chia; Gomes, Jose R. B.; ...

2016-04-04

A detailed theoretical understanding of the synthesis mechanism of periodic mesoporous silica has not yet been achieved. We present results of a multiscale simulation strategy that, for the first time, describes the molecular-level processes behind the formation of silica/surfactant mesophases in the synthesis of templated MCM-41 materials. The parameters of a new coarse-grained explicit-solvent model for the synthesis solution are calibrated with reference to a detailed atomistic model, which itself is based on quantum mechanical calculations. This approach allows us to reach the necessary time and length scales to explicitly simulate the spontaneous formation of mesophase structures while maintaining amore » level of realism that allows for direct comparison with experimental systems. Our model shows that silica oligomers are a necessary component in the formation of hexagonal liquid crystals from low-concentration surfactant solutions. Because they are multiply charged, silica oligomers are able to bridge adjacent micelles, thus allowing them to overcome their mutual repulsion and form aggregates. This leads the system to phase separate into a dilute solution and a silica/surfactant-rich mesophase, which leads to MCM-41 formation. Before extensive silica condensation takes place, the mesophase structure can be controlled by manipulation of the synthesis conditions. Our modeling results are in close agreement with experimental observations and strongly support a cooperative mechanism for synthesis of this class of materials. Furthermore, this work paves the way for tailored design of nanoporous materials using computational models.« less

Evidence-based surgery: barriers, solutions, and the role of evidence synthesis.

PubMed

Garas, George; Ibrahim, Amel; Ashrafian, Hutan; Ahmed, Kamran; Patel, Vanash; Okabayashi, Koji; Skapinakis, Petros; Darzi, Ara; Athanasiou, Thanos

2012-08-01

Surgery is a rapidly evolving field, making the rigorous testing of emerging innovations vital. However, most surgical research fails to employ randomized controlled trials (RCTs) and has particularly been based on low-quality study designs. Subsequently, the analysis of data through meta-analysis and evidence synthesis is particularly difficult. Through a systematic review of the literature, this article explores the barriers to achieving a strong evidence base in surgery and offers potential solutions to overcome the barriers. Many barriers exist to evidence-based surgical research. They include enabling factors, such as funding, time, infrastructure, patient preference, ethical issues, and additionally barriers associated with specific attributes related to researchers, methodologies, or interventions. Novel evidence synthesis techniques in surgery are discussed, including graphics synthesis, treatment networks, and network meta-analyses that help overcome many of the limitations associated with existing techniques. They offer the opportunity to assess gaps and quantitatively present inconsistencies within the existing evidence of RCTs. Poorly or inadequately performed RCTs and meta-analyses can give rise to incorrect results and thus fail to inform clinical practice or revise policy. The above barriers can be overcome by providing academic leadership and good organizational support to ensure that adequate personnel, resources, and funding are allocated to the researcher. Training in research methodology and data interpretation can ensure that trials are conducted correctly and evidence is adequately synthesized and disseminated. The ultimate goal of overcoming the barriers to evidence-based surgery includes the improved quality of patient care in addition to enhanced patient outcomes.

Synthesis of oligonucleotides on a soluble support

PubMed Central

2017-01-01

Oligonucleotides are usually prepared in lab scale on a solid support with the aid of a fully automated synthesizer. Scaling up of the equipment has allowed industrial synthesis up to kilogram scale. In spite of this, solution-phase synthesis has received continuous interest, on one hand as a technique that could enable synthesis of even larger amounts and, on the other hand, as a gram scale laboratory synthesis without any special equipment. The synthesis on a soluble support has been regarded as an approach that could combine the advantageous features of both the solution and solid-phase syntheses. The critical step of this approach is the separation of the support-anchored oligonucleotide chain from the monomeric building block and other small molecular reagents and byproducts after each coupling, oxidation and deprotection step. The techniques applied so far include precipitation, extraction, chromatography and nanofiltration. As regards coupling, all conventional chemistries, viz. phosphoramidite, H-phosphonate and phosphotriester strategies, have been attempted. While P(III)-based phosphoramidite and H-phosphonate chemistries are almost exclusively used on a solid support, the “outdated” P(V)-based phosphotriester chemistry still offers one major advantage for the synthesis on a soluble support; the omission of the oxidation step simplifies the coupling cycle. Several of protocols developed for the soluble-supported synthesis allow the preparation of both DNA and RNA oligomers of limited length in gram scale without any special equipment, being evidently of interest for research groups that need oligonucleotides in large amounts for research purposes. However, none of them has really tested at such a scale that the feasibility of their industrial use could be critically judged. PMID:28781703

Energetics of amino acid synthesis in hydrothermal ecosystems

NASA Technical Reports Server (NTRS)

Amend, J. P.; Shock, E. L.

1998-01-01

Thermodynamic calculations showed that the autotrophic synthesis of all 20 protein-forming amino acids was energetically favored in hot (100 degrees C), moderately reduced, submarine hydrothermal solutions relative to the synthesis in cold (18 degrees C), oxidized, surface seawater. The net synthesis reactions of 11 amino acids were exergonic in the hydrothermal solution, but all were endergonic in surface seawater. The synthesis of the requisite amino acids of nine thermophilic and hyperthermophilic proteins in a 100 degreesC hydrothermal solution yielded between 600 and 8000 kilojoules per mole of protein, which is energy that is available to drive the intracellular synthesis of enzymes and other biopolymers in hyperthermophiles thriving in these ecosystems.

Study of the self-organization processes in lead sulfide quantum dots

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

Tarasov, S. A., E-mail: SATarasov@mail.ru; Aleksandrova, O. A.; Maksimov, A. I.

A procedure is described for the synthesis of nanoparticles based on lead chalcogenides. The procedure combines the synthesis of colloidal quantum dots (QDs) in aqueous solutions with simultaneous organization of the QDs into ordered arrays. The processes of the self-organization of QDs are analyzed at the nano- and microscopic levels by the photoluminescence method, atomic-force microscopy, and optical microscopy.

Nanoporous films: From conventional to the conformal

DOE PAGES

Allendorf, Mark D.; Stavila, Vitalie

2015-12-14

Here, thin and continuous films of porous metal-organic frameworks can now be conformally deposited on various substrates using a vapor-phase synthesis approach that departs from conventional solution-based routes.

An improved synthesis of haloaceteamidine-based inactivators of protein arginine deiminase 4 (PAD4)

PubMed Central

Causey, Corey P.; Thompson, Paul R.

2008-01-01

Protein arginine deiminase 4 (PAD4) is an enzyme that hydrolyzes peptidyl arginine residues to form citrulline and ammonia. This enzyme has been implicated in several disease states, e.g. rheumatoid arthritis, and therefore represents a unique target for the development of a novel therapeutic. A solution-phase synthesis of Cl-amidine, the most potent PAD4 inactivator described to date, has been developed. This synthesis proceeds in 80% yield over 4 steps at a significantly (12-fold) lower cost. PMID:19587776

Synthesis and Characterisation of Hollow Spherical Nano- and Microparticles with Silica and Magnetite

NASA Astrophysics Data System (ADS)

Gorbyk, P. P.; Dubrovin, I. V.; Demchenko, Yu. A.

The main principles and methods of synthesis of hollow structures with inorganic nanomaterials are described. Synthesis of hollow spherical silica particles was based on hydrolysis of Si(CH3)2Cl2 and SiCl4 in nonpolar solvents at a surface of aerosol drops. To synthesise hollow magnetite nano- and microparticles with magnetite, saturated solution of iron chlorides in acetone was used. Phase and element composition, morphology and structure of samples were studied using XRD, Auger electron spectroscopy, scanning electron and atom force microscopies.

Self-Supporting, Hydrophobic, Ionic Liquid-Based Reference Electrodes Prepared by Polymerization-Induced Microphase Separation

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

Chopade, Sujay A.; Anderson, Evan L.; Schmidt, Peter W.

Interfaces of ionic liquids and aqueous solutions exhibit stable electrical potentials over a wide range of aqueous electrolyte concentrations. This makes ionic liquids suitable as bridge materials that separate in electroanalytical measurements the reference electrode from samples with low and/or unknown ionic strengths. However, methods for the preparation of ionic liquid-based reference electrodes have not been explored widely. We have designed a convenient and reliable synthesis of ionic liquid-based reference electrodes by polymerization-induced microphase separation. This technique allows for a facile, single-pot synthesis of ready-to-use reference electrodes that incorporate ion conducting nanochannels filled with either 1-octyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide or 1-dodecyl-3-methylimidazolium bis(trifluoromethylmore » sulfonyl)imide as ionic liquid, supported by a mechanically robust cross-linked polystyrene phase. This synthesis procedure allows for the straightforward design of various reference electrode geometries. These reference electrodes exhibit a low resistance as well as good reference potential stability and reproducibility when immersed into aqueous solutions varying from deionized, purified water to 100 mM KCl, while requiring no correction for liquid junction potentials.« less

A statistical-based scheduling algorithm in automated data path synthesis

NASA Technical Reports Server (NTRS)

Jeon, Byung Wook; Lursinsap, Chidchanok

1992-01-01

In this paper, we propose a new heuristic scheduling algorithm based on the statistical analysis of the cumulative frequency distribution of operations among control steps. It has a tendency of escaping from local minima and therefore reaching a globally optimal solution. The presented algorithm considers the real world constraints such as chained operations, multicycle operations, and pipelined data paths. The result of the experiment shows that it gives optimal solutions, even though it is greedy in nature.

Cationic hemicellulose-based hydrogels for arsenic and chromium removal from aqueous solutions.

PubMed

Dax, Daniel; Chávez, María Soledad; Xu, Chunlin; Willför, Stefan; Mendonça, Regis Teixeira; Sánchez, Julio

2014-10-13

In this work the synthesis of hemicellulose-based hydrogels and their application for the removal of arsenic and chromium ions is described. In a first step O-acetyl galactoglucomannan (GGM) was subjected to a transesterification applying glycidyl methacrylate (GMA) for the synthesis of novel GGM macromonomers. Two distinguished and purified GGM fractions with molar mass of 7.1 and 28 kDa were used as starting materials. The resulting GGM macromonomers (GGM-MA) contained well-defined amounts of methacrylate groups as determined by (1)H NMR spectroscopy. Selected GGM-MA derivatives were consecutively applied as a crosslinker in the synthesis of tailored hydrogels using [2-(methacryloyloxy)ethyl]trimethylammonium chloride (MeDMA) as monomer. The swelling rate of the hydrogels was determined and the coherence between the swelling rate and the hydrogel composition was examined. The morphology of the GGM-based hydrogels was analysed by SEM and the hydrogels revealed a high surface area and were assessed in respect to their ability to remove arsenate and chromate ions from aqueous solutions. The presented bio-based hydrogels are of high interest especially for the mining industries as a sustainable material for the treatment of their highly contaminated wastewaters. Copyright © 2014 Elsevier Ltd. All rights reserved.

Two-Swim Operators in the Modified Bacterial Foraging Algorithm for the Optimal Synthesis of Four-Bar Mechanisms

PubMed Central

Hernández-Ocaña, Betania; Pozos-Parra, Ma. Del Pilar; Mezura-Montes, Efrén; Portilla-Flores, Edgar Alfredo; Vega-Alvarado, Eduardo; Calva-Yáñez, Maria Bárbara

2016-01-01

This paper presents two-swim operators to be added to the chemotaxis process of the modified bacterial foraging optimization algorithm to solve three instances of the synthesis of four-bar planar mechanisms. One swim favors exploration while the second one promotes fine movements in the neighborhood of each bacterium. The combined effect of the new operators looks to increase the production of better solutions during the search. As a consequence, the ability of the algorithm to escape from local optimum solutions is enhanced. The algorithm is tested through four experiments and its results are compared against two BFOA-based algorithms and also against a differential evolution algorithm designed for mechanical design problems. The overall results indicate that the proposed algorithm outperforms other BFOA-based approaches and finds highly competitive mechanisms, with a single set of parameter values and with less evaluations in the first synthesis problem, with respect to those mechanisms obtained by the differential evolution algorithm, which needed a parameter fine-tuning process for each optimization problem. PMID:27057156

Two-Swim Operators in the Modified Bacterial Foraging Algorithm for the Optimal Synthesis of Four-Bar Mechanisms.

PubMed

Hernández-Ocaña, Betania; Pozos-Parra, Ma Del Pilar; Mezura-Montes, Efrén; Portilla-Flores, Edgar Alfredo; Vega-Alvarado, Eduardo; Calva-Yáñez, Maria Bárbara

2016-01-01

This paper presents two-swim operators to be added to the chemotaxis process of the modified bacterial foraging optimization algorithm to solve three instances of the synthesis of four-bar planar mechanisms. One swim favors exploration while the second one promotes fine movements in the neighborhood of each bacterium. The combined effect of the new operators looks to increase the production of better solutions during the search. As a consequence, the ability of the algorithm to escape from local optimum solutions is enhanced. The algorithm is tested through four experiments and its results are compared against two BFOA-based algorithms and also against a differential evolution algorithm designed for mechanical design problems. The overall results indicate that the proposed algorithm outperforms other BFOA-based approaches and finds highly competitive mechanisms, with a single set of parameter values and with less evaluations in the first synthesis problem, with respect to those mechanisms obtained by the differential evolution algorithm, which needed a parameter fine-tuning process for each optimization problem.

Calcium hydride synthesis of Ti-Nb-based alloy powders

NASA Astrophysics Data System (ADS)

Kasimtsev, A. V.; Shuitsev, A. V.; Yudin, S. N.; Levinskii, Yu. V.; Sviridova, T. A.; Alpatov, A. V.; Novosvetlova, E. E.

2017-09-01

The metallothermic (calcium hydride) synthesis of Ti-Nb alloy powders alloyed with tantalum and zirconium is experimentally studied under various conditions. Chemical, X-ray diffraction, and metallographic analyses of the synthesized products show that initial oxides are completely reduced and a homogeneous β-Ti-based alloy powder forms under the optimum synthesis conditions at a temperature of 1200°C. At a lower synthesis temperature, the end products have a high oxygen content. The experimental results are used to plot the thermokinetic dependences o formation of a bcc solid solution at various times of isothermal holding of Ti-22Nb-6Ta and Ti-22Nb-6Zr (at %) alloys. The physicochemical and technological properties of the Ti-22Nb-6Ta and Ti-22Nb-6Zr alloy powders synthesized by calcium hydride reduction under the optimum conditions are determined.

Molecular Mechanisms of Adaptation of the Moderately Halophilic Bacterium Halobacillis halophilus to Its Environment

PubMed Central

Hänelt, Inga; Müller, Volker

2013-01-01

The capability of osmoadaptation is a prerequisite of organisms that live in an environment with changing salinities. Halobacillus halophilus is a moderately halophilic bacterium that grows between 0.4 and 3 M NaCl by accumulating both chloride and compatible solutes as osmolytes. Chloride is absolutely essential for growth and, moreover, was shown to modulate gene expression and activity of enzymes involved in osmoadaptation. The synthesis of different compatible solutes is strictly salinity- and growth phase-dependent. This unique hybrid strategy of H. halophilus will be reviewed here taking into account the recently published genome sequence. Based on identified genes we will speculate about possible scenarios of the synthesis of compatible solutes and the uptake of potassium ion which would complete our knowledge of the fine-tuned osmoregulation and intracellular osmolyte balance in H. halophilus. PMID:25371341

Cyclotron production of Ga-68 for human use from liquid targets: From theory to practice

NASA Astrophysics Data System (ADS)

Alves, F.; Alves, V. H.; Neves, A. C. B.; do Carmo, S. J. C.; Nactergal, B.; Hellas, V.; Kral, E.; Gonçalves-Gameiro, C.; Abrunhosa, A. J.

2017-05-01

A fully automated system for the production of 68Ga based on commercially available cyclotron liquid target and synthesis modules is described. A solution containing enriched 68Zn dissolved in a nitric solution is irradiated in a Cyclone 18/9 IBA cyclotron leading to the production of up to about 25 GBq of 68Ga. The irradiated solution is transferred to a Synthera synthesis module in which 68Ga is separated and purified with a yield superior to 85 % and where further labelling is achieved with yields no inferior to 70 %. The developed and implemented method presents an improved approach for the production of 68Ga-radiopharmaceuticals suitable for human use, in a process that takes less than 2 hours. This technique represents an economically viable alternative to 68Ge/68Ga generators with improved characteristics.

Paramagnetic iron-doped hydroxyapatite nanoparticles with improved metal sorption properties. A bioorganic substrates-mediated synthesis.

PubMed

Mercado, D Fabio; Magnacca, Giuliana; Malandrino, Mery; Rubert, Aldo; Montoneri, Enzo; Celi, Luisella; Bianco Prevot, Alessandra; Gonzalez, Mónica C

2014-03-26

This paper describes the synthesis of paramegnetic iron-containing hydroxyapatite nanoparticles and their increased Cu(2+) sorbent capacity when using Ca(2+) complexes of soluble bioorganic substrates from urban wastes as synthesis precursors. A thorough characterization of the particles by TEM, XRD, FTIR spectroscopy, specific surface area, TGA, XPS, and DLS indicates that loss of crystallinity, a higher specific area, an increased surface oxygen content, and formation of surface iron phases strongly enhance Cu(2+) adsorption capacity of hydroxyapatite-based materials. However, the major effect of the surface and morphologycal modifications is the size diminution of the aggregates formed in aqueous solutions leading to an increased effective surface available for Cu(2+) adsorption. Maximum sorption values of 550-850 mg Cu(2+) per gram of particles suspended in an aqueous solution at pH 7 were determined, almost 10 times the maximum values observed for hydroxyapatite nanoparticles suspensions under the same conditions.

An in-situ phosphorus source for the synthesis of Cu 3P and the subsequent conversion to Cu 3PS 4 nanoparticle clusters

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

Sheets, Erik J.; Stach, Eric A.; Yang, Wei -Chang

2015-09-20

The search for alternative earth abundant semiconducting nanocrystals for sustainable energy applications has brought forth the need for nanoscale syntheses beyond bulk synthesis routes. Of particular interest are metal phosphides and derivative I-V-VI chalcogenides including copper phosphide (Cu 3P) and copper thiophosphate (Cu 3PS 4). Herein, we report a one-pot, solution-based synthesis of Cu 3P nanocrystals utilizing an in-situ phosphorus source: phosphorus pentasulfide (P 2S 5) in trioctylphosphine (TOP). By injecting this phosphorus source into a copper solution in oleylamine (OLA), uniform and size controlled Cu 3P nanocrystals with a phosphorous-rich surface are synthesized. The subsequent reaction of the Cumore » 3P nanocrystals with decomposing thiourea forms nanoscale Cu 3PS 4 particles having p-type conductivity and an effective optical band gap of 2.36 eV.« less

Dinitrosyl iron complexes with natural thiol-containing ligands in aqueous solutions: Synthesis and some physico-chemical characteristics (A methodological review).

PubMed

Vanin, Anatoly F; Borodulin, Rostislav R; Mikoyan, Vasak D

2017-06-01

Two approaches to the synthesis of dinitrosyl iron complexes (DNIC) with glutathione and l-cysteine in aqueous solutions based on the use of gaseous NO and appropriate S-nitrosothiols, viz., S-nitrosoglutathione (GS-NO) or S-nitrosocysteine (Cys-NO), respectively, are considered. A schematic representation of a vacuum unit for generation and accumulation of gaseous NO purified from the NO 2 admixture and its application for obtaining aqueous solutions of DNIC in a Thunberg apparatus is given. To achieve this, a solution of bivalent iron in distilled water is loaded into the upper chamber of the Thunberg apparatus, while the thiol solution in an appropriate buffer (рН 7.4) is loaded into its lower chamber. Further steps, which include degassing, addition of gaseous NO, shaking of both solutions and formation of the Fe 2+ -thiol mixture, culminate in the synthesis of DNIC. The second approach consists in a stepwise addition of Fe 2+ salts and nitrite to aqueous solutions of glutathione or cysteine. In the presence of Fe 2+ and after the increase in рН to the physiological level, GS-NO or Cys-NO generated at acid media (pH < 4) are converted into DNIC with glutathione or cysteine. Noteworthy, irrespective of the procedure used for their synthesis DNIC with glutathione manifest much higher stability than DNIC with cysteine. The pattern of spin density distribution in iron-dinitrosyl fragments of DNIC characterized by the d 7 electronic configuration of the iron atom and described by the formula Fe + (NO + ) 2 is unique in that it provides a plausible explanation for the ability of DNIC to generate NO and nitrosonium ions (NO + ) and the peculiar characteristics of the EPR signal of their mononuclear form (M-DNIC). Copyright © 2017. Published by Elsevier Inc.

Effect of the raw material type and the reaction time on the synthesis of halloysite based Zeolite Na-P1

NASA Astrophysics Data System (ADS)

Meftah, Mahdi; Oueslati, Walid; Chorfi, Nejmeddine; Ben Haj Amara, Abdesslem

Zeolites are currently one of the most important classes of inorganic materials because of their multiple applications not only as ions exchangers and molecular sieves, but also as catalysts. This works focus the synthesis and the characterization of Zeolite Na-P1 using halloysite (collected near Ain Khemouda, western Tunisia) as the starting material. Two parameters, such as the host materials type (natural or treated) and the reaction time, involved in the synthesis process are investigated. The intermediate phases and final products were characterized by X-ray diffraction, Infrared IR spectroscopy, scanning electron microscopy and high-resolution 29Si and 27Al MAS NMR. Obtained results show that the hydrothermal synthesis from natural and heated-halloysite leads to formation of homogenous Zeolite Na-P1. The difference in the crystallization/transformation time process is explained by the effect of the dissolution rate of the starting materials in sodium hydroxide solution. In the case of heated halloysite, the synthesis reaction with alkali solution occurs very readily and achieved without prior thermal activation at high temperature. The optimal conditions of Zeolite Na-P1 crystallization, from heated-halloysite, are reached at 120 °C.

Burst nucleation by hot injection for size controlled synthesis of ε-cobalt nanoparticles.

PubMed

Zacharaki, Eirini; Kalyva, Maria; Fjellvåg, Helmer; Sjåstad, Anja Olafsen

2016-01-01

Reproducible growth of narrow size distributed ε-Co nanoparticles with a specific size requires full understanding and identification of the role of essential synthesis parameters for the applied synthesis method. For the hot injection methodology, a significant discrepancy with respect to obtained sizes and applied reaction conditions is reported. Currently, a systematic investigation controlling key synthesis parameters as injection-temperature and time, metal to surfactant ratio and reaction holding time in terms of their impact on mean ([Formula: see text]mean) and median ([Formula: see text]median) particle diameter using dichlorobenzene (DCB), Co2(CO)8 and oleic acid (OA) as the reactant matrix is lacking. A series of solution-based ε-Co nanoparticles were synthesized using the hot injection method. Suspensions and obtained particles were analyzed by DLS, ICP-OES, (synchrotron)XRD and TEM. Rietveld refinements were used for structural analysis. Mean ([Formula: see text]mean) and median ([Formula: see text]median) particle diameters were calculated with basis in measurements of 250-500 particles for each synthesis. 95 % bias corrected confidence intervals using bootstrapping were calculated for syntheses with three or four replicas. ε-Co NPs in the size range ~4-10 nm with a narrow size distribution are obtained via the hot injection method, using OA as the sole surfactant. Typically the synthesis yield is ~75 %, and the particles form stable colloidal solutions when redispersed in hexane. Reproducibility of the adopted synthesis procedure on replicate syntheses was confirmed. We describe in detail the effects of essential synthesis parameters, such as injection-temperature and time, metal to surfactant ratio and reaction holding time in terms of their impact on mean ([Formula: see text]mean) and median ([Formula: see text]median) particle diameter. The described synthesis procedure towards ε-Co nanoparticles (NPs) is concluded to be robust when controlling key synthesis parameters, giving targeted particle diameters with a narrow size distribution. We have identified two major synthesis parameters which control particle size, i.e., the metal to surfactant molar ratio and the injection temperature of the hot OA-DCB solution into which the cobalt precursor is injected. By increasing the metal to surfactant molar ratio, the mean particle diameter of the ε-Co NPs has been found to increase. Furthermore, an increase in the injection temperature of the hot OA-DCB solution into which the cobalt precursor is injected, results in a decrease in the mean particle diameter of the ε-Co NPs, when the metal to surfactant molar ratio [Formula: see text] is fixed at ~12.9.

The Synthesis of Polymer Precursors and Exploratory Research Based on Acetylene Displacement Reaction

DTIC Science & Technology

1980-10-01

the addition of solids, a soluble base, potassium 2,6-dimethylphenoxide was tried. It was felt that the two ortho -methyl groups would sterically...was obtained, but as a mixture of all three nitro -isomers. Moreover, direct crystallization from the nitration media could not be induced even by...transferred to a dropping funnel. This solution was added dropwise over ca. 1 hr to a solution of 1220 g 4- nitro - benzil in 5.1 1 DMSO in a 22-1 pot held

One-pot synthesis of fluorescent polysaccharides: adenine grafted agarose and carrageenan.

PubMed

Oza, Mihir D; Prasad, Kamalesh; Siddhanta, A K

2012-08-01

New fluorescent polysaccharides were synthesized by grafting the nucleobase adenine on to the backbones of agarose and κ-carrageenan, which were characterized by FT-IR, (13)C NMR, TGA, XRD, UV, and fluorescence properties. The synthesis involved a rapid water based potassium persulfate (KPS) initiated method under microwave irradiation. The emission spectra of adenine grafted agarose and κ-carrageenan were recorded in aqueous (5×10(-5) M) solution, exhibiting λ(em,max) 347 nm by excitation at 261 nm, affording ca. 30% and 40% enhanced emission intensities, respectively compared to that of pure adenine solution in the same concentration. Similar emission intensity was recorded in the pure adenine solution at its molar equivalent concentrations present in the 5×10(-5) M solution of the agarose and carrageenan grafted products, that is, 3.28×10(-5) M and 4.5×10(-5) M respectively. These fluorescent adenine grafted products may have potential utility in various sensor applications. Copyright © 2012. Published by Elsevier Ltd.

Computer Synthesis Approaches of Hyperboloid Gear Drives with Linear Contact

NASA Astrophysics Data System (ADS)

Abadjiev, Valentin; Kawasaki, Haruhisa

2014-09-01

The computer design has improved forming different type software for scientific researches in the field of gearing theory as well as performing an adequate scientific support of the gear drives manufacture. Here are attached computer programs that are based on mathematical models as a result of scientific researches. The modern gear transmissions require the construction of new mathematical approaches to their geometric, technological and strength analysis. The process of optimization, synthesis and design is based on adequate iteration procedures to find out an optimal solution by varying definite parameters. The study is dedicated to accepted methodology in the creation of soft- ware for the synthesis of a class high reduction hyperboloid gears - Spiroid and Helicon ones (Spiroid and Helicon are trademarks registered by the Illinois Tool Works, Chicago, Ill). The developed basic computer products belong to software, based on original mathematical models. They are based on the two mathematical models for the synthesis: "upon a pitch contact point" and "upon a mesh region". Computer programs are worked out on the basis of the described mathematical models, and the relations between them are shown. The application of the shown approaches to the synthesis of commented gear drives is illustrated.

Bismuth-based oxide semiconductors: Mild synthesis and practical applications

NASA Astrophysics Data System (ADS)

Timmaji, Hari Krishna

In this dissertation study, bismuth based oxide semiconductors were prepared using 'mild' synthesis techniques---electrodeposition and solution combustion synthesis. Potential environmental remediation and solar energy applications of the prepared oxides were evaluated. Bismuth vanadate (BiVO4) was prepared by electrodeposition and solution combustion synthesis. A two step electrosynthesis strategy was developed and demonstrated for the first time. In the first step, a Bi film was first electrodeposited on a Pt substrate from an acidic BiCl3 medium. Then, this film was anodically stripped in a medium containing hydrolyzed vanadium precursor, to generate Bi3+, and subsequent BiVO4 formation by in situ precipitation. The photoelectrochemical data were consistent with the in situ formation of n-type semiconductor films. In the solution combustion synthesis procedure, BiVO4 powders were prepared using bismuth nitrate pentahydrate as the bismuth precursor and either vanadium chloride or vanadium oxysulfate as the vanadium precursor. Urea, glycine, or citric acid was used as the fuel. The effect of the vanadium precursor on the photocatalytic activity of combustion synthesized BiVO 4 was evaluated in this study. Methyl orange was used as a probe to test the photocatalytic attributes of the combustion synthesized (CS) samples, and benchmarked against a commercial bismuth vanadate sample. The CS samples showed superior activity to the commercial benchmark sample, and samples derived from vanadium chloride were superior to vanadium oxysulfate counterparts. The photoelectrochemical properties of the various CS samples were also studied and these samples were shown to be useful both for environmental photocatalytic remediation and water photooxidation applications. Silver bismuth tungstate (AgBiW2O8) nanoparticles were prepared for the first time by solution combustion synthesis by using silver nitrate, bismuth nitrate, sodium tungstate as precursors for Ag, Bi, and W respectively and urea as the fuel. The photocatalytic activity of these nanoparticles was superior to a sample prepared by solid-state synthesis. The combustion-synthesized particles were subsequently modified with Pt catalyst islands using a photodeposition technique and then used for the photo-generation of syngas (CO + H2). Formic acid was used in these experiments for in situ generation of CO2 and its subsequent reduction to CO. In the absence of Pt modification, H2 was not obtained. These results were compared with those obtained with acetic acid in place of formic acid, and finally the mechanistic pathways for syngas and methane photogeneration are presented.

Bacterial cellulose based hydrogel (BC-g-AA) and preliminary result of swelling behavior

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

Hakam, Adil; Lazim, Azwan Mat; Abdul Rahman, I. Irman

2013-11-27

In this study, hydrogel based on Bacterial cellulose (BC) or local known as Nata de Coco, which grafted with monomer: Acrylic acid (AA) is synthesis by using gamma radiation technique. These hydrogel (BC-g-AA) has unique characteristic whereby responsive to pH buffer solution.

Fabrication routes for one-dimensional nanostructures via block copolymers

NASA Astrophysics Data System (ADS)

Tharmavaram, Maithri; Rawtani, Deepak; Pandey, Gaurav

2017-05-01

Nanotechnology is the field which deals with fabrication of materials with dimensions in the nanometer range by manipulating atoms and molecules. Various synthesis routes exist for the one, two and three dimensional nanostructures. Recent advancements in nanotechnology have enabled the usage of block copolymers for the synthesis of such nanostructures. Block copolymers are versatile polymers with unique properties and come in many types and shapes. Their properties are highly dependent on the blocks of the copolymers, thus allowing easy tunability of its properties. This review briefly focusses on the use of block copolymers for synthesizing one-dimensional nanostructures especially nanowires, nanorods, nanoribbons and nanofibers. Template based, lithographic, and solution based approaches are common approaches in the synthesis of nanowires, nanorods, nanoribbons, and nanofibers. Synthesis of metal, metal oxides, metal oxalates, polymer, and graphene one dimensional nanostructures using block copolymers have been discussed as well.

Synthesis of Copper-Antimony-Sulfide Nanocrystals for Solution-Processed Solar Cells.

PubMed

Suehiro, Satoshi; Horita, Keisuke; Yuasa, Masayoshi; Tanaka, Tooru; Fujita, Katsuhiko; Ishiwata, Yoichi; Shimanoe, Kengo; Kida, Tetsuya

2015-08-17

The p-type nanocrystals (NCs) of copper-based chalcogenides, such as CuInSe2 and Cu2ZnSnS4, have attracted increasing attention in photovoltaic applications due to their potential to produce cheap solution-processed solar cells. Herein, we report the synthesis of copper-antimony-sulfide (CAS) NCs with different crystal phases including CuSbS2, Cu3SbS4, and Cu12Sb4S13. In addition, their morphology, crystal phase, and optical properties were characterized using transmission electron microscopy, X-ray diffractometry, UV-vis-near-IR spectroscopy, and photoemission yield spectroscopy. The morphology, crystal phase, and electronic structure were significantly dependent on the chemical composition in the CAS system. Devices were fabricated using particulate films consisting of CAS NCs prepared by spin coating without a high-temperature treatment. The CAS NC-based devices exhibited a diode-like current-voltage characteristic when coupled with an n-type CdS layer. In particular, the CuSbS2 NC devices exhibited photovoltaic responses under simulated sunlight, demonstrating its applicability for use in solution-processed solar cells.

On the suitability and development of layout templates for analog layout reuse and layout-aware synthesis

NASA Astrophysics Data System (ADS)

Castro-Lopez, Rafael; Fernandez, Francisco V.; Rodriguez Vazquez, Angel

2005-06-01

Accelerating the synthesis of increasingly complex analog integrated circuits is key to bridge the widening gap between what we can integrate and what we can design while meeting ever-tightening time-to-market constraints. It is a well-known fact in the semiconductor industry that such goal can only be attained by means of adequate CAD methodologies, techniques, and accompanying tools. This is particularly important in analog physical synthesis (a.k.a. layout generation), where large sensitivities of the circuit performances to the many subtle details of layout implementation (device matching, loading and coupling effects, reliability, and area features are of utmost importance to analog designers), render complete automation a truly challenging task. To approach the problem, two directions have been traditionally considered, knowledge-based and optimization-based, both with their own pros and cons. Besides, recently reported solutions oriented to speed up the overall design flow by means of reuse-based practices or by cutting off time-consuming, error-prone spins between electrical and layout synthesis (a technique known as layout-aware synthesis), rely on a outstandingly rapid yet efficient layout generation method. This paper analyses the suitability of procedural layout generation based on templates (a knowledge-based approach) by examining the requirements that both layout reuse and layout-aware solutions impose, and how layout templates face them. The ability to capture the know-how of experienced layout designers and the turnaround times for layout instancing are considered main comparative aspects in relation to other layout generation approaches. A discussion on the benefit-cost trade-off of using layout templates is also included. In addition to this analysis, the paper delves deeper into systematic techniques to develop fully reusable layout templates for analog circuits, either for a change of the circuit sizing (i.e., layout retargeting) or a change of the fabrication process (i.e., layout migration). Several examples implemented with the Cadence's Virtuoso tool suite are provided as demonstration of the paper's contributions.

Parallel solution-phase synthesis of a 2-aminothiazole library including fully automated work-up.

PubMed

Buchstaller, Hans-Peter; Anlauf, Uwe

2011-02-01

A straightforward and effective procedure for the solution phase preparation of a 2-aminothiazole combinatorial library is described. Reaction, work-up and isolation of the title compounds as free bases was accomplished in a fully automated fashion using the Chemspeed ASW 2000 automated synthesizer. The compounds were obtained in good yields and excellent purities without any further purification procedure.

Neural-genetic synthesis for state-space controllers based on linear quadratic regulator design for eigenstructure assignment.

PubMed

da Fonseca Neto, João Viana; Abreu, Ivanildo Silva; da Silva, Fábio Nogueira

2010-04-01

Toward the synthesis of state-space controllers, a neural-genetic model based on the linear quadratic regulator design for the eigenstructure assignment of multivariable dynamic systems is presented. The neural-genetic model represents a fusion of a genetic algorithm and a recurrent neural network (RNN) to perform the selection of the weighting matrices and the algebraic Riccati equation solution, respectively. A fourth-order electric circuit model is used to evaluate the convergence of the computational intelligence paradigms and the control design method performance. The genetic search convergence evaluation is performed in terms of the fitness function statistics and the RNN convergence, which is evaluated by landscapes of the energy and norm, as a function of the parameter deviations. The control problem solution is evaluated in the time and frequency domains by the impulse response, singular values, and modal analysis.

Cellulose acetate fibers prepared from different raw materials with rapid synthesis method.

PubMed

Chen, Jinghuan; Xu, Jikun; Wang, Kun; Cao, Xuefei; Sun, Runcang

2016-02-10

Transesterification is a mild process to prepare cellulose acetate (CA) as compared with the traditional method. In this study, CA fibers were produced from six cellulose raw materials based on a simple and rapid transesterification method. The properties of the CA solutions and the obtained CA fibers were investigated in detail. Results showed that all of the cellulose raw materials were esterified within 15 min, and spinning dopes could be obtained by concentrating the CA solutions via vacuum distillation. The XRD, FT-IR, (1)H, (13)C and HSQC NMR analysis confirmed the successful synthesis of CA. The degree of substitution (DS) of the obtained CA was significantly affected by the degree of polymerization (DP) of cellulose raw materials, which further influenced the viscosity of CA solutions as well as the structural, thermal and mechanical properties of the CA fibers. Copyright © 2015 Elsevier Ltd. All rights reserved.

Coassembly of Lysozyme and Amphiphilic Biomolecules Driven by Unimer-Aggregate Equilibrium.

PubMed

Tao, Yuanyuan; Ma, Xiaoteng; Cai, Yaqian; Liu, Li; Zhao, Hanying

2018-04-12

Synthesis and self-assembly of bioconjugates composed of proteins and synthetic molecules have been widely studied because of the potential applications in medicine, biotechnology, and nanotechnology. One of the challenging research studies in this area is to develop organic solvent-free approaches to the synthesis and self-assembly of amphiphilic bioconjugates. In this research, dialysis-assisted approach, a method based on unimer-aggregate equilibrium, was applied in the coassembly of lysozyme and conjugate of cholesterol and glutathione (Ch-GSH). In phosphate buffer solution, amphiphilic Ch-GSH conjugate self-assembles into vesicles, and the vesicle solution is dialyzed against lysozyme solution. Negatively charged Ch-GSH unimers produced in the unimer-vesicle exchange equilibrium, diffuse across the dialysis membrane and have electrostatic interaction with positively charged lysozyme, resulting in the formation of Ch-GSH-lysozyme bioconjugate. Above a critical concentration, the three-component bioconjugate molecules self-assemble into bioactive vesicles.

Structure-Property Evaluation of Thermally and Chemically Gelling Injectable Hydrogels for Tissue Engineering

PubMed Central

Ekenseair, Adam K.; Boere, Kristel W. M.; Tzouanas, Stephanie N.; Vo, Tiffany N.; Kasper, F. Kurtis; Mikos, Antonios G.

2012-01-01

The impact of synthesis and solution formulation parameters on the swelling and mechanical properties of a novel class of thermally and chemically gelling hydrogels combining poly(N-isopropylacrylamide)-based thermogelling macromers containing pendant epoxy rings with polyamidoamine-based hydrophilic and degradable diamine crosslinking macromers was evaluated. Through variation of network hydrophilicity and capacity for chain rearrangement, the often problematic tendency of thermogelling hydrogels to undergo significant syneresis was addressed. The demonstrated ability to easily tune post-formation dimensional stability at both the synthesis and formulation stages represents a significant novel contribution towards efforts to utilize poly(N-isopropylacrylamide)-based polymers as injectable biomaterials. Furthermore, the cytocompatibility of the hydrogel system under relevant conditions was established, while demonstrating time- and dose-dependent cytotoxicity at high solution osmolality. Such injectable in situ forming degradable hydrogels with tunable water content are promising candidates for many tissue engineering applications, particularly for cell delivery to promote rapid tissue regeneration in non-load-bearing defects. PMID:22881074

Large-Scale Surfactant-Free Synthesis of p-Type SnTe Nanoparticles for Thermoelectric Applications

PubMed Central

Han, Guang; Zhang, Ruizhi; Popuri, Srinivas R.; Greer, Heather F.; Reece, Michael J.; Bos, Jan-Willem G.; Zhou, Wuzong; Knox, Andrew R.; Gregory, Duncan H.

2017-01-01

A facile one-pot aqueous solution method has been developed for the fast and straightforward synthesis of SnTe nanoparticles in more than ten gram quantities per batch. The synthesis involves boiling an alkaline Na2SnO2 solution and a NaHTe solution for short time scales, in which the NaOH concentration and reaction duration play vital roles in controlling the phase purity and particle size, respectively. Spark plasma sintering of the SnTe nanoparticles produces nanostructured compacts that have a comparable thermoelectric performance to bulk counterparts synthesised by more time- and energy-intensive methods. This approach, combining an energy-efficient, surfactant-free solution synthesis with spark plasma sintering, provides a simple, rapid, and inexpensive route to p-type SnTe nanostructured materials. PMID:28772593

Effect of alkali ions (Na+, K+, Cs+) on reaction mechanism of CZTS nano-particles synthesis

NASA Astrophysics Data System (ADS)

Kumar, Suresh; Altosaar, Mare; Grossberg, Maarja; Mikli, Valdek

2018-04-01

The control of morphology, elemental composition and phase composition of Cu2ZnSnS4 (CZTS) nano-crystals depends on the control of complex formation and surface stabilization of nano-particles in solution-based synthesis in oleylamine. At temperatures ≥280 °C, the control of nano-crystal's morphology and homogenous growth is difficult because of fast poly-nuclear growth occurring at higher temperatures. In the present work the effect of oleylamine complex formation with different alkali ions (Na+, K+ and Cs+) on nano-crystals growth at synthesis temperature of 280 °C was studied. It was found that nano-powders synthesized in the presence of Na+ and K+ ions showed the formation of crystals of different sizes - small nano-particles (18 nm-30 nm), large aggregated crystals (few nm to 1 μm) and large single crystals (1 μm - 4 μm). The presence of Cs+ ions in the nano-powder synthesis in oleylamine-metal precursor-CsOH solution promoted growth of nano-crystals of homogenous size. It is proposed that the formed oleylamine-Cs complexes a) enhance the formation and stabilization of oleylamine-metal (Cu, Zn and Sn) complexes before the injection of sulphur precursor into the oleylamine-metal precursor solution and b) after addition of sulphur stabilize the fast nucleated nano-particles and promote diffusion limited growth.

Piezoelectric Ceramics of the (1 − x)Bi0.50Na0.50TiO3–xBa0.90Ca0.10TiO3 Lead-Free Solid Solution: Chemical Shift of the Morphotropic Phase Boundary, a Case Study for x = 0.06

PubMed Central

Vivar-Ocampo, Rodrigo; Pardo, Lorena; Ávila, David; Morán, Emilio; González, Amador M.; Bucio, Lauro; Villafuerte-Castrejón, María-Elena

2017-01-01

Research and development of lead-free piezoelectric materials are still the hottest topics in the field of piezoelectricity. One of the most promising lead-free family of compounds to replace lead zirconate–titanate for actuators is that of Bi0.50Na0.50TiO3 (BNT) based solid solutions. The pseudo-binary (1 − x)Bi0.50Na0.50TiO3–xBa1 − yCayTiO3 system has been proposed for high temperature capacitors and not yet fully explored as piezoelectric material. In this work, the solid solution with x = 0.06 and y = 0.10 was obtained by two different synthesis routes: solid state and Pechini, aiming at using reduced temperatures, both in synthesis (<800 °C) and sintering (<1150 °C), while maintaining appropriated piezoelectric performance. Crystal structure, ceramic grain size, and morphology depend on the synthesis route and were analyzed by X-ray diffraction, together with scanning and transmission electron microscopy. The effects of processing and ceramic microstructure on the structural, dielectric, ferroelectric, and piezoelectric properties were discussed in terms of a shift of the Morphotropic Phase Boundary, chemically induced by the synthesis route. PMID:28773096

Piezoelectric Ceramics of the (1 - x)Bi0.50Na0.50TiO₃-xBa0.90Ca0.10TiO₃ Lead-Free Solid Solution: Chemical Shift of the Morphotropic Phase Boundary, a Case Study for x = 0.06.

PubMed

Vivar-Ocampo, Rodrigo; Pardo, Lorena; Ávila, David; Morán, Emilio; González, Amador M; Bucio, Lauro; Villafuerte-Castrejón, María-Elena

2017-07-01

Research and development of lead-free piezoelectric materials are still the hottest topics in the field of piezoelectricity. One of the most promising lead-free family of compounds to replace lead zirconate-titanate for actuators is that of Bi 0.50 Na 0.50 TiO₃ (BNT) based solid solutions. The pseudo-binary (1 - x )Bi 0.50 Na 0.50 TiO₃- x Ba 1 - y Ca y TiO₃ system has been proposed for high temperature capacitors and not yet fully explored as piezoelectric material. In this work, the solid solution with x = 0.06 and y = 0.10 was obtained by two different synthesis routes: solid state and Pechini, aiming at using reduced temperatures, both in synthesis (<800 °C) and sintering (<1150 °C), while maintaining appropriated piezoelectric performance. Crystal structure, ceramic grain size, and morphology depend on the synthesis route and were analyzed by X-ray diffraction, together with scanning and transmission electron microscopy. The effects of processing and ceramic microstructure on the structural, dielectric, ferroelectric, and piezoelectric properties were discussed in terms of a shift of the Morphotropic Phase Boundary, chemically induced by the synthesis route.

Solution based synthesis of mixed-phase materials in the Li2TiO3-Li4SiO4 system

NASA Astrophysics Data System (ADS)

Hanaor, Dorian A. H.; Kolb, Matthias H. H.; Gan, Yixiang; Kamlah, Marc; Knitter, Regina

2015-01-01

As candidate tritium breeder materials for use in the ITER helium cooled pebble bed, ceramic multiphasic compounds lying in the region of the quasi-binary lithium metatitanate-lithium orthosilicate system may exhibit mechanical and physical advantages relative to single phase materials. Here we present an organometallic solution-based synthesis procedure for the low-temperature fabrication of compounds in the Li2TiO3-Li4SiO4 region and investigate phase stability and transformations through temperature varied X-ray diffraction and scanning calorimetry. Results demonstrate that the metatitanate and metasilicate phases Li2TiO3 and Li2SiO3 readily crystallise in nanocrystalline form at temperatures below 180 °C. Lithium deficiency in the region of 5% results from Li sublimation from Li4SiO4 and/or from excess Li incorporation in the metatitanate phase and brings about a stoichiometry shift, with product compounds exhibiting mixed lithium orthosilicate/metasilicate content towards the Si rich region and predominantly Li2TiO3 content towards the Ti rich region. Above 1150 °C the transformation of monoclinic to cubic γ-Li2TiO3 disordered solid-solution occurs while the melting of silicate phases indicates a likely monotectic type system with a solidus line in the region 1050-1100 °C. Synthesis procedures involving a lithium chloride precursor are not likely to be a viable option for breeder pebble synthesis as this route was found to yield materials with a more significant Li-deficiency exhibiting the crystallisation of the Li2TiSiO5 phase at intermediate compositions.

Zeolite Coating System for Corrosion Control to Eliminate Hexavalent Chromium from DoD Applications

DTIC Science & Technology

2009-08-01

Beving D.; Munoz R.; Yushan Y. 2005, Hydrothermal Synthesis and Corrosion Resistance of Vanadium ZSM-5 Films, The American Institute of Chemical...Engineers National Meeting, October 30 - November 4, Cincinnati, Ohio. 8) Mao Y.; Beving D.; Munoz R.; Yushan Y. 2005, Hydrothermal Synthesis of...directly at the solid-liquid interface from a synthesis solution during the coating formation process (Figure 2-4)12. The synthesis solution used is a

Ant colony optimisation-direct cover: a hybrid ant colony direct cover technique for multi-level synthesis of multiple-valued logic functions

NASA Astrophysics Data System (ADS)

Abd-El-Barr, Mostafa

2010-12-01

The use of non-binary (multiple-valued) logic in the synthesis of digital systems can lead to savings in chip area. Advances in very large scale integration (VLSI) technology have enabled the successful implementation of multiple-valued logic (MVL) circuits. A number of heuristic algorithms for the synthesis of (near) minimal sum-of products (two-level) realisation of MVL functions have been reported in the literature. The direct cover (DC) technique is one such algorithm. The ant colony optimisation (ACO) algorithm is a meta-heuristic that uses constructive greediness to explore a large solution space in finding (near) optimal solutions. The ACO algorithm mimics the ant's behaviour in the real world in using the shortest path to reach food sources. We have previously introduced an ACO-based heuristic for the synthesis of two-level MVL functions. In this article, we introduce the ACO-DC hybrid technique for the synthesis of multi-level MVL functions. The basic idea is to use an ant to decompose a given MVL function into a number of levels and then synthesise each sub-function using a DC-based technique. The results obtained using the proposed approach are compared to those obtained using existing techniques reported in the literature. A benchmark set consisting of 50,000 randomly generated 2-variable 4-valued functions is used in the comparison. The results obtained using the proposed ACO-DC technique are shown to produce efficient realisation in terms of the average number of gates (as a measure of chip area) needed for the synthesis of a given MVL function.

A new route for the prebiotic synthesis of nucleobases and hydantoins in water/ice solutions involving the photochemistry of acetylene.

PubMed

Menor-Salván, César; Marín-Yaseli, Margarita R

2013-05-10

The origin of nucleobases and other heterocycles is a classic question in the chemistry of the origins of life. The construction of laboratory models for the abiotic synthesis of nitrogen heterocycles in plausible natural conditions also aids the understanding and prediction of chemical species in the Solar System. Here, we report a new explanation for the origin of hydantoins, purines, and pyrimidines in eutectic water/ice/urea solutions driven by ultraviolet irradiation (in the 185-254 nm range, UVC) of acetylene under anoxic conditions. An analysis of the products indicates the synthesis of hydantoin and 5-hydroxyhydantoin, the purines uric acid, xanthine, and guanine, and the pyrimidines uracil and cytosine. The synthesis occurred together with the photo-oxidation of bases in a complex process for which possible pathways are proposed. In conclusion, an acetylene-containing atmosphere could contribute to the origin of nucleobases in the presence of a urea/water system by an HCN-independent mechanism. The presence of ice has a dual role as a favorable medium for the synthesis of nucleobases and protection against degradation and as a source of free radicals for the synthesis of highly oxidized heterocycles. A mechanism for the origin of hydantoins and uracil from urea in plausible conditions for prebiotic chemistry is also proposed. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Towards medicinal mechanochemistry: evolution of milling from pharmaceutical solid form screening to the synthesis of active pharmaceutical ingredients (APIs).

PubMed

Tan, Davin; Loots, Leigh; Friščić, Tomislav

2016-06-14

This overview highlights the emergent area of mechanochemical reactions for making active pharmaceutical ingredients (APIs), and covers the latest advances in the recently established area of mechanochemical screening and synthesis of pharmaceutical solid forms, specifically polymorphs, cocrystals, salts and salt cocrystals. We also provide an overview of the most recent developments in pharmaceutical uses of mechanochemistry, including real-time reaction monitoring, techniques for polymorph control and approaches for continuous manufacture using twin screw extrusion, and more. Most importantly, we show how the overlap of previously unrelated areas of mechanochemical screening for API solid forms, organic synthesis by milling, and mechanochemical screening for molecular recognition, enables the emergence of a new research discipline in which different aspects of pharmaceutical and medicinal chemistry are addressed through mechanochemistry rather than through conventional solution-based routes. The emergence of such medicinal mechanochemistry is likely to have a strong impact on future pharmaceutical and medicinal chemistry, as it offers not only access to materials and reactivity that are sometimes difficult or even impossible to access from solution, but can also provide a general answer to the demands of the pharmaceutical industry for cleaner, safer and efficient synthetic solutions.

The in situ synthesis of PbS nanocrystals from lead(II) n-octylxanthate within a 1,3-diisopropenylbenzene–bisphenol A dimethacrylate sulfur copolymer

PubMed Central

Bear, J. C.; Mayes, A. G.; Parkin, I. P.; O'Brien, P.

2017-01-01

The synthesis of lead sulfide nanocrystals within a solution processable sulfur ‘inverse vulcanization’ polymer thin film matrix was achieved from the in situ thermal decomposition of lead(II) n-octylxanthate, [Pb(S2COOct)2]. The growth of nanocrystals within polymer thin films from single-source precursors offers a faster route to networks of nanocrystals within polymers when compared with ex situ routes. The ‘inverse vulcanization’ sulfur polymer described herein contains a hybrid linker system which demonstrates high solubility in organic solvents, allowing solution processing of the sulfur-based polymer, ideal for the formation of thin films. The process of nanocrystal synthesis within sulfur films was optimized by observing nanocrystal formation by X-ray photoelectron spectroscopy and X-ray diffraction. Examination of the film morphology by scanning electron microscopy showed that beyond a certain precursor concentration the nanocrystals formed were not only within the film but also on the surface suggesting a loading limit within the polymer. We envisage this material could be used as the basis of a new generation of materials where solution processed sulfur polymers act as an alternative to traditional polymers. PMID:28878986

Combined flame and solution synthesis of nanoscale tungsten-oxide and zinc/tin-oxide heterostructures

NASA Astrophysics Data System (ADS)

Dong, Zhizhong; Huo, Di; Kear, Bernard H.; Tse, Stephen D.

2015-12-01

Heterostructures of tungsten-oxide nanowires decorated with zinc/tin-oxide nanostructures are synthesized via a combined flame and solution synthesis approach. Vertically well-aligned tungsten-oxide nanowires are grown on a tungsten substrate by a flame synthesis method. Here, tetragonal WO2.9 nanowires (diameters of 20-50 nm, lengths >10 μm, and coverage density of 109-1010 cm-2) are produced by the vapor-solid mechanism at 1720 K. Various kinds of Zn/Sn-oxide nanostructures are grown or deposited on the WO2.9 nanowires by adjusting the Sn2+ : Zn2+ molar ratio in an aqueous ethylenediamine solution at 65 °C. With WO2.9 nanowires serving as the base structures, sequential growth or deposition on them of hexagonal ZnO nanoplates, Zn2SnO4 nanocubes, and SnO2 nanoparticles are attained for Sn2+ : Zn2+ ratios of 0 : 1, 1 : 10, and 10 : 1, respectively, along with different saturation conditions. High-resolution transmission electron microscopy of the interfaces at the nanoheterojunctions shows abrupt interfaces for ZnO/WO2.9 and Zn2SnO4/WO2.9, despite lattice mismatches of >20%.

Sol-gel type synthesis of Bi.sub.2 (Sr,Ta.sub.2)O.sub.9 using an acetate based system

DOEpatents

Boyle, Timothy J.

1997-01-01

A method of forming a layered-perovskite bismuth-strontium-tantalum oxide (SBT) ferroelectric material is performed by dissolving a bismuth compound in a first solvent to form a first solution, mixing a strontium compound and a tantalum compound to form a binary mixture, dissolving the binary mixture in a second solvent to form a second solution, mixing the first solution with the second solution to form a SBT precursor solution, evaporating the first and second solvents to form a SBT precursor material and subsequently sintering said SBT precursor material in the presence of oxygen.

Sol-gel type synthesis of Bi{sub 2}(Sr,Ta{sub 2})O{sub 9} using an acetate based system

DOEpatents

Boyle, T.J.

1997-11-04

A method of forming a layered-perovskite bismuth-strontium-tantalum oxide (SBT) ferroelectric material is performed by dissolving a bismuth compound in a first solvent to form a first solution, mixing a strontium compound and a tantalum compound to form a binary mixture, dissolving the binary mixture in a second solvent to form a second solution, mixing the first solution with the second solution to form a SBT precursor solution, evaporating the first and second solvents to form a SBT precursor material and subsequently sintering said SBT precursor material in the presence of oxygen. 6 figs.

Synthesis of 4-triazolopyrimidinone nucleotide and its application in synthesis of 5-methylcytosine-containing oligodeoxyribonucleotides.

PubMed Central

Sung, W L

1981-01-01

5'-0-Dimethoxytritylthymidine (2) was phosphorylated and base-modified simultaneously to yield the 4-triazolopyrimidinone nucleotide (3). Coupling between (3) and other common deoxyribonucleotides gave a fully protected nonamer (4). Deblocking under different conditions yielded the nonamer as phosphodiester with concomitant conversion of 4-triazolopyrimidinone to 5-methylcytosine (aqueous ammonia) or thymine (N1,N1,N3,N3-tetramethyl-guanidinium syn-4-nitrobenzaldoximate solution). Images PMID:7312633

Mathematical programming formulations for satellite synthesis

NASA Technical Reports Server (NTRS)

Bhasin, Puneet; Reilly, Charles H.

1987-01-01

The problem of satellite synthesis can be described as optimally allotting locations and sometimes frequencies and polarizations, to communication satellites so that interference from unwanted satellite signals does not exceed a specified threshold. In this report, mathematical programming models and optimization methods are used to solve satellite synthesis problems. A nonlinear programming formulation which is solved using Zoutendijk's method and a gradient search method is described. Nine mixed integer programming models are considered. Results of computer runs with these nine models and five geographically compatible scenarios are presented and evaluated. A heuristic solution procedure is also used to solve two of the models studied. Heuristic solutions to three large synthesis problems are presented. The results of our analysis show that the heuristic performs very well, both in terms of solution quality and solution time, on the two models to which it was applied. It is concluded that the heuristic procedure is the best of the methods considered for solving satellite synthesis problems.

Prebiotic syntheses of purines and pyrimidines

NASA Technical Reports Server (NTRS)

Basile, B.; Oro, J.; Lazcano, A.

1984-01-01

The results of experimental and theoretical investigations of the prebiotic synthesis of purines and pyramidines are surveyed. Topics examined include the synthesis of purines from HCN via 4,5-disubstituted imidazole derivatives in aqueous solutions or liquid NH3, simultaneous formation of amino acids and purines by electron irradiation of CH4-NH3-H2O mixtures, synthesis of pyrimadines from cynoacetylene, energetics, formation of bases under anhydrous or concentrated conditions, formation of bases under dilute conditions, Fischer-Tropsch-type reactions, and the role of activated intermediates. It is pointed out that the precursor compounds have been detected in the interstellar medium, on Titan, and in other solar-system bodies, and that solar-nebula HCN concentrations of the order of 1-10 mM have been estimated on the basis of meteorite measurements.

Scope and Limitations of Fmoc Chemistry SPPS-Based Approaches to the Total Synthesis of Insulin Lispro via Ester Insulin.

PubMed

Dhayalan, Balamurugan; Mandal, Kalyaneswar; Rege, Nischay; Weiss, Michael A; Eitel, Simon H; Meier, Thomas; Schoenleber, Ralph O; Kent, Stephen B H

2017-01-31

We have systematically explored three approaches based on 9-fluorenylmethoxycarbonyl (Fmoc) chemistry solid phase peptide synthesis (SPPS) for the total chemical synthesis of the key depsipeptide intermediate for the efficient total chemical synthesis of insulin. The approaches used were: stepwise Fmoc chemistry SPPS; the "hybrid method", in which maximally protected peptide segments made by Fmoc chemistry SPPS are condensed in solution; and, native chemical ligation using peptide-thioester segments generated by Fmoc chemistry SPPS. A key building block in all three approaches was a Glu[O-β-(Thr)] ester-linked dipeptide equipped with a set of orthogonal protecting groups compatible with Fmoc chemistry SPPS. The most effective method for the preparation of the 51 residue ester-linked polypeptide chain of ester insulin was the use of unprotected peptide-thioester segments, prepared from peptide-hydrazides synthesized by Fmoc chemistry SPPS, and condensed by native chemical ligation. High-resolution X-ray crystallography confirmed the disulfide pairings and three-dimensional structure of synthetic insulin lispro prepared from ester insulin lispro by this route. Further optimization of these pilot studies could yield an efficient total chemical synthesis of insulin lispro (Humalog) based on peptide synthesis by Fmoc chemistry SPPS. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Niobate-based octahedral molecular sieves

DOEpatents

Nenoff, Tina M.; Nyman, May D.

2006-10-17

Niobate-based octahedral molecular sieves having significant activity for multivalent cations and a method for synthesizing such sieves are disclosed. The sieves have a net negatively charged octahedral framework, comprising niobium, oxygen, and octahedrally coordinated lower valence transition metals. The framework can be charge balanced by the occluded alkali cation from the synthesis method. The alkali cation can be exchanged for other contaminant metal ions. The ion-exchanged niobate-based octahedral molecular sieve can be backexchanged in acidic solutions to yield a solution concentrated in the contaminant metal. Alternatively, the ion-exchanged niobate-based octahedral molecular sieve can be thermally converted to a durable perovskite phase waste form.

Niobate-based octahedral molecular sieves

DOEpatents

Nenoff, Tina M.; Nyman, May D.

2003-07-22

Niobate-based octahedral molecular sieves having significant activity for multivalent cations and a method for synthesizing such sieves are disclosed. The sieves have a net negatively charged octahedral framework, comprising niobium, oxygen, and octahedrally coordinated lower valence transition metals. The framework can be charge balanced by the occluded alkali cation from the synthesis method. The alkali cation can be exchanged for other contaminant metal ions. The ion-exchanged niobate-based octahedral molecular sieve can be backexchanged in acidic solutions to yield a solution concentrated in the contaminant metal. Alternatively, the ion-exchanged niobate-based octahedral molecular sieve can be thermally converted to a durable perovskite phase waste form.

Scope & Limitations of Fmoc Chemistry SPPS-Based Approaches to the Total Synthesis of Insulin Lispro via Ester Insulin

PubMed Central

Dhayalan, Balamurugan; Mandal, Kalyaneswar; Rege, Nischay; Weiss, Michael A.; Eitel, Simon H.; Meier, Thomas; Schoenleber, Ralph O.; Kent, Stephen B.H.

2017-01-01

We have systematically explored three approaches based on Fmoc chemistry SPPS for the total chemical synthesis of the key depsipeptide intermediate for the efficient total chemical synthesis of insulin. The approaches used were: stepwise Fmoc chemistry SPPS; the ‘hybrid method’, in which maximally-protected peptide segments made by Fmoc chemistry SPPS are condensed in solution; and, native chemical ligation using peptide-thioester segments generated by Fmoc chemistry SPPS. A key building block in all three approaches was a Glu[Oβ(Thr)] ester-linked dipeptide equipped with a set of orthogonal protecting groups compatible with Fmoc chemistry SPPS. The most effective method for the preparation of the 51 residue ester-linked polypeptide chain of ester insulin was the use of unprotected peptide-thioester segments, prepared from peptide-hydrazides synthesized by Fmoc chemistry SPPS, and condensed by native chemical ligation. High resolution X-ray crystallography confirmed the disulfide pairings and three-dimensional structure of synthetic insulin lispro prepared from ester insulin lispro by this route. Further optimization of these pilot studies should yield an effective total chemical synthesis of insulin lispro (Humalog) based on peptide synthesis by Fmoc chemistry SPPS. PMID:27905149

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

Maxwell, D.P.; Richardson, C.F.

Three mercury measurement techniques were performed on synthesis gas streams before and after an amine-based sulfur removal system. The syngas was sampled using (1) gas impingers containing a nitric acid-hydrogen peroxide solution, (2) coconut-based charcoal sorbent, and (3) an on-line atomic absorption spectrophotometer equipped with a gold amalgamation trap and cold vapor cell. Various impinger solutions were applied upstream of the gold amalgamation trap to remove hydrogen sulfide and isolate oxidized and elemental species of mercury. The results from these three techniques are compared to provide an assessment of these measurement techniques in reducing gas atmospheres.

Synthesis of 1D Bragg gratings by a layer-aggregation method.

PubMed

Capmany, José; Muriel, Miguel A; Sales, Salvador

2007-08-15

We present what we believe to be a novel method for the synthesis of complex 1D (fiber and waveguide) Bragg gratings, which is based on an impedance reconstruction layer aggregation technique. The main advantage brought by the method is the possibility of synthesizing structures containing defects or discontinuities of the size of the local period, a feature that is not possible with prior reported methods. In addition, this enhanced spatial resolution allows the synthesis of very strong fiber Bragg grating devices providing convergent solutions. The method directly renders the refractive index profile n(z) as it does not rely on the coupled-mode theory.

Synthesis of sub-millimeter calcite from aqueous solution

NASA Astrophysics Data System (ADS)

Reimi, M. A.; Morrison, J. M.; Burns, P. C.

2011-12-01

A novel aqueous synthesis that leads to the formation of calcite (CaCO3) crystals, up to 500μm in diameter, will be used to facilitate the study of contaminant transport in aqueous environmental systems. Existing processes tend to be complicated and often yield nanometer-sized or amorphous CaCO3. The synthesis method presented here, which involves slow mixing of concentrated solutions of CaCl2 ¬and (NH4)2CO3, produces single crystals of rhombohedral calcite in 2 to 4 days. Variations on the experimental method, including changes in pH and solution concentration, were explored to optimize the synthesis. Scanning Electron Microscope images show the differences in size and purity observed when the crystals are grown at pH values ranging from 2 to 6. The crystals grown from solutions of pH 2 were large (up to 500 micrometers in diameter) with minimal polycrystalline calcium carbonate, while crystals grown from solutions with pH values beyond 4 were smaller (up to 100 micrometers in diameter) with significant polycrystalline calcium carbonate. The synthesis method, materials characterization, and use in future actinide contaminant studies will be discussed.

Solution-Phase Synthesis of Dipeptides: A Capstone Project That Employs Key Techniques in an Organic Laboratory Course

ERIC Educational Resources Information Center

Marchetti, Louis; DeBoef, Brenton

2015-01-01

A contemporary approach to the synthesis and purification of several UV-active dipeptides has been developed for the second-year organic laboratory. This experiment exposes students to the important technique of solution-phase peptide synthesis and allows an instructor to highlight the parallel between what they are accomplishing in the laboratory…

One-step microwave synthesis of photoluminescent carbon nanoparticles from sodium dextran sulfate water solution

NASA Astrophysics Data System (ADS)

Kokorina, Alina A.; Goryacheva, Irina Y.; Sapelkin, Andrei V.; Sukhorukov, Gleb B.

2018-04-01

Photoluminescent (PL) carbon nanoparticles (CNPs) have been synthesized by one-step microwave irradiation from water solution of sodium dextran sulfate (DSS) as the sole carbon source. Microwave (MW) method is very simple and cheap and it provides fast synthesis of CNPs. We have varied synthesis time for obtaining high luminescent CNPs. The synthesized CNPs exhibit excitation-dependent photoluminescent. Final CNPs water solution has a blue- green luminescence. CNPs have low cytotoxicity, good photostability and can be potentially suitable candidates for bioimaging, analysis or analytical tests.

Step-by-step growth of complex oxide microstructures

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

Datskos, Panos G.; Cullen, David A.; Sharma, Jaswinder K.

The synthesis of complex and hybrid oxide microstructures is of fundamental interest and practical applications. However, the design and synthesis of such structures is a challenging task. A solution-phase process to synthesize complex silica and silica-titania hybrid microstructures was developed by exploiting the emulsion-droplet-based step-by-step growth featuring shape control. Lastly, the strategy is robust and can be extended to the preparation of complex hybrid structures consisting of two or more materials, with each having its own shape.

Step-by-step growth of complex oxide microstructures

DOE PAGES

Datskos, Panos G.; Cullen, David A.; Sharma, Jaswinder K.

2015-06-10

The synthesis of complex and hybrid oxide microstructures is of fundamental interest and practical applications. However, the design and synthesis of such structures is a challenging task. A solution-phase process to synthesize complex silica and silica-titania hybrid microstructures was developed by exploiting the emulsion-droplet-based step-by-step growth featuring shape control. Lastly, the strategy is robust and can be extended to the preparation of complex hybrid structures consisting of two or more materials, with each having its own shape.

Synthesis, Morphological and Electrical Characterization of Solution Processable Low Bandgap Organic Materials

DTIC Science & Technology

2008-12-05

bandgap: 1.98 eV Okamoto, Toshihiro; Senatore, Michelle L.; Ling, Mang-Mang; Mallik , Abhijit B.; Tang, Ming L.; Bao, Zhenan. Synthesis...grant: 1. R.A.B. Devine, M.M. Ling, A. Mallik , M.Roberts, Z. Bao, "X-irradiation Effects on Top Contact, Pentacene Based Field Effect Transistors...Semiconductors: Asymmetric Linear Acenes Containing Sulphur ",J. Am. Chem. Soc., 128, 160002-160003,2006. 3. T. Okamoto, M.L. Senatore, M.M. Ling, A.B. Mallik

Convergent solid-phase and solution approaches in the synthesis of the cysteine-rich Mdm2 RING finger domain.

PubMed

Vasileiou, Zoe; Barlos, Kostas; Gatos, Dimitrios

2009-12-01

The RING finger domain of the Mdm2, located at the C-terminus of the protein, is necessary for regulation of p53, a tumor suppressor protein. The 48-residues long Mdm2 peptide is an important target for studying its interaction with small anticancer drug candidates. For the chemical synthesis of the Mdm2 RING finger domain, the fragment condensation on solid-phase and the fragment condensation in solution were studied. The latter method was performed using either protected or free peptides at the C-terminus as the amino component. Best results were achieved using solution condensation where the N-component was applied with the C-terminal carboxyl group left unprotected. The developed method is well suited for large-scale synthesis of Mdm2 RING finger domain, combining the advantages of both solid-phase and solution synthesis. (c) 2009 European Peptide Society and John Wiley & Sons, Ltd.

Multiple Representations-Based Face Sketch-Photo Synthesis.

PubMed

Peng, Chunlei; Gao, Xinbo; Wang, Nannan; Tao, Dacheng; Li, Xuelong; Li, Jie

2016-11-01

Face sketch-photo synthesis plays an important role in law enforcement and digital entertainment. Most of the existing methods only use pixel intensities as the feature. Since face images can be described using features from multiple aspects, this paper presents a novel multiple representations-based face sketch-photo-synthesis method that adaptively combines multiple representations to represent an image patch. In particular, it combines multiple features from face images processed using multiple filters and deploys Markov networks to exploit the interacting relationships between the neighboring image patches. The proposed framework could be solved using an alternating optimization strategy and it normally converges in only five outer iterations in the experiments. Our experimental results on the Chinese University of Hong Kong (CUHK) face sketch database, celebrity photos, CUHK Face Sketch FERET Database, IIIT-D Viewed Sketch Database, and forensic sketches demonstrate the effectiveness of our method for face sketch-photo synthesis. In addition, cross-database and database-dependent style-synthesis evaluations demonstrate the generalizability of this novel method and suggest promising solutions for face identification in forensic science.

Synthesis of sodium lignosulphonate from oil palm empty fruit bunches's lignin

NASA Astrophysics Data System (ADS)

Prakoso, Nurcahyo Iman; Purwono, Suryo; Rochmadi

2017-03-01

Synthesis of sodium lignosulphonate have been done by using batch method. Optimation of synthesis method was achieved through this study. The study was conducted on the optimation of mass ratio of lignin to the NaHSO3 solution, the concentration of NaHSO3 solution, reaction temperature, and reaction time. Of all the treatments, it was found that the optimum mass ratio of lignin to the NaHSO3 solution, concentration of NaHSO3 solution, reaction temperature, and reaction time respectively, 0.3 M, 0.1 M 97 °C, and the reaction was carried out for 4 hours. Excellent yields and selective products were obtained (90-92%)

Solution-Phase Synthesis of Cesium Lead Halide Perovskite Nanowires.

PubMed

Zhang, Dandan; Eaton, Samuel W; Yu, Yi; Dou, Letian; Yang, Peidong

2015-07-29

Halide perovskites have attracted much attention over the past 5 years as a promising class of materials for optoelectronic applications. However, compared to hybrid organic-inorganic perovskites, the study of their pure inorganic counterparts, like cesium lead halides (CsPbX3), lags far behind. Here, a catalyst-free, solution-phase synthesis of CsPbX3 nanowires (NWs) is reported. These NWs are single-crystalline, with uniform growth direction, and crystallize in the orthorhombic phase. Both CsPbBr3 and CsPbI3 are photoluminescence active, with composition-dependent temperature and self-trapping behavior. These NWs with a well-defined morphology could serve as an ideal platform for the investigation of fundamental properties and the development of future applications in nanoscale optoelectronic devices based on all-inorganic perovskites.

Peritoneal dialysis solution attenuates microvascular leukocyte adhesion induced by nitric oxide synthesis inhibition.

PubMed

White, R; Ram, S

1996-01-01

In the mesenteric microcirculation, inhibition of nitric oxide (NO) synthesis results in an inflammatory response through increased leukocyte adherence to the microvascular postcapillary venular endothelium. Recent studies have demonstrated that elevated concentrations of endogenous NO synthesis inhibitors are present in renal failure. How peritoneal dialysis solutions may affect leukocyte-endothelial interactions during inflammation induced by NO synthesis inhibition has been previously unknown. Using in vivo intravital microscopy of the rat mesenteric postcapillary venules, microvascular leukocyte adherence was quantitated during baseline conditions in which the mesentery was superfused with a buffer solution, followed by the superfusion of a NO synthesis inhibitor NG-nitro-L-ARGININE methyl ester (L-NAME) added to the buffer, followed by 4.25% Dianeal (4.25% D). When compared to baseline, L-NAME increased the mean number of adherent leukocytes by fivefold (2.2 +/- 0.9 vs 11.6 +/- 3.6 leukocytes/100 microns venule/10 min, p < 0.05), while 4.25% D quickly reversed the L-NAME-induced inflammatory response, returning the number of adherent leukocytes back to baseline values (11.6 +/- 3.6 vs 2.4 +/- 1.3 leukocytes/100 microns venule/ 10 min, p < 0.05). These results confirm that NO synthesis inhibition induces inflammation in mesenteric postcapillary venules. Superfusion of 4.25% D reverses leukocyte adhesion induced by NO synthesis inhibition. Thus, a standard peritoneal dialysis solution (4.25% D) reverses the leukocyte-adhesive effects of NO synthesis inhibition in the mesenteric microcirculation.

Optimization of low cost, non toxic, earth abundant p-type Cu2SnS3 thin film for Photovoltaic application

NASA Astrophysics Data System (ADS)

Chaudhari, J. J.; Patel, S.; Joshi, U. S.

2016-09-01

Cu2SnS3 (CTS) is one of promising candidate as an absorber material for thin film solar cell. Because of relatively higher prize of Indium and hazardous environmental impact of processing of Gallium, CTS is suitable alternative candidate to Cu2SnS3 (CIGS) based solar cell as its constituent elements such as copper, tin and sulphur are abundantly available in earth's crust. CTS is ternary semiconductor and its energy band gap is 1.5eV, which is perfectly matched with solar energy spectrum for maximum transfer of solar energy into electrical energy through photovoltaic action. The primary methods for the synthesis of CTS are Thermal evaporation, electrochemical, sputtering and wet chemical methods. Here in this paper we have optimized a low cost non-vacuum solution process method for the synthesis of CTS without any external sulfurization. The X-ray diffraction studies showed the formation of phase with the peaks corresponding to (112), (220) and (312) planes. Chemical Solution Deposition (CSD) for the synthesis of CTS is suitable for large area deposition and it includes several routes like solvothermal methods, direct liquid coating and nano ink based technique. The metal Chloride salts and thiourea is used as a source of sulphur to synthesize CTS solution and homogeneous thin films of CTS deposited on glass substrate using spin coating method. Use of abrasive solvent like hydrazine and hydrogen sulphide gas which are used to synthesize CTS thin film have detrimental effect on environment, we report eco friendly solvent based approach to synthesize CTS at low temperature 200 °C.

Synthesis and characterization of an effective organic/inorganic hybrid green corrosion inhibitive complex based on zinc acetate/Urtica Dioica

NASA Astrophysics Data System (ADS)

Salehi, E.; Naderi, Reza; Ramezanzadeh, B.

2017-02-01

This study aims at synthesis and characterization of an effective corrosion inhibitive complex based on zinc acetate/Urtica Dioica (ZnA-U.D) for corrosion protection of mild steel in chloride solution. The chemical structure and morphology of the complex were characterized by Fourier transform infrared spectroscopy (FT-IR), UV-vis, thermal gravimetric analysis (TGA), X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM). The corrosion protection performance of the mild steel samples dipped in 3.5 wt.% NaCl solutions with and without ZnA-U.D extract was investigated by visual observations, open circuit potential (OCP) measurements, electrochemical impedance spectroscopy (EIS) and polarization test. Results revealed that the ZnA successfully chelated with organic inhibitive compounds (i.e Quercetin, Quinic acid, Caffeic acid, Hystamine and Serotonin) present in the U.D extract. The electrochemical measurements revealed the effective inhibition action of ZnA-U.D complex in the sodium chloride solution on the mild steel. The synergistic effect between Zn2+ and organic compounds present in the U.D extract resulted in protective film deposition on the steel surface, which was proved by SEM and XPS analyses.

Determination of epichlorohydrin and 1,3-dichloro-2-propanol in synthesis of cationic etherifying reagent by headspace gas chromatography.

PubMed

Tao, Zheng-Yi; Chai, Xin-Sheng; Wu, Shu-Bin

2011-09-16

This study demonstrates a headspace gas chromatographic(HS-GC) technique for the determination of residual epichlorohydrin (ECH) and generated 1,3-dichloro-2-propanol (DCP) in synthesis process of 3-chloro-2-hydroxypropyltrimethylammonium chloride (CHTAC). By a weight-based sampling method, coupled with significant dilution in 15.8% sodium sulfate and 0.1% silver nitrate mixed solution rapidly, the sample for HS-GC analysis is prepared. Based on the reaction stoichiometry, the conversion (R) of CHTAC during the synthesis process can be calculated from sampling weight and GC peak area. The results showed that the method has a good measurement precision (RSD<2.5%) and accuracy (recovery=101-104%) for the quantification of both ECH and DCP in the process samples. The present method is simple and accurate, which can be used for the efficient determination of the CHTAC conversion in the synthesis research. Copyright © 2011 Elsevier B.V. All rights reserved.

Chemical synthesis of the precursor molecule of the Aequorea green fluorescent protein, subsequent folding, and development of fluorescence

PubMed Central

Nishiuchi, Yuji; Inui, Tatsuya; Nishio, Hideki; Bódi, József; Kimura, Terutoshi; Tsuji, Frederick I.; Sakakibara, Shumpei

1998-01-01

The present paper describes the total chemical synthesis of the precursor molecule of the Aequorea green fluorescent protein (GFP). The molecule is made up of 238 amino acid residues in a single polypeptide chain and is nonfluorescent. To carry out the synthesis, a procedure, first described in 1981 for the synthesis of complex peptides, was used. The procedure is based on performing segment condensation reactions in solution while providing maximum protection to the segment. The effectiveness of the procedure has been demonstrated by the synthesis of various biologically active peptides and small proteins, such as human angiogenin, a 123-residue protein analogue of ribonuclease A, human midkine, a 121-residue protein, and pleiotrophin, a 136-residue protein analogue of midkine. The GFP precursor molecule was synthesized from 26 fully protected segments in solution, and the final 238-residue peptide was treated with anhydrous hydrogen fluoride to obtain the precursor molecule of GFP containing two Cys(acetamidomethyl) residues. After removal of the acetamidomethyl groups, the product was dissolved in 0.1 M Tris⋅HCl buffer (pH 8.0) in the presence of DTT. After several hours at room temperature, the solution began to emit a green fluorescence (λmax = 509 nm) under near-UV light. Both fluorescence excitation and fluorescence emission spectra were measured and were found to have the same shape and maxima as those reported for native GFP. The present results demonstrate the utility of the segment condensation procedure in synthesizing large protein molecules such as GFP. The result also provides evidence that the formation of the chromophore in GFP is not dependent on any external cofactor. PMID:9811837

Sunlight mediated synthesis of silver nanoparticles by a novel actinobacterium (Sinomonas mesophila MPKL 26) and its antimicrobial activity against multi drug resistant Staphylococcus aureus.

PubMed

Manikprabhu, Deene; Cheng, Juan; Chen, Wei; Sunkara, Anil Kumar; Mane, Sunilkumar B; Kumar, Ram; das, Mousumi; N Hozzein, Wael; Duan, Yan-Qing; Li, Wen-Jun

2016-05-01

Synthesis of silver nanoparticles using microorganism are many, but there are only scanty reports using actinobacteria. In the present study, the actinobacterium of the genus Sinomonas was reported to synthesis silver nanoparticles for the first time. A photo-irradiation based method was developed for the synthesis of silver nanoparticles, which includes two day old cultural supernatant of novel species Sinomonas mesophila MPKL 26 and silver nitrate solution, exposed to sunlight. The preliminary synthesis of silver nanoparticles was noted by the color change of the solution from colorless to brown; the synthesis was further confirmed using UV-visible spectroscopy which shows a peak between 400 and 450nm. Spherical shape silver nanoparticles of size range 4-50nm were synthesized, which were characterized using transmission electron microscopy. The Fourier transform infrared spectroscopy result indicates that, the metabolite produced by the novel species S. mesophila MPKL 26 was the probable reducing/capping agent involved in the synthesis of silver nanoparticles. The synthesized silver nanoparticles maintained consistent shape with respect to different time periods. The synthesized silver nanoparticles were evaluated for the antimicrobial activity against multi drug resistant Staphylococcus aureus which show good antimicrobial activity. The method developed for synthesis is easy, requires less time (20min) and produces spherical shape nanoparticles of size as small as 4nm, having good antimicrobial activity. Hence, our study enlarges the scope of actinobacteria for the rapid biosynthesis of silver nanoparticles and can be used in formulating remedies for multi drug resistant S. aureus. Copyright © 2016 Elsevier B.V. All rights reserved.

Perspective: Toward "synthesis by design": Exploring atomic correlations during inorganic materials synthesis

NASA Astrophysics Data System (ADS)

Soderholm, L.; Mitchell, J. F.

2016-05-01

Synthesis of inorganic extended solids is a critical starting point from which real-world functional materials and their consequent technologies originate. However, unlike the rich mechanistic foundation of organic synthesis, with its underlying rules of assembly (e.g., functional groups and their reactivities), the synthesis of inorganic materials lacks an underpinning of such robust organizing principles. In the latter case, any such rules must account for the diversity of chemical species and bonding motifs inherent to inorganic materials and the potential impact of mass transport on kinetics, among other considerations. Without such assembly rules, there is less understanding, less predictive power, and ultimately less control of properties. Despite such hurdles, developing a mechanistic understanding for synthesis of inorganic extended solids would dramatically impact the range of new material discoveries and resulting new functionalities, warranting a broad call to explore what is possible. Here we discuss our recent approaches toward a mechanistic framework for the synthesis of bulk inorganic extended solids, in which either embryonic atomic correlations or fully developed phases in solutions or melts can be identified and tracked during product selection and crystallization. The approach hinges on the application of high-energy x-rays, with their penetrating power and large Q-range, to explore reaction pathways in situ. We illustrate this process using two examples: directed assembly of Zr clusters in aqueous solution and total phase awareness during crystallization from K-Cu-S melts. These examples provide a glimpse of what we see as a larger vision, in which large scale simulations, data-driven science, and in situ studies of atomic correlations combine to accelerate materials discovery and synthesis, based on the assembly of well-defined, prenucleated atomic correlations.

Perspective: Toward “synthesis by design”: Exploring atomic correlations during inorganic materials synthesis

DOE PAGES

Soderholm, L.; Mitchell, J. F.

2016-05-26

Synthesis of inorganic extended solids is a critical starting point from which real-world functional materials and their consequent technologies originate. However, unlike the rich mechanistic foundation of organic synthesis, with its underlying rules of assembly (e.g., functional groups and their reactivities), the synthesis of inorganic materials lacks an underpinning of such robust organizing principles. In the latter case, any such rules must account for the diversity of chemical species and bonding motifs inherent to inorganic materials and the potential impact of mass transport on kinetics, among other considerations. Without such assembly rules, there is less understanding, less predictive power, andmore » ultimately less control of properties. Despite such hurdles, developing a mechanistic understanding for synthesis of inorganic extended solids would dramatically impact the range of new material discoveries and resulting new functionalities, warranting a broad call to explore what is possible. Here we discuss our recent approaches toward a mechanistic framework for the synthesis of bulk inorganic extended solids, in which either embryonic atomic correlations or fully developed phases in solutions or melts can be identified and tracked during product selection and crystallization. The approach hinges on the application of high-energy x-rays, with their penetrating power and large Q-range, to explore reaction pathways in situ. We illustrate this process using two examples: directed assembly of Zr clusters in aqueous solution and total phase awareness during crystallization from K–Cu–S melts. These examples provide a glimpse of what we see as a larger vision, in which large scale simulations, data-driven science, and in situ studies of atomic correlations combine to accelerate materials discovery and synthesis, based on the assembly of well-defined, prenucleated atomic correlations.« less

Plasma synthesis of lithium based intercalation powders for solid polymer electrolyte batteries

DOEpatents

Kong, Peter C [Idaho Falls, ID; Pink, Robert J [Pocatello, ID; Nelson, Lee O [Idaho Falls, ID

2005-01-04

The invention relates to a process for preparing lithium intercalation compounds by plasma reaction comprising the steps of: forming a feed solution by mixing lithium nitrate or lithium hydroxide or lithium oxide and the required metal nitrate or metal hydroxide or metal oxide and between 10-50% alcohol by weight; mixing the feed solution with O.sub.2 gas wherein the O.sub.2 gas atomizes the feed solution into fine reactant droplets, inserting the atomized feed solution into a plasma reactor to form an intercalation powder; and if desired, heating the resulting powder to from a very pure single phase product.

Triphenylamine-Based Push–Pull Molecule for Photovoltaic Applications: From Synthesis to Ultrafast Device Photophysics

PubMed Central

2017-01-01

Small push–pull molecules attract much attention as prospective donor materials for organic solar cells (OSCs). By chemical engineering, it is possible to combine a number of attractive properties such as broad absorption, efficient charge separation, and vacuum and solution processabilities in a single molecule. Here we report the synthesis and early time photophysics of such a molecule, TPA-2T-DCV-Me, based on the triphenylamine (TPA) donor core and dicyanovinyl (DCV) acceptor end group connected by a thiophene bridge. Using time-resolved photoinduced absorption and photoluminescence, we demonstrate that in blends with [70]PCBM the molecule works both as an electron donor and hole acceptor, thereby allowing for two independent channels of charge generation. The charge-generation process is followed by the recombination of interfacial charge transfer states that takes place on the subnanosecond time scale as revealed by time-resolved photoluminescence and nongeminate recombination as follows from the OSC performance. Our findings demonstrate the potential of TPA-DCV-based molecules as donor materials for both solution-processed and vacuum-deposited OSCs. PMID:28413568

Study of Colloidal Gold Synthesis Using Turkevich Method

NASA Astrophysics Data System (ADS)

Rohiman, Asep; Anshori, Isa; Surawijaya, Akhmadi; Idris, Irman

2011-12-01

The synthesis of colloidal gold or Au-nanoparticles (Au-NPs) by reduction of chloroauric acid (HAuCl4) with sodium citrate was done using Turkevich method. We prepare HAuCl4 solution by dissolving gold wires (99.99%) into aqua regia solution. To initiate the Au-NPs synthesis 0.17 ml of 1 % chloroauric acid solution was heated to the boiling point and then 10 ml of 1 % sodium citrate was added to the boiling solution with a constant stirring in order to maintain a homogenous solution. A color of faint gray was observed in the solution approximately one minute and in a period of 2-3 minutes later, it further darkened to deep wine and red color. It showed that the gold solution has reduced to Au-NPs. The effect of process temperature on the size of Au-NPs prepared by sodium citrate reduction has also been investigated. With increasing temperature of Au-NPs synthesis, smaller-size Au-NPs were obtained. The higher temperatures shorten the time needed to achieve activation energy for reduction process. The resulting Au-NPs has been characterized by scanning Electron Microscope (SEM), showing the size of Au-NPs average diameter is ˜20-27 nm. The resulting colloidal gold will be used as catalyst for Si nanowires growth using VLS method.

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

Nurmikko, Arto V

Synthesis of semiconductor nanomaterials by low-cost, solution-based methods is shown to lead to new classes of thin film light emitting materials. These materials have been integrated to demonstrative compact laser device testbeds to illustrate their potential for coherent emitters across the visible spectrum to disrupt established photonics technologies, particularly semiconductor lasers?

Carbohydrate-Assisted Combustion Synthesis To Realize High-Performance Oxide Transistors.

PubMed

Wang, Binghao; Zeng, Li; Huang, Wei; Melkonyan, Ferdinand S; Sheets, William C; Chi, Lifeng; Bedzyk, Michael J; Marks, Tobin J; Facchetti, Antonio

2016-06-08

Owing to high carrier mobilities, good environmental/thermal stability, excellent optical transparency, and compatibility with solution processing, thin-film transistors (TFTs) based on amorphous metal oxide semiconductors (AOSs) are promising alternatives to those based on amorphous silicon (a-Si:H) and low-temperature (<600 °C) poly-silicon (LTPS). However, solution-processed display-relevant indium-gallium-tin-oxide (IGZO) TFTs suffer from low carrier mobilities and/or inferior bias-stress stability versus their sputtered counterparts. Here we report that three types of environmentally benign carbohydrates (sorbitol, sucrose, and glucose) serve as especially efficient fuels for IGZO film combustion synthesis to yield high-performance TFTs. The results indicate that these carbohydrates assist the combustion process by lowering the ignition threshold temperature and, for optimal stoichiometries, enhancing the reaction enthalpy. IGZO TFT mobilities are increased to >8 cm(2) V(-1) s(-1) on SiO2/Si gate dielectrics with significantly improved bias-stress stability. The first correlations between precursor combustion enthalpy and a-MO densification/charge transport are established.

Facile synthesis of "green" gold nanocrystals using cynarin in an aqueous solution

NASA Astrophysics Data System (ADS)

Katircioğlu, Zeynep; Şakalak, Hüseyin; Ulaşan, Mehmet; Gören, Ahmet Ceyhan; Yavuz, Mustafa Selman

2014-11-01

Herein we describe a water-based protocol that generates Au nanoparticles (AuNPs) by mixing aqueous solutions of HAuCl4 and cynarin (a natural product extract from artichoke leaf). Based on the observations from 1H NMR spectrum of AuNPs, a polyol oxidation mechanism by metal ions which eventually results in AuNPs formation, is proposed. Basically, the aromatic alcohol groups (1,2-benzenediol) of cynarin are oxidized to α-hydroxy ketone intermediate product, and then further oxidized to the vicinal diketone final product while the Au3+ ions are reduced to its atomic form (Au0) which leads the generation of Au nanoparticles. This new protocol has also been employed to prepare multiply twinned Pd nanoparticles and Ag cubical aggregates. Due to exclusion of organic solvent, surfactant, or stabilizer for all these synthesis, this protocol may provide a simple, versatile, and environmentally benign route to fabricate noble-metal nanoparticles having various compositions and morphologies.

Sound field reproduction as an equivalent acoustical scattering problem.

PubMed

Fazi, Filippo Maria; Nelson, Philip A

2013-11-01

Given a continuous distribution of acoustic sources, the determination of the source strength that ensures the synthesis of a desired sound field is shown to be identical to the solution of an equivalent acoustic scattering problem. The paper begins with the presentation of the general theory that underpins sound field reproduction with secondary sources continuously arranged on the boundary of the reproduction region. The process of reproduction by a continuous source distribution is modeled by means of an integral operator (the single layer potential). It is then shown how the solution of the sound reproduction problem corresponds to that of an equivalent scattering problem. Analytical solutions are computed for two specific instances of this problem, involving, respectively, the use of a secondary source distribution in spherical and planar geometries. The results are shown to be the same as those obtained with analyses based on High Order Ambisonics and Wave Field Synthesis, respectively, thus bringing to light a fundamental analogy between these two methods of sound reproduction. Finally, it is shown how the physical optics (Kirchhoff) approximation enables the derivation of a high-frequency simplification for the problem under consideration, this in turn being related to the secondary source selection criterion reported in the literature on Wave Field Synthesis.

Broadcasting satellite service synthesis using gradient and cyclic coordinate search procedures

NASA Technical Reports Server (NTRS)

Reilly, C. H.; Mount-Campbell, C. A.; Gonsalvez, D. J.; Martin, C. H.; Levis, C. A.; Wang, C. W.

1986-01-01

Two search techniques are considered for solving satellite synthesis problems. Neither is likely to find a globally optimal solution. In order to determine which method performs better and what factors affect their performance, we design an experiment and solve the same problem under a variety of starting solution configuration-algorithm combinations. Since there is no randomization in the experiment, we present results of practical, rather than statistical, significance. Our implementation of a cyclic coordinate search procedure clearly finds better synthesis solutions than our implementation of a gradient search procedure does with our objective of maximizing the minimum C/I ratio computed at test points on the perimeters of the intended service areas. The length of the available orbital arc and the configuration of the starting solution are shown to affect the quality of the solutions found.

Broadcasting satellite service synthesis using gradient and cyclic coordinate search procedures

NASA Technical Reports Server (NTRS)

Reilly, C. H.; Mount-Campbell, C. A.; Gonsalvez, D. J.; Martin, C. H.; Levis, C. A.

1986-01-01

Two search techniques are considered for solving satellite synthesis problems. Neither is likely to find a globally optimal solution. In order to determine which method performs better and what factors affect their performance, an experiment is designed and the same problem is solved under a variety of starting solution configuration-algorithm combinations. Since there is no randomization in the experiment, results of practical, rather than statistical, significance are presented. Implementation of a cyclic coordinate search procedure clearly finds better synthesis solutions than implementation of a gradient search procedure does with the objective of maximizing the minimum C/I ratio computed at test points on the perimeters of the intended service areas. The length of the available orbital arc and the configuration of the starting solution are shown to affect the quality of the solutions found.

Controlled synthesis of titania using water-soluble titanium complexes: A review

NASA Astrophysics Data System (ADS)

Truong, Quang Duc; Dien, Luong Xuan; Vo, Dai-Viet N.; Le, Thanh Son

2017-07-01

The development of human society has led to the increase in energy and resources consumption as well as the arising problems of environmental damage and the toxicity to the human health. The development of novel synthesis method which tolerates utilization of toxic solvents and chemicals would fulfill the demand of the society for safer, softer, and environmental friendly technologies. For the past decades, a remarkable progress has been attained in the development of new water-soluble titanium complexes (WSTC) and their use for the synthesis of nanocrystalline titanium dioxide materials by aqueous solution-based approaches. The progress of synthesis of nanocrystalline titanium dioxide using such WSTCs is reviewed in this work. The key structural features responsible for the successfully controlled synthesis of TiO2 are discussed to provide guidelines for the morphology-controlled synthesis. Finally, this review ends with a summary and some perspectives on the challenges as well as new directions in this fascinating research.

Pyrrole-Imidazole Polyamides: Manual Solid-Phase Synthesis.

PubMed

Pauff, Steven M; Fallows, Andrew J; Mackay, Simon P; Su, Wu; Cullis, Paul M; Burley, Glenn A

2015-12-01

Pyrrole-imidazole polyamides (PAs) are a family of DNA-binding peptides that bind in the minor groove of double-stranded DNA (dsDNA) in a sequence-selective, programmable fashion. This protocol describes a detailed manual procedure for the solid-phase synthesis of this family of compounds. The protocol entails solution-phase synthesis of the Boc-protected pyrrole (Py) and imidazole (Im) carboxylic acid building blocks. This unit also describes the importance of choosing the appropriate condensing agent to form the amide linkages between each building block. Finally, a monomeric coupling protocol and a fragment-based approach are described that delivers PAs in 13% to 30% yield in 8 days. Copyright © 2015 John Wiley & Sons, Inc.

Comparison of the solid-phase fragment condensation and phase-change approaches in the synthesis of salmon I calcitonin.

PubMed

Gatos, D; Tzavara, C

2001-02-01

Salmon I calcitonin was synthesized using both phase-change and conventional solid-phase fragment condensation (SPFC) approaches, utilizing the Rink amide linker (Fmoc-amido-2,4-dimethoxybenzyl-4-phenoxyacetic acid) combined with 2-chlorotrityl resin and the Fmoc/tBu(Trt)-based protection scheme. Phase-change synthesis, performed by the selective detachment of the fully protected C-terminal 22-mer peptide-linker from the resin and subsequent condensation in solution with the N-terminal 1-10 fragment, gave a product of slightly less purity (85 vs. 92%) than the corresponding synthesis on the solid-phase. In both cases salmon I calcitonin was easily obtained in high purity.

Synthesis of Ge-nanoparticles in organic solution

NASA Astrophysics Data System (ADS)

Pugsley, Andrew James

Much interest is focused on the synthesis of semiconductor particles from organic solution, in order to provide luminescent tracers for biological assays. However, group IV semiconductors have been largely neglected be cause of the lack of suitable nanoparticle formation reactions by solution-phase chemistries. A potentially useful new route to solution-based synthesis of nanocrystalline-Si,Ge involves the reaction between Zintl phases (NaSi, Mg 2Ge) that formally contain anionic semiconducting group species (Si-, Ge4-) and liquid phase SiCU, GeCU, etc. Luminescent nanoparticles formed by these reactions in organic solvents (e.g. diglyme) have been decribed in work from the Kauzlarich group at UC Davis (California, USA). The aim of this project has been to characterise the structural chemistry and luminescent properties of the products of the reaction, as well as following the course of the reaction in situ via synchrotron measurements. The product of the reaction has been characterised by TEM and x-ray absorption spectroscopy as well as other techniques. In order to analyse the x-ray absorption spectroscopy data, a number of model compounds have been studied, including the precursor material which was previously uncharacterised by this technique. An in situ reaction cell has been designed and built and used at a number of synchrotron beamlines to follow the course of the reaction. It has been found that the presence of even low concentrations of water can greatly affect the formation reaction, this is described herein.

Sequential-Optimization-Based Framework for Robust Modeling and Design of Heterogeneous Catalytic Systems

DOE PAGES

Rangarajan, Srinivas; Maravelias, Christos T.; Mavrikakis, Manos

2017-11-09

Here, we present a general optimization-based framework for (i) ab initio and experimental data driven mechanistic modeling and (ii) optimal catalyst design of heterogeneous catalytic systems. Both cases are formulated as a nonlinear optimization problem that is subject to a mean-field microkinetic model and thermodynamic consistency requirements as constraints, for which we seek sparse solutions through a ridge (L 2 regularization) penalty. The solution procedure involves an iterative sequence of forward simulation of the differential algebraic equations pertaining to the microkinetic model using a numerical tool capable of handling stiff systems, sensitivity calculations using linear algebra, and gradient-based nonlinear optimization.more » A multistart approach is used to explore the solution space, and a hierarchical clustering procedure is implemented for statistically classifying potentially competing solutions. An example of methanol synthesis through hydrogenation of CO and CO 2 on a Cu-based catalyst is used to illustrate the framework. The framework is fast, is robust, and can be used to comprehensively explore the model solution and design space of any heterogeneous catalytic system.« less

Sequential-Optimization-Based Framework for Robust Modeling and Design of Heterogeneous Catalytic Systems

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

Rangarajan, Srinivas; Maravelias, Christos T.; Mavrikakis, Manos

Here, we present a general optimization-based framework for (i) ab initio and experimental data driven mechanistic modeling and (ii) optimal catalyst design of heterogeneous catalytic systems. Both cases are formulated as a nonlinear optimization problem that is subject to a mean-field microkinetic model and thermodynamic consistency requirements as constraints, for which we seek sparse solutions through a ridge (L 2 regularization) penalty. The solution procedure involves an iterative sequence of forward simulation of the differential algebraic equations pertaining to the microkinetic model using a numerical tool capable of handling stiff systems, sensitivity calculations using linear algebra, and gradient-based nonlinear optimization.more » A multistart approach is used to explore the solution space, and a hierarchical clustering procedure is implemented for statistically classifying potentially competing solutions. An example of methanol synthesis through hydrogenation of CO and CO 2 on a Cu-based catalyst is used to illustrate the framework. The framework is fast, is robust, and can be used to comprehensively explore the model solution and design space of any heterogeneous catalytic system.« less

Novel salicylic acid-oriented thiourea-type receptors as colorimetric chemosensor: Synthesis, characterizations and selective naked-eye recognition properties

NASA Astrophysics Data System (ADS)

Li, Shaowei; Cao, Xiufang; Chen, Changshui; Ke, Shaoyong

2012-10-01

Based on the salicylic acid backbone, three highly sensitive and selective colorimetric chemosensors with an acylthiourea binding unit have been designed, synthesized and characterized. These chemosensors have been utilized for selective recognition of fluoride anions in dry DMSO solution by typical spectroscopic titration techniques. Furthermore, the obtained chemosensors AR1-3 have shown naked-eye sensitivity for detection of biologically important fluoride ion over other anions in solution.

Conversion of Carbon Dioxide into Ethanol by Electrochemical Synthesis Method Using Cu-Zn Electrode

NASA Astrophysics Data System (ADS)

Riyanto; Ramadan, S.; Fariduddin, S.; Aminudin, A. R.; Hayatri, A. K.

2018-01-01

Research on conversion of carbon dioxide into ethanol has been done. The conversion process is carried out in a sodium bicarbonate electrolyte solution in an electrochemical synthesis reactor. As cathode was used Cu-Zn, while as anode carbon was utilized. Variations of voltage, concentration of sodium bicarbonate electrolyte solution and time of electrolysis were performed to determine the optimum conditions to convert carbon dioxide into ethanol. Sample of the electrochemical synthesis process was analyzed by gas chromatography. From the result, it is found that the optimum conditions of the electrochemical synthesis process of carbon dioxide conversion into ethanol are voltage, concentration of sodium bicarbonate electrolyte solution and time of electrolysis are 3 volts, 0.4 M and 90 minutes with the ethanol concentration of 10.44%.

FOURTH SEMINAR TO THE MEMORY OF D.N. KLYSHKO: Algebraic solution of the synthesis problem for coded sequences

NASA Astrophysics Data System (ADS)

Leukhin, Anatolii N.

2005-08-01

The algebraic solution of a 'complex' problem of synthesis of phase-coded (PC) sequences with the zero level of side lobes of the cyclic autocorrelation function (ACF) is proposed. It is shown that the solution of the synthesis problem is connected with the existence of difference sets for a given code dimension. The problem of estimating the number of possible code combinations for a given code dimension is solved. It is pointed out that the problem of synthesis of PC sequences is related to the fundamental problems of discrete mathematics and, first of all, to a number of combinatorial problems, which can be solved, as the number factorisation problem, by algebraic methods by using the theory of Galois fields and groups.

Recycling of surfactant template in mesoporous MCM-41 synthesis

NASA Astrophysics Data System (ADS)

Lai, J. Y.; Twaiq, F.; Ngu, L. H.

2017-06-01

The recycling of surfactant template is investigated through the reuse of the surfactant template in the mesoporous MCM-41 synthesis process. In the synthesis of MCM-41, tetraethylorthosilicate (TEOS) solution in water was utilized as the silica source while hexadecyltrimethylammonium bromide (CTAB) solution in ethyl alcohol was used as a surfactant template. The synthesized gel is formed thoroughly by mixing the two solutions under acid conditions with a pH value of 0.5 for 1 hour and kept for crystallization for 48 hours. The as-synthesized MCM-41 powder is recovered by filtration while the filtrate (mother liquor) was then reused for the second synthesis cycle. The synthesis procedure was repeated till no further solid product was formed. The synthesized gel was not produced in the unifying solution in the fifth cycle of MCM-41 synthesis. The quality of the calcined MCM-41 powder produced in each synthesis cycle was evaluated by calculating the amount of MCM-41 produced and the surface area of the powder product. The result showed that 1.28, 0.37, 1.64, 1.90 and 0.037 g were obtained in the 1st, 2nd, 3rd, 4th and 5th synthesis cycle, respectively. The surface area of the powder produced was found to be 1170, 916, 728, and 508 m2/g for 1st, 2nd, 3rd and 4th respectively. The concentration of the surfactant template has reached value lower than the critical micelle concentration (CMC) and remained constant after the 4th cycle. There was no further formation of gel due to low availability in the interaction between silicate anions and surfactant cations when the amount of TEOS was fixed for every synthesis cycle.

Prebiotic Amino Acid Thioester Synthesis: Thiol-Dependent Amino Acid Synthesis from Formose substrates (Formaldehyde and Glycolaldehyde) and Ammonia

NASA Technical Reports Server (NTRS)

Weber, Arthur L.

1998-01-01

Formaldehyde and glycolaldehyde (substrates of the formose autocatalytic cycle) were shown to react with ammonia yielding alanine and homoserine under mild aqueous conditions in the presence of thiol catalysts. Since similar reactions carried out without ammonia yielded alpha-hydroxy acid thioesters, the thiol-dependent synthesis of alanine and homoserine is presumed to occur via amino acid thioesters-intermediates capable of forming peptides. A pH 5.2 solution of 20 mM formaldehyde, 20 mM glycolaldehyde, 20 mM ammonium chloride, 23 mM 3-mercaptopropionic acid, and 23 mM acetic acid that reacted for 35 days at 40 C yielded (based on initial formaldehyde) 1.8% alanine and 0.08% homoserine. In the absence of thiol catalyst, the synthesis of alanine and homoserine was negligible. Alanine synthesis required both formaldehyde and glycolaldehyde, but homoserine synthesis required only glycolaldehyde. At 25 days the efficiency of alanine synthesis calculated from the ratio of alanine synthesized to formaldehyde reacted was 2.1%, and the yield (based on initial formaldehyde) of triose and tetrose intermediates involved in alanine and homoserine synthesis was 0.3 and 2.1%, respectively. Alanine synthesis was also seen in similar reactions containing only 10 mM each of aldehyde substrates, ammonia, and thiol. The prebiotic significance of these reactions that use the formose reaction to generate sugar intermediates that are converted to reactive amino acid thioesters is discussed.

Synthesis of Energetic Materials by Rapid Expansion of a Supercritical Solution into Aqueous Solution (RESS-AS) Process

DTIC Science & Technology

2010-12-02

1366-1373, (2005). 16. Young, T . J ., Mawson , S., Johnston, K. P., Henriksen, I. B., Pace, G. W., and Mishra, A. K., Rapid Expansion from...Synthesis of Energetic Materials by Rapid Expansion of a Supercritical Solution into Aqueous Solution (RESS-AS) Process* J . T . Essel, A. C...Cortopassi, K. K. Kuo, J . H. Adair, and C. G. Leh The Pennsylvania State University University Park, PA 16802 USA T . M. Klapötke Ludwig Maximilian

On orbital allotments for geostationary satellites

NASA Technical Reports Server (NTRS)

Gonsalvez, David J. A.; Reilly, Charles H.; Mount-Campbell, Clark A.

1986-01-01

The following satellite synthesis problem is addressed: communication satellites are to be allotted positions on the geostationary arc so that interference does not exceed a given acceptable level by enforcing conservative pairwise satellite separation. A desired location is specified for each satellite, and the objective is to minimize the sum of the deviations between the satellites' prescribed and desired locations. Two mixed integer programming models for the satellite synthesis problem are presented. Four solution strategies, branch-and-bound, Benders' decomposition, linear programming with restricted basis entry, and a switching heuristic, are used to find solutions to example synthesis problems. Computational results indicate the switching algorithm yields solutions of good quality in reasonable execution times when compared to the other solution methods. It is demonstrated that the switching algorithm can be applied to synthesis problems with the objective of minimizing the largest deviation between a prescribed location and the corresponding desired location. Furthermore, it is shown that the switching heuristic can use no conservative, location-dependent satellite separations in order to satisfy interference criteria.

High-Density Magnetic Recording and Integrated Magneto-Optics: Materials and Devices; Symposium Held in San Francisco, California, on April 12-16 1998

DTIC Science & Technology

1998-04-01

Kido •Solution Flow System for Hydrothermal -Electrochemical Synthesis : New Opportunities for Multilayered Oxide Films 639 VI. Suchanek, T...FLOW SYSTEM FOR HYDROTHERMAL -ELECTROCHEMICAL SYNTHESIS : NEW OPPORTUNITIES FOR MULTTLAYERED OXIDE FILMS W. SUCHANEK, T. WATANABE, B. SAKURAI, M...ABSTRACT A solution flow system for hydrothermal -electrochemical synthesis has been constructed in our laboratory. This equipment can operate at 20

Solution-phase parallel synthesis of aryloxyimino amides via a novel multicomponent reaction among aromatic (Z)-chlorooximes, isocyanides, and electron-deficient phenols.

PubMed

Mercalli, Valentina; Giustiniano, Mariateresa; Del Grosso, Erika; Varese, Monica; Cassese, Hilde; Massarotti, Alberto; Novellino, Ettore; Tron, Gian Cesare

2014-11-10

A library of 41 aryloxyimino amides was prepared via solution phase parallel synthesis by extending the multicomponent reaction of (Z)-chlorooximes and isocyanides to the use of electron-deficient phenols. The resulting aryloxyiminoamide derivatives can be used as intermediates for the synthesis of benzo[d]isoxazole-3-carboxamides, dramatically reducing the number of synthetic steps required by other methods reported in literature.

Mycorrhizal synthesis between Boletus edulis species complex and rockroses (Cistus sp.).

PubMed

Águeda, Beatriz; Parladé, Javier; Fernández-Toirán, Luz Marina; Cisneros, Óscar; de Miguel, Ana María; Modrego, María Pilar; Martínez-Peña, Fernando; Pera, Joan

2008-10-01

Ectomycorrhizas of Boletus aereus, Boletus edulis, and Boletus reticulatus were synthesized with Cistus sp. under laboratory conditions using synthesis tubes filled with a mixture of sterilized peat-vermiculite and nutrient solution. The fungal strains isolated from sporocarps were identified by molecular techniques. The inoculated seedlings were grown for 4-5 months. The ectomycorrhizas formed were described based on standard morphological and anatomical characters. The three ectomycorrhizas described were very similar, with white monopodial-pinnate morphology, a three-layered plectenchymatous mantle on plan view and boletoid rhizomorphs.

Synthesis of Biodiesel from Crude Palm Oil by Using Contact Glow Discharge Electrolysis

NASA Astrophysics Data System (ADS)

Saksono, Nelson; Aditya Siswosoebrotho, Danar; Pranata, Jeremia J. C.; Bismo, Setijo

2018-03-01

This research has evaluated the use of Contact Glow Discharge Electrolysis method in the synthesis of biodiesel. The purpose of this research is to get the synthesis process and biodiesel product. The solution used is the mix of Crude Palm Oil and methanol with molar ratio of 1:24, and catalyst of NaOH and KOH with variation of concentration 0.5% - 1.5%-wt. The result shows that the biodiesel can be made from transesterification reaction that may be initiated by radical methoxide. The use of electrolyte KOH is better than NaOH based on the yield of biodiesel and the energy consumption. The optimum yield reaches 97%, at the synthesis for 30 minutes with the use of KOH 1%-wt with the energy consumption of 1.32 kJ/mL.

Designing a multiroute synthesis scheme in combinatorial chemistry.

PubMed

Akavia, Adi; Senderowitz, Hanoch; Lerner, Alon; Shamir, Ron

2004-01-01

Solid-phase mix-and-split combinatorial synthesis is often used to produce large arrays of compounds to be tested during the various stages of the drug development process. This method can be represented by a synthesis graph in which nodes correspond to grow operations and arcs to beads transferred among the different reaction vessels. In this work, we address the problem of designing such a graph which maximizes the number of produced target compounds (namely, compounds out of an input library of desired molecules), given constraints on the number of beads used for library synthesis and on the number of reaction vessels available for concurrent grow steps. We present a heuristic based on a discrete search for solving this problem, test our solution on several data sets, explore its behavior, and show that it achieves good performance.

A remote-controlled adaptive medchem lab: an innovative approach to enable drug discovery in the 21st Century.

PubMed

Godfrey, Alexander G; Masquelin, Thierry; Hemmerle, Horst

2013-09-01

This article describes our experiences in creating a fully integrated, globally accessible, automated chemical synthesis laboratory. The goal of the project was to establish a fully integrated automated synthesis solution that was initially focused on minimizing the burden of repetitive, routine, rules-based operations that characterize more established chemistry workflows. The architecture was crafted to allow for the expansion of synthetic capabilities while also providing for a flexible interface that permits the synthesis objective to be introduced and manipulated as needed under the judicious direction of a remote user in real-time. This innovative central synthesis suite is herein described along with some case studies to illustrate the impact such a system is having in expanding drug discovery capabilities. Copyright © 2013 Elsevier Ltd. All rights reserved.

Refined Synthesis and Characterization of Controlled Diameter, Narrow Size Distribution Microparticles for Aerospace Research Applications

NASA Technical Reports Server (NTRS)

Tiemsin, Pacita I.; Wohl, Christopher J.

2012-01-01

Flow visualization using polystyrene microspheres (PSL)s has enabled researchers to learn a tremendous amount of information via particle based diagnostic techniques. To better accommodate wind tunnel researchers needs, PSL synthesis via dispersion polymerization has been carried out at NASA Langley Research Center since the late 1980s. When utilizing seed material for flow visualization, size and size distribution are of paramount importance. Therefore, the work described here focused on further refinement of PSL synthesis and characterization. Through controlled variation of synthetic conditions (chemical concentrations, solution stirring speed, temperature, etc.) a robust, controllable procedure was developed. The relationship between particle size and salt concentration, MgSO4, was identified enabling the determination of PSL diameters a priori. Suggestions of future topics related to PSL synthesis, stability, and size variation are also described.

Structural characteristics and sorption properties of lithium-selective composite materials based on TiO2 and MnO2

NASA Astrophysics Data System (ADS)

Chaban, M. O.; Rozhdestvenska, L. M.; Palchyk, O. V.; Dzyazko, Y. S.; Dzyazko, O. G.

2018-04-01

A number of nanomaterials containing titanium dioxide and manganese dioxide were synthesized. The effect of synthesis conditions on structural and sorption characteristics for the selective extraction of lithium ions from solutions was studied. The ion-exchange materials were investigated with the methods of electron microscopy, thermogravimetric and X-ray analyses. During thermal synthesis phases of lithium manganese titanium spinel and TiO2 are being formed. Replacing a part of manganese with titanium ions leads to a decrease in the dissolution of Mn and to an increase in chemical stability. Composites with optimal values of selectivity and sorption rates were used to remove lithium ions from solutions with high salt background. The recovery degree of lithium ions under dynamic conditions reached 99%, the highest sorption capacity was found at pH 10.

Eco-friendly graphene synthesis on Cu foil electroplated by reusing Cu etchants

PubMed Central

Kwon, Ki Chang; Ham, Juyoung; Kim, Sungjun; Lee, Jong-Lam; Kim, Soo Young

2014-01-01

Graphene film grown by chemical vapor deposition using Cu substrate is promising for industrial applications. After etching the Cu substrate, which is essential step in graphene transfer process, the etchant solution must be chemically treated to prevent water pollution. Here we investigated that a method of reusing Cu etchant used to synthesize graphene, the synthesis of graphene on the resulting reused Cu films (R-G), and the application of R-G to organic light-emitting diodes (OLEDs) and organic photovoltaic cells (OPVs). The turn-on voltage of OLEDs based on the R-G electrode was 4.2 V, and the efficiencies of OPVs based on the R-G electrode were 5.9–5.95%, that are similar to or better than those of the indium-tin-oxide-based devices. These results suggest that the reusing of Cu foil by the electroplating method could reduce the cost of graphene synthesis, thus opening a wide range of applications in graphene electronics. PMID:24777344

Cooperative solution in the synthesis of multidegree-of-freedom shock isolation systems

NASA Astrophysics Data System (ADS)

Hati, S. K.; Rao, S. S.

1983-01-01

It is noted that there are essentially two major criteria in the synthesis of shock isolation stems. One is related to the minimization of the relative displacement between the main mass (which is to be isolated from vibration) and the base (where disturbance is given); the other concerns the minimization of force transmitted to the main mass. From the available literature, it is observed that nearly all the investigators have considered the design problem by treating one of these factors as the objective and the other as a constraint. This problem is treated here as a multicriteria optimization problem, and the trade-off between the two objectives is determined by using a game theory approach. The synthesis of a multidegree-of-freedom shock isolation system under a sinusoidal base disturbance is given as an example problem to illustrate the theory.

P25-graphene hydrogels: room-temperature synthesis and application for removal of methylene blue from aqueous solution.

PubMed

Hou, Chengyi; Zhang, Qinghong; Li, Yaogang; Wang, Hongzhi

2012-02-29

Herein we report a room-temperature synthesis of chemically bonded TiO2 (P25)-graphene composite hydrogels and their use as high performance visible light photocatalysts. The three-dimensional (3D) TiO2-carbon composite exhibits a significant enhancement in the reaction rate in the decontamination of methylene blue, compared to the bare P25. The 3D P25-graphene hydrogel is much easier to prepare and apply as a macroscopic device, compared to the 2D P25-graphene sheets. This work could provide new insights into the room-temperature synthesis of graphene-based materials. As a kind of the novel 3D graphene-based composite, the obtained high performance P25-graphene gel could be widely used in the environmental protection issues. Copyright © 2012. Published by Elsevier B.V.

Combinatorial codon scrambling enables scalable gene synthesis and amplification of repetitive proteins

NASA Astrophysics Data System (ADS)

Tang, Nicholas C.; Chilkoti, Ashutosh

2016-04-01

Most genes are synthesized using seamless assembly methods that rely on the polymerase chain reaction (PCR). However, PCR of genes encoding repetitive proteins either fails or generates nonspecific products. Motivated by the need to efficiently generate new protein polymers through high-throughput gene synthesis, here we report a codon-scrambling algorithm that enables the PCR-based gene synthesis of repetitive proteins by exploiting the codon redundancy of amino acids and finding the least-repetitive synonymous gene sequence. We also show that the codon-scrambling problem is analogous to the well-known travelling salesman problem, and obtain an exact solution to it by using De Bruijn graphs and a modern mixed integer linear programme solver. As experimental proof of the utility of this approach, we use it to optimize the synthetic genes for 19 repetitive proteins, and show that the gene fragments are amenable to PCR-based gene assembly and recombinant expression.

Reusable electrochemical cell for rapid separation of [18F]fluoride from [18O]water for flow-through synthesis of 18F-labeled tracers

PubMed Central

Sadeghi, Saman; Liang, Vincent; Cheung, Shilin; Woo, Suh; Wu, Curtis; Ly, Jimmy; Deng, Yuliang; Eddings, Mark; van Dam, R. Michael

2015-01-01

A brass-platinum electrochemical micro flow cell was developed to extract [18F]fluoride from an aqueous solution and release it into an organic based solution, suitable for subsequent radio-synthesis, in a fast and reliable manner. This cell does not suffer electrode erosion and is thus reusable while operating faster by enabling increased voltages. By optimizing temperature, trapping and release potentials, flow rates, and electrode materials, an overall [18F]fluoride trapping and release efficiency of 84±5% (n=7) was achieved. X-ray photoelectron spectroscopy (XPS) was used to analyze electrode surfaces of various metal-metal systems and the findings were correlated with the performance of the electrochemical cell. To demonstrate the reactivity of the released [18F]fluoride, the cell was coupled to a flow-through reactor and automated synthesis of [18F]FDG with a repeatable decay-corrected yield of 56±4% (n=4) was completed in <15 min. A multi-human dose of 5.92 GBq [18F]FDG was also demonstrated. PMID:23474380

Large Marks-decahedral Pd nanoparticles synthesized by a modified hydrothermal method using a homogeneous reactor

NASA Astrophysics Data System (ADS)

Zhao, Haiqiang; Qi, Weihong; Ji, Wenhai; Wang, Tianran; Peng, Hongcheng; Wang, Qi; Jia, Yanlin; He, Jieting

2017-05-01

Fivefold symmetry appears only in small particles and quasicrystals because internal stress in the particles increases with the particle size. However, a typical Marks decahedron with five re-entrant grooves located at the ends of the twin boundaries can further reduce the strain energy. During hydrothermal synthesis, it is difficult to stir the reaction solution contained in a digestion high-pressure tank because of the relatively small size and high-temperature and high-pressure sealed environment. In this work, we optimized a hydrothermal reaction system by replacing the conventional drying oven with a homogeneous reactor to shift the original static reaction solution into a full mixing state. Large Marks-decahedral Pd nanoparticles ( 90 nm) have been successfully synthesized in the optimized hydrothermal synthesis system. Additionally, in the products, round Marks-decahedral Pd particles were also found for the first time. While it remains a challenge to understand the growth mechanism of the fivefold twinned structure, we proposed a plausible growth-mediated mechanism for Marks-decahedral Pd nanoparticles based on observations of the synthesis process.

Ferroelectric devices using lead zirconate titanate (PZT) nanoparticles.

PubMed

Paik, Young Hun; Kojori, Hossein Shokri; Kim, Sung Jin

2016-02-19

We successfully demonstrate the synthesis of lead zirconate titanate nanoparticles (PZT NPs) and a ferroelectric device using the synthesized PZT NPs. The crystalline structure and the size of the nanocrystals are studied using x-ray diffraction and transmission electron microscopy, respectively. We observe <100 nm of PZT NPs and this result matches dynamic light scattering measurements. A solution-based low-temperature process is used to fabricate PZT NP-based devices on an indium tin oxide substrate. The fabricated ferroelectric devices are characterized using various optical and electrical measurements and we verify ferroelectric properties including ferroelectric hysteresis and the ferroelectric photovoltaic effect. Our approach enables low-temperature solution-based processes that could be used for various applications. To the best of our knowledge, this low-temperature solution processed ferroelectric device using PZT NPs is the first successful demonstration of its kind.

Ferroelectric devices using lead zirconate titanate (PZT) nanoparticles

NASA Astrophysics Data System (ADS)

Paik, Young Hun; Shokri Kojori, Hossein; Kim, Sung Jin

2016-02-01

We successfully demonstrate the synthesis of lead zirconate titanate nanoparticles (PZT NPs) and a ferroelectric device using the synthesized PZT NPs. The crystalline structure and the size of the nanocrystals are studied using x-ray diffraction and transmission electron microscopy, respectively. We observe <100 nm of PZT NPs and this result matches dynamic light scattering measurements. A solution-based low-temperature process is used to fabricate PZT NP-based devices on an indium tin oxide substrate. The fabricated ferroelectric devices are characterized using various optical and electrical measurements and we verify ferroelectric properties including ferroelectric hysteresis and the ferroelectric photovoltaic effect. Our approach enables low-temperature solution-based processes that could be used for various applications. To the best of our knowledge, this low-temperature solution processed ferroelectric device using PZT NPs is the first successful demonstration of its kind.

PETI-298 Prepared by Microwave Synthesis: Neat Resin and Composite Properties

NASA Technical Reports Server (NTRS)

Smith, Joseph G.; Connell, John W.; Li, Chao-Jun; Wu, Wei; Criss, Jim M., Jr.

2004-01-01

PETI-298 is a high temperature/high performance matrix resin that is processable into composites by resin transfer molding (RTM), resin infusion and vacuum assisted RTM techniques. It is typically synthesized in a polar aprotic solvent from the reaction of an aromatic anhydride and a combination of diamines and endcapped with phenylethynylphthalic anhydride. Microwave synthesis of PETI-298 was investigated as a means to eliminate solvent and decrease reaction time. The monomers were manually mixed and placed in a microwave oven for various times to determine optimum reaction conditions. The synthetic process was subsequently scaled-up to 330g. Three batches were synthesized and combined to give 1 kg of material that was characterized for thermal and rheological properties and compared to PETI-298 prepared by the classic solution based synthetic method. The microwave synthesized PETI-298 was subsequently used to fabricate flat laminates on T650 carbon fabric by RTM. The composite panels were analyzed and mechanical properties determined and compared with those fabricated from PETI-298 prepared by the classic solution method. The microwave synthesis process and characterization of neat resin and carbon fiber reinforced composites fabricated by RTM will be presented. KEY WORDS: Resin Transfer Molding, High Temperature Polymers, Phenylethynyl Terminated Imides, Microwave Synthesis

Emulsion Synthesis of Size-Tunable CH3NH3PbBr3 Quantum Dots: An Alternative Route toward Efficient Light-Emitting Diodes.

PubMed

Huang, Hailong; Zhao, Fangchao; Liu, Lige; Zhang, Feng; Wu, Xian-gang; Shi, Lijie; Zou, Bingsuo; Pei, Qibing; Zhong, Haizheng

2015-12-30

We report a facile nonaqueous emulsion synthesis of colloidal halide perovskite quantum dots by controlled addition of a demulsifier into an emulsion of precursors. The size of resulting CH3NH3PbBr3 quantum dots can be tuned from 2 to 8 nm by varying the amount of demulsifier. Moreover, this emulsion synthesis also allows the purification of these quantum dots by precipitation from the colloidal solution and obtains solid-state powder which can be redissolved for thin film coating and device fabrication. The photoluminescence quantum yields of the quantum dots is generally in the range of 80-92%, and can be well-preserved after purification (∼80%). Green light-emitting diodes fabricated comprising a spin-cast layer of the colloidal CH3NH3PbBr3 quantum dots exhibited maximum current efficiency of 4.5 cd/A, power efficiency of 3.5 lm/W, and external quantum efficiency of 1.1%. This provides an alternative route toward high efficient solution-processed perovskite-based light-emitting diodes. In addition, the emulsion synthesis is versatile and can be extended for the fabrication of inorganic halide perovskite colloidal CsPbBr3 nanocrystals.

Process for production of solution-derived (Pb,La)(Nb,Sn,Zr,Ti)O{sub 3} thin films and powders

DOEpatents

Boyle, T.J.

1999-01-12

A simple and rapid process for synthesizing (Pb,La)(Nb,Sn,Zr,Ti)O{sub 3} precursor solutions and subsequent ferroelectric thin films and powders of the perovskite phase of these materials has been developed. This process offers advantages over standard methods, including: rapid solution synthesis (<10 minutes), use of commercially available materials, film production under ambient conditions, ease of lanthanum dissolution at high concentrations, and no heating requirements during solution synthesis. For lanthanum-doped ferroelectric materials, the lanthanum source can be added with total synthesis time less than 10 minutes. Films and powders are crystallized at approximately 650 C and exhibit ferroelectric properties comparable to films and powders produced by other techniques which require higher crystallization temperatures. 2 figs.

Process for production of solution-derived (Pb,La)(Nb,Sn,Zr,Ti)O.sub.3 thin films and powders

DOEpatents

Boyle, Timothy J.

1999-01-01

A simple and rapid process for synthesizing (Pb,La)(Nb,Sn,Zr,Ti)O.sub.3 precursor solutions and subsequent ferroelectric thin films and powders of the perovskite phase of these materials has been developed. This process offers advantages over standard methods, including: rapid solution synthesis (<10 minutes), use of commercially available materials, film production under ambient conditions, ease of lanthanum dissolution at high concentrations, and no heating requirements during solution synthesis. For lanthanum-doped ferroelectric materials, the lanthanum source can be added with total synthesis time less than 10 minutes. Films and powders are crystallized at approximately 650.degree. C. and exhibit ferroelectric properties comparable to films and powders produced by other techniques which require higher crystallization temperatures.

Facile synthesis of nanostructured TiNb2O7 anode materials with superior performance for high-rate lithium ion batteries.

PubMed

Lou, Shuaifeng; Ma, Yulin; Cheng, Xinqun; Gao, Jinlong; Gao, Yunzhi; Zuo, Pengjian; Du, Chunyu; Yin, Geping

2015-12-18

One-dimensional nanostructured TiNb2O7 was prepared by a simple solution-based process and subsequent thermal annealing. The obtained anode materials exhibited excellent electrochemical performance with superior reversible capacity, rate capability and cyclic stability.

Machine-Vision Aids for Improved Flight Operations

NASA Technical Reports Server (NTRS)

Menon, P. K.; Chatterji, Gano B.

1996-01-01

The development of machine vision based pilot aids to help reduce night approach and landing accidents is explored. The techniques developed are motivated by the desire to use the available information sources for navigation such as the airport lighting layout, attitude sensors and Global Positioning System to derive more precise aircraft position and orientation information. The fact that airport lighting geometry is known and that images of airport lighting can be acquired by the camera, has lead to the synthesis of machine vision based algorithms for runway relative aircraft position and orientation estimation. The main contribution of this research is the synthesis of seven navigation algorithms based on two broad families of solutions. The first family of solution methods consists of techniques that reconstruct the airport lighting layout from the camera image and then estimate the aircraft position components by comparing the reconstructed lighting layout geometry with the known model of the airport lighting layout geometry. The second family of methods comprises techniques that synthesize the image of the airport lighting layout using a camera model and estimate the aircraft position and orientation by comparing this image with the actual image of the airport lighting acquired by the camera. Algorithms 1 through 4 belong to the first family of solutions while Algorithms 5 through 7 belong to the second family of solutions. Algorithms 1 and 2 are parameter optimization methods, Algorithms 3 and 4 are feature correspondence methods and Algorithms 5 through 7 are Kalman filter centered algorithms. Results of computer simulation are presented to demonstrate the performance of all the seven algorithms developed.

Method for the synthesis of chiral allylic alcohols utilizing selone based chiral derivatizing agents

DOEpatents

Silks, III, Louis A.

2002-01-01

Molecules containing a chiral 1,2-diol unit are synthesized from reactions between aldehydes and N-acyl selones. A chilled N-acyl selone is reacted with a Lewis acid such as TiCl.sub.4 and mixed with a tertiary amine such as diisopropylethylamine to generate an enolate solution. Upon further chilling of the enolate solution a desired aldehyde is added and after an acceptable reaction period a quencher is introduced and the product isolated.

Glycine Betaine Catabolism Contributes to Pseudomonas syringae Tolerance to Hyperosmotic Stress by Relieving Betaine-Mediated Suppression of Compatible Solute Synthesis

PubMed Central

Li, Shanshan; Yu, Xilan

2013-01-01

Many bacteria can accumulate glycine betaine for osmoprotection and catabolize it as a growth substrate, but how they regulate these opposing roles is poorly understood. In Pseudomonas syringae B728a, expression of the betaine catabolism genes was reduced by an osmotic upshift to an intermediate stress level, consistent with betaine accumulation, but was increased by an upshift to a high stress level, as confirmed by an accompanying increase in degradation of radiolabeled betaine. Deletion of the gbcAB betaine catabolism genes reduced osmotolerance at a high osmolarity, and this reduction was due to the relief of betaine-mediated suppression of compatible solute synthesis. This conclusion was supported by the findings that, at high osmolarity, the ΔgbcAB mutant accumulated high betaine levels and low endogenous solutes and exhibited reduced expression of the solute synthesis genes. Moreover, the ΔgbcAB mutant and a mutant deficient in the synthesis of the compatible solutes NAGGN and trehalose exhibited similar reductions in osmotolerance and also in fitness on bean leaves. Activation of betaine catabolism at high osmotic stress resulted, in part, from induction of gbdR, which encodes the transcriptional activator GbdR. Betaine catabolism was subject to partial repression by succinate under hyperosmotic stress conditions, in contrast to strong repression in the absence of stress, suggesting that betaine functions both in nutrition and as an intracellular signal modulating solute synthesis under hyperosmotic stress conditions. Collectively, these results begin to provide a detailed mechanistic understanding of how P. syringae transitions from reliance on exogenously derived betaine to the use of endogenous solutes during adaptation to hyperosmotic conditions. PMID:23524610

Fastest Formation Routes of Nanocarbons in Solution Plasma Processes.

PubMed

Morishita, Tetsunori; Ueno, Tomonaga; Panomsuwan, Gasidit; Hieda, Junko; Yoshida, Akihito; Bratescu, Maria Antoaneta; Saito, Nagahiro

2016-11-14

Although solution-plasma processing enables room-temperature synthesis of nanocarbons, the underlying mechanisms are not well understood. We investigated the routes of solution-plasma-induced nanocarbon formation from hexane, hexadecane, cyclohexane, and benzene. The synthesis rate from benzene was the highest. However, the nanocarbons from linear molecules were more crystalline than those from ring molecules. Linear molecules decomposed into shorter olefins, whereas ring molecules were reconstructed in the plasma. In the saturated ring molecules, C-H dissociation proceeded, followed by conversion into unsaturated ring molecules. However, unsaturated ring molecules were directly polymerized through cation radicals, such as benzene radical cation, and were converted into two- and three-ring molecules at the plasma-solution interface. The nanocarbons from linear molecules were synthesized in plasma from small molecules such as C 2 under heat; the obtained products were the same as those obtained via pyrolysis synthesis. Conversely, the nanocarbons obtained from ring molecules were directly synthesized through an intermediate, such as benzene radical cation, at the interface between plasma and solution, resulting in the same products as those obtained via polymerization. These two different reaction fields provide a reasonable explanation for the fastest synthesis rate observed in the case of benzene.

Fastest Formation Routes of Nanocarbons in Solution Plasma Processes

PubMed Central

Morishita, Tetsunori; Ueno, Tomonaga; Panomsuwan, Gasidit; Hieda, Junko; Yoshida, Akihito; Bratescu, Maria Antoaneta; Saito, Nagahiro

2016-01-01

Although solution-plasma processing enables room-temperature synthesis of nanocarbons, the underlying mechanisms are not well understood. We investigated the routes of solution-plasma-induced nanocarbon formation from hexane, hexadecane, cyclohexane, and benzene. The synthesis rate from benzene was the highest. However, the nanocarbons from linear molecules were more crystalline than those from ring molecules. Linear molecules decomposed into shorter olefins, whereas ring molecules were reconstructed in the plasma. In the saturated ring molecules, C–H dissociation proceeded, followed by conversion into unsaturated ring molecules. However, unsaturated ring molecules were directly polymerized through cation radicals, such as benzene radical cation, and were converted into two- and three-ring molecules at the plasma–solution interface. The nanocarbons from linear molecules were synthesized in plasma from small molecules such as C2 under heat; the obtained products were the same as those obtained via pyrolysis synthesis. Conversely, the nanocarbons obtained from ring molecules were directly synthesized through an intermediate, such as benzene radical cation, at the interface between plasma and solution, resulting in the same products as those obtained via polymerization. These two different reaction fields provide a reasonable explanation for the fastest synthesis rate observed in the case of benzene. PMID:27841288

Chemical oxidative and solid state synthesis of low molecular weight polymers for organic field effect transistors

NASA Astrophysics Data System (ADS)

Mahale, Rajashree Y.; Dharmapurikar, Satej S.; Chini, Mrinmoy Kumar

2018-03-01

Solution processability of the precursor molecules is a major issue owing to their limited solubility for the synthesis of conjugated polymers. Therefore, we favour the solvent free solid state chemical oxidative polymerization route for the synthesis of diketopyrrolopyrrole (DPP) based donor-acceptor (D-A) type conjugated polymers. D-A type polymer Poly(S-OD-EDOT) which contains DPP coupled with EDOT donor units is synthesized via solid state polymerization method. The polymer is employed as an active layer for organic field-effect transistors to measure charge transport properties. The Polymer shows good hole mobility 3.1 × 10-2 cm2 V-1 s-1, with a on/off ratio of 1.1 × 103.

Apparatus and method for polymer synthesis using arrays

DOEpatents

Brennan, Thomas M.

1995-01-01

A polymer synthesis apparatus (20) for building a polymer chain including a head assembly (21) having an array of nozzles (22) with each nozzle coupled to a reservoir (23) of liquid reagent (24) , and a base assembly (25) having an array of reaction wells (26). A transport mechanism (27) aligns the reaction wells (26) and selected nozzles (22) for deposition of the liquid reagent (24) into selected reaction wells (26). A sliding seal (30) is positioned between the head assembly (21) and the base assembly (25) to form a common chamber (31) enclosing both the reaction well (26) and the nozzles (22) therein. A gas inlet (70) into the common chamber (31), upstream from the nozzles (22), and a gas outlet (71) out of the common chamber (31) , downstream from the nozzles (22) , sweeps the common chamber ( 31 ) of toxic fumes emitted by the reagents. Each reaction well (26) includes an orifice (74) extending into the well (26) which is of a size and dimension to form a capillary liquid seal to retain the reagent solution (76) in the well (26) for polymer chain growth therein. A pressure regulating device (82) is provided for controlling a pressure differential, between a first gas pressure exerted on the reaction well (26) and a second gas pressure exerted on an exit (80) of the orifice, such that upon the pressure differential exceeding a predetermined amount, the reagent solution (76) is expelled from the well (26) through the orifice (74). A method of synthesis of a polymer chain in a synthesis apparatus (20) is also included.

Apparatus and method for polymer synthesis using arrays

DOEpatents

Brennan, Thomas M.

1996-01-01

A polymer synthesis apparatus (20) for building a polymer chain including a head assembly (21) having an array of nozzles (22) with each nozzle coupled to a reservoir (23) of liquid reagent (24), and a base assembly (25) having an array of reaction wells (26). A transport mechanism (27) aligns the reaction wells (26) and selected nozzles (22) for deposition of the liquid reagent (24) into selected reaction wells (26). A sliding seal (30) is positioned between the head assembly (21) and the base assembly (25) to form a common chamber (31) enclosing both the reaction well (26) and the nozzles (22) therein. A gas inlet (70) into the common chamber (31), upstream from the nozzles (22), and a gas outlet (71) out of the common chamber (31), downstream from the nozzles (22), sweeps the common chamber (31) of toxic fumes emitted by the reagents. Each reaction well ( 26) includes an orifice (74) extending into the well (26) which is of a size and dimension to form a capillary liquid seal to retain the reagent solution (76) in the well (26) for polymer chain growth therein. A pressure regulating device (82 ) is provided for controlling a pressure differential, between a first gas pressure exerted on the reaction well (26) and a second gas pressure exerted on an exit (80) of the orifice, such that upon the pressure differential exceeding a predetermined amount, the reagent solution (76) is expelled from the well (26) through the orifice (74). A method of synthesis of a polymer chain in a synthesis apparatus (20) is also included.

It's Complicated: Negotiating Between Traditional Research and Community-Based Participatory Research in a Translational Study.

PubMed

Hopkins, Allison L; Moore-Monroy, Martha; Wilkinson-Lee, Ada M; Nuño, Velia Leybas; Armenta, Alexandra; Lopez, Elvia; Vanzzini, Susan; Garcia, Francisco A

2016-01-01

The Interactive Systems Framework (ISF), a guide for translational research, encourages the balancing of traditional research and community-based participatory research (CBPR) approaches. This paper focuses on the challenges, solutions, and lessons learned in applying the ISF to our translational research project. A community-campus partnership translated evidence-based screening guidelines on sexually transmitted infections (STIs) and depression into culturally relevant educational materials. Community health workers (CHWs) disseminated the information through a cross-over design to Hispanic women in Pima County, Arizona. Challenges, solutions, and lessons learned were identified throughout this process. We identified challenges in the areas of research design, and in the ISF systems of prevention synthesis and translation, prevention support, and prevention delivery. We successfully negotiate solutions between the scientific and local community that resulted in acceptable compromises for both groups. The model presented by the ISF is difficult to achieve, but we offer concrete solutions to community members and scientists to move toward that ideal.

Bulk properties of solution-synthesized chevron-like graphene nanoribbons.

PubMed

Vo, Timothy H; Shekhirev, Mikhail; Lipatov, Alexey; Korlacki, Rafal A; Sinitskii, Alexander

2014-01-01

Graphene nanoribbons (GNRs) have received a great deal of attention due to their promise for electronic and optoelectronic applications. Several recent studies have focused on the synthesis of GNRs by the bottom-up approaches that could yield very narrow GNRs with atomically precise edges. One type of GNRs that has received a considerable attention is the chevron-like GNR with a very distinct periodic structure. Surface-assisted and solution-based synthetic approaches for the chevron-like GNRs have been developed, but their electronic properties have not been reported yet. In this work, we synthesized chevron-like GNRs in bulk by a solution-based method, characterized them by a number of spectroscopic techniques and measured their bulk conductivity. We demonstrate that solution-synthesized chevron-like GNRs are electrically conductive in bulk, which makes them a potentially promising material for applications in organic electronics and photovoltaics.

Single-phase and well-dispersed Cu1.75S nanocrystals by ambient pressure diethylene glycol solution synthesis

NASA Astrophysics Data System (ADS)

Zheng, Xuerong; Jin, Zhengguo; Liu, Hui; Wang, Yueqiu; Wang, Xin; Du, Haiyan

2013-02-01

Single-phase, well-dispersed Cu1.75S nanocrystals were synthesized by an ambient pressure, hydrazine hydrate and ethylenediamine co-assisted diethylene glycol based solution chemical process using copper chloride and thioacetamide as precursors at the temperature range from 180 to 210 °C. Influence of hydrazine hydrate and ethylenediamine adding amounts, synthetic temperature on crystal growth, size distribution and optical properties of the synthesized Cu1.75S nanocrystals were investigated by XRD, TEM, HRTEM, EDX and UV-vis measurements. The synthetic reaction at above 200 °C grew flaky-shaped nanocrystals with relatively narrow size distribution. The formation of single-phase Cu1.75S nanocrystals in the diethylene glycol based solution process might be involved in the presence of intermediate [Cu(en)n]1+ and [Cu(NH3)4]2+ complexes in reaction solution, providing a stable Cu(I) and Cu(II) valent-mixed precursor.

Laser-processing of VO2 thin films synthesized by polymer-assisted-deposition

NASA Astrophysics Data System (ADS)

Breckenfeld, Eric; Kim, Heungsoo; Gorzkowski, Edward P.; Sutto, Thomas E.; Piqué, Alberto

2017-03-01

We investigate a novel route for synthesis and laser-sintering of VO2 thin films via solution-based polymer-assisted-deposition (PAD). By replacing the traditional solvent for PAD (water) with propylene glycol, we are able to control the viscosity and improve the environmental stability of the precursor. The solution stability and ability to control the viscosity makes for an ideal solution to pattern simple or complex shapes via direct-write methods. We demonstrate the potential of our precursor for printing applications by combining PAD with laser induced forward transfer (LIFT). We also demonstrate large-area film synthesis on 4 in. diameter glass wafers. By varying the annealing temperature, we identify the optimal synthesis conditions, obtaining optical transmittance changes of 60% at a 2500 nm wavelength and a two-order-of-magnitude semiconductor-to-metal transition. We go on to demonstrate two routes for improved semiconductor-to-metal characteristics. The first method uses a multi-coating process to produce denser films with large particles. The second method uses a pulsed-UV-laser sintering step in films annealed at low temperatures (<450° C) to promote particle growth and improve the semiconductor-to-metal transition. By comparing the hysteresis width and semiconductor-to-metal transition magnitude in these samples, we demonstrate that both methods yield high quality VO2 with a three-order-of-magnitude transition.

Elucidating the reaction pathways in the synthesis of organolead trihalide perovskite for high-performance solar cells.

PubMed

Wang, Baohua; Young Wong, King; Xiao, Xudong; Chen, Tao

2015-05-28

The past two years have witnessed unprecedentedly rapid development of organic-inorganic halide perovskite-based solar cells. The solution-processability and high efficiency make this technology extraordinarily attractive. The intensive investigations have accumulated rich experiences in the perovskite fabrication; while the mechanism of the chemical synthesis still remains unresolved. Here, we set up the chemical equation of the synthesis and elucidate the reactions from both thermodynamic and kinetic perspectives. Our study shows that gaseous products thermodynamically favour the reaction, while the activation energy and "collision" probability synergistically determine the reaction rate. These understandings enable us to finely tune the crystal size for high-quality perovskite film, leading to a record fill factor among similar device structures in the literature. This investigation provides a general strategy to explore the mechanism of perovskite synthesis and benefits the fabrication of high-efficiency perovskite photoactive layer.

Synthesis and characterization of luminescent materials for thermal sensing and proton dosimetry

NASA Astrophysics Data System (ADS)

Doull, Brandon Arthur

The work presented in this thesis is the materials synthesis, investigation of synthesis parameters, and basic luminescent characterizations of MgB 4O7, Li2B4O7, and MgO for the applications of thermal sensing using thermoluminescence (TL) and proton dosimetry using optically stimulated luminescence (OSL). The materials were synthesized using solution combustion synthesis and characterized by x-ray diffraction, radioluminescence, thermoluminescence, and optically stimulated luminescence. Based upon the basic characterizations MgB 4O7:Li,Dy and Li2B4O7:Cu,Ag were selected for their potential for use as TL materials for thermal sensing while MgB4O7:Li,Ce and MgO:Li were chosen for use as OSL materials in proton dosimetry. Furthermore, MgB4O7:Li,Ce and MgO:Li were fabricated into detector assemblies and exposed to a clinical proton beam for analysis.

'Beautiful' unconventional synthesis and processing technologies of superconductors and some other materials.

PubMed

Badica, Petre; Crisan, Adrian; Aldica, Gheorghe; Endo, Kazuhiro; Borodianska, Hanna; Togano, Kazumasa; Awaji, Satoshi; Watanabe, Kazuo; Sakka, Yoshio; Vasylkiv, Oleg

2011-02-01

Superconducting materials have contributed significantly to the development of modern materials science and engineering. Specific technological solutions for their synthesis and processing helped in understanding the principles and approaches to the design, fabrication and application of many other materials. In this review, we explore the bidirectional relationship between the general and particular synthesis concepts. The analysis is mostly based on our studies where some unconventional technologies were applied to different superconductors and some other materials. These technologies include spray-frozen freeze-drying, fast pyrolysis, field-assisted sintering (or spark plasma sintering), nanoblasting, processing in high magnetic fields, methods of control of supersaturation and migration during film growth, and mechanical treatments of composite wires. The analysis provides future research directions and some key elements to define the concept of 'beautiful' technology in materials science. It also reconfirms the key position and importance of superconductors in the development of new materials and unconventional synthesis approaches.

Materials for n-type organic electronics: synthesis and properties of fluoroarene-thiophene semiconductors

NASA Astrophysics Data System (ADS)

Facchetti, Antonio; Yoon, Myung-Han; Katz, Howard E.; Marks, Tobin J.

2003-11-01

Recent progress in the field of organic electronics is due to a fruitful combination of both innovative molecular design and promising low-cost material/device assembly. Targeting the first strategy, we present here the general synthesis of fluoroarene-containing thiophene-based semiconductors and the study of their properties with respect to the corresponding fluorine-free hole-transporting analogues. The new compounds have been characterized by elemental analysis, mass spectrometry, and 1H- and 19F NMR. The dramatic influence of fluorine substitution and molecular architecture has been investigated by solution/film optical absorption, fluorescence emission, and cyclic voltammetry. Single crystal data for all of the oligomers have been obtained and will be presented. Film microstructure and morphology of this new class of materials have been studied by XRD and SEM. Particular emphasis will be posed on the solution-processable oligomers and polymers.

Synthesis, molecular docking and anticancer studies of peptides and iso-peptides.

PubMed

Jabeen, Farukh; Panda, Siva S; Kondratyuk, Tamara P; Park, Eun-Jung; Pezzuto, John M; Ihsan-ul-Haq; Hall, C Dennis; Katritzky, Alan R

2015-08-01

Chiral peptides and iso-peptides were synthesized in excellent yield by using benzotriazole mediated solution phase synthesis. Benzotriazole acted both as activating and leaving group, eliminating frequent use of protection and subsequent deprotection. The procedure was based on the hypothesis that epimerization should be suppressed in solution due to a faster coupling rate than SPPS. All the synthesized peptides complied with Lipinski's Ro5 except for the rotatable bonds. Inhibition of cell proliferation of cancer cell lines is one of the most commonly used methods to study the effectiveness of any anticancer agents. Synthesized peptides and iso-peptides were tested against three cancer cell lines (MCF-7, MDA-MB 231) to determine their anti-proliferative potential. NFkB was also determined. Molecular docking studies were also carried out to complement the experimental results. Copyright © 2015 Elsevier Ltd. All rights reserved.

Optimization of three- and four-component reactions for polysubstituted piperidines: application to the synthesis and preliminary biological screening of a prototype library.

PubMed

Ulaczyk-Lesanko, Agnieszka; Pelletier, Eric; Lee, Maria; Prinz, Heino; Waldmann, Herbert; Hall, Dennis G

2007-01-01

Several solid- and solution-phase strategies were evaluated for the preparation of libraries of polysubstituted piperidines of type 7 using the tandem aza[4+2]cycloaddition/allylboration multicomponent reaction between 1-aza-4-boronobutadienes, maleimides, and aldehydes. A novel four-component variant of this chemistry was developed in solution phase, and it circumvents the need for pre-forming the azabutadiene component. A parallel synthesis coupled with compound purification by HPLC with mass-based fraction collection allowed the preparation of a library of 944 polysubstituted piperidines in a high degree of purity suitable for biological screening. A representative subset of 244 compounds was screened against a panel of phosphatase enzymes, and despite the modest levels of activity obtained, this study demonstrated that piperidines of type 7 display the right physical properties (e.g., solubility) to be assayed effectively in high-throughput enzymatic tests.

A reliable algorithm for optimal control synthesis

NASA Technical Reports Server (NTRS)

Vansteenwyk, Brett; Ly, Uy-Loi

1992-01-01

In recent years, powerful design tools for linear time-invariant multivariable control systems have been developed based on direct parameter optimization. In this report, an algorithm for reliable optimal control synthesis using parameter optimization is presented. Specifically, a robust numerical algorithm is developed for the evaluation of the H(sup 2)-like cost functional and its gradients with respect to the controller design parameters. The method is specifically designed to handle defective degenerate systems and is based on the well-known Pade series approximation of the matrix exponential. Numerical test problems in control synthesis for simple mechanical systems and for a flexible structure with densely packed modes illustrate positively the reliability of this method when compared to a method based on diagonalization. Several types of cost functions have been considered: a cost function for robust control consisting of a linear combination of quadratic objectives for deterministic and random disturbances, and one representing an upper bound on the quadratic objective for worst case initial conditions. Finally, a framework for multivariable control synthesis has been developed combining the concept of closed-loop transfer recovery with numerical parameter optimization. The procedure enables designers to synthesize not only observer-based controllers but also controllers of arbitrary order and structure. Numerical design solutions rely heavily on the robust algorithm due to the high order of the synthesis model and the presence of near-overlapping modes. The design approach is successfully applied to the design of a high-bandwidth control system for a rotorcraft.

The effect of particle size on the toxic action of silver nanoparticles

NASA Astrophysics Data System (ADS)

Sosenkova, L. S.; Egorova, E. M.

2011-04-01

Silver nanoparticles in AOT reverse micelles were obtained by means of the biochemical synthesis. Synthesis of nanoparticles was carried out with variation of the three parameters of reverse-micellar systems: concentration of silver ions, concentration of the stabilizer (AOT) and hydration extent w = [H2O]/[AOT]. The combinations of varied parameters have been found, allowing to prepare micellar solutions of spherical silver nanoparticles with average sizes 4.6 and 9.5 nm and narrow size distribution. From micellar solution the nanoparticles were transferred into the water phase; water solutions of the nanoparticles were used for testing their biological activity. Our assay is based on negative chemotaxis, a motile reaction of cells to an unfavorable chemical environment. Plasmodium of the slime mold Physarum polycephalum used as an object is a multinuclear amoeboid cell with unlimited growth and the auto-oscillatory mode of locomotion. In researches of chemotaxis on plasmodium it is learned that silver nanoparticles of smaller size exhibit a higher biological activity (behave as stronger repellent) and this correlates with the literary data obtained in studies of silver nanoparticles interaction with other biological objects.

Methodology for the specification of communication activities within the framework of a multi-layered architecture: Toward the definition of a knowledge base

NASA Astrophysics Data System (ADS)

Amyay, Omar

A method defined in terms of synthesis and verification steps is presented. The specification of the services and protocols of communication within a multilayered architecture of the Open Systems Interconnection (OSI) type is an essential issue for the design of computer networks. The aim is to obtain an operational specification of the protocol service couple of a given layer. Planning synthesis and verification steps constitute a specification trajectory. The latter is based on the progressive integration of the 'initial data' constraints and verification of the specification originating from each synthesis step, through validity constraints that characterize an admissible solution. Two types of trajectories are proposed according to the style of the initial specification of the service protocol couple: operational type and service supplier viewpoint; knowledge property oriented type and service viewpoint. Synthesis and verification activities were developed and formalized in terms of labeled transition systems, temporal logic and epistemic logic. The originality of the second specification trajectory and the use of the epistemic logic are shown. An 'artificial intelligence' approach enables a conceptual model to be defined for a knowledge base system for implementing the method proposed. It is structured in three levels of representation of the knowledge relating to the domain, the reasoning characterizing synthesis and verification activities and the planning of the steps of a specification trajectory.

A Base-Resistant Metalloporphyrin Metal–Organic Framework for C–H Bond Halogenation

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

Lv, Xiu-Liang; Wang, Kecheng; Wang, Bin

A base-resistant porphyrin metal–organic framework (MOF), namely PCN-602 has been constructed with 12-connected [Ni 8(OH) 4(H 2O) 2Pz 12] (Pz = pyrazolate) cluster and a newly designed pyrazolate-based porphyrin ligand, 5,10,15,20-tetrakis(4-(pyrazolate-4-yl)phenyl)porphyrin under the guidance of the reticular synthesis strategy. Besides its robustness in hydroxide solution, PCN-602 also shows excellent stability in aqueous solutions of F –, CO 3 2–, and PO 4 3– ions. Interestingly, the Mn 3+-porphyrinic PCN-602, as a recyclable MOF catalyst, presents high catalytic activity for the C–H bond halogenation reaction in a basic system, significantly outperforming its homogeneous counterpart. For the first time, a porphyrinic MOFmore » was thus used as an efficient catalyst in a basic solution with coordinating anions, to the best of our knowledge.« less

Synthesis of GaN:ZnO solid solution by solution combustion method and characterization for photocatalytic application

NASA Astrophysics Data System (ADS)

Menon, Sumithra Sivadas; Anitha, R.; Gupta, Bhavana; Baskar, K.; Singh, Shubra

2016-05-01

GaN-ZnO solid solution has emerged as a successful and reproducible photocatalyst for overall water splitting by one-step photoexcitation, with a bandgap in visible region. When the solid solution is formed, some of the Zn and O ions are replaced by Ga and N ions respectively and there is a narrowing of bandgap which is hypothesized as due to Zn3d-N2p repulsion. The traditional method of synthesis of GaN-ZnO solid solution is by nitridation of the starting oxides under constant ammonia flow. Here we report a solution combustion technique for the synthesis of the solid solution at a temperature about 500 ° C in a muffle furnace with metal nitrates as precursors and urea as the fuel. The as prepared samples showed change in color with the increased concentration of ZnO in the solution. The structural, microstructural, morphological and optical properties of the samples were realized by Powder X ray diffraction, Scanning electron microscopy, Energy dispersive X ray analysis, Transmission electron microscopy and Photoluminescence. Finally the hydrogen production efficiency of the GaN-ZnO nanopowders by water splitting was found, using methanol as a scavenger. The apparent quantum yield (AQY) of 0.048% is obtained for GaN-ZnO solid solution.

Radiolabeling of DOTA-like conjugated peptides with generator-produced 68Ga and using NaCl-based cationic elution method

PubMed Central

Mueller, Dirk; Breeman, Wouter A P; Klette, Ingo; Gottschaldt, Michael; Odparlik, Andreas; Baehre, Manfred; Tworowska, Izabela; Schultz, Michael K

2017-01-01

Gallium-68 (68Ga) is a generator-produced radionuclide with a short half-life (t½ = 68 min) that is particularly well suited for molecular imaging by positron emission tomography (PET). Methods have been developed to synthesize 68Ga-labeled imaging agents possessing certain drawbacks, such as longer synthesis time because of a required final purification step, the use of organic solvents or concentrated hydrochloric acid (HCl). In our manuscript, we provide a detailed protocol for the use of an advantageous sodium chloride (NaCl)-based method for radiolabeling of chelator-modified peptides for molecular imaging. By working in a lead-shielded hot-cell system, 68Ga3+ of the generator eluate is trapped on a cation exchanger cartridge (100 mg, ∼8 mm long and 5 mm diameter) and then eluted with acidified 5 M NaCl solution directly into a sodium acetate-buffered solution containing a DOTA (1,4,7,10-tetraazacyclododecane-1,4,7,10-tetraacetic acid) or DOTA-like chelator-modified peptide. The main advantages of this procedure are the high efficiency and the absence of organic solvents. It can be applied to a variety of peptides, which are stable in 1 M NaCl solution at a pH value of 3–4 during reaction. After labeling, neutralization, sterile filtration and quality control (instant thin-layer chromatography (iTLC), HPLC and pH), the radiopharmaceutical can be directly administered to patients, without determination of organic solvents, which reduces the overall synthesis-to-release time. This procedure has been adapted easily to automated synthesis modules, which leads to a rapid preparation of 68Ga radiopharmaceuticals (12–16 min). PMID:27172166

Radiolabeling of DOTA-like conjugated peptides with generator-produced (68)Ga and using NaCl-based cationic elution method.

PubMed

Mueller, Dirk; Breeman, Wouter A P; Klette, Ingo; Gottschaldt, Michael; Odparlik, Andreas; Baehre, Manfred; Tworowska, Izabela; Schultz, Michael K

2016-06-01

Gallium-68 ((68)Ga) is a generator-produced radionuclide with a short half-life (t½ = 68 min) that is particularly well suited for molecular imaging by positron emission tomography (PET). Methods have been developed to synthesize (68)Ga-labeled imaging agents possessing certain drawbacks, such as longer synthesis time because of a required final purification step, the use of organic solvents or concentrated hydrochloric acid (HCl). In our manuscript, we provide a detailed protocol for the use of an advantageous sodium chloride (NaCl)-based method for radiolabeling of chelator-modified peptides for molecular imaging. By working in a lead-shielded hot-cell system,(68)Ga(3+) of the generator eluate is trapped on a cation exchanger cartridge (100 mg, ∼8 mm long and 5 mm diameter) and then eluted with acidified 5 M NaCl solution directly into a sodium acetate-buffered solution containing a DOTA (1,4,7,10-tetraazacyclododecane-1,4,7,10-tetraacetic acid) or DOTA-like chelator-modified peptide. The main advantages of this procedure are the high efficiency and the absence of organic solvents. It can be applied to a variety of peptides, which are stable in 1 M NaCl solution at a pH value of 3-4 during reaction. After labeling, neutralization, sterile filtration and quality control (instant thin-layer chromatography (iTLC), HPLC and pH), the radiopharmaceutical can be directly administered to patients, without determination of organic solvents, which reduces the overall synthesis-to-release time. This procedure has been adapted easily to automated synthesis modules, which leads to a rapid preparation of (68)Ga radiopharmaceuticals (12-16 min).

Solution-Based Electro-Orientation Spectroscopy (EOS) for Contactless Measurement of Semiconductor Nanowires

NASA Astrophysics Data System (ADS)

Yuan, Wuhan; Mohabir, Amar; Tutuncuoglu, Gozde; Filler, Michael; Feldman, Leonard; Shan, Jerry

2017-11-01

Solution-based, contactless methods for determining the electrical conductivity of nanowires and nanotubes have unique advantages over conventional techniques in terms of high throughput and compatibility with further solution-based processing and assembly methods. Here, we describe the solution-based electro-orientation spectroscopy (EOS) method, in which nanowire conductivity is measured from the AC-electric-field-induced alignment rate of the nanowire in a suspending fluid. The particle conductivity is determined from the measured crossover frequency between conductivity-dominated, low-frequency alignment to the permittivity-dominated, high-frequency regime. We discuss the extension of the EOS measurement range by an order-of-magnitude, taking advantage of the high dielectric constant of deionized water. With water and other fluids, we demonstrate that EOS can quantitatively characterize the electrical conductivities of nanowires over a 7-order-of-magnitude range, 10-5 to 102 S/m. We highlight the efficiency and utility of EOS for nanomaterial characterization by statistically characterizing the variability of semiconductor nanowires of the same nominal composition, and studying the connection between synthesis parameters and properties. NSF CBET-1604931.

Manufacturing of Smart Structures Using Fiber Placement Manufacturing Processes

NASA Technical Reports Server (NTRS)

Thomas, Matthew M.; Glowasky, Robert A.; McIlroy, Bruce E.; Story, Todd A.

1996-01-01

Smart structures research and development, with the ultimate aim of rapid commercial and military production of these structures, are at the forefront of the Synthesis and Processing of Intelligent Cost-Effective Structures (SPICES) program. As part of this ARPA-sponsored program, MDA-E is using fiber placement processes to manufacture integrated smart structure systems. These systems comprise advanced composite structures with embedded fiber optic sensors, shape memory alloys, piezoelectric actuators, and miniature accelerometers. Cost-effective approaches and solutions to smart material synthesis in the fiber-placement process, based upon integrated product development, are discussed herein.

Pilot-optimal augmentation synthesis

NASA Technical Reports Server (NTRS)

Schmidt, D. K.

1978-01-01

An augmentation synthesis method usable in the absence of quantitative handling qualities specifications, and yet explicitly including design objectives based on pilot-rating concepts, is presented. The algorithm involves the unique approach of simultaneously solving for the stability augmentation system (SAS) gains, pilot equalization and pilot rating prediction via optimal control techniques. Simultaneous solution is required in this case since the pilot model (gains, etc.) depends upon the augmented plant dynamics, and the augmentation is obviously not a priori known. Another special feature is the use of the pilot's objective function (from which the pilot model evolves) to design the SAS.

Two Alternative Pathways for the Synthesis of the Rare Compatible Solute Mannosylglucosylglycerate in Petrotoga mobilis▿

PubMed Central

Fernandes, Chantal; Mendes, Vitor; Costa, Joana; Empadinhas, Nuno; Jorge, Carla; Lamosa, Pedro; Santos, Helena; da Costa, Milton S.

2010-01-01

The compatible solute mannosylglucosylglycerate (MGG), recently identified in Petrotoga miotherma, also accumulates in Petrotoga mobilis in response to hyperosmotic conditions and supraoptimal growth temperatures. Two functionally connected genes encoding a glucosyl-3-phosphoglycerate synthase (GpgS) and an unknown glycosyltransferase (gene Pmob_1143), which we functionally characterized as a mannosylglucosyl-3-phosphoglycerate synthase and designated MggA, were identified in the genome of Ptg. mobilis. This enzyme used the product of GpgS, glucosyl-3-phosphoglycerate (GPG), as well as GDP-mannose to produce mannosylglucosyl-3-phosphoglycerate (MGPG), the phosphorylated precursor of MGG. The MGPG dephosphorylation was determined in cell extracts, and the native enzyme was partially purified and characterized. Surprisingly, a gene encoding a putative glucosylglycerate synthase (Ggs) was also identified in the genome of Ptg. mobilis, and an active Ggs capable of producing glucosylglycerate (GG) from ADP-glucose and d-glycerate was detected in cell extracts and the recombinant enzyme was characterized, as well. Since GG has never been identified in this organism nor was it a substrate for the MggA, we anticipated the existence of a nonphosphorylating pathway for MGG synthesis. We putatively identified the corresponding gene, whose product had some sequence homology with MggA, but it was not possible to recombinantly express a functional enzyme from Ptg. mobilis, which we named mannosylglucosylglycerate synthase (MggS). In turn, a homologous gene from Thermotoga maritima was successfully expressed, and the synthesis of MGG was confirmed from GDP-mannose and GG. Based on the measurements of the relevant enzyme activities in cell extracts and on the functional characterization of the key enzymes, we propose two alternative pathways for the synthesis of the rare compatible solute MGG in Ptg. mobilis. PMID:20061481

Synthesis and supramolecular assembly of biomimetic polymers

NASA Astrophysics Data System (ADS)

Marciel, Amanda Brittany

A grand challenge in materials chemistry is the synthesis of macromolecules and polymers with precise shapes and architectures. Polymer microstructure and architecture strongly affect the resulting functionality of advanced materials, yet understanding the static and dynamic properties of these complex macromolecules in bulk has been difficult due to their inherit polydispersity. Single molecule studies have provided a wealth of information on linear flexible and semi-flexible polymers in dilute solutions. However, few investigations have focused on industrially relevant complex topologies (e.g., star, comb, hyperbranched polymers) in industrially relevant solution conditions (e.g., semi-dilute, concentrated). Therefore, from this perspective there is a strong need to synthesize precision complex architectures for bulk studies as well as complex architectures compatible with current single molecule techniques to study static and dynamic polymer properties. In this way, we developed a hybrid synthetic strategy to produce branched polymer architectures based on chemically modified DNA. Overall, this approach enables control of backbone length and flexibility, as well as branch grafting density and chemical identity. We utilized a two-step scheme based on enzymatic incorporation of non-natural nucleotides containing bioorthogonal dibenzocyclooctyne (DBCO) functional groups along the main polymer backbone, followed by copper-free "click" chemistry to graft synthetic polymer branches or oligonucleotide branches to the DNA backbone, thereby allowing for the synthesis of a variety of polymer architectures, including three-arm stars, H-polymers, graft block copolymers, and comb polymers for materials assembly and single molecule studies. Bulk materials properties are also affected by industrial processing conditions that alter polymer morphology. Therefore, in an alternative strategy we developed a microfluidic-based approach to assemble highly aligned synthetic oligopeptides nanostructures using microscale extensional flows. This strategy enabled reproducible, reliable fabrication of aligned hierarchical constructs that do not form spontaneously in solution. In this way, fluidic-directed assembly of supramolecular structures allows for unprecedented manipulation at the nano- and mesoscale, which has the potential to provide rapid and efficient control of functional materials properties.

Titanium(IV) isopropoxide mediated solution phase reductive amination on an automated platform: application in the generation of urea and amide libraries.

PubMed

Bhattacharyya, S; Fan, L; Vo, L; Labadie, J

2000-04-01

Amine libraries and their derivatives are important targets for high throughput synthesis because of their versatility as medicinal agents and agrochemicals. As a part of our efforts towards automated chemical library synthesis, a titanium(IV) isopropoxide mediated solution phase reductive amination protocol was successfully translated to automation on the Trident(TM) library synthesizer of Argonaut Technologies. An array of 24 secondary amines was prepared in high yield and purity from 4 primary amines and 6 carbonyl compounds. These secondary amines were further utilized in a split synthesis to generate libraries of ureas, amides and sulfonamides in solution phase on the Trident(TM). The automated runs included 192 reactions to synthesize 96 ureas in duplicate and 96 reactions to synthesize 48 amides and 48 sulfonamides. A number of polymer-assisted solution phase protocols were employed for parallel work-up and purification of the products in each step.

Immobilization methods for the rapid total chemical synthesis of proteins on microtiter plates.

PubMed

Zitterbart, Robert; Krumrey, Michael; Seitz, Oliver

2017-07-01

The chemical synthesis of proteins typically involves the solid-phase peptide synthesis of unprotected peptide fragments that are stitched together in solution by native chemical ligation (NCL). The process is slow, and throughput is limited because of the need for repeated high performance liquid chromatography purification steps after both solid-phase peptide synthesis and NCL. With an aim to provide faster access to functional proteins and to accelerate the functional analysis of synthetic proteins by parallelization, we developed a method for the high performance liquid chromatography-free synthesis of proteins on the surface of microtiter plates. The method relies on solid-phase synthesis of unprotected peptide fragments, immobilization of the C-terminal fragment and on-surface NCL with an unprotected peptide thioester in crude form. Herein, we describe the development of a suitable immobilization chemistry. We compared (i) formation of nickel(II)-oligohistidine complexes, (ii) Cu-based [2 + 3] alkine-azide cycloaddition and (iii) hydrazone ligation. The comparative study identified the hydrazone ligation as most suitable. The sequence of immobilization via hydrazone ligation, on-surface NCL and radical desulfurization furnished the targeted SH3 domains in near quantitative yield. The synthetic proteins were functional as demonstrated by an on-surface fluorescence-based saturation binding analysis. Copyright © 2017 European Peptide Society and John Wiley & Sons, Ltd. Copyright © 2017 European Peptide Society and John Wiley & Sons, Ltd.

Automated Synthesis of 68Ga-DOTA-TOC: Methodological Aspects and Suitable Technical Solutions for a Cationic Purification System.

PubMed

Uccelli, Licia; Boschi, Alessandra; Cittanti, Corrado; Martini, Petra; Lodi, Luca; Zappaterra, Elisa; Romani, Simona; Zaccaria, Samanta; Cecconi, Davide; Rambaldi, Ilaria; Santi, Ivan; Panareo, Stefano; Giganti, Melchiore; Bartolomei, Mirco

2018-05-08

The PET Gallium-68 isotope has the advantage of being produced from a generator, so it is also available in nuclear medicine departments without a cyclotron. The preparation of Ga-68 DOTA-labelled compounds is actually performed by remotely controlled automated systems developed in order to assure production efficiency, reproducibility of the results, guarantee fast reaction time, to facilitate the synthesis and minimize the radiation exposure. Many automatic synthesis systems are available on the radiopharmaceutical market, and each of these requires the realization of some technical adaptations for routine use. We reported the Ga-68 DOTATOC production by automated cassette-based theranostic synthesizer system used in combination with a disposable GMP grade cassette system for cationic purification. The synthesizer is integrated with the 68Ge/68Ga generator systems and it allows to perform elution, eluate purification and radiolabeling in about 38 minutes. We have performed between January 2016 and January 2017 over 100 [68Ga]Ga-DOTA-TOC preparation and of these only three have failed. The average synthesis yield of radiopharmaceutical production was 54.4 ± 2.3 % and the average radiochemical purity was 96.94 ± 0.74 %. The methodology and the technical solutions adopted have allowed to obtain a high quality radiopharmaceutical product as required by the European Pharmacopoeia. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

Synthesis of carbon nanotubes from waste polyethylene plastics

NASA Astrophysics Data System (ADS)

Zhuo, Chuanwei

Generation of non-biodegradable wastes, such as plastics, and resulting land as well as water pollution therefrom discarded plastics have been continuously increasing, while landfill space decreases and recycling markets dwindle. Exploration of novel uses of such materials becomes therefore imperative. Here I present an innovative and unique partial conversion of plastic waste to valuable carbon nanomaterials. It is an overall exothermic and scalable process based on feeding waste plastics to a multi-stage, pyrolysis/combustion-synthesis reactor. Plain stainless steel screens are used as substrates as well as low-cost catalyst for both carbon nanomaterials synthesis and pyrolyzates generation. Nano carbon yields of as high as 13.6% of the weight of the polymer precursor were recorded. This demonstration provides a sustainable solution to both plastic waste utilization, and carbon nanomaterials mass production.

Controlled soft-template synthesis of ultrathin C@FeS nanosheets with high-Li-storage performance.

PubMed

Xu, Chen; Zeng, Yi; Rui, Xianhong; Xiao, Ni; Zhu, Jixin; Zhang, Wenyu; Chen, Jing; Liu, Weiling; Tan, Huiteng; Hng, Huey Hoon; Yan, Qingyu

2012-06-26

We report a facile approach to prepare carbon-coated troilite FeS (C@FeS) nanosheets via surfactant-assisted solution-based synthesis. 1-Dodecanethiol is used as both the sulfur source and the surfactant, which may form different-shaped micelles to direct the growth of nanostructures. Under appropriate growth conditions, the iron and sulfur atoms react to form thin layers of FeS while the hydrocarbon tails of 1-dodecanethiol separate the thin FeS layers, which turn to carbon after annealing in Ar. Such an approach can be extended to grow C@FeS nanospheres and nanoplates by modifying the synthesis parameters. The C@FeS nanosheets display excellent Li storage properties with high specific capacities and stable charge/discharge cyclability, especially at fast charge/discharge rates.

Peptide synthesis on glass substrate using acoustic droplet ejector.

PubMed

Youngki Choe; Shih-Jui Chen; Eun Sok Kim

2014-03-01

This paper describes the synthesis of a 9-mers-long peptide ladder structure of glycine on a modified glass surface using a nanoliter droplet ejector. To synthesize peptide on a glass substrate, SPOT peptide synthesis protocol was followed with a nozzleless acoustic droplet ejector being used to eject about 300 droplets of preactivated amino acid solution to dispense 60 nL of the solution per mer. The coupling efficiency of each mer was measured with FITC fluorescent tag to be 96%, resulting in net 70% efficiency for the whole 9-mer-long peptide of glycine. Usage of a nanoliter droplet ejector for SPOT peptide synthesis increases the density of protein array on a chip.

PH Tester Gauge Repeatability and Reproducibility Study for WO3 Nanostructure Hydrothermal Growth Process

NASA Astrophysics Data System (ADS)

Abd Rashid, Amirul; Hayati Saad, Nor; Bien Chia Sheng, Daniel; Yee, Lee Wai

2014-06-01

PH value is one of the important variables for tungsten trioxide (WO3) nanostructure hydrothermal synthesis process. The morphology of the synthesized nanostructure can be properly controlled by measuring and controlling the pH value of the solution used in this facile synthesis route. Therefore, it is very crucial to ensure the gauge used for pH measurement is reliable in order to achieve the expected result. In this study, gauge repeatability and reproducibility (GR&R) method was used to assess the repeatability and reproducibility of the pH tester. Based on ANOVA method, the design of experimental metrics as well as the result of the experiment was analyzed using Minitab software. It was found that the initial GR&R value for the tester was at 17.55 % which considered as acceptable. To further improve the GR&R level, a new pH measuring procedure was introduced. With the new procedure, the GR&R value was able to be reduced to 2.05%, which means the tester is statistically very ideal to measure the pH of the solution prepared for WO3 hydrothermal synthesis process.

Facile Fabrication of Platinum-Cobalt Alloy Nanoparticles with Enhanced Electrocatalytic Activity for a Methanol Oxidation Reaction

NASA Astrophysics Data System (ADS)

Huang, Huihong; Hu, Xiulan; Zhang, Jianbo; Su, Nan; Cheng, Jiexu

2017-03-01

Decreasing the cost associated with platinum-based catalysts along with improving their catalytic properties is a major challenge for commercial direct methanol fuel cells. In this work, a simple and facile strategy was developed for the more efficient preparation of multi-walled carbon nanotube (MWCNT) -supported Pt/CoPt composite nanoparticles (NPs) via solution plasma sputtering with subsequent thermal annealing. Quite different from general wet synthesis methods, Pt/CoPt composite NPs were directly derived from metal wire electrodes without any additions. The obtained Pt/CoPt/MWCNTs composite catalysts exhibited tremendous improvement in the electro-oxidation of methanol in acidic media with mass activities of 1719 mA mg-1Pt. This value is much higher than that of previous reports of Pt-Co alloy and commercial Pt/C (3.16 times) because of the many active sites and clean surface of the catalysts. The catalysts showed good stability due to the special synergistic effects of the CoPt alloy. Pt/CoPt/MWCNTs can be used as a promising catalyst for direct methanol fuel cells. In addition, this solution plasma sputtering-assisted synthesis method introduces a general and feasible route for the synthesis of binary alloys.

Facile Fabrication of Platinum-Cobalt Alloy Nanoparticles with Enhanced Electrocatalytic Activity for a Methanol Oxidation Reaction.

PubMed

Huang, Huihong; Hu, Xiulan; Zhang, Jianbo; Su, Nan; Cheng, JieXu

2017-03-30

Decreasing the cost associated with platinum-based catalysts along with improving their catalytic properties is a major challenge for commercial direct methanol fuel cells. In this work, a simple and facile strategy was developed for the more efficient preparation of multi-walled carbon nanotube (MWCNT) -supported Pt/CoPt composite nanoparticles (NPs) via solution plasma sputtering with subsequent thermal annealing. Quite different from general wet synthesis methods, Pt/CoPt composite NPs were directly derived from metal wire electrodes without any additions. The obtained Pt/CoPt/MWCNTs composite catalysts exhibited tremendous improvement in the electro-oxidation of methanol in acidic media with mass activities of 1719 mA mg -1 Pt . This value is much higher than that of previous reports of Pt-Co alloy and commercial Pt/C (3.16 times) because of the many active sites and clean surface of the catalysts. The catalysts showed good stability due to the special synergistic effects of the CoPt alloy. Pt/CoPt/MWCNTs can be used as a promising catalyst for direct methanol fuel cells. In addition, this solution plasma sputtering-assisted synthesis method introduces a general and feasible route for the synthesis of binary alloys.

An Algorithm for Integrated Subsystem Embodiment and System Synthesis

NASA Technical Reports Server (NTRS)

Lewis, Kemper

1997-01-01

Consider the statement,'A system has two coupled subsystems, one of which dominates the design process. Each subsystem consists of discrete and continuous variables, and is solved using sequential analysis and solution.' To address this type of statement in the design of complex systems, three steps are required, namely, the embodiment of the statement in terms of entities on a computer, the mathematical formulation of subsystem models, and the resulting solution and system synthesis. In complex system decomposition, the subsystems are not isolated, self-supporting entities. Information such as constraints, goals, and design variables may be shared between entities. But many times in engineering problems, full communication and cooperation does not exist, information is incomplete, or one subsystem may dominate the design. Additionally, these engineering problems give rise to mathematical models involving nonlinear functions of both discrete and continuous design variables. In this dissertation an algorithm is developed to handle these types of scenarios for the domain-independent integration of subsystem embodiment, coordination, and system synthesis using constructs from Decision-Based Design, Game Theory, and Multidisciplinary Design Optimization. Implementation of the concept in this dissertation involves testing of the hypotheses using example problems and a motivating case study involving the design of a subsonic passenger aircraft.

Analytical Devices Based on Direct Synthesis of DNA on Paper.

PubMed

Glavan, Ana C; Niu, Jia; Chen, Zhen; Güder, Firat; Cheng, Chao-Min; Liu, David; Whitesides, George M

2016-01-05

This paper addresses a growing need in clinical diagnostics for parallel, multiplex analysis of biomarkers from small biological samples. It describes a new procedure for assembling arrays of ssDNA and proteins on paper. This method starts with the synthesis of DNA oligonucleotides covalently linked to paper and proceeds to assemble microzones of DNA-conjugated paper into arrays capable of simultaneously capturing DNA, DNA-conjugated protein antigens, and DNA-conjugated antibodies. The synthesis of ssDNA oligonucleotides on paper is convenient and effective with 32% of the oligonucleotides cleaved and eluted from the paper substrate being full-length by HPLC for a 32-mer. These ssDNA arrays can be used to detect fluorophore-linked DNA oligonucleotides in solution, and as the basis for DNA-directed assembly of arrays of DNA-conjugated capture antibodies on paper, detect protein antigens by sandwich ELISAs. Paper-anchored ssDNA arrays with different sequences can be used to assemble paper-based devices capable of detecting DNA and antibodies in the same device and enable simple microfluidic paper-based devices.

The use of methods of structural optimization at the stage of designing high-rise buildings with steel construction

NASA Astrophysics Data System (ADS)

Vasilkin, Andrey

2018-03-01

The more designing solutions at the search stage for design for high-rise buildings can be synthesized by the engineer, the more likely that the final adopted version will be the most efficient and economical. However, in modern market conditions, taking into account the complexity and responsibility of high-rise buildings the designer does not have the necessary time to develop, analyze and compare any significant number of options. To solve this problem, it is expedient to use the high potential of computer-aided designing. To implement automated search for design solutions, it is proposed to develop the computing facilities, the application of which will significantly increase the productivity of the designer and reduce the complexity of designing. Methods of structural and parametric optimization have been adopted as the basis of the computing facilities. Their efficiency in the synthesis of design solutions is shown, also the schemes, that illustrate and explain the introduction of structural optimization in the traditional design of steel frames, are constructed. To solve the problem of synthesis and comparison of design solutions for steel frames, it is proposed to develop the computing facilities that significantly reduces the complexity of search designing and based on the use of methods of structural and parametric optimization.

Application of solution-processed V2O5 in inverted polymer solar cells based on fluorine-doped tin oxide substrate.

PubMed

Wu, Jian; Zhang, Yupeng; He, Yeyuan; Liu, Chunyu; Guolt, Wenbin; Ruan, Shengping

2014-06-01

We used a hydrothermal method to synthesis the solution-processed V2O5 as anode buffer layer, which applied on inverted polymer solar cells based on FTO substrate. The structure of the device is glass/FTO/TiO2/P3HT:PCBM/V2O5/Ag. We discussed the dependence of device performance on the concentrations of V2O5 solution. It is found that when the concentration of V2O5 is 300 microg/ml, the power conversion efficiency (PCE of 2.38%) is the highest, which is much higher than that of the device without anode buffer layer (PCE of only 0.87%). Moreover, it can significantly reduce the energy consumption and make it more cost-effective.

Scalable continuous flow synthesis of ZnO nanorod arrays in 3-D ceramic honeycomb substrates for low-temperature desulfurization

DOE PAGES

Wang, Sibo; Wu, Yunchao; Miao, Ran; ...

2017-07-26

Scalable and cost-effective synthesis and assembly of technologically important nanostructures in three-dimensional (3D) substrates hold keys to bridge the demonstrated nanotechnologies in academia with industrially relevant scalable manufacturing. In this paper, using ZnO nanorod arrays as an example, a hydrothermal-based continuous flow synthesis (CFS) method is successfully used to integrate the nano-arrays in multi-channeled monolithic cordierite. Compared to the batch process, CFS enhances the average growth rate of nano-arrays by 125%, with the average length increasing from 2 μm to 4.5 μm within the same growth time of 4 hours. The precursor utilization efficiency of CFS is enhanced by 9more » times compared to that of batch process by preserving the majority of precursors in recyclable solution. Computational fluid dynamic simulation suggests a steady-state solution flow and mass transport inside the channels of honeycomb substrates, giving rise to steady and consecutive growth of ZnO nano-arrays with an average length of 10 μm in 12 h. The monolithic ZnO nano-array-integrated cordierite obtained through CFS shows enhanced low-temperature (200 °C) desulfurization capacity and recyclability in comparison to ZnO powder wash-coated cordierite. This can be attributed to exposed ZnO {101¯0} planes, better dispersion and stronger interactions between sorbent and reactant in the ZnO nanorod arrays, as well as the sintering-resistance of nano-array configurations during sulfidation–regeneration cycles. Finally, with the demonstrated scalable synthesis and desulfurization performance of ZnO nano-arrays, a promising, industrially relevant integration strategy is provided to fabricate metal oxide nano-array-based monolithic devices for various environmental and energy applications.« less

Scalable continuous flow synthesis of ZnO nanorod arrays in 3-D ceramic honeycomb substrates for low-temperature desulfurization

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

Wang, Sibo; Wu, Yunchao; Miao, Ran

Scalable and cost-effective synthesis and assembly of technologically important nanostructures in three-dimensional (3D) substrates hold keys to bridge the demonstrated nanotechnologies in academia with industrially relevant scalable manufacturing. In this paper, using ZnO nanorod arrays as an example, a hydrothermal-based continuous flow synthesis (CFS) method is successfully used to integrate the nano-arrays in multi-channeled monolithic cordierite. Compared to the batch process, CFS enhances the average growth rate of nano-arrays by 125%, with the average length increasing from 2 μm to 4.5 μm within the same growth time of 4 hours. The precursor utilization efficiency of CFS is enhanced by 9more » times compared to that of batch process by preserving the majority of precursors in recyclable solution. Computational fluid dynamic simulation suggests a steady-state solution flow and mass transport inside the channels of honeycomb substrates, giving rise to steady and consecutive growth of ZnO nano-arrays with an average length of 10 μm in 12 h. The monolithic ZnO nano-array-integrated cordierite obtained through CFS shows enhanced low-temperature (200 °C) desulfurization capacity and recyclability in comparison to ZnO powder wash-coated cordierite. This can be attributed to exposed ZnO {101¯0} planes, better dispersion and stronger interactions between sorbent and reactant in the ZnO nanorod arrays, as well as the sintering-resistance of nano-array configurations during sulfidation–regeneration cycles. Finally, with the demonstrated scalable synthesis and desulfurization performance of ZnO nano-arrays, a promising, industrially relevant integration strategy is provided to fabricate metal oxide nano-array-based monolithic devices for various environmental and energy applications.« less

Titanium compounds as catalysts of higher alpha-olefin-based super-high-molecular polymers synthesis

NASA Astrophysics Data System (ADS)

Konovalov, K. B.; Kazaryan, M. A.; Manzhay, V. N.; Vetrova, O. V.

2016-01-01

The synthesis of polymers of 10 million or more molecular weight is a difficult task even in a chemical lab. Higher α-olefin-based polymer agents of such kind have found a narrow but quite important niche, the reduction of drag in the turbulent flow of hydrocarbon fluids such as oil and oil-products. In its turn, searching for a catalytic system capable to produce molecules of such a high length and to synthesize polymers of a low molecular-mass distribution is part of a global task of obtaining a high-quality product. In this paper we had observed a number of industrial catalysts with respect to their suitability for higher poly-α- olefins synthesis. A number samples representing copolymers of 1-hexene with 1-decene obtained on a previous generation catalyst, a microsphere titanium chloride catalytic agent had been compared to samples synthesized using a titanium-magnesium catalyst both in solution and in a polymer medium.

OPTICON: Pro-Matlab software for large order controlled structure design

NASA Technical Reports Server (NTRS)

Peterson, Lee D.

1989-01-01

A software package for large order controlled structure design is described and demonstrated. The primary program, called OPTICAN, uses both Pro-Matlab M-file routines and selected compiled FORTRAN routines linked into the Pro-Matlab structure. The program accepts structural model information in the form of state-space matrices and performs three basic design functions on the model: (1) open loop analyses; (2) closed loop reduced order controller synthesis; and (3) closed loop stability and performance assessment. The current controller synthesis methods which were implemented in this software are based on the Generalized Linear Quadratic Gaussian theory of Bernstein. In particular, a reduced order Optimal Projection synthesis algorithm based on a homotopy solution method was successfully applied to an experimental truss structure using a 58-state dynamic model. These results are presented and discussed. Current plans to expand the practical size of the design model to several hundred states and the intention to interface Pro-Matlab to a supercomputing environment are discussed.

Synthesis of GaN:ZnO solid solution by solution combustion method and characterization for photocatalytic application

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

Menon, Sumithra Sivadas; Anitha, R.; Baskar, K.

2016-05-23

GaN-ZnO solid solution has emerged as a successful and reproducible photocatalyst for overall water splitting by one-step photoexcitation, with a bandgap in visible region. When the solid solution is formed, some of the Zn and O ions are replaced by Ga and N ions respectively and there is a narrowing of bandgap which is hypothesized as due to Zn3d-N2p repulsion. The traditional method of synthesis of GaN-ZnO solid solution is by nitridation of the starting oxides under constant ammonia flow. Here we report a solution combustion technique for the synthesis of the solid solution at a temperature about 500 °more » C in a muffle furnace with metal nitrates as precursors and urea as the fuel. The as prepared samples showed change in color with the increased concentration of ZnO in the solution. The structural, microstructural, morphological and optical properties of the samples were realized by Powder X ray diffraction, Scanning electron microscopy, Energy dispersive X ray analysis, Transmission electron microscopy and Photoluminescence. Finally the hydrogen production efficiency of the GaN-ZnO nanopowders by water splitting was found, using methanol as a scavenger. The apparent quantum yield (AQY) of 0.048% is obtained for GaN-ZnO solid solution.« less

Immobilization, Regiospecificity Characterization and Application of Aspergillus oryzae Lipase in the Enzymatic Synthesis of the Structured Lipid 1,3-Dioleoyl-2-Palmitoylglycerol.

PubMed

Cai, Haiying; Li, Yang; Zhao, Minjie; Fu, Guanwen; Lai, Jia; Feng, Fengqin

2015-01-01

The enzymatic synthesis of 1,3-dioleoyl-2-palmitoylglycerol (OPO), one of the main components of human milk fats, has been hindered by the relatively high cost of sn-1,3-specific lipases and the deficiency in biocatalyst stability. The sn-1,3-specific lipase from Aspergillus oryzae (AOL) is highly and efficiently immobilized with the polystyrene-based hydrophobic resin D3520, with a significant 49.54-fold increase in specific lipase activity compared with the AOL powder in catalyzing the synthesis of OPO through the acidolysis between palm stearin and oleic acid (OA). The optimal immobilization conditions were investigated, including time course, initial protein concentration and solution pH. The sn-1,3 specificity of lipases under different immobilization conditions was evaluated and identified as positively associated with the lipase activity, and the pH of the immobilization solution influenced the regiospecificity and synthetic activity of these lipases. Immobilized AOL D3520, as the biocatalyst, was used for the enzymatic synthesis of the structured lipid OPO through the acidolysis between palm stearin and OA. The following conditions were optimized for the synthesis of structured lipid OPO: 65 °C temperature; 1:8 substrate molar ratio between palm stearin and OA; 8% (w/w) enzyme load; 3.5% water content of the immobilized lipase; and 1 h reaction time. Under these conditions, highly efficient C52 production (45.65%) was achieved, with a tripalmitin content of 2.75% and a sn-2 palmitic acid (PA) proportion of 55.08% in the system.

Controlling the growth of palladium aerogels with high-performance toward bioelectrocatalytic oxidation of glucose.

PubMed

Wen, Dan; Herrmann, Anne-Kristin; Borchardt, Lars; Simon, Frank; Liu, Wei; Kaskel, Stefan; Eychmüller, Alexander

2014-02-19

We report the controllable synthesis of Pd aerogels with high surface area and porosity by destabilizing colloidal solutions of Pd nanoparticles with variable concentrations of calcium ions. Enzyme electrodes based on Pd aerogels co-immobilized with glucose oxidase show high activity toward glucose oxidation and are promising materials for applications in bioelectronics.

Bio-Inspired Nanomaterials: Protein Cage Nano-Architectures

DTIC Science & Technology

2008-04-01

chemical modification of protein cage materials and controlled chemical synthesis under mild biological conditions. High- resolution structural...properties based on a combination of controlled mobility and metal ligand interactions. Using the exterior surface of the CCMV viral cage we have chemically ...follows: Patterning by microplotter was achieved by depositing a preselected antibody solution directly onto chemically activated silicon or gold

Library Automation Design for Visually Impaired People

ERIC Educational Resources Information Center

Yurtay, Nilufer; Bicil, Yucel; Celebi, Sait; Cit, Guluzar; Dural, Deniz

2011-01-01

Speech synthesis is a technology used in many different areas in computer science. This technology can bring a solution to reading activity of visually impaired people due to its text to speech conversion. Based on this problem, in this study, a system is designed needed for a visually impaired person to make use of all the library facilities in…

Synthesis of kaolinite-filled EPDM rubber composites by solution intercalation: structural characterization and studies on mechanical properties

NASA Astrophysics Data System (ADS)

Ginil Mon, S.; Jaya Vinse Ruban, Y.; Vetha Roy, D.

2011-09-01

In the large field of nanotechnology, polymer matrix-based nanocomposites have become a prominent area of current research and development. Exfoliated clay-based nanocomposites have dominated the polymer world with excellent characteristics. EPDM rubber composites have been synthesized by solution-intercalation using the easily available kaolinite as filler. The composite structure has been elucidated by X-ray diffraction (XRD), Fourier transform IR, and scanning electron microscope studies. The molecular level dispersion of clay layers has been verified by the disappearance of basal XRD peak of kaolinite in the EPDM/kaolinite composites. The mechanical properties showed significant improvement of EPDM/kaolinite composites with respect to neat EPDM.

Algorithms for synthesizing management solutions based on OLAP-technologies

NASA Astrophysics Data System (ADS)

Pishchukhin, A. M.; Akhmedyanova, G. F.

2018-05-01

OLAP technologies are a convenient means of analyzing large amounts of information. An attempt was made in their work to improve the synthesis of optimal management decisions. The developed algorithms allow forecasting the needs and accepted management decisions on the main types of the enterprise resources. Their advantage is the efficiency, based on the simplicity of quadratic functions and differential equations of only the first order. At the same time, the optimal redistribution of resources between different types of products from the assortment of the enterprise is carried out, and the optimal allocation of allocated resources in time. The proposed solutions can be placed on additional specially entered coordinates of the hypercube representing the data warehouse.

Accelerate synthesis in ecology and environmental sciences

USDA-ARS?s Scientific Manuscript database

Synthesis of diverse knowledge is a central part of all sciences, but especially those such as ecology and environmental sciences which draw information from many disciplines. Research and education in ecology are intrinsically synthetic, and synthesis is increasingly needed to find solutions for en...

Biochar-based nano-composites for the decontamination of wastewater: A review.

PubMed

Tan, Xiao-Fei; Liu, Yun-Guo; Gu, Yan-Ling; Xu, Yan; Zeng, Guang-Ming; Hu, Xin-Jiang; Liu, Shao-Bo; Wang, Xin; Liu, Si-Mian; Li, Jiang

2016-07-01

Synthesizing biochar-based nano-composites can obtain new composites and combine the advantages of biochar with nano-materials. The resulting composites usually exhibit great improvement in functional groups, pore properties, surface active sites, catalytic degradation ability and easy to separation. These composites have excellent abilities to adsorb a range of contaminants from aqueous solutions. Particularly, catalytic material-coated biochar can exert simultaneous adsorption and catalytic degradation function for organic contaminants removal. Synthesizing biochar-based nano-composites has become an important practice for expanding the environmental applications of biochar and nanotechnology. This paper aims to review and summarize the various synthesis techniques for biochar-based nano-composites and their effects on the decontamination of wastewater. The characteristic and advantages of existing synthesis methods are summarized and discussed. Application of biochar-based nano-composites for different contaminants removal and the underlying mechanisms are reviewed. Furthermore, knowledge gaps that exist in the fabrication and application of biochar-based nano-composites are also identified. Copyright © 2016 Elsevier Ltd. All rights reserved.

Efficacy of a Solution-Based Approach for Making Sodalite Waste Forms for an Oxide Reduction Salt Utilized in the Reprocessing of Used Uranium Oxide Fuel

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

Riley, Brian J.; Pierce, David A.; Frank, Steven M.

2015-04-01

This paper describes various approaches for making sodalite with a LiCl-Li2O oxide reduction salt used to recover uranium from used oxide fuel. The approaches include sol-gel and solution-based synthesis processes. As-made products were mixed with 5 and 10 mass% of a Na2O-B2O3-SiO2 glass binder and these, along with product without a binder, were heated using either a cold-press-and-sinter method or hot uniaxial pressing. The results demonstrate the limitation of sodalite yield due to the fast intermediate reactions between Na+ and Cl- to form halite in solution and Li2O and SiO2 to form lithium silicates (e.g., Li2SiO3 or Li2Si2O5) in themore » calcined and sintered pellets. The results show that pellets can be made with high sodalite fractions (~92 mass%) and low porosities using a solution-based approach and this LiCl-Li2O salt.« less

Experiments on and Numerical Modeling of the Capture and Concentration of Transcription-Translation Machinery inside Vesicles.

PubMed

Mavelli, Fabio; Stano, Pasquale

2015-01-01

Synthetic or semi-synthetic minimal cells are those cell-like artificial compartments that are based on the encapsulation of molecules inside lipid vesicles (liposomes). Synthetic cells are currently used as primitive cell models and are very promising tools for future biotechnology. Despite the recent experimental advancements and sophistication reached in this field, the complete elucidation of many fundamental physical aspects still poses experimental and theoretical challenges. The interplay between solute capture and vesicle formation is one of the most intriguing ones. In a series of studies, we have reported that when vesicles spontaneously form in a dilute solution of proteins, ribosomes, or ribo-peptidic complexes, then, contrary to statistical predictions, it is possible to find a small fraction of liposomes (<1%) that contain a very large number of solutes, so that their local (intravesicular) concentrations largely exceed the expected value. More recently, we have demonstrated that this effect (spontaneous crowding) operates also on multimolecular mixtures, and can drive the synthesis of proteins inside vesicles, whereas the same reaction does not proceed at a measurable rate in the external bulk phase. Here we firstly introduce and discuss these already published observations. Then, we present a computational investigation of the encapsulation of transcription-translation (TX-TL) machinery inside vesicles, based on a minimal protein synthesis model and on different solute partition functions. Results show that experimental data are compatible with an entrapment model that follows a power law rather than a Gaussian distribution. The results are discussed from the viewpoint of origin of life, highlighting open questions and possible future research directions.

Methods for synthesis of semiconductor nanocrystals and thermoelectric compositions

DOEpatents

Ren, Zhifeng [Newton, MA; Chen, Gang [Carlisle, MA; Poudel, Bed [Watertown, MA; Kumar, Shankar [Watertown, MA; Wang, Wenzhong [Newton, MA; Dresselhaus, Mildred [Arlington, MA

2007-08-14

The present invention provides methods for synthesis of IV VI nanostructures, and thermoelectric compositions formed of such structures. In one aspect, the method includes forming a solution of a Group IV reagent, a Group VI reagent and a surfactant. A reducing agent can be added to the solution, and the resultant solution can be maintained at an elevated temperature, e.g., in a range of about 20.degree. C. to about 360.degree. C., for a duration sufficient for generating nanoparticles as binary alloys of the IV VI elements.

Synthesis and Reactivity of a New (Methylene)Phosphine.

DTIC Science & Technology

1981-01-27

the synthesis of a variety of alkyl(silylamino)- 8phosphines Similarly, if two equivalents of the silylmethyl Grignard reagent were used (eq 3), the...n-BuLi (hexane solution), and t-BuLi (pentane solution). The Grignard reagent Me 3SiCH2 MgCl was prepared in Et 0 2 2 solution from Me3SiCH 2C and Mg...trimethylsilyl)amino] (chloro)- (trimethylsilylmethyl)phosphine (1) was prepared by the "one-pot" Grignard method (eqs 1 and 2) which we have used previously for

Methods for synthesis of semiconductor nanocrystals and thermoelectric compositions

NASA Technical Reports Server (NTRS)

Chen, Gang (Inventor); Poudel, Bed (Inventor); Kumar, Shankar (Inventor); Dresselhaus, Mildred (Inventor); Ren, Zhifeng (Inventor); Wang, Wenzhong (Inventor)

2007-01-01

The present invention provides methods for synthesis of IV VI nanostructures, and thermoelectric compositions formed of such structures. In one aspect, the method includes forming a solution of a Group IV reagent, a Group VI reagent and a surfactant. A reducing agent can be added to the solution, and the resultant solution can be maintained at an elevated temperature, e.g., in a range of about 20.degree. C. to about 360.degree. C., for a duration sufficient for generating nanoparticles as binary alloys of the IV VI elements.

Synthesis and triplex forming properties of pyrimidine derivative containing extended functionality.

PubMed

Gianolio, D A; McLaughlin, L W

1999-08-01

Two pyrimidine nucleosides have been synthesized containing extended hydrogen bonding functionality. In one case the side chain is based upon semicarbazide and in the second monoacetylated carbohydrazide was employed. DNA sequences could be prepared using both analogue nucleosides in a reverse coupling protocol, and provided that the normal capping step was eliminated and that the iodine-based oxidizing solution was replaced with one based upon 10-camphorsulfonyl oxaziridine. Both derivatives exhibited moderate effects in targeting selectively C-G base pairs embedded within a polypurine target sequence.

Design of Distributed Controllers Seeking Optimal Power Flow Solutions Under Communication Constraints

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

Dall'Anese, Emiliano; Simonetto, Andrea; Dhople, Sairaj

This paper focuses on power distribution networks featuring inverter-interfaced distributed energy resources (DERs), and develops feedback controllers that drive the DER output powers to solutions of time-varying AC optimal power flow (OPF) problems. Control synthesis is grounded on primal-dual-type methods for regularized Lagrangian functions, as well as linear approximations of the AC power-flow equations. Convergence and OPF-solution-tracking capabilities are established while acknowledging: i) communication-packet losses, and ii) partial updates of control signals. The latter case is particularly relevant since it enables asynchronous operation of the controllers where DER setpoints are updated at a fast time scale based on local voltagemore » measurements, and information on the network state is utilized if and when available, based on communication constraints. As an application, the paper considers distribution systems with high photovoltaic integration, and demonstrates that the proposed framework provides fast voltage-regulation capabilities, while enabling the near real-time pursuit of solutions of AC OPF problems.« less

Design of Distributed Controllers Seeking Optimal Power Flow Solutions under Communication Constraints: Preprint

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

Dall'Anese, Emiliano; Simonetto, Andrea; Dhople, Sairaj

This paper focuses on power distribution networks featuring inverter-interfaced distributed energy resources (DERs), and develops feedback controllers that drive the DER output powers to solutions of time-varying AC optimal power flow (OPF) problems. Control synthesis is grounded on primal-dual-type methods for regularized Lagrangian functions, as well as linear approximations of the AC power-flow equations. Convergence and OPF-solution-tracking capabilities are established while acknowledging: i) communication-packet losses, and ii) partial updates of control signals. The latter case is particularly relevant since it enables asynchronous operation of the controllers where DER setpoints are updated at a fast time scale based on local voltagemore » measurements, and information on the network state is utilized if and when available, based on communication constraints. As an application, the paper considers distribution systems with high photovoltaic integration, and demonstrates that the proposed framework provides fast voltage-regulation capabilities, while enabling the near real-time pursuit of solutions of AC OPF problems.« less

Synthesis and Examination of Nanocomposites Based on Poly(2-hydroxyethyl methacrylate) for Medicinal Use

NASA Astrophysics Data System (ADS)

Kukolevska, Olena S.; Gerashchenko, Igor I.; Borysenko, Mykola V.; Pakhlov, Evgenii M.; Machovsky, Michal; Yushchenko, Tetyana I.

2017-02-01

Preparation of poly(2-hydroxyethyl methacrylate) (PHEMA) based nanocomposites using different approaches such as synthesis with water as the porogen, filling of polymer matrix by silica and formation of interpenetrating polymer networks with polyurethane was demonstrated. Incorporation of various biologically active compounds (BAC) such as metronidazole, decamethoxin, zinc sulphate, silver nitrate or amino acids glycine and tryptophan into nanocomposites was achieved. BAC were introduced into the polymer matrix either (1) directly, or (2) with a solution of colloidal silica, or (3) through immobilization on silica (sol-densil). Morphology of prepared materials was investigated by laser scanning microscopy and low-vacuum scanning electron microscopy. In vacuum freeze-drying, prior imaging was proposed for improving visualization of the porous structure of composites. The interaction between PHEMA matrix and silica filler was investigated by IR spectroscopy. Adsorption of 2-hydroxyethyl methacrylate and BAC from aqueous solution on the silica surface was also examined. Phase composition and thermal stability of composites were studied by the differential thermogravimetry/differential thermal analysis. Release of BAC into water medium from prepared composites were shown to depend on the synthetic method and differed significantly. Obtained PHEMA-base materials which are characterized by controlled release of BAC have a strong potential for application in manufacturing of different surgical devices like implants, catheters and drainages.

Synthesis of 4-(5-iodo-3-methylpyrazolyl) phenylsulfonamide and its elaboration to a COX II inhibitor library by solution-phase suzuki coupling using Pd/C as a solid-supported catalyst.

PubMed

Organ, Michael G; Mayer, Stanislas

2003-01-01

An effective synthesis of 4-(5-iodo-3-methylpyrazolyl) phenylsulfonamide has been developed. This aromatic iodide template served as an efficient oxidative addition partner for the preparation of a solution-phase library of Celecoxib analogues via Suzuki coupling using Pd/C, a readily filterable catalyst.

Facile room-temperature solution-phase synthesis of a spherical covalent organic framework for high-resolution chromatographic separation.

PubMed

Yang, Cheng-Xiong; Liu, Chang; Cao, Yi-Meng; Yan, Xiu-Ping

2015-08-07

A simple and facile room-temperature solution-phase synthesis was developed to fabricate a spherical covalent organic framework with large surface area, good solvent stability and high thermostability for high-resolution chromatographic separation of diverse important industrial analytes including alkanes, cyclohexane and benzene, α-pinene and β-pinene, and alcohols with high column efficiency and good precision.

Surface-complexation synthesis of silica-supported high-loading well-dispersed reducible nano-Co3O4 catalysts using CoIII ammine hydroxo complexes

NASA Astrophysics Data System (ADS)

Zhang, Weidong; Pan, Feng; Li, Jinjun; Wang, Zhen; Ding, Wei; Qin, Yi; Wu, Feng

2018-06-01

Silica-supported highly dispersed cobalt oxides prepared by adsorption are likely to be poorly reducible Co-phyllosilicates or CoO species. Here we report the synthesis of silica-supported monodispersed spinel nano-Co3O4 catalysts by inner-sphere complexation using CoIII ammine hydroxo complexes as precursors. The precursors were facilely prepared by stirring ammoniacal CoII solutions exposed to air. The cobalt loadings (up to 188 mg/g) and particle sizes (3-10 nm) were tailored by successive complexation-calcination cycles. Such catalysts showed significantly superior reducibility and catalytic activity in complete propane oxidation in comparison to supported Co-phyllosilicates and CoO. A further development of this synthesis process may provide a variety of cobalt-based catalysts for important catalytic applications.

Green synthesis of silver nanoparticles using a Melissa officinalis leaf extract with antibacterial properties

NASA Astrophysics Data System (ADS)

de Jesús Ruíz-Baltazar, Álvaro; Reyes-López, Simón Yobbany; Larrañaga, Daniel; Estévez, Miriam; Pérez, Ramiro

The exceptional properties of the silver nanoparticles offer several applications in the biomedicine field. The development of antibiotics which are clinically useful against bacteria and drug resistant microorganisms, it is one of the main approaches of silver nanoparticles. However, it is necessary to develop environmentally friendly methods for their synthesis. In this sense, the main objective of this work is focused on to propose a simplified and efficient green synthesis of silver nanoparticles with proven antibacterial properties. The green synthesis route is based on the use of the Melissa officinalis as reducing agent of the silver ions in aqueous solution at room temperature. Complementary, the antibacterial activity of the silver nanoparticles against Staphylococcus aureus and Escherichia coli was confirmed. The silver nanoparticles obtained were characterized by transmission electron microscopy, X-ray diffraction, UV-vis, Raman and FT-IR spectroscopy. The observed results suggested that using Melissa officinalis, it is possible to performed silver nanoparticles with controlled characteristics and with significant inhibitory activity against the Staphylococcus aureus and Escherichia coli.

Flow chemistry to control the synthesis of nano and microparticles for biomedical applications.

PubMed

Hassan, Natalia; Oyarzun-Ampuero, Felipe; Lara, Pablo; Guerrero, Simón; Cabuil, Valérie; Abou-Hassan, Ali; Kogan, Marcelo J

2014-03-01

In this article we review the flow chemistry methodologies for the controlled synthesis of different kind of nano and microparticles for biomedical applications. Injection mechanism has emerged as new alternative for the synthesis of nanoparticles due to this strategy allows achieving superior levels of control of self-assemblies, leading to higher-ordered structures and rapid chemical reactions. Self-assembly events are strongly dependent on factors such as the local concentration of reagents, the mixing rates, and the shear forces, which can be finely tuned, as an example, in a microfluidic device. Injection methods have also proved to be optimal to elaborate microsystems comprising polymer solutions. Concretely, extrusion based methods can provide controlled fluid transport, rapid chemical reactions, and cost-saving advantages over conventional reactors. We provide an update of synthesis of nano and microparticles such as core/shell, Janus, nanocrystals, liposomes, and biopolymeric microgels through flow chemistry, its potential bioapplications and future challenges in this field are discussed.

Spray-combustion synthesis: Efficient solution route to high-performance oxide transistors

PubMed Central

Yu, Xinge; Smith, Jeremy; Zhou, Nanjia; Zeng, Li; Guo, Peijun; Xia, Yu; Alvarez, Ana; Aghion, Stefano; Lin, Hui; Yu, Junsheng; Chang, Robert P. H.; Bedzyk, Michael J.; Ferragut, Rafael; Marks, Tobin J.; Facchetti, Antonio

2015-01-01

Metal-oxide (MO) semiconductors have emerged as enabling materials for next generation thin-film electronics owing to their high carrier mobilities, even in the amorphous state, large-area uniformity, low cost, and optical transparency, which are applicable to flat-panel displays, flexible circuitry, and photovoltaic cells. Impressive progress in solution-processed MO electronics has been achieved using methodologies such as sol gel, deep-UV irradiation, preformed nanostructures, and combustion synthesis. Nevertheless, because of incomplete lattice condensation and film densification, high-quality solution-processed MO films having technologically relevant thicknesses achievable in a single step have yet to be shown. Here, we report a low-temperature, thickness-controlled coating process to create high-performance, solution-processed MO electronics: spray-combustion synthesis (SCS). We also report for the first time, to our knowledge, indium-gallium-zinc-oxide (IGZO) transistors having densification, nanoporosity, electron mobility, trap densities, bias stability, and film transport approaching those of sputtered films and compatible with conventional fabrication (FAB) operations. PMID:25733848

Spray-combustion synthesis: efficient solution route to high-performance oxide transistors.

PubMed

Yu, Xinge; Smith, Jeremy; Zhou, Nanjia; Zeng, Li; Guo, Peijun; Xia, Yu; Alvarez, Ana; Aghion, Stefano; Lin, Hui; Yu, Junsheng; Chang, Robert P H; Bedzyk, Michael J; Ferragut, Rafael; Marks, Tobin J; Facchetti, Antonio

2015-03-17

Metal-oxide (MO) semiconductors have emerged as enabling materials for next generation thin-film electronics owing to their high carrier mobilities, even in the amorphous state, large-area uniformity, low cost, and optical transparency, which are applicable to flat-panel displays, flexible circuitry, and photovoltaic cells. Impressive progress in solution-processed MO electronics has been achieved using methodologies such as sol gel, deep-UV irradiation, preformed nanostructures, and combustion synthesis. Nevertheless, because of incomplete lattice condensation and film densification, high-quality solution-processed MO films having technologically relevant thicknesses achievable in a single step have yet to be shown. Here, we report a low-temperature, thickness-controlled coating process to create high-performance, solution-processed MO electronics: spray-combustion synthesis (SCS). We also report for the first time, to our knowledge, indium-gallium-zinc-oxide (IGZO) transistors having densification, nanoporosity, electron mobility, trap densities, bias stability, and film transport approaching those of sputtered films and compatible with conventional fabrication (FAB) operations.

Synthesis of hexavalent molybdenum formo- and aceto-hydroxamates and deferoxamine via liquid-liquid metal partitioning

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

Breshears, Andrew T.; Brown, M. Alex; Bloom, Ira

We report a new method of crystal growth and synthesis based on liquid-liquid partitioning that allows for isolation and in-depth characterization of molybdenyl bis(formohydroxamate), Mo-FHA, molybdenyl bis(acetohydroxamate), Mo-AHA, and molybdenyl deferoxamine, Mo-DFO, for the first time. This novel approach affords shorter crystal growth time (hourly timeframe) without sacrificing crystal size or integrity when other methods of crystallization were unsuccessful. All three Mo complexes are characterized in solution via FTIR, NMR, UV-vis, and EXAFS spectroscopy. Mo-AHA and Mo-FHA structures are resolved by single crystal X-ray diffraction. Using the molybdenyl hydroxamate structural information, the speciation of Mo in a siderophore complex (Mo-DFO)more » is determined via complimentary spectroscopic methods and confirmed by DFT calculations. ESI-MS verifies that a complex of 1:1 molybdenum to deferoxamine is present in solution. Additionally, the Mo solution speciation in the precursor organic phase, MoO2(NO3)2HEH[EHP]2 (where HEH[EHP] is 2-ethylhexylphosphonic acid mono-2-ethylhexyl ester), is characterized by FTIR and EXAFS spectroscopy as well as DFT calculations.« less

Solution combustion synthesis of oxide semiconductors

NASA Astrophysics Data System (ADS)

Thomas, Abegayl Lorenda Shara-Lynn

The quest for stable and efficient photocatalytic materials beyond TiO2 and WO3 has over the years led to the development of new materials that possess varied interfacial energetics. This dissertation study focused on using for the first time a novel method, solution combustion synthesis (SCS), to prepare two distinct families of binary metal-based oxide semiconductor materials. Detailed studies on material characteristics and applications were carried out on tungsten- and niobium-based oxide semiconductors with varying principal metals. Initial emphasis was placed on the SCS of tungsten-based oxide semiconductors (ZnWO4, CuWO4, and Ag2WO4). The influence of different tungsten precursor's on the resultant product was of particular relevance to this study, with the most significant effects highlighted. Upon characterization, each sample's photocatalytic activity towards methyl orange dye degradation was studied, and benchmarked against their respective commercial oxide sample, obtained by solid-state ceramic synthesis. Detailed analysis highlighted the importance of the SCS process as a time- and energy-efficient method to produce crystalline nano-sized materials even without additional or excessive heat treatment. It was observed that using different tungstate precursors does influence the structural and morphological make-up of the resulting materials. The as-synthesized tungstate materials showed good photocatalytic performance for the degradation of methyl orange dye, while taking into account specific surface area and adsorbed dye amount on the surface of the material. Like the tungstate's, niobium-based oxide semiconductors CuNb 2O6 and ZnNb2O6 were the first to be synthesized via solution combustion synthesis. Particular attention was placed on the crystal structures formed while using an oxalate niobium precursor during the reaction process. X-ray patterns yielded a multiphase structure for the ZnNb2O6 and a single phase structure for CuNb 2O6. Photoelectrochemical (PEC) measurements were used both as a characterization tool as well as an application for CO2 reduction. The PEC data was consistent with an n-type and p-type semiconductor for ZnNb 2O6 and CuNb2O6 respectively. Good phototelectrochemical behavior was observed for CuNb2O6 with stable, high photocurrents suggesting a suitable material for CO 2 reduction while in a 0.1 M NaHCO3 + CO2 medium. All in all, this dissertation study expounds on metal ion insertion into various structural frameworks (e.g. WO3) which may open sustainable materials chemistry avenues to solar energy conversion and environmental remediation.

Secondary Crystal Growth on a Cracked Hydrotalcite-Based Film Synthesized by the Sol-Gel Method.

PubMed

Lee, Wooyoung; Lee, Chan Hyun; Lee, Ki Bong

2016-05-02

The sol-gel synthesis method is an attractive technology for the fabrication of ceramic films due to its preparation simplicity and ease of varying the metal composition. However, this technique presents some limitations in relation to the film thickness. Notably, when the film thickness exceeds the critical limit, large tensile stresses occur, resulting in a cracked morphology. In this study, a secondary crystal growth method was introduced as a post-treatment process for Mg/Al hydrotalcite-based films synthesized by the sol-gel method, which typically present a cracked morphology. The cracked hydrotalcite-based film was hydrothermally treated for the secondary growth of hydrotalcite crystals. In the resulting film, hydrotalcite grew with a vertical orientation, and the gaps formed during the sol-gel synthesis were filled with hydrotalcite after the crystal growth. The secondary crystal growth method provides a new solution for cracked ceramic films synthesized by the sol-gel method.

Lipase Catalysed Synthesis of Furan Based Oligoesters and their Self-Assembly Assisted Polymerization.

PubMed

Subbiah, Nagarajan; K, Muthusamy; Krishnamoorthy, Lalitha; Yadavali, Siva Prasad; Ayyapillai, Thamizhanban; Vellaisamy, Sridharan; C Uma, Maheswari

2018-05-11

Bio-based polyesters are well-known biodegradable materials that are frequently used in our daily life, which include food industries and biomedical fields. The journey towards the development of sustainable polymer materials and technology postulate the replacement of traditionally using petrochemical-based monomers, transition metal catalyst, and more intensive purification techniques, which do not agree with the green chemistry principles. This contribution investigates the synthesis of bio-based hydrophilic and hydrophobic oligoesters, which in turn derived from easily accessible monomers of natural resources. In addition to the selection of renewable monomers, Novozyme 435, an immobilized lipase B from Candida antarctica was used for the oligomerization of monomers. The reaction condition for oligomerization using Novozyme 435 was established to get moderate to good yield. To our delight, oligoester derived from hydrophilic monomer was found to self-assemble to form a viscous solution, which on further heating resulted in the formation of polymer via the intermolecular Diels-Alder reaction. The viscosity of solution and assembly of oligoester to form fibrous structure was investigated by rheological studies, XRD and SEM. Both oligoesters and polymers were completely characterized. For the first time we are reporting the assembly assisted polymerization of oligoester using intermolecular Diels-Alder reaction, which would initiate a new avenue in polymer science field. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Synthesis and Base Hydrolysis of a Cobalt(III) Complex Coordinated by a Thioether Ligand

ERIC Educational Resources Information Center

Roecker, Lee

2008-01-01

A two-week laboratory experiment for students in advanced inorganic chemistry is described. Students prepare and characterize a cobalt(III) complex coordinated by a thioether ligand during the first week of the experiment and then study the kinetics of Co-S bond cleavage in basic solution during the second week. The synthetic portion of the…

Base induced chemical conversion of 3-carbamoyl-2-isoxazolines.

PubMed

Nishiwaki, Nagatoshi; Maki, Asaka; Ariga, Masahiro

2009-01-01

3-Carbamoyl-2-isoxazolines, prepared by cycloaddition of functionalized nitrile oxide, serve as masked 3-unsubstituted isoxazolines to afford 2-isoxazoline-3-carboxylic acid, beta-cyanoalcohol, alpha,beta-unsaturated nitrile, and alpha,beta-unsaturated amide upon heating in the alkaline solution. The present reaction is also applicable to synthesis of 3,4-difunctionalized isoxazoles and beta-hydroxy-gamma-lactone.

Chemical synthesis of oriented ferromagnetic LaSr-2 × 4 manganese oxide molecular sieve nanowires

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

Carretero-Genevrier, Adrián; Gazquez, Jaume; Magen, Cesar

2012-04-25

Here we report a chemical solution based method using nanoporous track-etched polymer templates for producing long and oriented LaSr-2 × 4 manganese oxide molecular sieve nanowires. Scanning transmission electron microscopy and electron energy loss spectroscopy analyses show that the nanowires are ferromagnetic at room temperature, single crystalline, epitaxially grown and self-aligned.

Low-temperature metal-oxide thin-film transistors formed by directly photopatternable and combustible solution synthesis.

PubMed

Rim, You Seung; Lim, Hyun Soo; Kim, Hyun Jae

2013-05-01

We investigated the formation of ultraviolet (UV)-assisted directly patternable solution-processed oxide semiconductor films and successfully fabricated thin-film transistors (TFTs) based on these films. An InGaZnO (IGZO) solution that was modified chemically with benzoylacetone (BzAc), whose chelate rings decomposed via a π-π* transition as result of UV irradiation, was used for the direct patterning. A TFT was fabricated using the directly patterned IGZO film, and it had better electrical characteristics than those of conventional photoresist (PR)-patterned TFTs. In addition, the nitric acid (HNO3) and acetylacetone (AcAc) modified In2O3 (NAc-In2O3) solution exhibited both strong UV absorption and high exothermic reaction. This method not only resulted in the formation of a low-energy path because of the combustion of the chemically modified metal-oxide solution but also allowed for photoreaction-induced direct patterning at low temperatures.

Extraction of Boron Nitride Nanotubes and Fabrication of Macroscopic Articles Using Chlorosulfonic Acid.

PubMed

Adnan, Mohammed; Marincel, Daniel M; Kleinerman, Olga; Chu, Sang-Hyon; Park, Cheol; Hocker, Samuel J A; Fay, Catharine; Arepalli, Sivaram; Talmon, Yeshayahu; Pasquali, Matteo

2018-03-14

Due to recent advances in high-throughput synthesis, research on boron nitride nanotubes (BNNTs) is moving toward applications. One future goal is the assembly of macroscopic articles of high-aspect-ratio, pristine BNNTs. However, these articles are presently unattainable because of insufficient purification and fabrication methods. We introduce a solution process for extracting BNNTs from synthesis impurities without sonication or the use of surfactants and proceed to convert the extracted BNNTs into thin films. The solution process can also be used to convert as-synthesized material-which contains significant amounts of hexagonal boron nitride ( h-BN)-into mats and aerogels with controllable structure and dimension. The solution extraction method, combined with further advances in synthesis and purification, contributes to the development of all-BNNT macroscopic articles, such as fibers and 3-D structures.

Structural and optical properties of novel surfactant-coated Yb@TiO2 nanoparticles

NASA Astrophysics Data System (ADS)

Calandra, P.; Lombardo, D.; Pistone, A.; Turco Liveri, V.; Trusso, S.

2011-11-01

In this paper a novel hybrid approach to synthesise composite nanoparticles is presented. It is based on the laser ablation of a bulk target (Yb) immersed in a reversed micellar solution which contains nanoparticles of a different host material (TiO2 nanoparticles) previously synthesised by chemical method. This approach thus exploits the advantages of the chemical synthesis through reversed micellar solution (size control, nanoparticle stabilisation), and of the laser ablation ("clean" synthesis, no side reactions). Central role is played by the microscopic processes controlling the deposition of the ablated Yb atoms onto the surface of TiO2 nanoparticles which actually behave as nucleation seeds. The structural features of the resulting Yb@TiO2 composite nanoparticles have been studied by Transmission Electron Microscopy, whereas their peculiar optical properties have been explored by UV-Vis spectroscopy and steady-state fluorescence. Results consistently show the formation of Yb and TiO2 glued nanodomains to form nearly spherical and non-interacting nanoparticles with enhanced photophysical properties.

Synthesis and characterization of magnetic of Ni/ABS nanocomposites by electrical explosion of wire in liquid and solution blending methods

NASA Astrophysics Data System (ADS)

Thuyet-Nguyen, Minh; Hai-Nguyen, Hong; Kim, Won Joo; Kim, Ho Yoon; Kim, Jin-Chun

2017-03-01

Nanomaterials have attracted great attention from chemists, physicists and materials scientists because of their application benefits and special properties. Thermoplastics have been used in many applications such as molding of non-electrical components, conducting, magnetic field and 3D printing. Nanocomposites are known as a material which blends the best properties of components, a high performance material exhibits unusual property combinations and unique design possibilities. In this research, we focused to investigate and report primary results in the synthesis of magnetic nanocomposites based on acrylonitrile butadiene styrene (ABS), which are useful and important thermoplastics. Nickel nanopowder was prepared by electrical explosion of wire in a liquid were used as magnetic component. The composites were prepared by following steps, first the obtained Ni nanopowders were incorporated into the ABS matrix via a solution blending method (drop-casting), and then the solvent was evaporated. The characterizations of obtaining composites were analyzed by field emission scanning electron microscopy, X-Ray Diffraction analysis and vibrating sample magnetometer.

Solvothermal synthesis of nanocrystalline TiO 2 in toluene with surfactant

NASA Astrophysics Data System (ADS)

Kim, Chung-Sik; Moon, Byung Kee; Park, Jong-Ho; Choi, Byung-Chun; Seo, Hyo-Jin

2003-10-01

Synthesis of narrow-dispersed nanocrystalline TiO 2 was investigated by surfactant-aided solvothermal synthetic method in toluene solutions. Titanium isopropoxide (TIP) was used as precursor, which was decomposed at high temperature in the surfactant-dissolved solution. After the solution was thermally treated at 250°C for 20 h in an autoclave, low-dispersed TiO 2 nanocrystalline particles with average size of <6 nm were synthesized. When sufficient amount of TIP or surfactant was added in the solution, long dumbbell-shaped nanorods were formed, which may be due to the oriented growth of particles along [0 0 1] axis. Characterization of products was investigated by X-ray diffraction and transmission electron microscopy.

A facile synthesis of α-MnO2 used as a supercapacitor electrode material: The influence of the Mn-based precursor solutions on the electrochemical performance

NASA Astrophysics Data System (ADS)

Li, Wenyao; Xu, Jiani; Pan, Yishuang; An, Lei; Xu, Kaibing; Wang, Guangjin; Yu, Zhishui; Yu, Li; Hu, Junqing

2015-12-01

Three types of α-MnO2 nanomaterials are synthesized in different Mn-based precursor solutions by using a facile electrochemical deposition at the same depositional condition. The relationships between the precursor solutions and corresponding MnO2 nanomaterials' morphology as well as the electrochemical performance have been studied. As an electrode, electrochemical measurements show that the MnO2 deposited in MnCl2 precursor solution (MnO2-P3) exhibits an enhanced specific capacitance (318.9 F g-1 at 2 mV s-1). Moreover, this electrode demonstrates a good rate capability with 44% retention, which is higher than the MnO2-P1 deposited with Mn(CH3COOH)2 solution and the MnO2-P2 deposited with Mn(NO3)2 precursor solution. Besides, the specific capacitance of the MnO2-P3 electrode nearly has 98.2% retention after 2000 cycles, showing good long-term cycle stability. These findings show that the MnO2-P3 is a promising electrode material for supercapacitors.

Synthesis and characterization of dextran-coated iron oxide nanoparticles

NASA Astrophysics Data System (ADS)

Predescu, Andra Mihaela; Matei, Ecaterina; Berbecaru, Andrei Constantin; Pantilimon, Cristian; Drăgan, Claudia; Vidu, Ruxandra; Predescu, Cristian; Kuncser, Victor

2018-03-01

Synthesis and characterization of iron oxide nanoparticles coated with a large molar weight dextran for environmental applications are reported. The first experiments involved the synthesis of iron oxide nanoparticles which were coated with dextran at different concentrations. The synthesis was performed by a co-precipitation technique, while the coating of iron oxide nanoparticles was carried out in solution. The obtained nanoparticles were characterized by using scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction spectrometry, Fourier transform infrared spectroscopy and superconducting quantum interference device magnetometry. The results demonstrated a successful coating of iron oxide nanoparticles with large molar weight dextran, of which agglomeration tendency depended on the amount of dextran in the coating solution. SEM and TEM observations have shown that the iron oxide nanoparticles are of about 7 nm in size.

The Synthesis of Copper(II) Carboxylates Revisited

ERIC Educational Resources Information Center

Kushner, Kevin; Spangler, Robert E.; Salazar, Ralph A., Jr.; Lagowski, J. J.

2006-01-01

An electrochemical synthesis of copper(II) carboxylates has been developed and used in the general chemistry laboratory course for chemistry majors. This synthesis, using nonaqueous solutions, supplements the strategy of providing experiences in synthetic chemistry described by Yoder et al. ("J. Chem. Educ." 1995, 72, 267). (Contains 1 table.)

A Novel Thermal Electrochemical Synthesis Method for Production of Stable Colloids of "Naked" Metal (Ag) Nanocrystals

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

Hu, Michael Z.; Easterly, Clay E

Solution synthesis of nanocrystal silver is reviewed. This paper reports a novel thermal electrochemical synthesis (TECS) for producing metal Ag nanocrystals as small as a few nanometers. The TECS method requires mild conditions (25-100oC), low voltage (1-50 V DC) on Ag electrodes, and simple water or aqueous solutions as reaction medium. Furthermore, a tubular dialysis membrane surround electrodes proves favorable to produce nanosized (<10 nm) Ag nanocrystals. Different from those nanocrystals reported in literature, our nanocrystals have several unique features: (1) small nanometer size, (2) nakedness , i.e., surfaces of metal nanocrystals are free of organic ligands or capping moleculesmore » and no need of dispersant in synthesis solutions, and (3) colloidally stable in water solutions. It was discovered that Ag nanoparticles with initially large size distribution can be homogenized into near-monodispersed system by a low power (< 15 mW) He-Ne laser exposure treatment. The combination of the TECS technique and the laser treatment could lead to a new technology that produces metal nanoparticles that are naked, stable, and uniform sized. In the presence of stabilizing agent (also as supporting electrolyte) such as polyvinyl alcohol (PVA), large yield of silver nanoparticles (<100nm) in the form of thick milky sols are produced.« less

Combustion synthesis continuous flow reactor

DOEpatents

Maupin, G.D.; Chick, L.A.; Kurosky, R.P.

1998-01-06

The present invention is a reactor for combustion synthesis of inorganic powders. The reactor includes a reaction vessel having a length and a first end and a second end. The reaction vessel further has a solution inlet and a carrier gas inlet. The reactor further has a heater for heating both the solution and the carrier gas. In a preferred embodiment, the reaction vessel is heated and the solution is in contact with the heated reaction vessel. It is further preferred that the reaction vessel be cylindrical and that the carrier gas is introduced tangentially into the reaction vessel so that the solution flows helically along the interior wall of the reaction vessel. As the solution evaporates and combustion produces inorganic material powder, the carrier gas entrains the powder and carries it out of the reactor. 10 figs.

Combustion synthesis continuous flow reactor

DOEpatents

Maupin, Gary D.; Chick, Lawrence A.; Kurosky, Randal P.

1998-01-01

The present invention is a reactor for combustion synthesis of inorganic powders. The reactor includes a reaction vessel having a length and a first end and a second end. The reaction vessel further has a solution inlet and a carrier gas inlet. The reactor further has a heater for heating both the solution and the carrier gas. In a preferred embodiment, the reaction vessel is heated and the solution is in contact with the heated reaction vessel. It is further preferred that the reaction vessel be cylindrical and that the carrier gas is introduced tangentially into the reaction vessel so that the solution flows helically along the interior wall of the reaction vessel. As the solution evaporates and combustion produces inorganic material powder, the carrier gas entrains the powder and carries it out of the reactor.

A Review of RedOx Cycling of Solid Oxide Fuel Cells Anode

PubMed Central

Faes, Antonin; Hessler-Wyser, Aïcha; Zryd, Amédée; Van Herle, Jan

2012-01-01

Solid oxide fuel cells are able to convert fuels, including hydrocarbons, to electricity with an unbeatable efficiency even for small systems. One of the main limitations for long-term utilization is the reduction-oxidation cycling (RedOx cycles) of the nickel-based anodes. This paper will review the effects and parameters influencing RedOx cycles of the Ni-ceramic anode. Second, solutions for RedOx instability are reviewed in the patent and open scientific literature. The solutions are described from the point of view of the system, stack design, cell design, new materials and microstructure optimization. Finally, a brief synthesis on RedOx cycling of Ni-based anode supports for standard and optimized microstructures is depicted. PMID:24958298

Modular synthesis of a dual metal-dual semiconductor nano-heterostructure

DOE PAGES

Amirav, Lilac; Oba, Fadekemi; Aloni, Shaul; ...

2015-04-29

Reported is the design and modular synthesis of a dual metal-dual semiconductor heterostructure with control over the dimensions and placement of its individual components. Analogous to molecular synthesis, colloidal synthesis is now evolving into a series of sequential synthetic procedures with separately optimized steps. Here we detail the challenges and parameters that must be considered when assembling such a multicomponent nanoparticle, and their solutions.

Gum ghatti mediated, one pot green synthesis of optimized gold nanoparticles: Investigation of process-variables impact using Box-Behnken based statistical design.

PubMed

Alam, Md Sabir; Garg, Arun; Pottoo, Faheem Hyder; Saifullah, Mohammad Khalid; Tareq, Abu Izneid; Manzoor, Ovais; Mohsin, Mohd; Javed, Md Noushad

2017-11-01

Due to unique inherent catalytic characteristics of different size, shape and surface functionalized gold nanoparticles, their potential applications, are being explored in various fields such as drug delivery, biosensor, diagnosis and theranostics. However conventional process for synthesis of these metallic nanoparticles utilizes toxic reagents as reducing agents, additional capping agent for stability as well as surface functionalization for drug delivery purposes. Hence, in this work suitability of gum Ghatti for reducing, capping and surface functionalization during the synthesis of stable Gold nanoparticles were duly explored. Role and impact of key process variables i.e. volume of chloroauric acid solution, gum solution and temperature at their respective three different levels, as well as mechanism of formation of optimized gold nanoparticles were also investigated using Box- Behnken design. These novel synthesized optimized Gold nanoparticles were further characterized by UV spectrophotometer for its surface plasmon resonance (SPR) at around ∼530nm, dynamic light scattering (DLS) for its hydrodynamic size (112.5nm), PDI (0.222) and zeta potential (-21.3mV) while, transmission electron microscopy (TEM) further revealed surface geometry of these nanoparticles being spherical in shape. Copyright © 2017 Elsevier B.V. All rights reserved.

Facile Fabrication of Platinum-Cobalt Alloy Nanoparticles with Enhanced Electrocatalytic Activity for a Methanol Oxidation Reaction

PubMed Central

Huang, Huihong; Hu, Xiulan; Zhang, Jianbo; Su, Nan; Cheng, JieXu

2017-01-01

Decreasing the cost associated with platinum-based catalysts along with improving their catalytic properties is a major challenge for commercial direct methanol fuel cells. In this work, a simple and facile strategy was developed for the more efficient preparation of multi-walled carbon nanotube (MWCNT) -supported Pt/CoPt composite nanoparticles (NPs) via solution plasma sputtering with subsequent thermal annealing. Quite different from general wet synthesis methods, Pt/CoPt composite NPs were directly derived from metal wire electrodes without any additions. The obtained Pt/CoPt/MWCNTs composite catalysts exhibited tremendous improvement in the electro-oxidation of methanol in acidic media with mass activities of 1719 mA mg−1Pt. This value is much higher than that of previous reports of Pt-Co alloy and commercial Pt/C (3.16 times) because of the many active sites and clean surface of the catalysts. The catalysts showed good stability due to the special synergistic effects of the CoPt alloy. Pt/CoPt/MWCNTs can be used as a promising catalyst for direct methanol fuel cells. In addition, this solution plasma sputtering-assisted synthesis method introduces a general and feasible route for the synthesis of binary alloys. PMID:28358143

Green synthesis of palm oil mill effluent-based graphenic adsorbent for the treatment of dye-contaminated wastewater.

PubMed

Teow, Yeit Haan; Nordin, Nadzirah Ilyiani; Mohammad, Abdul Wahab

2018-05-12

Textile wastewater contains methylene blue (MB), a major coloring agent in textile industry. Activated carbon (AC) is the most widely used adsorbent in removing dyes from industrial wastewater. However, high production cost of AC is the major obstacle for its wide application in dye wastewater treatment. In this study, a sustainable approach in synthesizing graphenic adsorbent from palm oil mill effluent (POME), a potential carbonaceous source, has been explored. This new development in adsorption technique is considered as green synthesis as it does not require any binder during the synthesis process, and at the same time, it helps to solve the bottleneck of palm oil industry as POME is the main cause contributed to Malaysia's water pollution problem. The synthesized GSC was characterized through XRD, FESEM, and EDX. The adsorption performance of the synthesized GSC was evaluated by adsorption of MB. The effect of initial concentration of synthetic MB solution (1-20 mg/L) and weight of GSC (5-20 g) were investigated. A remarkable change in color of synthetic MB solution from blue to crystal clear was observed at the end of adsorption study. High efficiency of the synthesized GSC for dye-contaminated wastewater treatment is concluded.

Effect of reaction solvent on hydroxyapatite synthesis in sol-gel process

NASA Astrophysics Data System (ADS)

Nazeer, Muhammad Anwaar; Yilgor, Emel; Yagci, Mustafa Baris; Unal, Ugur; Yilgor, Iskender

2017-12-01

Synthesis of hydroxyapatite (HA) through sol-gel process in different solvent systems is reported. Calcium nitrate tetrahydrate (CNTH) and diammonium hydrogen phosphate (DAHP) were used as calcium and phosphorus precursors, respectively. Three different synthesis reactions were carried out by changing the solvent media, while keeping all other process parameters constant. A measure of 0.5 M aqueous DAHP solution was used in all reactions while CNTH was dissolved in distilled water, tetrahydrofuran (THF) and N,N-dimethylformamide (DMF) at a concentration of 0.5 M. Ammonia solution (28-30%) was used to maintain the pH of the reaction mixtures in the 10-12 range. All reactions were carried out at 40 ± 2°C for 4 h. Upon completion of the reactions, products were filtered, washed and calcined at 500°C for 2 h. It was clearly demonstrated through various techniques that the dielectric constant and polarity of the solvent mixture strongly influence the chemical structure and morphological properties of calcium phosphate synthesized. Water-based reaction medium, with highest dielectric constant, mainly produced β-calcium pyrophosphate (β-CPF) with a minor amount of HA. DMF/water system yielded HA as the major phase with a very minor amount of β-CPF. THF/water solvent system with the lowest dielectric constant resulted in the formation of pure HA.

Drastic nickel ion removal from aqueous solution by curcumin-capped Ag nanoparticles

NASA Astrophysics Data System (ADS)

Bettini, S.; Pagano, R.; Valli, L.; Giancane, G.

2014-08-01

A completely green synthesis protocol has been adopted to obtain silver nanoaggregates capped by the natural compound (1E, 6E)-1,7-bis(4-hydroxy-3-methoxyphenyl)-1,6-heptadiene-3,5-diene), also known as curcumin. The synthesis has been monitored by infrared, Raman, visible and fluorescence spectroscopies. Characterization confirms that curcumin reduces and caps the nanoparticles, and such a procedure allows its solubility in water and drastically increases curcumin stability. Silver nanoparticles (AgNPs)/curcumin complex has been dispersed in a water solution containing a known nickel ion concentration. After three days, a grey precipitate is observed and nickel concentration in the solution is reduced by about 70%.A completely green synthesis protocol has been adopted to obtain silver nanoaggregates capped by the natural compound (1E, 6E)-1,7-bis(4-hydroxy-3-methoxyphenyl)-1,6-heptadiene-3,5-diene), also known as curcumin. The synthesis has been monitored by infrared, Raman, visible and fluorescence spectroscopies. Characterization confirms that curcumin reduces and caps the nanoparticles, and such a procedure allows its solubility in water and drastically increases curcumin stability. Silver nanoparticles (AgNPs)/curcumin complex has been dispersed in a water solution containing a known nickel ion concentration. After three days, a grey precipitate is observed and nickel concentration in the solution is reduced by about 70%. Electronic supplementary information (ESI) available. See DOI: 10.1039/c4nr02583k

Polarization-sensitive nanowire photodetectors based on solution-synthesized CdSe quantum-wire solids.

PubMed

Singh, Amol; Li, Xiangyang; Protasenko, Vladimir; Galantai, Gabor; Kuno, Masaru; Xing, Huili Grace; Jena, Debdeep

2007-10-01

Polarization-sensitive photodetectors are demonstrated using solution-synthesized CdSe nanowire (NW) solids. Photocurrent action spectra taken with a tunable white light source match the solution linear absorption spectra of the NWs, showing that the NW network is responsible for the device photoconductivity. Temperature-dependent transport measurements reveal that carriers responsible for the dark current through the nanowire solids are thermally excited across CdSe band gap. The NWs are aligned using dielectrophoresis between prepatterned electrodes using conventional optical photolithography. The photocurrent through the NW solid is found to be polarization-sensitive, consistent with complementary absorption (emission) measurements of both single wires and their ensembles. The range of solution-processed semiconducting NW materials, their facile synthesis, ease of device fabrication, and compatibility with a variety of substrates make them attractive for potential nanoscale polarization-sensitive photodetectors.

Ultrathin SnO2 nanorods: template- and surfactant-free solution phase synthesis, growth mechanism, optical, gas-sensing, and surface adsorption properties.

PubMed

Xi, Guangcheng; Ye, Jinhua

2010-03-01

A novel template- and surfactant-free low temperature solution-phase method has been successfully developed for the controlled synthesis of ultrathin SnO(2) single-crystalline nanorods for the first time. The ultrathin SnO(2) single-crystalline nanorods are 2.0 +/- 0.5 nm in diameter, which is smaller than its exciton Bohr radius. The ultrathin SnO(2) nanorods show a high specific area (191.5 m(2) g(-1)). Such a thin SnO(2) single-crystalline nanorod is new in the family of SnO(2) nanostrucures and presents a strong quantum confinement effect. Its formation depends on the reaction temperature as well as on the concentration of the urea solution. A nonclassical crystallization process, Ostwald ripening process followed by an oriented attachment mechanism, is proposed based on the detailed observations from a time-dependent crystal evolution process. Importantly, such structured SnO(2) has shown a strong structure-induced enhancement of gas-sensing properties and has exhibited greatly enhanced gas-sensing property for the detection of ethanol than that of other structured SnO(2), such as the powders of nanobelts and microrods. Moreover, these ultrathin SnO(2) nanorods exhibit excellent ability to remove organic pollutant in wastewater by enormous surface adsorption. These properties are mainly attributed to its higher surface-to-volume ratio and ultrathin diameter. This work provides a novel low temperature, green, and inexpensive pathway to the synthesis of ultrathin nanorods, offering a new material form for sensors, solar cells, catalysts, water treatments, and other applications.

Wavelet-based adaptive thresholding method for image segmentation

NASA Astrophysics Data System (ADS)

Chen, Zikuan; Tao, Yang; Chen, Xin; Griffis, Carl

2001-05-01

A nonuniform background distribution may cause a global thresholding method to fail to segment objects. One solution is using a local thresholding method that adapts to local surroundings. In this paper, we propose a novel local thresholding method for image segmentation, using multiscale threshold functions obtained by wavelet synthesis with weighted detail coefficients. In particular, the coarse-to- fine synthesis with attenuated detail coefficients produces a threshold function corresponding to a high-frequency- reduced signal. This wavelet-based local thresholding method adapts to both local size and local surroundings, and its implementation can take advantage of the fast wavelet algorithm. We applied this technique to physical contaminant detection for poultry meat inspection using x-ray imaging. Experiments showed that inclusion objects in deboned poultry could be extracted at multiple resolutions despite their irregular sizes and uneven backgrounds.

Synthesis, structures, and solution dynamics of tetrasubstituted nine-atom germanium deltahedral clusters.

PubMed

Li, Feng; Sevov, Slavi C

2014-08-27

Reported are the rational synthesis, structures, and solution dynamics of three tetrasubstituted and neutral Ge9-based deltahedral clusters [Ge9R3R'](0), where R = Si(SiMe3)3 and R' = Et (1), Sn(n)Bu3 (2), or Tl (3). The first step of the synthesis is a reaction of an acetonitrile suspension of the intermetallic precursor compound K4Ge9 with {Si(SiMe3)3}Cl which produces the trisubstituted monoanions [Ge9{Si(SiMe3)3}](-). A benzene suspension of the latter is then reacted with Sn(n)Bu3Cl or TlCp to produce 2 and 3, respectively, while the same acetonitrile solution is reacted with EtBr in order to produce 1. All three structures can be viewed as tricapped trigonal prisms of Ge9 with the three "hypersilyl" substituents, Si(SiMe3)3, exo-bonded to the capping atoms. The fourth substituent in 1, the ethyl group, is exo-bonded to one of the six available Ge atoms with the Ge-C bond positioned radially to the Ge9 core. In the case of 2, on the other hand, the tin fragment is found above one of the triangular bases of the prism interacting with one or more Ge atoms in three crystallographically different molecules in the structure. Lastly, the Tl atom in the structure of 3 is found capping a pseudosquare face between two hypersilyl substituents. NMR spectroscopy indicates that all three compounds are dynamic at room temperature. Variable-temperature studies suggest that the process in 1 and 2 is intramolecular while the process in 3 involves dissociation of the Tl(+) ion from the molecule followed by association at the same or another equivalent pseudosquare face of the molecule. Thus, the latter compound may be considered to a large extent to be ionic as it is made of a thallium cation and a trisubstituted cluster anion.

Surface acetylation of bamboo cellulose: preparation and rheological properties.

PubMed

Cai, Jie; Fei, Peng; Xiong, Zhouyi; Shi, Yongjun; Yan, Kai; Xiong, Hanguo

2013-01-30

In this study, purified bamboo cellulose was used to synthesize cellulose diacetate (B-CDA). The synthesis was controlled by determination of the degree of substitution and insoluble residue content. The product then was characterized by FTIR. The rheological properties of B-CDA solutions in acetone/N,N-dimethylacetamide (DMAc) solvent system were systematically investigated on an advanced rheometer, including the dependence of apparent viscosity η(α), non-Newtonian index n, and structural viscosity index Δη on the concentration and temperature of the solutions. B-CDA-acetone/DMAc solution is a shear-thinning fluid. With increasing solution concentration and decreasing temperature, Δη increased, whereas n decreased, which indicates a deteriorating spinnability. Moreover, the values of the viscous flow activation energy E(η) based on the Arrhenius equation increased when the shear rate γ was enhanced, which indicates that the η(α) of the solution is more sensitive to temperature in the higher γ values. The results are favorable for predicting the B-CDA solution spinnability. Copyright © 2012 Elsevier Ltd. All rights reserved.

Synthesis of Synthetic Hydrocarbons Via Alpha Olefins.

DTIC Science & Technology

1985-05-01

THF complex, 0OC; (e) Pyridinium chlorochromate , dry CH2 CL29 room temperature; b (f) methyltriphenylphosphonium bromide, dimethyl sulfoxide, room...vigorously stirred solution of pyridinium chlorochromate (27.91 g, 0.13 mol) in dry methylene chloride (175 mL) was added all at once a solution of l... pyridinium chlorochroniate. 3 Our four-step synthesis of l-decene-2-1 3 C from 1-bromooctane is outlined in the Scheme. This synthetic sequence provides the

Formation of hollow nanoshells in solution-based reactions via collision coalescence of nanobubble-particle systems

NASA Astrophysics Data System (ADS)

Vongehr, Sascha; Tang, Shaochun

2016-06-01

Research on hollow nanoshells has, for years, claimed to involve free, pre-existing nanobubbles as soft templates. It is a challenge to demonstrate this due to the difficulty of in situ observation during solution-based reactions. We show that no available free-bubble theory can describe the mysterious behavior of the bubble number density n. A new mechanism of collision coalescence of bubble-particle systems is suggested to form hollow nanoshells. By approximating relative velocity as ˜R -z (R is bubble radius), numerical simulations can reproduce the counterintuitive observations in the regime 1 < z < 2. We discuss the mechanism based on successful synthesis of grain-monolayer thin, fractal-like incomplete, multi-metallic nanoshells with superior catalytic activity. The behaviors of n, R, and shell thickness h are closely reproduced by z = 1.6.

Hierarchically Mesoporous o-Hydroxyazobenzene Polymers: Synthesis and Their Applications in CO2 Capture and Conversion.

PubMed

Ji, Guipeng; Yang, Zhenzhen; Zhang, Hongye; Zhao, Yanfei; Yu, Bo; Ma, Zhishuang; Liu, Zhimin

2016-08-08

The synthesis of hierarchically mesoporous polymers with multiple functionalities is challenging. Herein we reported a template-free strategy for synthesis of phenolic azo-polymers with hierarchical porous structures based on diazo-coupling reaction in aqueous solution under mild conditions. The resultant polymers have surface areas up to 593 m(2)  g(-1) with the mesopore ratio of >80 %, and a good ability to complex with metal ions, such as Cu(2+) , Zn(2+) ,Ni(2+) , achieving a metal loading up to 26.24 wt %. Moreover, the polymers complexed with Zn showed excellent performance for catalyzing the reaction of CO2 with epoxide, affording a TOF of 2570 h(-1) in the presence of tetrabutyl ammonium bromide (7.2 mol %). The polymer complexed with Cu could catalyze the oxidation of alcohol with high efficiency. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Synthesis and screening of one-bead-one-compound cyclic peptide libraries.

PubMed

Qian, Ziqing; Upadhyaya, Punit; Pei, Dehua

2015-01-01

Cyclic peptides have been a rich source of biologically active molecules. Herein we present a method for the combinatorial synthesis and screening of large one-bead-one-compound (OBOC) libraries of cyclic peptides against biological targets such as proteins. Up to ten million different cyclic peptides are rapidly synthesized on TentaGel microbeads by the split-and-pool synthesis method and subjected to a multistage screening protocol which includes magnetic sorting, on-bead enzyme-linked and fluorescence-based assays, and in-solution binding analysis of cyclic peptides selectively released from single beads by fluorescence anisotropy. Finally, the most active hit(s) is identified by the partial Edman degradation-mass spectrometry (PED-MS) method. This method allows a single researcher to synthesize and screen up to ten million cyclic peptides and identify the most active ligand(s) in ~1 month, without the time-consuming and expensive hit resynthesis or the use of any special equipment.

Synthesis of Mikto-Arm Star Peptide Conjugates.

PubMed

Koo, Jin Mo; Su, Hao; Lin, Yi-An; Cui, Honggang

2018-01-01

Mikto-arm star peptide conjugates are an emerging class of self-assembling peptide-based structural units that contain three or more auxiliary segments of different chemical compositions and/or functionalities. This group of molecules exhibit interesting self-assembly behavior in solution due to their chemically asymmetric topology. Here we describe the detailed procedure for synthesis of an ABC Mikto-arm star peptide conjugate in which two immiscible entities (a saturated hydrocarbon and a hydrophobic and lipophobic fluorocarbon) are conjugated onto a short β-sheet forming peptide sequence, GNNQQNY, derived from the Sup35 prion, through a lysine junction. Automated and manual Fmoc-solid phase synthesis techniques are used to synthesize the Mikto-arm star peptide conjugates, followed by HPLC purification. We envision that this set of protocols can afford a versatile platform to synthesize a new class of peptidic building units for diverse applications.

Parallel Computer System for 3D Visualization Stereo on GPU

NASA Astrophysics Data System (ADS)

Al-Oraiqat, Anas M.; Zori, Sergii A.

2018-03-01

This paper proposes the organization of a parallel computer system based on Graphic Processors Unit (GPU) for 3D stereo image synthesis. The development is based on the modified ray tracing method developed by the authors for fast search of tracing rays intersections with scene objects. The system allows significant increase in the productivity for the 3D stereo synthesis of photorealistic quality. The generalized procedure of 3D stereo image synthesis on the Graphics Processing Unit/Graphics Processing Clusters (GPU/GPC) is proposed. The efficiency of the proposed solutions by GPU implementation is compared with single-threaded and multithreaded implementations on the CPU. The achieved average acceleration in multi-thread implementation on the test GPU and CPU is about 7.5 and 1.6 times, respectively. Studying the influence of choosing the size and configuration of the computational Compute Unified Device Archi-tecture (CUDA) network on the computational speed shows the importance of their correct selection. The obtained experimental estimations can be significantly improved by new GPUs with a large number of processing cores and multiprocessors, as well as optimized configuration of the computing CUDA network.

Flocculation characteristics of polyacrylamide grafted cellulose from Phyllostachys heterocycla: An efficient and eco-friendly flocculant.

PubMed

Liu, Hongyi; Yang, Xiaogang; Zhang, Yong; Zhu, Hangcheng; Yao, Juming

2014-08-01

This work presents a synthesis process and flocculation characteristics of an eco-friendly flocculant based on bamboo pulp cellulose (BPC) from Phyllostachys heterocycla. Ployacrylamide (PAM) was grafted onto the BPC by free-radical graft copolymerization in homogeneous aqueous solution. The optimal synthesis conditions of the bamboo pulp cellulose-graft-ployacrylamide flocculant (BPC-g-PAM) and its performance on wastewater treatments were investigated. A UV-based method was used to rapidly determine the degree of substitution (DS) of BPC. The results showed that, under the optimal synthesis conditions, the obtained BPC-g-PAM held a grafting ratio of 43.8% and DS of 1.31. Turbidity removal of the product reached 98.0% accompanying with the significant flocculation and sedimentation in target suspensions. The flocculation mechanism was explored by means of zeta potential method. For negatively charged contaminants, like kaolin clay particles, the BPC-g-PAM could remove the contaminants efficiently via bridging and charge neutralization in acidic or neutral environment. Copyright © 2014 Elsevier Ltd. All rights reserved.

Supercritical carbon dioxide-assisted rapid synthesis of few-layer black phosphorus for hydrogen peroxide sensing.

PubMed

Yan, Shancheng; Wang, Bojun; Wang, Zhulan; Hu, Dong; Xu, Xin; Wang, Junzhuan; Shi, Yi

2016-06-15

Solutions with large-scale dispersions of 2D black phosphorus (BP), often referred to as phosphorene, are obtained through solvent exfoliation. But, rapid phosphorene synthesis remains a challenge. Furthermore, although the chemical sensing capability of BP-based sensors has been theoretically predicted, its experimental verification remains lacking. In this study, we demonstrate the use of supercritical carbon dioxide-assisted rapid synthesis (5h) of few-layer BP. In addition, we construct a non-enzymatic hydrogen peroxide (H2O2) sensor based on few-layer BP for the first time to utilize BP degradation under ambient conditions. The proposed H2O2 sensor exhibits a considerably lower detection limit of 1 × 10(-7) M compared with the general detection limit of 1 × 10(-7) M-5 × 10(-5)M via electrochemical methods. Overall, the results of this study will not only expand the coverage of BP research but will also identify the important sensing characteristics of BP. Copyright © 2016 Elsevier B.V. All rights reserved.

Fabrication of heterogeneous nanomaterial array by programmable heating and chemical supply within microfluidic platform towards multiplexed gas sensing application

PubMed Central

Yang, Daejong; Kang, Kyungnam; Kim, Donghwan; Li, Zhiyong; Park, Inkyu

2015-01-01

A facile top-down/bottom-up hybrid nanofabrication process based on programmable temperature control and parallel chemical supply within microfluidic platform has been developed for the all liquid-phase synthesis of heterogeneous nanomaterial arrays. The synthesized materials and locations can be controlled by local heating with integrated microheaters and guided liquid chemical flow within microfluidic platform. As proofs-of-concept, we have demonstrated the synthesis of two types of nanomaterial arrays: (i) parallel array of TiO2 nanotubes, CuO nanospikes and ZnO nanowires, and (ii) parallel array of ZnO nanowire/CuO nanospike hybrid nanostructures, CuO nanospikes and ZnO nanowires. The laminar flow with negligible ionic diffusion between different precursor solutions as well as localized heating was verified by numerical calculation and experimental result of nanomaterial array synthesis. The devices made of heterogeneous nanomaterial array were utilized as a multiplexed sensor for toxic gases such as NO2 and CO. This method would be very useful for the facile fabrication of functional nanodevices based on highly integrated arrays of heterogeneous nanomaterials. PMID:25634814

Synthesis, Spectral and Photophysical Properties of Anthracene Substituted Phthalocyanines; A Study as Polyurethane Electrospun Nanofibers.

PubMed

Ku, Kyo-Sun; Kumar, Rangaraju Satish; Son, Young-A

2018-03-01

We have designed and synthesized novel symmetrical anthracene substituted zinc(II), copper(II), cobalt(II) and nickel(II) phthalocyanines (PC1, PC2, PC3 and PC4) in this work. For this synthesis, we started from base-catalysed aromatic displacement reaction of 4-nitrophthalonitrile with 9-hydroxyanthracene. The resulting four phthalocyanines (PCs) have been fully characterized by a series of spectroscopic methods including electronic absorption, elemental analysis, MALDI-TOF mass, and IR spectroscopy. The aggregation behavior of these PCs was investigated in different concentrations of chloroform solution. Further thermal stability also investigated by TG analysis. Finally we successfully made phthalocyanine (PC1) blended polyurethane electrospun (ES) nanofibers.

Peptide-Decorated Tunable-Fluorescence Graphene Quantum Dots.

PubMed

Sapkota, Bedanga; Benabbas, Abdelkrim; Lin, Hao-Yu Greg; Liang, Wentao; Champion, Paul; Wanunu, Meni

2017-03-22

We report here the synthesis of graphene quantum dots with tunable size, surface chemistry, and fluorescence properties. In the size regime 15-35 nm, these quantum dots maintain strong visible light fluorescence (mean quantum yield of 0.64) and a high two-photon absorption (TPA) cross section (6500 Göppert-Mayer units). Furthermore, through noncovalent tailoring of the chemistry of these quantum dots, we obtain water-stable quantum dots. For example, quantum dots with lysine groups bind strongly to DNA in solution and inhibit polymerase-based DNA strand synthesis. Finally, by virtue of their mesoscopic size, the quantum dots exhibit good cell permeability into living epithelial cells, but they do not enter the cell nucleus.

Increased short circuit current in an azafullerene-based organic solar cell.

PubMed

Cambarau, Werther; Fritze, Urs F; Viterisi, Aurélien; Palomares, Emilio; von Delius, Max

2015-01-21

We report the synthesis of a solution-processable, dodecyloxyphenyl-substituted azafullerene monoadduct (DPC59N) and its application as electron acceptor in bulk heterojunction organic solar cells (BHJ-OSCs). Due to its relatively strong absorption of visible light, DPC59N outperforms PC60BM in respect to short circuit current (JSC) and external quantum efficiency (EQE) in blends with donor P3HT.

Hybrid Inorganic/Organic Photovoltaics: Translating Fundamental Nanostructure Research to Enhanced Solar Conversion Efficiency

DTIC Science & Technology

2010-03-18

quantum dots composed of a photopolymerizable outer corona constituting methacrylate and an inner siloxane layer, with a view making them photo...nanostructures. The inherent properties of photopolymerizable QDs such as their stability, PL, and ease of solution processability, make them suitable...Thiophenes are important compounds that are used as building blocks in many chemical synthesis. The thiophene oligomers and thiophene-based

Course Management Systems as Tools for the Creation of Online Learning Environments: Evaluation from a Social Constructivist Perspective and Implications for Their Design

ERIC Educational Resources Information Center

Papastergiou, Marina

2006-01-01

The Internet and the Web offer academic institutions solutions for covering the massive demand for education and transition towards student-centered, social constructivist educational models, in accordance with the demands of the knowledge-based society. This article reports on an investigation aimed at presenting a synthesis of recent research on…

Efficacy of a solution-based approach for making sodalite waste forms for an oxide reduction salt utilized in the reprocessing of used uranium oxide fuel

NASA Astrophysics Data System (ADS)

Riley, Brian J.; Pierce, David A.; Frank, Steven M.; Matyáš, Josef; Burns, Carolyne A.

2015-04-01

This paper describes the various approaches evaluated for making solution-derived sodalite with a LiCl-Li2O oxide reduction salt selected to dissolve used uranium oxide fuel so the uranium can be recovered and recycled. The approaches include modified sol-gel and solution-based synthesis processes. As-made products were mixed with 5 and 10 mass% of a Na2O-B2O3-SiO2 glass binder and these, along with product without a binder, were heated using either a cold-press-and-sinter method or hot uniaxial pressing. The results demonstrate the limitation of sodalite yield due to the fast intermediate reactions between Na+ and Cl- to form halite in solution and Li2O and SiO2 to form lithium silicates (e.g., Li2SiO3 or Li2Si2O5) in the calcined and sintered pellets. The results show that pellets can be made with high sodalite fractions in the crystalline product (∼92 mass%) and low porosities using a solution-based approach and this LiCl-Li2O salt but that the incorporation of Li into the sodalite is low.

A mathematical framework for yield (vs. rate) optimization in constraint-based modeling and applications in metabolic engineering.

PubMed

Klamt, Steffen; Müller, Stefan; Regensburger, Georg; Zanghellini, Jürgen

2018-05-01

The optimization of metabolic rates (as linear objective functions) represents the methodical core of flux-balance analysis techniques which have become a standard tool for the study of genome-scale metabolic models. Besides (growth and synthesis) rates, metabolic yields are key parameters for the characterization of biochemical transformation processes, especially in the context of biotechnological applications. However, yields are ratios of rates, and hence the optimization of yields (as nonlinear objective functions) under arbitrary linear constraints is not possible with current flux-balance analysis techniques. Despite the fundamental importance of yields in constraint-based modeling, a comprehensive mathematical framework for yield optimization is still missing. We present a mathematical theory that allows one to systematically compute and analyze yield-optimal solutions of metabolic models under arbitrary linear constraints. In particular, we formulate yield optimization as a linear-fractional program. For practical computations, we transform the linear-fractional yield optimization problem to a (higher-dimensional) linear problem. Its solutions determine the solutions of the original problem and can be used to predict yield-optimal flux distributions in genome-scale metabolic models. For the theoretical analysis, we consider the linear-fractional problem directly. Most importantly, we show that the yield-optimal solution set (like the rate-optimal solution set) is determined by (yield-optimal) elementary flux vectors of the underlying metabolic model. However, yield- and rate-optimal solutions may differ from each other, and hence optimal (biomass or product) yields are not necessarily obtained at solutions with optimal (growth or synthesis) rates. Moreover, we discuss phase planes/production envelopes and yield spaces, in particular, we prove that yield spaces are convex and provide algorithms for their computation. We illustrate our findings by a small example and demonstrate their relevance for metabolic engineering with realistic models of E. coli. We develop a comprehensive mathematical framework for yield optimization in metabolic models. Our theory is particularly useful for the study and rational modification of cell factories designed under given yield and/or rate requirements. Copyright © 2018 The Authors. Published by Elsevier Inc. All rights reserved.

Method to synthesize metal chalcogenide monolayer nanomaterials

DOEpatents

Hernandez-Sanchez, Bernadette A.; Boyle, Timothy J.

2016-12-13

Metal chalcogenide monolayer nanomaterials can be synthesized from metal alkoxide precursors by solution precipitation or solvothermal processing. The synthesis routes are more scalable, less complex and easier to implement than other synthesis routes.

Induction of Crassulacean Acid Metabolism in Mesembryanthemum crystallinum by High Salinity: Mass Increase and de Novo Synthesis of PEP-Carboxylase 1

PubMed Central

Höfner, Roswitha; Vazquez-Moreno, Luz; Winter, Klaus; Bohnert, Hans J.; Schmitt, Jürgen M.

1987-01-01

Intact plants of the halophilic species Mesembryanthemum crystallinum were induced to exhibit Crassulacean acid metabolism by irrigation with nutrient solution containing 500 millimolar NaCl. During the induction period, the extractable activity of phosphoenolpyruvate carboxylase (PEPcase) increased approximately 40-fold. This increase was linearly correlated with a mass increase of PEPcase protein as measured by single radial immunodiffusion. De novo synthesis of PEPcase protein was shown by immunoprecipitation of the newly synthesized, radioactively labeled protein in leaf discs from salt-treated plants. Nontreated plants were characterized by a low level of the enzyme and low rates of PEPcase synthesis. Synthesis of this enzyme in leaf discs was correlated with the concentration of NaCl in the nutrient solution during growth. Images Fig. 1 Fig. 2 Fig. 3 PMID:16665363

One-dimensional zinc oxide nanomaterials synthesis and photovoltaic applications

NASA Astrophysics Data System (ADS)

Weintraub, Benjamin A.

As humanly engineered materials systems approach the atomic scale, top-down manufacturing approaches breakdown and following nature's example, bottom-up or self-assembly methods have the potential to emerge as the dominant paradigm. Synthesis of one-dimensional nanomaterials takes advantage of such self-assembly manufacturing techniques, but until now most efforts have relied on high temperature vapor phase schemes which are limited in scalability and compatibility with organic materials. The solution-phase approach is an attractive low temperature alternative to overcome these shortcomings. To this end, this thesis is a study of the rationale solution-phase synthesis of ZnO nanowires and applications in photovoltaics. The following thesis goals have been achieved: rationale synthesis of a single ZnO nanowire on a polymer substrate without seeding, design of a wafer-scale technique to control ZnO nanowire array density using layer-by-layer polymers, determination of optimal nanowire field emitter density to maximize the field enhancement factor, design of bridged nanowires across metal electrodes to order to circumvent post-synthesis manipulation steps, electrical characterization of bridged nanowires, rationale solution-phase synthesis of long ZnO nanowires on optical fibers, fabrication of ZnO nanowire dye-sensitized solar cells on optical fibers, electrical and optical characterization of solar cell devices, comparison studies of 2-D versus 3-D nanowire dye-sensitized solar cell devices, and achievement of 6-fold solar cell power conversion efficiency enhancement using a 3-D approach. The thesis results have implications in nanomanufacturing scale-up and next generation photovoltaics.

Novel synthesis and characterization of a collagen-based biopolymer initiated by hydroxyapatite nanoparticles.

PubMed

Bhuiyan, D; Jablonsky, M J; Kolesov, I; Middleton, J; Wick, T M; Tannenbaum, R

2015-03-01

In this study, we developed a novel synthesis method to create a complex collagen-based biopolymer that promises to possess the necessary material properties for a bone graft substitute. The synthesis was carried out in several steps. In the first step, a ring-opening polymerization reaction initiated by hydroxyapatite nanoparticles was used to polymerize d,l-lactide and glycolide monomers to form poly(lactide-co-glycolide) co-polymer. In the second step, the polymerization product was coupled with succinic anhydride, and subsequently was reacted with N-hydroxysuccinimide in the presence of dicyclohexylcarbodiimide as the cross-linking agent, in order to activate the co-polymer for collagen attachment. In the third and final step, the activated co-polymer was attached to calf skin collagen type I, in hydrochloric acid/phosphate buffer solution and the precipitated co-polymer with attached collagen was isolated. The synthesis was monitored by proton nuclear magnetic resonance, infrared and Raman spectroscopies, and the products after each step were characterized by thermal and mechanical analysis. Calculations of the relative amounts of the various components, coupled with initial dynamic mechanical analysis testing of the resulting biopolymer, afforded a preliminary assessment of the structure of the complex biomaterial formed by this novel polymerization process. Copyright © 2015. Published by Elsevier Ltd.

Kinetics of the creatine kinase reaction in neonatal rabbit heart: An empirical analysis of the rate equation

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

McAuliffe, J.J.; Perry, S.B.; Brooks, E.E.

1991-03-12

Here the authors define the kinetics of the creatine kinase (CK) reaction in an intact mammalian heart containing the full rnage of CK isoenzymes. Previously derived kinetic constants were refit for the reaction occurring at 37C. Steady-state metabolite concentrations from {sup 31}P NMR and standard biochemical techniques were determined. {sup 31}P magnetization transfer data were obtained to determine unidirectional creatine kinase fluxes in hearts with differing total creatine contents and differing mitochondrial CK activities during KCl arrest and isovolumic work for both the forward reaction (MgATP synthesis) and reverse reaction (phosphocreatine synthesis). The NMR kinetic data and substrate concentrations datamore » were used in conjunction with a kinetic model based on MM-CK in solution to determine the applicability of the solution-based kinetic models to the CK kinetics of the intact heart. The results indicated that no single set of rate equation constants could describe both the KCl-arrested and working hearts. Analysis of the results indicated that the CK reaction is rate limited in the direction of ATP synthesis, the size of the guanidino substrate pool drives the measured CK flux in the intact heart, and during isovolumic work, the CK reaction operates under saturating conditions; that is, the substrate concentrations are at least 2-fold greater than the K{sub m} or K{sub im} for each substrate. However, during KCl arrest the reaction does not operate under saturating conditions and the CK reaction velocity is strongly influenced by the guanidino substrate pool size.« less

A Facile Synthesis of MPd (M=Co, Cu) Nanoparticles and Their Catalysis for Formic Acid Oxidation

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

Mazumder, Vismadeb; Chi, Miaofang; Mankin, Max

2012-01-01

Monodisperse CoPd nanoparticles (NPs) were synthesized and studied for catalytic formic acid (HCOOH) oxidation (FAO). The NPs were prepared by coreduction of Co(acac)2 (acac = acetylacetonate) and PdBr2 at 260 C in oleylamine and trioctylphosphine, and their sizes (5-12 nm) and compositions (Co10Pd90 to Co60Pd40) were controlled by heating ramp rate, metal salt concentration, or metal molar ratios. The 8 nm CoPd NPs were activated for HCOOH oxidation by a simple ethanol wash. In 0.1 M HClO4 and 2 M HCOOH solution, their catalytic activities followed the trend of Co50Pd50 > Co60Pd40 > Co10Pd90 > Pd. The Co50Pd50 NPs hadmore » an oxidation peak at 0.4 V with a peak current density of 774 A/gPd. As a comparison, commercial Pd catalysts showed an oxidation peak at 0.75 V with peak current density of only 254 A/gPd. The synthesis procedure could also be extended to prepare CuPd NPs when Co(acac)2 was replaced by Cu(ac)2 (ac = acetate) in an otherwise identical condition. The CuPd NPs were less active catalysts than CoPd or even Pd for FAO in HClO4 solution. The synthesis provides a general approach to Pd-based bimetallic NPs and will enable further investigation of Pd-based alloy NPs for electro-oxidation and other catalytic reactions.« less

Scoping Candidate Minerals for Stabilization of Arsenic-Bearing Solid Residuals

PubMed Central

Raghav, Madhumitha; Shan, Jilei; Sáez, A. Eduardo; Ela, Wendell P.

2014-01-01

Arsenic Crystallization Technology (ACT) is a potentially eco-friendly, effective technology for stabilization of arsenic-bearing solid residuals (ABSRs). The strategy is to convert ABSRs generated by water treatment facilities into minerals with a high arsenic capacity and long-term stability in mature, municipal solid waste landfills. Candidate minerals considered in this study include scorodite, arsenate hydroxyapatites, ferrous arsenates (symplesite-type minerals), tooeleite, and arsenated-schwertmannite. These minerals were evaluated as to ease of synthesis, applicability to use of iron-based ABSRs as a starting material, and arsenic leachability. The Toxicity Characteristic Leaching Procedure (TCLP) was used for preliminary assessment of candidate mineral leaching. Minerals that passed the TCLP and whose synthesis route was promising were subjected to a more aggressive leaching test using a simulated landfill leachate (SLL) solution. Scorodite and arsenate hydroxyapatites were not considered further because their synthesis conditions were not found to be favorable for general application. Tooeleite and silica-amended tooeleite showed high TCLP arsenic leaching and were also not investigated further. The synthesis process and leaching of ferrous arsenate and arsenated-schwertmannite were promising and of these, arsenated-schwertmannite was most stable during SLL testing. The latter two candidate minerals warrant synthesis optimization and more extensive testing. PMID:24231323

The use of physiological solutions or media in calcium phosphate synthesis and processing.

PubMed

Tas, A Cuneyt

2014-05-01

This review examined the literature to spot uses, if any, of physiological solutions/media for the in situ synthesis of calcium phosphates (CaP) under processing conditions (i.e. temperature, pH, concentration of inorganic ions present in media) mimicking those prevalent in the human hard tissue environments. There happens to be a variety of aqueous solutions or media developed for different purposes; sometimes they have been named as physiological saline, isotonic solution, cell culture solution, metastable CaP solution, supersaturated calcification solution, simulated body fluid or even dialysate solution (for dialysis patients). Most of the time such solutions were not used as the aqueous medium to perform the biomimetic synthesis of calcium phosphates, and their use was usually limited to the in vitro testing of synthetic biomaterials. This review illustrates that only a limited number of research studies used physiological solutions or media such as Earle's balanced salt solution, Bachra et al. solutions or Tris-buffered simulated body fluid solution containing 27mM HCO3(-) for synthesizing CaP, and these studies have consistently reported the formation of X-ray-amorphous CaP nanopowders instead of Ap-CaP or stoichiometric hydroxyapatite (HA, Ca10(PO4)6(OH)2) at 37°C and pH 7.4. By relying on the published articles, this review highlights the significance of the use of aqueous solutions containing 0.8-1.5 mMMg(2+), 22-27mM HCO3(-), 142-145mM Na(+), 5-5.8mM K(+), 103-133mM Cl(-), 1.8-3.75mM Ca(2+), and 0.8-1.67mM HPO4(2-), which essentially mimic the composition and the overall ionic strength of the human extracellular fluid (ECF), in forming the nanospheres of X-ray-amorphous CaP. Copyright © 2013 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Synthesis of two-dimensional titanium nitride Ti4N3 (MXene)

NASA Astrophysics Data System (ADS)

Urbankowski, Patrick; Anasori, Babak; Makaryan, Taron; Er, Dequan; Kota, Sankalp; Walsh, Patrick L.; Zhao, Mengqiang; Shenoy, Vivek B.; Barsoum, Michel W.; Gogotsi, Yury

2016-06-01

We report on the synthesis of the first two-dimensional transition metal nitride, Ti4N3-based MXene. In contrast to the previously reported MXene synthesis methods - in which selective etching of a MAX phase precursor occurred in aqueous acidic solutions - here a molten fluoride salt is used to etch Al from a Ti4AlN3 powder precursor at 550 °C under an argon atmosphere. We further delaminated the resulting MXene to produce few-layered nanosheets and monolayers of Ti4N3Tx, where T is a surface termination (F, O, or OH). Density functional theory calculations of bare, non-terminated Ti4N3 and terminated Ti4N3Tx were performed to determine the most energetically stable form of this MXene. Bare and functionalized Ti4N3 are predicted to be metallic. Bare Ti4N3 is expected to show magnetism, which is significantly reduced in the presence of functional groups.We report on the synthesis of the first two-dimensional transition metal nitride, Ti4N3-based MXene. In contrast to the previously reported MXene synthesis methods - in which selective etching of a MAX phase precursor occurred in aqueous acidic solutions - here a molten fluoride salt is used to etch Al from a Ti4AlN3 powder precursor at 550 °C under an argon atmosphere. We further delaminated the resulting MXene to produce few-layered nanosheets and monolayers of Ti4N3Tx, where T is a surface termination (F, O, or OH). Density functional theory calculations of bare, non-terminated Ti4N3 and terminated Ti4N3Tx were performed to determine the most energetically stable form of this MXene. Bare and functionalized Ti4N3 are predicted to be metallic. Bare Ti4N3 is expected to show magnetism, which is significantly reduced in the presence of functional groups. Electronic supplementary information (ESI) available. See DOI: 10.1039/c6nr02253g

Making Single-Source Precursors of Ternary Semiconductors

NASA Technical Reports Server (NTRS)

Hepp, Aloysius; Banger, Kulbindre K.

2007-01-01

A synthesis route has been developed for the commercial manufacture of single- source precursors of chalcopyrite semiconductor absorber layers of thin-film solar photovoltaic cells. A closely related class of single-source precursors of these semiconductors, and their synthesis routes, were reported in "Improved Single-Source Precursors for Solar-Cell Absorbers" (LEW-17445-1), NASA Tech Briefs, Vol. 31, No. 6 (June 2007), page 56. The present synthesis route is better suited to commercialization because it is simpler and involves the use of commercially available agents, yet offers the flexibility needed for synthesis of a variety of precursors. A single-source precursor of the type of interest here is denoted by the general formula L2M'(mu-ER)2M(ER)2, where L signifies a Lewis base; M signifies Al, In, or Ga; M' signifies Ag or Cu; R signifies an alkyl, aryl, silyl, or perfluorocarbon group; E signifies O, S, Se, or Te; and mu signifies a bridging ligand. This compound can be synthesized in a "one-pot" procedure from ingredients that are readily available from almost any chemical supplier. In a demonstration, the following synthesis was performed: Under anaerobic conditions, InCl3 was reacted with sodium ethanethiolate in methanol in a 1:4 molar ratio to afford the ionic stable intermediate compound Na+[In(SEt)4]- (where Et signifies ethyl group). After approximately 15 minutes, a heterogeneous solution of CuCl and the Lewis base PPh3 (where Ph signifies phenyl) in a 1:2 ratio in a mixture of CH3CN and CH2Cl2 was added directly to the freshly prepared Na+[In(SEt)4]-. After 24 hours, the reaction was essentially complete. The methanolic solution was concentrated, then the product was extracted with CH2Cl2, then the product was washed with dry ether and pentane. The product in its final form was a creamy white solid. Spectroscopic and elemental analysis confirmed that the product was (PPh3)2Cu(mu-SEt)2In(mu-SEt)2, which is known to be a precursor of the ternary semiconductor CuInS2.

A Family of Highly Efficient CuI-Based Lighting Phosphors Prepared by a Systematic, Bottom-up Synthetic Approach.

PubMed

Liu, Wei; Fang, Yang; Wei, George Z; Teat, Simon J; Xiong, Kecai; Hu, Zhichao; Lustig, William P; Li, Jing

2015-07-29

Copper(I) iodide (CuI)-based inorganic-organic hybrid materials in the general chemical formula of CuI(L) are well-known for their structural diversity and strong photoluminescence and are therefore considered promising candidates for a number of optical applications. In this work, we demonstrate a systematic, bottom-up precursor approach to developing a series of CuI(L) network structures built on CuI rhomboid dimers. These compounds combine strong luminescence due to the CuI inorganic modules and significantly enhanced thermal stability as a result of connecting individual building units into robust, extended networks. Examination of their optical properties reveals that these materials not only exhibit exceptionally high photoluminescence performance (with internal quantum yield up to 95%) but also that their emission energy and color are systematically tunable through modification of the organic component. Results from density functional theory calculations provide convincing correlations between these materials' crystal structures and chemical compositions and their optophysical properties. The advantages of cost-effective, solution-processable, easily scalable and fully controllable synthesis as well as high quantum efficiency with improved thermal stability, make this phosphor family a promising candidate for alternative, RE-free phosphors in general lighting and illumination. This solution-based precursor approach creates a new blueprint for the rational design and controlled synthesis of inorganic-organic hybrid materials.

Radio Frequency Magnetron Sputtering Deposition of TiO2 Thin Films and Their Perovskite Solar Cell Applications

PubMed Central

Chen, Cong; Cheng, Yu; Dai, Qilin; Song, Hongwei

2015-01-01

In this work, we report a physical deposition based, compact (cp) layer synthesis for planar heterojunction perovskite solar cells. Typical solution-based synthesis of cp layer for perovskite solar cells involves low-quality of thin films, high-temperature annealing, non-flexible devices, limitation of large-scale production and that the effects of the cp layer on carrier transport have not been fully understood. In this research, using radio frequency magnetron sputtering (RFMS), TiO2 cp layers were fabricated and the thickness could be controlled by deposition time; CH3NH3PbI3 films were prepared by evaporation & immersion (E & I) method, in which PbI2 films made by thermal evaporation technique were immersed in CH3NH3I solution. The devices exhibit power conversion efficiency (PCE) of 12.1% and the photovoltaic performance can maintain 77% of its initial PCE after 1440 h. The method developed in this study has the capability of fabricating large active area devices (40 × 40 mm2) showing a promising PCE of 4.8%. Low temperature and flexible devices were realized and a PCE of 8.9% was obtained on the PET/ITO substrates. These approaches could be used in thin film based solar cells which require high-quality films leading to reduced fabrication cost and improved device performance. PMID:26631493

Bioinspired synthesis of a soft-nanofilament-based coating consisting of polysilsesquioxanes/polyamine and its divergent surface control.

PubMed

Yuan, Jian-Jun; Kimitsuka, Nobuo; Jin, Ren-Hua

2013-04-24

The synthesis of polysilsesquioxanes coating with controllable one-dimensional nanostructure on substrates remains a major long-term challenge by conventional solution-phase method. The hydrolytic polycondensation of organosilanes in solution normally produces a mixture of incomplete cages, ladderlike, and network structures, resulting in the poor control of the formation of specific nanostructure. This paper describes a simple aqueous process to synthesize nanofilament-based coatings of polysilsesquioxanes possessing various organo-functional groups (for example, thiol, methyl, phenyl, vinyl, and epoxy). We utilized a self-assembled nanostructured polyamine layer as a biomimetically catalytic scaffold/template to direct the formation of one-dimensional nanofilament of polysilsesquioxanes by temporally and spatially controlled hydrolytic polycondensation of organosilane. The surface nanostructure and morphology of polysilsesquioxane coating could be modulated by changing hydrolysis and condensation reaction conditions, and the orientation of nanofilaments of polysilsesquioxanes on substrates could be controlled by simply adjusting the self-assembly conditions of polyamine layer. The nanostructure and polyamine@polysilsesquioxane hybrid composition of nanofilament-based coatings were examined by means of scanning electron microscopy (SEM), transmission electron microscopy (TEM), and X-ray photoelectron spectroscopy (XPS). The template role of nanostructured polyamine layer for the formation of polysilsesquioxane nanofilament was confirmed by combining thin film X-ray diffraction (XRD) and XPS measurements. Moreover, these nanotextured coatings with various organo-functional groups could be changed into superhydrophobic surfaces after surface modification with fluorocarbon molecule.

Synthesis and solution self-assembly of side-chain cobaltocenium-containing block copolymers.

PubMed

Ren, Lixia; Hardy, Christopher G; Tang, Chuanbing

2010-07-07

The synthesis of side-chain cobaltocenium-containing block copolymers and their self-assembly in solution was studied. Highly pure monocarboxycobaltocenium was prepared and subsequently attached to side chains of poly(tert-butyl acrylate)-block-poly(2-hydroxyethyl acrylate), yielding poly(tert-butyl acrylate)-block-poly(2-acryloyloxyethyl cobaltoceniumcarboxylate). The cobaltocenium block copolymers exhibited vesicle morphology in the mixture of acetone and water, while micelles of nanotubes were formed in the mixture of acetone and chloroform.

Synthesis of peptides from amino acids and ATP with lysine-rich proteinoid

NASA Technical Reports Server (NTRS)

Nakashima, T.; Fox, S. W.

1980-01-01

The paper examines the synthesis of peptides from aminoacids and ATP with a lysine-rich protenoid. The latter in aqueous solution catalyzes the formation of peptides from free amino acids and ATP; this catalytic activity is not found in acidic protenoids, even though the latter contain a basic aminoacid. The pH optimum for the synthesis is about 11, but it is appreciable below 8 and above 13. Temperature data indicate an optimum at 20 C or above, with little increase in rate up to 60 C. Pyrophosphate can be used instead of ATP, but the yields are lower. The ATP-aided syntheses of peptides in aqueous solution occur with several types of proteinous aminoacids.

Understanding facilitators and barriers to reengineering the clinical research enterprise in community-based practice settings.

PubMed

Kukafka, Rita; Allegrante, John P; Khan, Sharib; Bigger, J Thomas; Johnson, Stephen B

2013-09-01

Solutions are employed to support clinical research trial tasks in community-based practice settings. Using the IT Implementation Framework (ITIF), an integrative framework intended to guide the synthesis of theoretical perspectives for planning multi-level interventions to enhance IT use, we sought to understand the barriers and facilitators to clinical research in community-based practice settings preliminary to implementing new informatics solutions for improving clinical research infrastructure. The studies were conducted in practices within the Columbia University Clinical Trials Network. A mixed-method approach, including surveys, interviews, time-motion studies, and observations was used. The data collected, which incorporates predisposing, enabling, and reinforcing factors in IT use, were analyzed according to each phase of ITIF. Themes identified in the first phase of ITIF were 1) processes and tools to support clinical trial research and 2) clinical research peripheral to patient care processes. Not all of the problems under these themes were found to be amenable to IT solutions. Using the multi-level orientation of the ITIF, we set forth strategies beyond IT solutions that can have an impact on reengineering clinical research tasks in practice-based settings. Developing strategies to target enabling and reinforcing factors, which focus on organizational factors, and the motivation of the practice at large to use IT solutions to integrate clinical research tasks with patient care processes, is most challenging. The ITIF should be used to consider both IT and non-IT solutions concurrently for reengineering of clinical research in community-based practice settings. © 2013.

CSBB-ConeExclusion, adapting structure based solution virtual screening to libraries on solid support.

PubMed

Shave, Steven; Auer, Manfred

2013-12-23

Combinatorial chemical libraries produced on solid support offer fast and cost-effective access to a large number of unique compounds. If such libraries are screened directly on-bead, the speed at which chemical space can be explored by chemists is much greater than that addressable using solution based synthesis and screening methods. Solution based screening has a large supporting body of software such as structure-based virtual screening tools which enable the prediction of protein-ligand complexes. Use of these techniques to predict the protein bound complexes of compounds synthesized on solid support neglects to take into account the conjugation site on the small molecule ligand. This may invalidate predicted binding modes, the linker may be clashing with protein atoms. We present CSBB-ConeExclusion, a methodology and computer program which provides a measure of the applicability of solution dockings to solid support. Output is given in the form of statistics for each docking pose, a unique 2D visualization method which can be used to determine applicability at a glance, and automatically generated PyMol scripts allowing visualization of protein atom incursion into a defined exclusion volume. CSBB-ConeExclusion is then exemplarically used to determine the optimum attachment point for a purine library targeting cyclin-dependent kinase 2 CDK2.

Digital Sound Synthesis Algorithms: a Tutorial Introduction and Comparison of Methods

NASA Astrophysics Data System (ADS)

Lee, J. Robert

The objectives of the dissertation are to provide both a compendium of sound-synthesis methods with detailed descriptions and sound examples, as well as a comparison of the relative merits of each method based on ease of use, observed sound quality, execution time, and data storage requirements. The methods are classified under the general headings of wavetable-lookup synthesis, additive synthesis, subtractive synthesis, nonlinear methods, and physical modelling. The nonlinear methods comprise a large group that ranges from the well-known frequency-modulation synthesis to waveshaping. The final category explores computer modelling of real musical instruments and includes numerical and analytical solutions to the classical wave equation of motion, along with some of the more sophisticated time -domain models that are possible through the prudent combination of simpler synthesis techniques. The dissertation is intended to be understandable by a musician who is mathematically literate but who does not necessarily have a background in digital signal processing. With this limitation in mind, a brief and somewhat intuitive description of digital sampling theory is provided in the introduction. Other topics such as filter theory are discussed as the need arises. By employing each of the synthesis methods to produce the same type of sound, interesting comparisons can be made. For example, a struck string sound, such as that typical of a piano, can be produced by algorithms in each of the synthesis classifications. Many sounds, however, are peculiar to a single algorithm and must be examined independently. Psychoacoustic studies were conducted as an aid in the comparison of the sound quality of several implementations of the synthesis algorithms. Other psychoacoustic experiments were conducted to supplement the established notions of which timbral issues are important in the re -synthesis of the sounds of acoustic musical instruments.

Solution-Processed Metal Oxides as Efficient Carrier Transport Layers for Organic Photovoltaics.

PubMed

Choy, Wallace C H; Zhang, Di

2016-01-27

Carrier (electron and hole) transport layers (CTLs) are essential components for boosting the performance of various organic optoelectronic devices such as organic solar cells and organic light-emitting diodes. Considering the drawbacks of conventional CTLs (easily oxidized/unstable, demanding/costly fabrication, etc.), transition metal oxides with good carrier transport/extraction and superior stability have drawn extensive research interest as CTLs for next-generation devices. In recent years, many research efforts have been made toward the development of solution-based metal oxide CTLs with the focus on low- or even room-temperature processes, which can potentially be compatible with the deposition processes of organic materials and can significantly contribute to the low-cost and scale-up of organic devices. Here, the recent progress of different types of solution-processed metal oxide CTLs are systematically reviewed in the context of organic photovoltaics, from synthesis approaches to device performance. Different approaches for further enhancing the performance of solution-based metal oxide CTLs are also discussed, which may push the future development of this exciting field. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Rapid Nanoprobe Signal Enhancement by In Situ Gold Nanoparticle Synthesis.

PubMed

Dias, Jorge T; Svedberg, Gustav; Nystrand, Mats; Andersson-Svahn, Helene; Gantelius, Jesper

2018-03-07

The use of nanoprobes such as gold, silver, silica or iron-oxide nanoparticles as detection reagents in bioanalytical assays can enable high sensitivity and convenient colorimetric readout. However, high densities of nanoparticles are typically needed for detection. The available synthesis-based enhancement protocols are either limited to gold and silver nanoparticles or rely on precise enzymatic control and optimization. Here, we present a protocol to enhance the colorimetric readout of gold, silver, silica, and iron oxide nanoprobes. It was observed that the colorimetric signal can be improved by up to a 10000-fold factor. The basis for such signal enhancement strategies is the chemical reduction of Au 3+ to Au 0 . There are several chemical reactions that enable the reduction of Au 3+ to Au 0 . In the protocol, Good's buffers and H2O2 are used and it is possible to favor the deposition of Au 0 onto the surface of existing nanoprobes, in detriment of the formation of new gold nanoparticles. The protocol consists of the incubation of the microarray with a solution consisting of chloroauric acid and H2O2 in 2-(N-morpholino)ethanesulfonic acid pH 6 buffer following the nanoprobe-based detection assay. The enhancement solution can be applied to paper and glass-based sensors. Moreover, it can be used in commercially available immunoassays as demonstrated by the application of the method to a commercial allergen microarray. The signal development requires less than 5 min of incubation with the enhancement solution and the readout can be assessed by naked eye or low-end image acquisition devices such as a table-top scanner or a digital camera.

Improved inter-layer prediction for light field content coding with display scalability

NASA Astrophysics Data System (ADS)

Conti, Caroline; Ducla Soares, Luís.; Nunes, Paulo

2016-09-01

Light field imaging based on microlens arrays - also known as plenoptic, holoscopic and integral imaging - has recently risen up as feasible and prospective technology due to its ability to support functionalities not straightforwardly available in conventional imaging systems, such as: post-production refocusing and depth of field changing. However, to gradually reach the consumer market and to provide interoperability with current 2D and 3D representations, a display scalable coding solution is essential. In this context, this paper proposes an improved display scalable light field codec comprising a three-layer hierarchical coding architecture (previously proposed by the authors) that provides interoperability with 2D (Base Layer) and 3D stereo and multiview (First Layer) representations, while the Second Layer supports the complete light field content. For further improving the compression performance, novel exemplar-based inter-layer coding tools are proposed here for the Second Layer, namely: (i) an inter-layer reference picture construction relying on an exemplar-based optimization algorithm for texture synthesis, and (ii) a direct prediction mode based on exemplar texture samples from lower layers. Experimental results show that the proposed solution performs better than the tested benchmark solutions, including the authors' previous scalable codec.

From non-preemptive to preemptive scheduling using synchronization synthesis.

PubMed

Černý, Pavol; Clarke, Edmund M; Henzinger, Thomas A; Radhakrishna, Arjun; Ryzhyk, Leonid; Samanta, Roopsha; Tarrach, Thorsten

2017-01-01

We present a computer-aided programming approach to concurrency. The approach allows programmers to program assuming a friendly, non-preemptive scheduler, and our synthesis procedure inserts synchronization to ensure that the final program works even with a preemptive scheduler. The correctness specification is implicit, inferred from the non-preemptive behavior. Let us consider sequences of calls that the program makes to an external interface. The specification requires that any such sequence produced under a preemptive scheduler should be included in the set of sequences produced under a non-preemptive scheduler. We guarantee that our synthesis does not introduce deadlocks and that the synchronization inserted is optimal w.r.t. a given objective function. The solution is based on a finitary abstraction, an algorithm for bounded language inclusion modulo an independence relation, and generation of a set of global constraints over synchronization placements. Each model of the global constraints set corresponds to a correctness-ensuring synchronization placement. The placement that is optimal w.r.t. the given objective function is chosen as the synchronization solution. We apply the approach to device-driver programming, where the driver threads call the software interface of the device and the API provided by the operating system. Our experiments demonstrate that our synthesis method is precise and efficient. The implicit specification helped us find one concurrency bug previously missed when model-checking using an explicit, user-provided specification. We implemented objective functions for coarse-grained and fine-grained locking and observed that different synchronization placements are produced for our experiments, favoring a minimal number of synchronization operations or maximum concurrency, respectively.

Synthesis of Pyridine– and Pyrazine–BF 3 Complexes and Their Characterization in Solution and Solid State

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

Chénard, Etienne; Sutrisno, Andre; Zhu, Lingyang

2016-03-31

Following the discovery of the redox-active 1,4- bis-BF 3-quinoxaline complex, we undertook a structure- activity study with the objective to understand the active nature of the quinoxaline complex. Through systematic synthesis and characterization, we have compared complexes prepared from pyridine and pyrazine derivatives, as heterocyclic core analogues. This paper reports the structural requirements that give rise to the electrochemical features of the 1,4-bis-BF 3-quinoxaline adduct. Using solution and solidstate NMR spectroscopy, the role of aromatic ring fusion and nitrogen incorporation in bonding and electronics was elucidated. We establish the boron atom location and its interaction with its environment from 1Dmore » and 2D solution NMR, X-ray diffraction analysis, and 11B solid-state NMR experiments. Crystallographic analysis of single crystals helped to correlate the boron geometry with 11B quadrupolar coupling constant (CQ) and asymmetry parameter (ηQ), extracted from 11B solid-state NMR spectra. Additionally, computations based on density functional theory were performed to predict electrochemical behavior of the BF 3-heteroaromatic complexes. We then experimentally measured electrochemical potential using cyclic voltammetry and found that the redox potentials and CQ values are similarly affected by electronic changes in the complexes.« less

Surface Modification of Graphene Oxides by Plasma Techniques and Their Application for Environmental Pollution Cleanup.

PubMed

Wang, Xiangxue; Fan, Qiaohui; Chen, Zhongshan; Wang, Qi; Li, Jiaxing; Hobiny, Aatef; Alsaedi, Ahmed; Wang, Xiangke

2016-02-01

Graphene oxides (GOs) have come under intense multidisciplinary study because of their unique physicochemical properties and possible applications. The large amount of oxygen-containing functional groups on GOs leads to a high sorption capacity for the removal of various kinds of organic and inorganic pollutants from aqueous solutions in environmental pollution cleanup. However, the lack of selectivity results in difficulty in the selective removal of target pollutants from aqueous solutions in the presence of other coexisting pollutants. Herein, the surface grafting of GOs with special oxygen-containing functional groups using low-temperature plasma techniques and the application of the surface-modified GOs for the efficient removal of organic and inorganic pollutants in environmental pollution are reviewed. This paper gives an account of our research on the application of GO-based nanomaterials in environmental pollution cleanup, including: (1) the synthesis and surface grafting of functional groups on GOs, summarizing various types of low-temperature plasma techniques for the synthesis of graphene/GOs; and (2) the application of graphene/GOs and their composites for the efficient removal of organic and inorganic pollutants from aqueous solutions, including the interaction mechanism according to recently published results. © 2015 The Chemical Society of Japan & Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

High-performance carbon-coated ZnMn2O4 nanocrystallite supercapacitors with tailored microstructures enabled by a novel solution combustion method

NASA Astrophysics Data System (ADS)

Abdollahifar, Mozaffar; Huang, Sheng-Siang; Lin, Yu-Hsiang; Lin, Yan-Cheng; Shih, Bing-Yi; Sheu, Hwo-Shuenn; Liao, Yen-Fa; Wu, Nae-Lih

2018-02-01

Although ZnMn2O4 is widely studied as Li-ion battery anodes, it remains a challenge to tailor suitable microstructures of the oxide for supercapacitor applications. Carbon-coated ZnMn2O4 (C@ZMO) nanocrystallites showing high-performance pseudocapacitor behaviours in neutral aqueous electrolyte are for the first time successfully synthesised via a novel solution combustion process using polyethylene glycol as a multifunctional microstructure-directing agent. Controlling the molecular weight and amount of the polymer in the combustion solution enables the formation of highly-crystalline C@ZMO having substantially higher, by more than 5 folds, specific surface areas with mesoporous structures and conformal carbon coating via the one-pot synthesis process. The resulting C@ZMO supercapacitor electrodes in Na2SO4(aq) electrolyte exhibit ideal capacitive behaviours with specific capacitances up to 150 F g-1 and cycle stability showing no capacitance fade after 10,000 cycles at 60% of full capacity and >99% Coulombic efficiency. This study not only illustrates a new powerful synthesis route capable of producing conductive mesoporous crystalline oxide-based nanomaterials for energy storage applications but also reveals a new class of high-performance pseudocapacitive materials for neutral aqueous electrolytes.

Analytical solution of Luedeking-Piret equation for a batch fermentation obeying Monod growth kinetics.

PubMed

Garnier, Alain; Gaillet, Bruno

2015-12-01

Not so many fermentation mathematical models allow analytical solutions of batch process dynamics. The most widely used is the combination of the logistic microbial growth kinetics with Luedeking-Piret bioproduct synthesis relation. However, the logistic equation is principally based on formalistic similarities and only fits a limited range of fermentation types. In this article, we have developed an analytical solution for the combination of Monod growth kinetics with Luedeking-Piret relation, which can be identified by linear regression and used to simulate batch fermentation evolution. Two classical examples are used to show the quality of fit and the simplicity of the method proposed. A solution for the combination of Haldane substrate-limited growth model combined with Luedeking-Piret relation is also provided. These models could prove useful for the analysis of fermentation data in industry as well as academia. © 2015 Wiley Periodicals, Inc.

Synthesis and characterization of LTA nanozeolite using barley husk silica: Mercury removal from standard and real solutions

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

Azizi, Seyed Naser, E-mail: azizi@umz.ac.ir; Dehnavi, Ahmad Roozbehani, E-mail: Roozbehanisulfur@yahoo.com; Joorabdoozha, Amir

2013-05-15

Highlights: ► Silica extraction from barley husk with high purity for the synthesis of A nanozeolite. ► Free template A nanozeolite synthesized via new source of silica at low temperature. ► Optimization of SiO{sub 2}/Al{sub 2}O{sub 3}, Na{sub 2}O/SiO{sub 2} ratios, temperature and time of the synthesis. ► Utilizing of synthesized A nanozeolite for mercury removal from aqueous solutions. ► Mercury removal at optimized pH, contact time and adsorbent dose from real solution. - Abstract: In this study, synthesized Lined Type A (LTA) nanozeolite from barley husk silica (BHS) was used for mercury removal from standard and real aqueous solutions.more » The BHS in amorphous phase with 80% purity was extracted from barley husk ash (BHA), and used effectively as a new source of silica for the synthesis of NaA nanozeolite. The NaA nanocrystal in pure phase has been synthesized at low temperature, without adding any organic additives. The effects of heating time, reaction temperature, SiO{sub 2}/Al{sub 2}O{sub 3}, and Na{sub 2}O/SiO{sub 2} mole ratios on the crystallization of NaA nanozeolite were studied. The adsorption capacity of mercury (II) was studied as a function of pH, contact time, and amount of adsorbent. The crystallization of NaA nanozeolite from BHS was characterized by X-ray diffraction (XRD), X-ray fluorescence (XRF), scanning electron microscopy (SEM), energy-dispersive X-ray (EDX), Brunauer–Emmett–Teller (BET), and FTIR techniques. Moreover, concentration of Hg{sup 2+} ions in the aqueous solutions was analyzed by hydride generation atomic absorption spectroscopy method (HG-AAS). The standard and real samples analysis showed that NaA nanozeolite is capable of Hg{sup 2+} ions removal from the aqueous solutions. Efficiency of mercury (II) adsorption from real solutions onto the nano-sized NaA zeolite was 98%.« less

Force fields for describing the solution-phase synthesis of shape-selective metal nanoparticles

NASA Astrophysics Data System (ADS)

Zhou, Ya; Al-Saidi, Wissam; Fichthorn, Kristen

2013-03-01

Polyvinylpyrrolidone (PVP) and polyethylene oxide (PEO) are structure-directing agents that exhibit different performance in the polyol synthesis of Ag nanostructures. The success of these structure-directing agents in selective nanostructure synthesis is often attributed to their selective binding to Ag(100) facets. We use first-principles, density-functional theory (DFT) calculations in a vacuum environment to show that PVP has a stronger preference to bind to Ag(100) than to Ag(111), whereas PEO exhibits much weaker selectivity. To understand the role of solvent in the surface-sensitive binding, we develop classical force fields to describe the interactions of the structure-directing (PVP and PEO) and solvent (ethylene glycol) molecules with various Ag substrates. We parameterize the force fields through force-and-energy matching to DFT results using simulated annealing. We validate the force fields by comparisons to DFT and experimental binding energies. Our force fields reproduce the surface-sensitive binding predicted by DFT calculations. Molecular dynamics simulations based on these force fields can be used to reveal the role of solvent, polymer chain length, and polymer concentration in the selective synthesis of Ag nanostructures.

Biogenic silver nanoparticles using Rhinacanthus nasutus leaf extract: synthesis, spectral analysis, and antimicrobial studies

PubMed Central

Pasupuleti, Visweswara Rao; Prasad, TNVKV; Shiekh, Rayees Ahmad; Balam, Satheesh Krishna; Narasimhulu, Ganapathi; Reddy, Cirandur Suresh; Rahman, Ismail Ab; Gan, Siew Hua

2013-01-01

Nanotechnology is gaining momentum due to its ability to transform metals into nanoparticles. The synthesis, characterization, and applications of biologically synthesized nanomaterials have become an important branch of nanotechnology. Plant extracts are a cost-effective, ecologically friendly, and efficient alternative for the large-scale synthesis of nanoparticles. In this study, silver nanoparticles (AgNps) were synthesized using Rhinacanthus nasutus leaf extract. After exposing the silver ions to the leaf extract, the rapid reduction of silver ions led to the formation of AgNps in solution. The synthesis was confirmed by ultraviolet-visible spectroscopy, Fourier transform infrared spectroscopy, and transmission electron microscopy. The in vitro antimicrobial activity of the AgNps synthesized using R. nasutus leaf extract was investigated against Bacillus subtilis, Staphylococcus aureus, Pseudomonas aeruginosa, Klebsiella pneumonia, Escherichia coli, Aspergillus niger, and Aspergillus flavus using a disc diffusion method. The AgNps showed potential activity against all of the bacterial strains and fungal colonies, indicating that R. nasutus has the potential to be used in the development of value-added products in the biomedical and nanotechnology-based industries. PMID:24039419

Biogenic silver nanoparticles using Rhinacanthus nasutus leaf extract: synthesis, spectral analysis, and antimicrobial studies.

PubMed

Pasupuleti, Visweswara Rao; Prasad, T N V; Shiekh, Rayees Ahmad; Balam, Satheesh Krishna; Narasimhulu, Ganapathi; Reddy, Cirandur Suresh; Ab Rahman, Ismail; Gan, Siew Hua

2013-01-01

Nanotechnology is gaining momentum due to its ability to transform metals into nanoparticles. The synthesis, characterization, and applications of biologically synthesized nanomaterials have become an important branch of nanotechnology. Plant extracts are a cost-effective, ecologically friendly, and efficient alternative for the large-scale synthesis of nanoparticles. In this study, silver nanoparticles (AgNps) were synthesized using Rhinacanthus nasutus leaf extract. After exposing the silver ions to the leaf extract, the rapid reduction of silver ions led to the formation of AgNps in solution. The synthesis was confirmed by ultraviolet-visible spectroscopy, Fourier transform infrared spectroscopy, and transmission electron microscopy. The in vitro antimicrobial activity of the AgNps synthesized using R. nasutus leaf extract was investigated against Bacillus subtilis, Staphylococcus aureus, Pseudomonas aeruginosa, Klebsiella pneumonia, Escherichia coli, Aspergillus niger, and Aspergillus flavus using a disc diffusion method. The AgNps showed potential activity against all of the bacterial strains and fungal colonies, indicating that R. nasutus has the potential to be used in the development of value-added products in the biomedical and nanotechnology-based industries.

Synthesis of silicon containing materials using liquid hydrosilane compositions through direct injection

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

Srinivasan, Guruvenket; Sailer, Robert A.; Hoey, Justin

An apparatus and a non-vapor-pressure dependent method of chemical vapor deposition of Si based materials using direct injection of liquid hydrosilane(s) are presented. Liquid silane precursor solutions may also include metal, non-metal or metalloid dopants, nanomaterials and solvents. An illustrative apparatus has a precursor solution and carrier gas system, atomizer and deposit head with interior chamber and a hot plate supporting the substrate. Atomized liquid silane precursor solutions and carrier gas moves through a confined reaction zone that may be heated and the aerosol and vapor are deposited on a substrate to form a thin film. The substrate may bemore » heated prior to deposition. The deposited film may be processed further with thermal or laser processing.« less

LiGe(SiMe₃)₃: A New Substituent for the Synthesis of Metalloid Tin Clusters from Metastable Sn(I) Halide Solutions.

PubMed

Binder, Mareike; Schrenk, Claudio; Block, Theresa; Pöttgen, Rainer; Schnepf, Andreas

2018-04-26

The most fruitful synthetic route to metalloid tin clusters applies the disproportionation reaction of metastable Sn(I) halide solutions, whereby Si(SiMe₃)₃ is mostly used as the stabilizing substituent. Here, we describe the synthesis and application of the slightly modified substituent Ge(SiMe₃)₃, which can be used for the synthesis of metalloid tin clusters to give the neutral cluster Sn 10 [Ge(SiMe₃)₃]₆ as well as the charged clusters {Sn 10 [Ge(SiMe₃)₃]₅} − and {Sn 10 [Ge(SiMe₃)₃]₄} 2− . The obtained metalloid clusters are structurally similar to their Si(SiMe₃)₃ derivatives. However, differences with respect to the stability in solution are observed. Additionally, a different electronic situation for the tin atoms is realized as shown by 119m Sn Mössbauer spectroscopy, giving further insight into the different kinds of tin atoms within the metalloid cluster {Sn 10 [Ge(SiMe₃)₃]₄} 2− . The synthesis of diverse derivatives gives the opportunity to check the influence of the substituent for further investigations of metalloid tin cluster compounds.

Effects of synthesis techniques on chemical composition, microstructure and dielectric properties of Mg-doped calcium titanate

NASA Astrophysics Data System (ADS)

Jongprateep, Oratai; Sato, Nicha

2018-04-01

Calcium titanate (CaTiO3) has been recognized as a material for fabrication of dielectric components, owing to its moderate dielectric constant and excellent microwave response. Enhancement of dielectric properties of the material can be achieved through doping, compositional and microstructural control. This study, therefore, aimed at investigating effects of powder synthesis techniques on compositions, microstructure, and dielectric properties of Mg-doped CaTiO3. Solution combustion and solid-state reaction were powder synthesis techniques employed in preparation of undoped CaTiO3 and CaTiO3 doped with 5-20 at% Mg. Compositional analysis revealed that powder synthesis techniques did not exhibit a significant effect on formation of secondary phases. When Mg concentration did not exceed 5 at%, the powders prepared by both techniques contained only a single phase. An increase of MgO secondary phase was observed as Mg concentrations increased from 10 to 20 at%. Experimental results, on the contrary, revealed that powder synthesis techniques contributed to significant differences in microstructure. Solution combustion technique produced powders with finer particle sizes, which consequently led to finer grain sizes and density enhancement. High-density specimens with fine microstructure generally exhibit improved dielectric properties. Dielectric measurements revealed that dielectric constants of all samples ranged between 231 and 327 at 1 MHz, and that superior dielectric constants were observed in samples prepared by the solution combustion technique.

Citrate-capped superparamagnetic iron oxide (Fe3O4-CA) nanocatalyst for synthesis of pyrimidine derivative compound as antioxidative agent

NASA Astrophysics Data System (ADS)

Cahyana, A. H.; Pratiwi, D.; Ardiansah, B.

2017-04-01

The development of a recyclable catalyst based on magnetic nanoparticles has attracted an increasing interest as the emerging application in the heterogeneous catalyst field. Superparamagnetic iron oxide nanoparticle with citric acid as capping agent was successfully obtained from iron (III) chloride solution via two steps synthesis. The first step involving the formation of magnetite nanoparticle by bioreduction using Sargassum Sp, then its surface was modified by adding citric acid solution in the second step. The structural, surface morphology and magnetic properties of the nanocatalyst were investigated by various instrumentations such as scanning electron microscope with energy dispersive (SEM-EDS), and particle size analyser (PSA). Fe3O4-CA was then applied as reusable catalyst for Knoevenagel condensation of barbituric acid and cinnamaldehyde to produce (E)-5-(3-phenylallylidene)pyrimidine-2,4,6(1H,3H,5H)-trione. The optimum condition of this reaction was achieved by using 7.5% mole of catalyst at 50°C for 6 h to give 83% yield. Some spectroscopy techniques such as UV-Vis, FTIR, LC-MS and 1H-NMR were used to confirm the product’s structure. Furthermore, the synthesized compound has an attractive antioxidant activity based on the in-vitro analysis using DPPH method.

Combinatorial evolution of site- and enantioselective catalysts for polyene epoxidation

NASA Astrophysics Data System (ADS)

Lichtor, Phillip A.; Miller, Scott J.

2012-12-01

Selectivity in the catalytic functionalization of complex molecules is a major challenge in chemical synthesis. The problem is magnified when there are several possible stereochemical outcomes and when similar functional groups occur repeatedly within the same molecule. Selective polyene oxidation provides an archetypical example of this challenge. Historically, enzymatic catalysis has provided the only precedents. Although non-enzymatic catalysts that meet some of these challenges became known, a comprehensive solution has remained elusive. Here, we describe low molecular weight peptide-based catalysts, discovered through a combinatorial synthesis and screening protocol, that exhibit site- and enantioselective oxidation of certain positions of various isoprenols. This diversity-based approach, which exhibits features reminiscent of the directed evolution of enzymes, delivers catalysts that compare favourably to the state-of-the-art for the asymmetric oxidation of these compounds. Moreover, the approach culminated in catalysts that exhibit alternative-site selectivity in comparison to oxidation catalysts previously described.

Selective Production of Renewable para-Xylene by Tungsten Carbide Catalyzed Atom-Economic Cascade Reactions.

PubMed

Dai, Tao; Li, Changzhi; Li, Lin; Zhao, Zongbao Kent; Zhang, Bo; Cong, Yu; Wang, Aiqin

2018-02-12

Tungsten carbide was employed as the catalyst in an atom-economic and renewable synthesis of para-xylene with excellent selectivity and yield from 4-methyl-3-cyclohexene-1-carbonylaldehyde (4-MCHCA). This intermediate is the product of the Diels-Alder reaction between the two readily available bio-based building blocks acrolein and isoprene. Our results suggest that 4-MCHCA undergoes a novel dehydroaromatization-hydrodeoxygenation cascade process by intramolecular hydrogen transfer that does not involve an external hydrogen source, and that the hydrodeoxygenation occurs through the direct dissociation of the C=O bond on the W 2 C surface. Notably, this process is readily applicable to the synthesis of various (multi)methylated arenes from bio-based building blocks, thus potentially providing a petroleum-independent solution to valuable aromatic compounds. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Solution-Based Fabrication of Polycrystalline Si Thin-Film Transistors from Recycled Polysilanes.

PubMed

Sberna, Paolo M; Trifunovic, Miki; Ishihara, Ryoichi

2017-07-03

Currently, research has been focusing on printing and laser crystallization of cyclosilanes, bringing to life polycrystalline silicon (poly-Si) thin-film transistors (TFTs) with outstanding properties. However, the synthesis of these Si-based inks is generally complex and expensive. Here, we prove that a polysilane ink, obtained as a byproduct of silicon gases and derivatives, can be used successfully for the synthesis of poly-Si by laser annealing, at room temperature, and for n- and p-channel TFTs. The devices, fabricated according to CMOS compatible processes at 350 °C, showed field effect mobilities up to 8 and 2 cm 2 /(V s) for n- and p-type TFTs, respectively. The presented method combines a low-cost coating technique with the usage of recycled material, opening a route to a convenient and sustainable production of large-area, flexible, and even disposable/single-use electronics.

Rationalism, Empiricism, and Evidence-Based Medicine: A Call for a New Galenic Synthesis.

PubMed

Webb, William M

2018-04-25

Thirty years after the rise of the evidence-based medicine (EBM) movement, formal training in philosophy remains poorly represented among medical students and their educators. In this paper, I argue that EBM’s reception in this context has resulted in a privileging of empiricism over rationalism in clinical reasoning with unintended consequences for medical practice. After a limited review of the history of medical epistemology, I argue that a solution to this problem can be found in the method of the 2nd-century Roman physician Galen, who brought empiricism and rationalism together in a synthesis anticipating the scientific method. Next, I review several of the problems that have been identified as resulting from a staunch commitment to empiricism in medical practice. Finally, I conclude that greater epistemological awareness in the medical community would precipitate a Galenic shift toward a more epistemically balanced, scientific approach to clinical research.

Corrigendum to "Synthesis of hydroxyapatite/multi-walled carbon nanotubes for the removal of fluoride ions from solution" [Appl. Surf. Sci. 412 (2017) 578-590

NASA Astrophysics Data System (ADS)

Ruan, Zhongyuan; Tian, Yaxi; Ruan, Jifu; Cui, Guijia; Iqbal, Kanwal; Iqbal, Anam; Ye, Herui; Yang, Zhangzhong; Yan, Shiqiang

2018-04-01

In our recent paper [1], we reported the synthesis of hydroxyapatite/multi-walled carbon nanotubes (HA-MWCNTs) and studied their performance for the removal of fluoride ions from solution. However, we have made some writing mistakes, especially in the section on adsorption kinetics analysis. Our mistakes were spotted by Prof. Yuandong Huang, who graciously noticed these errors. We are grateful to him, and have decided to write a "Corrigendum".

A Physics-Based Vibrotactile Feedback Library for Collision Events.

PubMed

Park, Gunhyuk; Choi, Seungmoon

2017-01-01

We present PhysVib: a software solution on the mobile platform extending an open-source physics engine in a multi-rate rendering architecture for automatic vibrotactile feedback upon collision events. PhysVib runs concurrently with a physics engine at a low update rate and generates vibrotactile feedback commands at a high update rate based on the simulation results of the physics engine using an exponentially-decaying sinusoidal model. We demonstrate through a user study that this vibration model is more appropriate to our purpose in terms of perceptual quality than more complex models based on sound synthesis. We also evaluated the perceptual performance of PhysVib by comparing eight vibrotactile rendering methods. Experimental results suggested that PhysVib enables more realistic vibrotactile feedback than the other methods as to perceived similarity to the visual events. PhysVib is an effective solution for providing physically plausible vibrotactile responses while reducing application development time to great extent.

Control of size and aspect ratio in hydroquinone-based synthesis of gold nanorods

NASA Astrophysics Data System (ADS)

Morasso, Carlo; Picciolini, Silvia; Schiumarini, Domitilla; Mehn, Dora; Ojea-Jiménez, Isaac; Zanchetta, Giuliano; Vanna, Renzo; Bedoni, Marzia; Prosperi, Davide; Gramatica, Furio

2015-08-01

In this article, we describe how it is possible to tune the size and the aspect ratio of gold nanorods obtained using a highly efficient protocol based on the use of hydroquinone as a reducing agent by varying the amounts of CTAB and silver ions present in the "seed-growth" solution. Our approach not only allows us to prepare nanorods with a four times increased Au3+ reduction yield, when compared with the commonly used protocol based on ascorbic acid, but also allows a remarkable reduction of 50-60 % of the amount of CTAB needed. In fact, according to our findings, the concentration of CTAB present in the seed-growth solution do not linearly influence the final aspect ratio of the obtained nanorods, and an optimal concentration range between 30 and 50 mM has been identified as the one that is able to generate particles with more elongated shapes. On the optimized protocol, the effect of the concentration of Ag+ ions in the seed-growth solution and the stability of the obtained particles has also been investigated.

Hydrothermal synthesis of nanostructured Y2O3 and (Y0.75Gd0.25)2O3 based phosphors

NASA Astrophysics Data System (ADS)

Mančić, Lidija; Lojpur, Vesna; Marinković, Bojan A.; Dramićanin, Miroslav D.; Milošević, Olivera

2013-08-01

Examples of (Y2O3-Gd2O3):Eu3+ and Y2O3:(Yb3+/Er3+) rare earth oxide-based phosphors are presented to highlight the controlled synthesis of 1D and 2D nanostructures through simple hydrothermal method. Conversion of the starting nitrates mixture into carbonate hydrate phase is performed with the help of ammonium hydrogen carbonate solution during hydrothermal treatment at 200 °C/3 h. Morphological architectures of rare earth oxides obtained after subsequent powders thermal treatment at 600 and 1100 °C for 3 and 12 h and their correlation with the optical characteristics are discussed based on X-ray powder diffractometry, field emission scanning electron microscopy, infrared spectroscopy and photoluminescence measurements. Strong red and green emission followed by the superior decay times are attributed to the high powders purity and homogeneous dopants distribution over the host lattice matrix.

Lac-L-TTA, a novel lactose-based amino acid-sugar conjugate for anti-metastatic applications.

PubMed

Roviello, Giovanni N; Iannitti, Roberta; Palumbo, Rosanna; Simonyan, Hayarpi; Vicidomini, Caterina; Roviello, Valentina

2017-08-01

Here we describe the synthesis, chromatographic purification, MS and NMR characterization of a new lactosyl-derivative, i.e. a lactosyl thiophenyl-substituted triazolyl-thione L-alanine (Lac-L-TTA). This amino acid-sugar conjugate was prepared by solution synthesis in analogy to the natural fructosyl-amino acids. Furthermore, we investigated the inhibition of PC-3 prostate cancer cell colony formation by this lactose derivative in comparison with the less polar fructose-based derivative, Fru-L-TTA. This let us to compare the properties of the artificial derivative, object of the present work, with the monosaccharide-based counterpart and to obtain a preliminary information on the influence of polarity on such biological activity. A significantly higher anticancer effect of Lac-L-TTA with respect to the fructose analogue emerged from our study suggesting that the anti-metastatic potential of fructosyl-amino acids can be enhanced by increasing the polarity of the compounds, for example by introducing disaccharide moieties in place of fructose.

Determination of the Degree of Substitution of Cationic Guar Gum by Headspace-Based Gas Chromatography during Its Synthesis.

PubMed

Wan, Xiaofang; Guo, Congbao; Feng, Jiarui; Yu, Teng; Chai, Xin-Sheng; Chen, Guangxue; Xie, Wei-Qi

2017-08-16

This study reports on a headspace-based gas chromatography (HS-GC) technique for determining the degree of substitution (DS) of cationic guar gum during the synthesis process. The method is based on the determination of 2,3-epoxypropyltrimethylammonium chloride in the process medium. After a modest pretreatment procedure, the sample was added to a headspace vial containing bicarbonate solution for measurement of evolved CO 2 by HS-GC. The results showed that the method had a good precision (relative standard deviation of <3.60%) and accuracy for the 2,3-epoxypropyltrimethylammonium chloride measurement, with recoveries in the range of 96-102%, matching with the data obtained by a reference method, and were within 12% of the values obtained by the more arduous Kjeldahl method for the calculated DS of cationic guar gum. The HS-GC method requires only a small volume of sample and, thus, is suitable for determining the DS of cationic guar gum in laboratory-scale process-related applications.

Novel hierarchical microparticles super-assembled from nanoparticles with the induction of casein micelles

NASA Astrophysics Data System (ADS)

Xiong, Xiaopeng; Duan, Jiangjiang; Wang, Yong; Yu, Zhaoju

2013-08-01

We have demonstrated a solution-based synthesis of novel waxberry-like hierarchical ZnO microparticles in the presence casein micelles under mild conditions. The microstructures of the sub-micrometer-sized hierarchical microparticles were characterized, and the synthesis conditions were optimized. The formation mechanism of the hierarchical microparticle was analyzed through control experiments. The hierarchical ZnO microparticles are found to be super-assemblies of 30-70 nm ZnO nanoparticles, which are thought to be based on casein micelle induction followed by Ostwald ripening. In the same manner, copper-based hierarchical microparticles with a similar morphology have also been successfully synthesized. By controlling the synthetic time or temperature, solid or hollow microparticles can be fabricated. The narrowly distributed ZnO microparticles have a high specific surface area, exhibiting great potential application in fields such as photocatalytic and energy conversion. Our findings may meanwhile open a new bottom-up strategy in order to construct structurally sophisticated nanomaterials.

Differently Environment Stable Bio-Silver Nanoparticles: Study on Their Optical Enhancing and Antibacterial Properties

PubMed Central

Balachandran, Yekkuni L.; Girija, Shanmugam; Selvakumar, Rajendran; Tongpim, Saowanit; Gutleb, Arno C.; Suriyanarayanan, Sarvajeyakesavalu

2013-01-01

Generally, limited research is extended in studying stability and applicational properties of silver nanoparticles (Ag NPs) synthesized by adopting ‘green chemistry’ protocol. In this work, we report on the synthesis of stable Ag NPs using plant-derived materials such as leaf extract of Neem (Azadirachta indica) and biopolymer pectin from apple peel. In addition, the applicational properties of Ag NPs such as surface-enhanced Raman scattering (SERS) and antibacterial efficiencies were also investigated. As-synthesized nanoparticles (NPs) were characterized using various instrumentation techniques. Both the plant materials (leaf extract and biopolymer) favored the synthesis of well-defined NPs capped with biomaterials. The NPs were spherical in shape with an average particle size between 14-27 nm. These bio-NPs exhibited colloidal stability in most of the suspended solutions such as water, electrolyte solutions (NaCl; NaNO3), biological solution (bovine serum albumin), and in different pH solutions (pH 7; 9) for a reasonable time period of 120 hrs. Both the bio-NPs were observed to be SERS active through displaying intrinsic SERS signals of the Raman probe molecule (Nile blue A). The NPs were effective against the Escherichia coli bacterium when tested in nutrient broth and agar medium. Scanning and high-resolution transmission electron microscopy (SEM and HRTEM) images confirmed cellular membrane damage of nanoparticle treated E. coli cells. These environmental friendly template Ag NPs can be used as an antimicrobial agent and also for SERS based analytical applications. PMID:24130832

Sources of Chemical Toxics and Their Precursors in Pharmaceutical Industry

DTIC Science & Technology

2001-09-01

includes a lot of independent units specialized in synthesis of active substances, their processing as pharmaceutical forms, control of intermediate and...materials (ingredients), synthesis intermediates, intermediate forms (solutions, powders), analytical reactives, drugs itself, residues etc. Secondary...specialist scenario The simplest idea is to orient the attack against chemical synthesis facilities friom where a lot of volatile solvents could be spread

Synthesis of copper oxide nanowires and nanoporous copper via environmentally friendly transformation of bulk copper-calcium alloys.

PubMed

Zhang, X; Turcheniuk, K; Zusmann, B; Benson, J; Nelson, S; Luo, S; Magasinski, A; Yushin, G

2018-05-24

In this work, we report a novel, one-step, inexpensive and environmentally friendly synthesis of Cu nanostructures by means of chemical de-alloying of bulk Cu-Ca alloys in aqueous solutions. By controlling the synthesis conditions, we tune the morphology of the nanostructured Cu from nanoporous Cu to copper oxide nanowires.

Color appearance for photorealistic image synthesis

NASA Astrophysics Data System (ADS)

Marini, Daniele; Rizzi, Alessandro; Rossi, Maurizio

2000-12-01

Photorealistic Image Synthesis is a relevant research and application field in computer graphics, whose aim is to produce synthetic images that are undistinguishable from real ones. Photorealism is based upon accurate computational models of light material interaction, that allow us to compute the spectral intensity light field of a geometrically described scene. The fundamental methods are ray tracing and radiosity. While radiosity allows us to compute the diffuse component of the emitted and reflected light, applying ray tracing in a two pass solution we can also cope with non diffuse properties of the model surfaces. Both methods can be implemented to generate an accurate photometric distribution of light of the simulated environment. A still open problem is the visualization phase, whose purpose is to display the final result of the simulated mode on a monitor screen or on a printed paper. The tone reproduction problem consists of finding the best solution to compress the extended dynamic range of the computed light field into the limited range of the displayable colors. Recently some scholars have addressed this problem considering the perception stage of image formation, so including a model of the human visual system in the visualization process. In this paper we present a working hypothesis to solve the tone reproduction problem of synthetic image generation, integrating Retinex perception model into the photo realistic image synthesis context.

Phytosynthesis of intracellular and extracellular gold nanoparticles by living peanut plant (Arachis hypogaea L.).

PubMed

Raju, Dugyala; Mehta, Urmil J; Ahmad, Absar

2012-01-01

Inorganic nanomaterials of different chemical compositions are conventionally synthesized under harsh environments such as extremes of temperature, pressure, and pH. Moreover, these methods are eco-unfriendly and cumbersome, yield bigger particles, and agglomerate because of not being capped by capping agents. In contrast, biological synthesis of inorganic nanomaterials occurs under ambient conditions, namely room temperature, atmospheric pressure, and physiological pH. These methods are reliable, eco-friendly, and cheap. In this paper, we report for the first time the extracellular and intracellular synthesis of gold nanoparticles (GNPs) using living peanut seedlings. The formed GNPs were highly stable in solution and inside the plant tissue. Transmission electron microscopy revealed that extracellular GNPs distributions were in the form of monodispersed nanoparticles. The nanoparticles ranged from 4 to 6 nm in size. The intercellular nanoparticles were of oval shape and size ranged from 5 to 50 nm. Both extracellular and intracellular nanoparticles were further characterized by standard techniques. The formed GNPs inside the plant tissue were estimated by inductively coupled plasma spectrometry. This opens up an exciting possibility of a plant-based nanoparticle synthesis strategy, wherein the nanoparticles may be entrapped in the biomass in the form of a film or produced in the solution, both of which have interesting applications. © 2012 International Union of Biochemistry and Molecular Biology, Inc.

Fully automated SPE-based synthesis and purification of 2-[18F]fluoroethyl-choline for human use.

PubMed

Schmaljohann, Jörn; Schirrmacher, Esther; Wängler, Björn; Wängler, Carmen; Schirrmacher, Ralf; Guhlke, Stefan

2011-02-01

2-[(18)F]Fluoroethyl-choline ([(18)F]FECH) is a promising tracer for the detection of prostate cancer as well as brain tumors with positron emission tomography (PET). [(18)F]FECH is actively transported into mammalian cells, becomes phosphorylated by choline kinase and gets incorporated into the cell membrane after being metabolized to phosphatidylcholine. So far, its synthesis is a two-step procedure involving at least one HPLC purification step. To allow a wider dissemination of this tracer, finding a purification method avoiding HPLC is highly desirable and would result in easier accessibility and more reliable production of [(18)F]FECH. [(18)F]FECH was synthesized by reaction of 2-bromo-1-[(18)F]fluoroethane ([(18)F]BFE) with dimethylaminoethanol (DMAE) in DMSO. We applied a novel and very reliable work-up procedure for the synthesis of [(18)F]BFE. Based on a combination of three different solid-phase cartridges, the purification of [(18)F]BFE from its precursor 2-bromoethyl-4-nitrobenzenesulfonate (BENos) could be achieved without using HPLC. Following the subsequent reaction of the purified [(18)F]BFE with DMAE, the final product [(18)F]FECH was obtained as a sterile solution by passing the crude reaction mixture through a combination of two CM plus cartridges and a sterile filter. The fully automated synthesis was performed using as well a Raytest SynChrom module (Raytest, Germany) or a Scintomics HotboxIII module (Scintomics, Germany). The radiotracer [(18)F]FECH can be synthesized in reliable radiochemical yields (RCY) of 37±5% (Synchrom module) and 33±5% (Hotbox III unit) in less than 1 h using these two fully automated commercially available synthesis units without HPLC involvement for purification. Detailed quality control of the final injectable [(18)F]FECH solution proved the high radiochemical purity and the absence of Kryptofix2.2.2, DMAE and DMSO used in the course of synthesis. Sterility and bacterial endotoxin testing following standard procedures verified that the described production method for [(18)F]FECH is suitable for human applications. The routine production of [(18)F]FECH with sufficient RCYs was established by reliable and fast solid-phase extraction purifications of both the secondary labeling precursor [(18)F]BFE and the final product [(18)F]FECH, avoiding complex and sensitive HPLC equipment. The purity of the product was >95%, rendering the tracer suitable for human application. The newly developed purification procedure for [(18)F]BFE significantly reduces the complexity of the automated synthesis unit, hence reducing the cost for routine production in a clinical setup and allowing easy transfer to different synthesis modules. Copyright © 2011 Elsevier Inc. All rights reserved.

Microwave-Assisted Green Synthesis of Silver Nanostructures

EPA Science Inventory

This account summarizes a microwave (MW)-assisted synthetic approach for producing silver nanostructures. The rapid and in-core MW heating has received considerable attention as a promising new method for the one-pot synthesis of metallic nanostructures in solutions. Conceptually...

Application of modern control theory to the design of optimum aircraft controllers

NASA Technical Reports Server (NTRS)

Power, L. J.

1973-01-01

The synthesis procedure presented is based on the solution of the output regulator problem of linear optimal control theory for time-invariant systems. By this technique, solution of the matrix Riccati equation leads to a constant linear feedback control law for an output regulator which will maintain a plant in a particular equilibrium condition in the presence of impulse disturbances. Two simple algorithms are presented that can be used in an automatic synthesis procedure for the design of maneuverable output regulators requiring only selected state variables for feedback. The first algorithm is for the construction of optimal feedforward control laws that can be superimposed upon a Kalman output regulator and that will drive the output of a plant to a desired constant value on command. The second algorithm is for the construction of optimal Luenberger observers that can be used to obtain feedback control laws for the output regulator requiring measurement of only part of the state vector. This algorithm constructs observers which have minimum response time under the constraint that the magnitude of the gains in the observer filter be less than some arbitrary limit.

A nickel tripeptide as a metallodithiolate ligand anchor for resin-bound organometallics.

PubMed

Green, Kayla N; Jeffery, Stephen P; Reibenspies, Joseph H; Darensbourg, Marcetta Y

2006-05-17

The molecular structure of the acetyl CoA synthase enzyme has clarified the role of individual nickel atoms in the dinickel active site which mediates C-C and C-S coupling reactions. The NiN2S2 portion of the biocatalyst (N2S2 = a cysteine-glycine-cysteine or CGC4- tripeptide ligand) serves as an S-donor ligand comparable to classical bidentate ligands operative in organometallic chemistry, ligating the second nickel which is redox and catalytically active. Inspired by this biological catalyst, the synthesis of NiN2S2 metalloligands, including the solid-phase synthesis of resin-bound Ni(CGC)2-, and sulfur-based derivatization with W(CO)5 and Rh(CO)2+ have been carried out. Through comparison to analogous well-characterized, solution-phase complexes, Attenuated Total Reflectance FTIR spectroscopy establishes the presence of unique heterobimetallic complexes, of the form [Ni(CGC)]M(CO)x, both in solution and immobilized on resin beads. This work provides the initial step toward exploitation of such an evolutionarily optimized nickel peptide as a solid support anchor for hybrid bioinorganic-organometallic catalysts.

Acyl guanidine inhibitors of β-secretase (BACE-1): optimization of a micromolar hit to a nanomolar lead via iterative solid- and solution-phase library synthesis.

PubMed

Gerritz, Samuel W; Zhai, Weixu; Shi, Shuhao; Zhu, Shirong; Toyn, Jeremy H; Meredith, Jere E; Iben, Lawrence G; Burton, Catherine R; Albright, Charles F; Good, Andrew C; Tebben, Andrew J; Muckelbauer, Jodi K; Camac, Daniel M; Metzler, William; Cook, Lynda S; Padmanabha, Ramesh; Lentz, Kimberley A; Sofia, Michael J; Poss, Michael A; Macor, John E; Thompson, Lorin A

2012-11-08

This report describes the discovery and optimization of a BACE-1 inhibitor series containing an unusual acyl guanidine chemotype that was originally synthesized as part of a 6041-membered solid-phase library. The synthesis of multiple follow-up solid- and solution-phase libraries facilitated the optimization of the original micromolar hit into a single-digit nanomolar BACE-1 inhibitor in both radioligand binding and cell-based functional assay formats. The X-ray structure of representative inhibitors bound to BACE-1 revealed a number of key ligand:protein interactions, including a hydrogen bond between the side chain amide of flap residue Gln73 and the acyl guanidine carbonyl group, and a cation-π interaction between Arg235 and the isothiazole 4-methoxyphenyl substituent. Following subcutaneous administration in rats, an acyl guanidine inhibitor with single-digit nanomolar activity in cells afforded good plasma exposures and a dose-dependent reduction in plasma Aβ levels, but poor brain exposure was observed (likely due to Pgp-mediated efflux), and significant reductions in brain Aβ levels were not obtained.

Microwave assisted synthesis of luminescent carbonaceous nanoparticles from silk fibroin for bioimaging.

PubMed

Gao, Hongzhi; Teng, Choon Peng; Huang, Donghong; Xu, Wanqing; Zheng, Chaohui; Chen, Yisong; Liu, Minghuan; Yang, Da-Peng; Lin, Ming; Li, Zibiao; Ye, Enyi

2017-11-01

Bombyx mori silk as a natural protein based biopolymer with high nitrogen content, is abundant and sustainable because of its mass product all over the world per year. In this study, we developed a facile and fast microwave-assisted synthesis of luminescent carbonaceous nanoparticles using Bombyx mori silk fibroin and silk solution as the precursors. As a result, the obtained carbonaceous nanoparticles exhibit a photoluminescence quantum yield of ~20%, high stability, low cytotoxicity, high biocompatibility. Most importantly, we successfully demonstrated bioimaging using these luminescent carbonaceous nanoparticles with excitation dependent luminescence. In addition, the microwave-assisted hydrothermal method can be extended to convert other biomass into functional nanomaterials. Copyright © 2017 Elsevier B.V. All rights reserved.

Hollow nanotubular toroidal polymer microrings.

PubMed

Lee, Jiyeong; Baek, Kangkyun; Kim, Myungjin; Yun, Gyeongwon; Ko, Young Ho; Lee, Nam-Suk; Hwang, Ilha; Kim, Jeehong; Natarajan, Ramalingam; Park, Chan Gyung; Sung, Wokyung; Kim, Kimoon

2014-02-01

Despite the remarkable progress made in the self-assembly of nano- and microscale architectures with well-defined sizes and shapes, a self-organization-based synthesis of hollow toroids has, so far, proved to be elusive. Here, we report the synthesis of polymer microrings made from rectangular, flat and rigid-core monomers with anisotropically predisposed alkene groups, which are crosslinked with each other by dithiol linkers using thiol-ene photopolymerization. The resulting hollow toroidal structures are shape-persistent and mechanically robust in solution. In addition, their size can be tuned by controlling the initial monomer concentrations, an observation that is supported by a theoretical analysis. These hollow microrings can encapsulate guest molecules in the intratoroidal nanospace, and their peripheries can act as templates for circular arrays of metal nanoparticles.

Synthesis of Cd-free InP/ZnS Quantum Dots Suitable for Biomedical Applications.

PubMed

Ellis, Matthew A; Grandinetti, Giovanna; Fichter, Katye M; Fichter, Kathryn M

2016-02-06

Fluorescent nanocrystals, specifically quantum dots, have been a useful tool for many biomedical applications. For successful use in biological systems, quantum dots should be highly fluorescent and small/monodisperse in size. While commonly used cadmium-based quantum dots possess these qualities, they are potentially toxic due to the possible release of Cd(2+) ions through nanoparticle degradation. Indium-based quantum dots, specifically InP/ZnS, have recently been explored as a viable alternative to cadmium-based quantum dots due to their relatively similar fluorescence characteristics and size. The synthesis presented here uses standard hot-injection techniques for effective nanoparticle growth; however, nanoparticle properties such as size, emission wavelength, and emission intensity can drastically change due to small changes in the reaction conditions. Therefore, reaction conditions such temperature, reaction duration, and precursor concentration should be maintained precisely to yield reproducible products. Because quantum dots are not inherently soluble in aqueous solutions, they must also undergo surface modification to impart solubility in water. In this protocol, an amphiphilic polymer is used to interact with both hydrophobic ligands on the quantum dot surface and bulk solvent water molecules. Here, a detailed protocol is provided for the synthesis of highly fluorescent InP/ZnS quantum dots that are suitable for use in biomedical applications.

Synthesis of Cd-free InP/ZnS Quantum Dots Suitable for Biomedical Applications

PubMed Central

Ellis, Matthew A.; Grandinetti, Giovanna; Fichter, Katye M.

2016-01-01

Fluorescent nanocrystals, specifically quantum dots, have been a useful tool for many biomedical applications. For successful use in biological systems, quantum dots should be highly fluorescent and small/monodisperse in size. While commonly used cadmium-based quantum dots possess these qualities, they are potentially toxic due to the possible release of Cd2+ ions through nanoparticle degradation. Indium-based quantum dots, specifically InP/ZnS, have recently been explored as a viable alternative to cadmium-based quantum dots due to their relatively similar fluorescence characteristics and size. The synthesis presented here uses standard hot-injection techniques for effective nanoparticle growth; however, nanoparticle properties such as size, emission wavelength, and emission intensity can drastically change due to small changes in the reaction conditions. Therefore, reaction conditions such temperature, reaction duration, and precursor concentration should be maintained precisely to yield reproducible products. Because quantum dots are not inherently soluble in aqueous solutions, they must also undergo surface modification to impart solubility in water. In this protocol, an amphiphilic polymer is used to interact with both hydrophobic ligands on the quantum dot surface and bulk solvent water molecules. Here, a detailed protocol is provided for the synthesis of highly fluorescent InP/ZnS quantum dots that are suitable for use in biomedical applications. PMID:26891282

One-step solution combustion synthesis of pure Ni nanopowders with enhanced coercivity: The fuel effect

NASA Astrophysics Data System (ADS)

Khort, Alexander; Podbolotov, Kirill; Serrano-García, Raquel; Gun'ko, Yurii K.

2017-09-01

In this paper, we report a new modified one-step combustion synthesis technique for production of Ni metal nanoparticles. The main unique feature of our approach is the use of microwave assisted foam preparation. Also, the effect of different types of fuels (urea, citric acid, glycine and hexamethylenetetramine) on the combustion process and characteristics of resultant solid products were investigated. It is observed that the combination of microwave assisted foam preparation and using of hexamethylenetetramine as a fuel allows producing pure ferromagnetic Ni metal nanoparticles with enhanced coercivity (78 Oe) and high value of saturation magnetization (52 emu/g) by one-step solution combustion synthesis under normal air atmosphere without any post-reduction processing.

Synthesis of nanocrystalline TiO 2 in toluene by a solvothermal route

NASA Astrophysics Data System (ADS)

Kim, Chung-Sik; Moon, Byung Kee; Park, Jong-Ho; Tae Chung, Su; Son, Se-Mo

2003-07-01

A solvothermal synthetic method to TiO 2 nanoparticles has been investigated in toluene solutions with titanium isopropoxide (TIP) as precursor. Weight ratios of precursor to solvent prepared in the mixture are 5/100, 10/100, 20/100, 30/100 and 40/100. At the weight ratio of 10/100, 20/100 and 30/100, TiO 2 nanocrystalline particles were obtained after synthesis at 250°C for 3 h in an autoclave. X-ray diffraction and tranmission electron microscopy shows that the product has uniform anatase structure with average particle size below 20 nm. As the composition of TIP in the solution increases, the particle size of TiO 2 powder tends to increase. At 5/100 and 40/100, however, pale yellow colloidal solution is obtained after synthesis and crystalline phase of TiO 2 is not produced. The specific surface area of the TiO 2 nanocrystalline powder was also investigated using BET surface area analyzer.

A fundamental approach to adhesion: Synthesis, surface analysis, thermodynamics and mechanics. [acid-base properties of titanium 6-4 surfaces

NASA Technical Reports Server (NTRS)

Siriwardane, R.; Wightman, J. P.

1980-01-01

The acid-base properties of titanium 6-4 plates (low surface area) were investigated after three different pretreatments, namely Turco, phosphate-fluoride and Pasa-Jell. A series of indicators was used and color changes were detected using diffuse reflectance visible spectroscopy. Electron spectroscopy for chemical analysis was used to examine the indicator on the Ti 6-4 surface. Specular reflectance infra-red spectroscopy was used to study the adsorption of stearic acid from cyclohexane solutions on the Ti 6-4 surface.

Preparation of poly(N-vinylpyrrolidone)-stabilized ZnO colloid nanoparticles

PubMed Central

Gutul, Tatyana; Condur, Nadejda; Ursaki, Veaceslav; Goncearenco, Evgenii; Vlazan, Paulina

2014-01-01

Summary We propose a method for the synthesis of a colloidal ZnO solution with poly(N-vinylpyrrolidone) (PVP) as stabilizer. Stable colloidal solutions with good luminescence properties are obtained by using PVP as stabilizer in the synthesis of ZnO nanoparticles by a sol–gel method assisted by ultrasound. Nanoparticles with sizes of 30–40 nm in a PVP matrix are produced as a solid product. The colloidal ZnO/PVP/methanol solution, apart from the most intense PL band at 356 nm coming from the PVP, exhibits a strong PL band at 376 nm (3.30 eV) which corresponds to the emission of the free exciton recombination in ZnO nanoparticles. PMID:24778966

Volume-confined synthesis of ligand-free gold nanoparticles with tailored sizes for enhanced catalytic activity

NASA Astrophysics Data System (ADS)

Shaik, Firdoz; Zhang, Weiqing; Niu, Wenxin; Lu, Xianmao

2014-10-01

Ligand-free Au nanoparticles with controlled sizes are synthesized via a volume-confined method. In this synthesis, mesoporous hollow silica shells (mHSS) are used as nano-containers for the impregnation of HAuCl4 solution before they are separated from the bulk solution. With a simple heating process, the Au precursor confined within the cavity of the isolated hollow shells is converted into ligand-free Au nanoparticles. The size of the Au nanoparticles can be tuned precisely by loading HAuCl4 solution of different concentrations, or by using mHSS with different cavity volumes. The ligand-free Au nanoparticles demonstrate superior catalytic activity than sodium citrate-capped Au nanoparticles.

Fischer Indole Synthesis in the Gas Phase, the Solution Phase, and at the Electrospray Droplet Interface.

PubMed

Bain, Ryan M; Ayrton, Stephen T; Cooks, R Graham

2017-07-01

Previous reports have shown that reactions occurring in the microdroplets formed during electrospray ionization can, under the right conditions, exhibit significantly greater rates than the corresponding bulk solution-phase reactions. The observed acceleration under electrospray ionization could result from a solution-phase, a gas-phase, or an interfacial reaction. This study shows that a gas-phase ion/molecule (or ion/ion) reaction is not responsible for the observed rate enhancement in the particular case of the Fischer indole synthesis. The results show that the accelerated reaction proceeds in the microdroplets, and evidence is provided that an interfacial process is involved. Graphical Abstract .

Synthesis and Doping of Silicon Nanocrystals for Versatile Nanocrystal Inks

NASA Astrophysics Data System (ADS)

Kramer, Nicolaas Johannes

The impact of nanotechnology on our society is getting larger every year. Electronics are becoming smaller and more powerful, the "Internet of Things" is all around us, and data generation is increasing exponentially. None of this would have been possible without the developments in nanotechnology. Crystalline semiconductor nanoparticles (nanocrystals) are one of the latest developments in the field of nanotechnology. This thesis addresses three important challenges for the transition of silicon nanocrystals from the lab bench to the marketplace: A better understanding of the nanocrystal synthesis was obtained, the electronic properties of the nanocrystals were characterized and tuned, and novel silicon nanocrystal inks were formed and applied using simple coating technologies. Plasma synthesis of nanocrystals has numerous advantages over traditional solution-based synthesis methods. While the formation of nanoparticles in low pressure nonthermal plasmas is well known, the heating mechanism leading to their crystallization is poorly understood. A combination of comprehensive plasma characterization with a nanoparticle heating model presented here reveals the underlying plasma physics leading to crystallization. The model predicts that the nanoparticles reach temperatures as high as 900 K in the plasma as a result of heating reactions on the nanoparticle surface. These temperatures are well above the gas temperature and sufficient for complete nanoparticle crystallization. Moving the field of plasma nanoparticle synthesis to atmospheric pressures is important for lowering its cost and making the process attractive for industrial applications. The heating and charging model for silicon nanoparticles was adapted in Chapter 3 to study plasmas maintained over a wide range of pressures (10 -- 105 Pa). The model considers three collisionality regimes and determines the dominant contribution of each regime under various plasma conditions. Strong nanoparticle cooling at atmospheric pressures necessitates high plasma densities to reach temperatures required for crystallization of nanoparticles. Using experimentally determined plasma properties from the literature, the model estimates the nanoparticle temperature that is achieved during synthesis at atmospheric pressures. It was found that temperatures well above those required for crystallization can be achieved. Now that the synthesis of nanocrystals is understood, the second half of this thesis will focus on doping of the nanocrystals. The doping of semiconductor nanocrystals, which is vital for the optimization of nanocrystal-based devices, remains a challenge. Gas phase plasma approaches have been very successful in incorporating dopant atoms into nanocrystals by simply adding a dopant precursor during synthesis. However, little is known about the electronic activation of these dopants. This was investigated with field-effect transistor measurements using doped silicon nanocrystal films. It was found that, analogous to bulk silicon, boron and phosphorous electronically dope silicon nanocrystals. However, the dopant activation efficiency remains low as a result of self-purification of the dopants to the nanocrystal surface. Next the plasmonic properties of heavily doped silicon nanocrystals was explored. While the synthesis method was identical, the plasmonic behavior of phosphorus-doped and boron-doped nanocrystals was found the be significantly different. Phosphorus-doped nanocrystals exhibit a plasmon resonance immediately after synthesis, while boron-doped nanocrystals require a post-synthesis annealing or oxidation treatment. This is a result of the difference in dopant location. Phosphorus is more likely to be incorporated into the core of the nanocrystal, while the majority of boron is placed on the surface of the nanocrystal. The oxidized boron-doped particles exhibit stable plasmonic properties, and therefore this allows for the production of air-stable silicon-based plasmonic materials which is very interesting for certain applications. Finally the boron atoms were used to form a Lewis acidic nanocrystal surface chemistry allowing for the creation of ligand-less silicon nanocrystal solutions. This represents an immense step towards an abundant, non-toxic alternative to Pb and Cd-based nanocrystal technologies. The lack of long ligand chains enables the production of dense films with excellent electrical conductivity. This was demonstrated by forming uniform nanocrystal thin-films using simple and inexpensive spray coating techniques.

Tailoring indium oxide nanocrystal synthesis conditions for air-stable high-performance solution-processed thin-film transistors.

PubMed

Swisher, Sarah L; Volkman, Steven K; Subramanian, Vivek

2015-05-20

Semiconducting metal oxides (ZnO, SnO2, In2O3, and combinations thereof) are a uniquely interesting family of materials because of their high carrier mobilities in the amorphous and generally disordered states, and solution-processed routes to these materials are of particular interest to the printed electronics community. Colloidal nanocrystal routes to these materials are particularly interesting, because nanocrystals may be formulated with tunable surface properties into stable inks, and printed to form devices in an additive manner. We report our investigation of an In2O3 nanocrystal synthesis for high-performance solution-deposited semiconductor layers for thin-film transistors (TFTs). We studied the effects of various synthesis parameters on the nanocrystals themselves, and how those changes ultimately impacted the performance of TFTs. Using a sintered film of solution-deposited In2O3 nanocrystals as the TFT channel material, we fabricated devices that exhibit field effect mobility of 10 cm(2)/(V s) and an on/off current ratio greater than 1 × 10(6). These results outperform previous air-stable nanocrystal TFTs, and demonstrate the suitability of colloidal nanocrystal inks for high-performance printed electronics.

Synthesis of nanosized sodium titanates

DOEpatents

Hobbs, David T.; Taylor-Pashow, Kathryn M. L.; Elvington, Mark C.

2015-09-29

Methods directed to the synthesis and peroxide-modification of nanosized monosodium titanate are described. Methods include combination of reactants at a low concentration to a solution including a nonionic surfactant. The nanosized monosodium titanate can exhibit high selectivity for sorbing various metallic ions.

Chemical Synthesis of Proteins

PubMed Central

Nilsson, Bradley L.; Soellner, Matthew B.; Raines, Ronald T.

2010-01-01

Proteins have become accessible targets for chemical synthesis. The basic strategy is to use native chemical ligation, Staudinger ligation, or other orthogonal chemical reactions to couple synthetic peptides. The ligation reactions are compatible with a variety of solvents and proceed in solution or on a solid support. Chemical synthesis enables a level of control on protein composition that greatly exceeds that attainable with ribosome-mediated biosynthesis. Accordingly, the chemical synthesis of proteins is providing previously unattainable insight into the structure and function of proteins. PMID:15869385

Investigating the synthesis of ligated metal clusters in solution using a flow reactor and electrospray ionization mass spectrometry.

PubMed

Olivares, Astrid; Laskin, Julia; Johnson, Grant E

2014-09-18

The scalable synthesis of ligated subnanometer metal clusters containing an exact number of atoms is of interest due to the highly size-dependent catalytic, electronic, and optical properties of these species. While significant research has been conducted on the batch preparation of clusters through reduction synthesis in solution, the processes of metal complex reduction as well as cluster nucleation, growth, and postreduction etching are still not well understood. Herein, we demonstrate a prototype temperature-controlled flow reactor for qualitatively studying cluster formation in solution at steady-state conditions. Employing this technique, methanol solutions of a chloro(triphenylphosphine)gold precursor, 1,4-bis(diphenylphosphino)butane capping ligand, and borane-tert-butylamine reducing agent were combined in a mixing tee and introduced into a heated capillary with a known length. In this manner, the temperature dependence of the relative abundance of different ionic reactants, intermediates, and products synthesized in real time was characterized qualitatively using online mass spectrometry. A wide distribution of doubly and triply charged cationic gold clusters was observed as well as smaller singly charged organometallic complexes. The results demonstrate that temperature plays a crucial role in determining the relative population of cationic gold clusters and, in general, that higher temperature promotes the formation of doubly charged clusters and singly charged organometallic complexes while reducing the abundance of triply charged species. Moreover, the distribution of clusters observed at elevated temperatures is found to be consistent with that obtained at longer reaction times at room temperature, thereby demonstrating that heating may be used to access cluster distributions characteristic of different stages of batch reduction synthesis in solution.

Synthesis of quantum dots via microreaction: structure optimization for microreactor system

NASA Astrophysics Data System (ADS)

Yang, Hongwei; Luan, Weiling; Cheng, Rui; Chu, Haijian; Tu, Shan-tung

2011-08-01

Microreactor systems existed as a powerful tool for the continuous synthesis of quantum dots. However, the lack of structure optimization for the discrete units led to empirical determination of the length scale, and the properties of the formed products varied in different cases. In this article, the optimizations for the micromixer volume and capillary diameter were presented based on the synthesis of CdSe nanocrystals (NCs). Spectra investigation revealed that the application of a small convective mixer of 36 μL led to 1/3 increase of CdSe concentration in the crude solution. The enhanced mixing of the precursors in this case was also demonstrated favorable to achieve CdSe NCs with narrow PL width. Fast heating and uniform reaction condition achieved in a narrow channel favored the preparation of high quality CdSe NCs under short residence time. However, the application of wide channel did not necessarily result in CdSe NCs with poor quality. Here, we demonstrated that high-quality CdSe NCs with narrow full width at half maximum (FWHM) as 32 nm and high quantum yield (QY) 34.7% could be prepared using an 844 μm inner diameter capillary. Based on the obtained results, the scaled-up synthesis of CdSe NCs was demonstrated, and a high quantity of 0.8 g dry CdSe NCs powder (3.5 nm, σ 8.2%) was obtained within 1 h.

Building blocks for the solution phase synthesis of oligonucleotides: regioselective hydrolysis of 3',5'-Di-O-levulinylnucleosides using an enzymatic approach.

PubMed

García, Javier; Fernández, Susana; Ferrero, Miguel; Sanghvi, Yogesh S; Gotor, Vicente

2002-06-28

A short and convenient synthesis of 3'- and 5'-O-levulinyl-2'-deoxynucleosides has been developed from the corresponding 3',5'-di-O-levulinyl derivatives by regioselective enzymatic hydrolysis, avoiding several tedious chemical protection/deprotection steps. Thus, Candida antartica lipase B (CAL-B) was found to selectively hydrolyze the 5'-levulinate esters, furnishing 3'-O-levulinyl-2'-deoxynucleosides 3 in >80% isolated yields. On the other hand, immobilized Pseudomonas cepacia lipase (PSL-C) and Candida antarctica lipase A (CAL-A) exhibit the opposite selectivity toward the hydrolysis at the 3'-position, affording 5'-O-levulinyl derivatives 4 in >70% yields. A similar hydrolysis procedure was successfully extended to the synthesis of 3'- and 5'-O-levulinyl-protected 2'-O-alkylribonucleosides 7 and 8. This work demonstrates for the first time application of commercial CAL-B and PSL-C toward regioselective hydrolysis of levulinyl esters with excellent selectivity and yields. It is noteworthy that protected cytidine and adenosine base derivatives were not adequate substrates for the enzymatic hydrolysis with CAL-B, whereas PSL-C was able to accommodate protected bases during selective hydrolysis. In addition, we report an improved synthesis of dilevulinyl esters using a polymer-bound carbodiimide as a replacement for dicyclohexylcarbodiimide (DCC), thus considerably simplifying the workup for esterification reactions.

Click mechanochemistry: quantitative synthesis of "ready to use" chiral organocatalysts by efficient two-fold thiourea coupling to vicinal diamines.

PubMed

Štrukil, Vjekoslav; Igrc, Marina D; Eckert-Maksić, Mirjana; Friščić, Tomislav

2012-07-02

Mechanochemical methods of neat grinding and liquid-assisted grinding have been applied to the synthesis of mono- and bis(thiourea)s by using the click coupling of aromatic and aliphatic diamines with aromatic isothiocyanates. The ability to modify the reaction conditions allowed the optimization of each reaction, leading to the quantitative formation of chiral bis(thiourea)s with known uses as organocatalysts or anion sensors. Quantitative reaction yields, combined with the fact that mechanochemical reaction conditions avoid the use of bulk solvents, enabled solution-based purification methods (such as chromatography or recrystallization) to be completely avoided. Importantly, by using selected model reactions, we also show that the described mechanochemical reaction procedures can be readily scaled up to at least the one-gram scale. In that way, mechanochemical synthesis provides a facile method to fully transform valuable enantiomerically pure reagents into useful products that can immediately be applied in their designed purpose. This was demonstrated by using some of the mechanochemically prepared reagents as organocatalysts in a model Morita-Baylis-Hillman reaction and as cyanide ion sensors in organic solvents. The use of electronically and sterically hindered ortho-phenylenediamine revealed that mechanochemical reaction conditions can be readily optimized to form either the 1:1 or the 1:2 click-coupling product, demonstrating that reaction stoichiometry can be more efficiently controlled under these conditions than in solution-based syntheses. In this way, it was shown that excellent stoichiometric control by mechanochemistry, previously established for mechanochemical syntheses of cocrystals and coordination polymers, can also be achieved in the context of covalent-bond formation. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Application of heuristic satellite plan synthesis algorithms to requirements of the WARC-88 allotment plan

NASA Technical Reports Server (NTRS)

Heyward, Ann O.; Reilly, Charles H.; Walton, Eric K.; Mata, Fernando; Olen, Carl

1990-01-01

Creation of an Allotment Plan for the Fixed Satellite Service at the 1988 Space World Administrative Radio Conference (WARC) represented a complex satellite plan synthesis problem, involving a large number of planned and existing systems. Solutions to this problem at WARC-88 required the use of both automated and manual procedures to develop an acceptable set of system positions. Development of an Allotment Plan may also be attempted through solution of an optimization problem, known as the Satellite Location Problem (SLP). Three automated heuristic procedures, developed specifically to solve SLP, are presented. The heuristics are then applied to two specific WARC-88 scenarios. Solutions resulting from the fully automated heuristics are then compared with solutions obtained at WARC-88 through a combination of both automated and manual planning efforts.

Engineering calculations for communications satellite systems planning

NASA Technical Reports Server (NTRS)

Walton, E.; Aebker, E.; Mata, F.; Reilly, C.

1991-01-01

The final phase of a satellite synthesis project is described. Several methods for generating satellite positionings with improved aggregate carrier to interference characteristics were studied. Two general methods for modifying required separation values are presented. Also, two methods for improving aggregate carrier to interference (C/I) performance of given satellite synthesis solutions are presented. A perturbation of the World Administrative Radio Conference (WARC) synthesis is presented.

Synthesis and Size Dependent Reflectance Study of Water Soluble SnS Nanoparticles

PubMed Central

Xu, Ying; Al-Salim, Najeh; Tilley, Richard D.

2012-01-01

Near-monodispersed water soluble SnS nanoparticles in the diameter range of 3–6 nm are synthesized by a facile, solution based one-step approach using ethanolamine ligands. The optimal amount of triethanolamine is investigated. The effect of further heat treatment on the size of these SnS nanoparticles is discussed. Diffuse reflectance study of SnS nanoparticles agrees with predictions from quantum confinement model. PMID:28348295

Polyazulene based materials for heavy metal ions detection

NASA Astrophysics Data System (ADS)

Oprisanu, A.; Ungureanu, E. M.; Isopescu, R.; Birzan, L.; Mihai, M.; Vasiliu, C.

2017-06-01

Azulene is a special monomer used to functionalize electrodes, due to its spontaneous electron drift from the seven-membered ring to the five-membered ring. The seven-membered ring of the molecule may act as electron acceptor, while the five-membered ring - as electron donor. This leads to very attractive properties for the synthesis of functional advanced materials like: materials with nonlinear optical and photorefractive properties, cathode materials for lithium batteries, or light emitting diodes based on organic materials. Azulene derivatives have been used rarely to the metal ions electroanalysis. Our study concerns the synthesis and electrochemical characterization of a new azulene based monomer 4-(azulen-1-yl)-2,6-bis((E)-2-(thiophen-3-yl)vinyl)pyridine (L). L has been used to obtain modified electrodes by electrochemical polymerization. PolyL films modified electrodes have been characterized by cyclic voltammetry in ferrocene solutions. The complexing properties of polyL based functional materials have been investigated towards heavy metals (Pb, Cd Hg, Cu) by preconcentration - anodic stripping technique in order to analyze the content of these cations from water samples.

Scoping candidate minerals for stabilization of arsenic-bearing solid residuals.

PubMed

Raghav, Madhumitha; Shan, Jilei; Sáez, A Eduardo; Ela, Wendell P

2013-12-15

Arsenic Crystallization Technology (ACT) is a potentially eco-friendly, effective technology for stabilization of arsenic-bearing solid residuals (ABSRs). The strategy is to convert ABSRs generated by water treatment facilities into minerals with a high arsenic capacity and long-term stability in mature, municipal solid waste landfills. Candidate minerals considered in this study include scorodite, arsenate hydroxyapatites, ferrous arsenates (symplesite-type minerals), tooeleite, and arsenated-schwertmannite. These minerals were evaluated as to ease of synthesis, applicability to use of iron-based ABSRs as a starting material, and arsenic leachability. The Toxicity Characteristic Leaching Procedure (TCLP) was used for preliminary assessment of candidate mineral leaching. Minerals that passed the TCLP and whose synthesis route was promising were subjected to a more aggressive leaching test using a simulated landfill leachate (SLL) solution. Scorodite and arsenate hydroxyapatites were not considered further because their synthesis conditions were not found to be favorable for general application. Tooeleite and silica-amended tooeleite showed high TCLP arsenic leaching and were also not investigated further. The synthesis process and leaching of ferrous arsenate and arsenated-schwertmannite were promising and of these, arsenated-schwertmannite was most stable during SLL testing. The latter two candidate minerals warrant synthesis optimization and more extensive testing. Copyright © 2013 Elsevier B.V. All rights reserved.

Study of low-temperature active rare-earth oxide catalysts for automotive exhaust clean-up.

DOT National Transportation Integrated Search

2014-02-01

We report a facile onepot synthesis of CexZr1-xO2 (0x1) solid solution nanocrystals using hydrothermal reactions. A direct formation of oxide solid solutions in aqueous solution under pressure at low temperatures was clearly revealed by X-ra...

Swift adsorptive removal of Congo red from aqueous solution by K1.33Mn8O16 nanowires.

PubMed

Wu, Junshu; Li, Hongyi; Wang, Jinshu; Li, Zhifei

2013-08-01

A swift and efficient approach to converting organic dye effluents into fresh water could be of substantial benefit. In this study, we presented facile hydrothermal synthesis of K1.33Mn8O16 nanowires in ammonium fluoride (NH4F) aqueous solution. The crystallization process of K1.33Mn8O16 nanowires was investigated. The as-obtained K1.33Mn8O16 nanowires were used for swift adsorptive removal of Congo red from aqueous solution without adjusting pH value at room temperature. Adsorption kinetic experimental data are well described by pseudo-second-order rate kinetic model, and the adsorption isotherm fits Langmuir isotherm model. The present investigation provides an efficient approach to designing and fabricating manganese-based nanomaterials for environmental remediation.

Dead biomass of Amazon yeast: A new insight into bioremediation and recovery of silver by intracellular synthesis of nanoparticles.

PubMed

Salvadori, Marcia R; Ando, Rômulo A; Nascimento, Cláudio A Oller; Corrêa, Benedito

2017-09-19

This investigation was undertaken to describe a natural process for the removal of silver and the simultaneous recovery of Ag/Ag 2 O nanoparticles by dead biomass of the yeast Rhodotorula mucilaginosa. The removal of silver ions from aqueous solution and the synthesis of Ag/Ag 2 O nanoparticles were analyzed based on physicochemical factors and equilibrium concentration, combined with transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS), and infrared spectroscopy (FTIR). A successful process for the synthesis of Ag/Ag 2 O nanoparticles was obtained, following the Langmuir isotherm model, showing a high biosorption capacity of silver (49.0 mg g -1 ). The nanoparticles were spherical, had an average size of 11.0 nm, were synthesized intracellularly and capped by yeast proteins. This sustainable protocol is an attractive platform for the industrial-scale production of silver nanoparticles and of a silver nanobiosorbent.

Belite cement clinker from coal fly ash of high Ca content. Optimization of synthesis parameters.

PubMed

Guerrero, A; Goñi, S; Campillo, I; Moragues, A

2004-06-01

The optimization of parameters of synthesis of belite cement clinker from coal fly ash of high Ca content is presented in this paper. The synthesis process is based on the hydrothermal-calcination-route of the fly ash without extra additions. The hydrothermal treatment was carried out in demineralized water and a 1 M NaOH solution for 4 h at the temperatures of 100 degrees C, 150 degrees C, and 200 degrees C. The precursors obtained during the hydrothermal treatmentwere heated at temperatures of 700 degrees C, 800 degrees C, 900 degrees C, and 1000 degrees C. The changes of fly ash composition after the different treatments were characterized by X-ray diffraction (XRD), FT infrared (FTIR) spectroscopy, surface area (BET-N2), and thermal analyses. From the results obtained we concluded that the optimum temperature of the hydrothermal treatment was 200 degrees C, and the optimum temperature for obtaining the belite cement clinker was 800 degrees C.

Scalable One-pot Bacteria-templating Synthesis Route toward Hierarchical, Porous-Co3O4 Superstructures for Supercapacitor Electrodes

PubMed Central

Shim, Hyun-Woo; Lim, Ah-Hyeon; Kim, Jae-Chan; Jang, Eunjin; Seo, Seung-Deok; Lee, Gwang-Hee; Kim, T. Doohun; Kim, Dong-Wan

2013-01-01

Template-driven strategy has been widely used to synthesize inorganic nano/micro materials. Here, we used a bottom-up controlled synthesis route to develop a powerful solution-based method of fabricating three-dimensional (3D), hierarchical, porous-Co3O4 superstructures that exhibit the morphology of flower-like microspheres (hereafter, RT-Co3O4). The gram-scale RT-Co3O4 was facilely prepared using one-pot synthesis with bacterial templating at room temperature. Large-surface-area RT-Co3O4 also has a noticeable pseudocapacitive performance because of its high mass loading per area (~10 mg cm−2), indicating a high capacitance of 214 F g−1 (2.04 F cm−2) at 2 A g−1 (19.02 mA cm−2), a Coulombic efficiency averaging over 95%, and an excellent cycling stability that shows a capacitance retention of about 95% after 4,000 cycles. PMID:23900049

Wave field synthesis of a virtual source located in proximity to a loudspeaker array.

PubMed

Lee, Jung-Min; Choi, Jung-Woo; Kim, Yang-Hann

2013-09-01

For the derivation of 2.5-dimensional operator in wave field synthesis, a virtual source is assumed to be positioned far from a loudspeaker array. However, such far-field approximation inevitably results in a reproduction error when the virtual source is placed adjacent to an array. In this paper, a method is proposed to generate a virtual source close to and behind a continuous line array of loudspeakers. A driving function is derived by reducing a surface integral (Rayleigh integral) to a line integral based on the near-field assumption. The solution is then combined with the far-field formula of wave field synthesis by introducing a weighting function that can adjust the near- and far-field contribution of each driving function. This enables production of a virtual source anywhere in relation to the array. Simulations show the proposed method can reduce the reproduction error to below -18 dB, regardless of the virtual source position.

Magnetic Droplet Microfluidics as a Platform for the Concentration of [18F]Fluoride and Radiosynthesis of Sulfonyl [18F]Fluoride.

PubMed

Fiel, Somewhere A; Yang, Hua; Schaffer, Paul; Weng, Samuel; Inkster, James A H; Wong, Michael C K; Li, Paul C H

2015-06-17

The radioisotope 18F is often considered the best choice for positron emission tomography (PET) owing to its desirable chemical and radiochemical properties. However, nucleophilic 18F-fluorination of large, water-soluble biomolecules, based on C-F bond formation, has traditionally been difficult. Thus, several aqueous fluorination approaches that offer significant versatility in radiopharmaceutical synthesis with sensitive targeting vectors have been developed. Furthermore, because 18F decays rapidly, production of these 18F-labeled compounds requires an automated process to reduce production time, reduce radiation exposure, and minimize losses due to the transfer of reagents during tracer synthesis. Herein, we report the use of magnetic droplet microfluidics (MDM) as a means to concentrate [18F]fluoride from the cyclotron target solution, followed by the synthesis of an 18F-labeled compound on a microfluidic platform. Using this method, we have demonstrated 18F preconcentration in a small-volume droplet through the use of anion exchanging magnetic particles. By using MDM, the preconcentration step took approximately 5 min, and the [18F]fluoride solution was preconcentrated by 15-fold. After the preconcentration step, an 18F-labeling reaction was performed on the MDM platform using the S-F bond formation in aqueous conditions to produce an arylsulfonyl [18F]fluoride compound which can be used as a prosthetic group to label PET targeting ligands. The high radiochemical purity of 95±1% was comparable to the 96% previously reported using a conventional method. In addition, when MDM was used, the total synthesis time was improved to 15 min with lower reagent volumes (50-60 μL) used.

Access to small size distributions of nanoparticles by microwave-assisted synthesis. Formation of Ag nanoparticles in aqueous carboxymethylcellulose solutions in batch and continuous-flow reactors

NASA Astrophysics Data System (ADS)

Horikoshi, Satoshi; Abe, Hideki; Torigoe, Kanjiro; Abe, Masahiko; Serpone, Nick

2010-08-01

This article examines the effect(s) of the 2.45-GHz microwave (MW) radiation in the synthesis of silver nanoparticles in aqueous media by reduction of the diaminesilver(i) complex, [Ag(NH3)2]+, with carboxymethylcellulose (CMC) in both batch-type and continuous-flow reactor systems with a particular emphasis on the characteristics of the microwaves in this process and the size distributions. This microwave thermally-assisted synthesis is compared to a conventional heating (CH) method, both requiring a reaction temperature of 100 °C to produce the nanoparticles, in both cases leading to the formation of silver colloids with different size distributions. Reduction of the diaminesilver(i) precursor complex, [Ag(NH3)2]+, by CMC depended on the solution temperature. Cooling the reactor during the heating process driven with 390-Watt microwaves (MW-390W/Cool protocol) yielded silver nanoparticles with sizes spanning the range 1-2 nm. By contrast, the size distribution of Ag nanoparticles with 170-Watt microwaves (no cooling; MW-170W protocol) was in the range 1.4-3.6 nm (average size ~3 nm). The overall results suggest the potential for a scale-up process in the microwave-assisted synthesis of nanoparticles. Based on the present data, a flow-through microwave reactor system is herein proposed for the continuous production of silver nanoparticles. The novel flow reactor system (flow rate, 600 mL min-1) coupled to 1200-Watt microwave radiation generated silver nanoparticles with a size distribution 0.7-2.8 nm (average size ca. 1.5 nm).

Multivariable optimization of an auto-thermal ammonia synthesis reactor using genetic algorithm

NASA Astrophysics Data System (ADS)

Anh-Nga, Nguyen T.; Tuan-Anh, Nguyen; Tien-Dung, Vu; Kim-Trung, Nguyen

2017-09-01

The ammonia synthesis system is an important chemical process used in the manufacture of fertilizers, chemicals, explosives, fibers, plastics, refrigeration. In the literature, many works approaching the modeling, simulation and optimization of an auto-thermal ammonia synthesis reactor can be found. However, they just focus on the optimization of the reactor length while keeping the others parameters constant. In this study, the other parameters are also considered in the optimization problem such as the temperature of feed gas enters the catalyst zone. The optimal problem requires the maximization of a multivariable objective function which subjects to a number of equality constraints involving the solution of coupled differential equations and also inequality constraints. The solution of an optimization problem can be found through, among others, deterministic or stochastic approaches. The stochastic methods, such as evolutionary algorithm (EA), which is based on natural phenomenon, can overcome the drawbacks such as the requirement of the derivatives of the objective function and/or constraints, or being not efficient in non-differentiable or discontinuous problems. Genetic algorithm (GA) which is a class of EA, exceptionally simple, robust at numerical optimization and is more likely to find a true global optimum. In this study, the genetic algorithm is employed to find the optimum profit of the process. The inequality constraints were treated using penalty method. The coupled differential equations system was solved using Runge-Kutta 4th order method. The results showed that the presented numerical method could be applied to model the ammonia synthesis reactor. The optimum economic profit obtained from this study are also compared to the results from the literature. It suggests that the process should be operated at higher temperature of feed gas in catalyst zone and the reactor length is slightly longer.

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

Novikova, N. N., E-mail: nn-novikova07@yandex.ru; Kovalchuk, M. V.; Yakunin, S. N.

The processes of structural rearrangement in a model membrane, i.e., an arachic acid monolayer formed on a colloidal solution of cerium dioxide or magnetite, are studied in situ in real time by the methods of X-ray standing waves and 2D diffraction. It is shown that the character of the interaction of nanoparticles with the monolayer is determined by their nature and sizes and depends on the conditions of nanoparticle synthesis. In particular, the structure formation in the monolayer–particle system is greatly affected by the stabilizer (citric acid), which is introduced into the colloidal solution during synthesis.

Solution combustion synthesis and characterization of nanosized bismuth ferrite

NASA Astrophysics Data System (ADS)

Sai Kumar, V. Sesha; Rao, K. Venkateswara; Krishnaveni, T.; Kishore Goud, A. Shiva; Reddy, P. Ranjith

2012-06-01

The present paper describes a simple method of nanosized BiFeO3 by the solution combustion synthesis using bismuth and iron nitrates as oxidizers and the combination fuel of citric acid and ammonium hydroxide, with fuel to oxidizer ratio (Ψ = 1) one. The X-ray Diffraction results indicated rhombohedral phase (R3m) with JCPDS data card no: 72-2035. The ferroelectric transition of the sample at 8310C was detected by differential thermal analysis. Thermal analysis was done by Thermal gravimetric-Differential thermal analyzer and obtained results were presented in this paper.

Synthesis and characterization of CoPt nanoparticles prepared by room temperature chemical reduction with PAMAM dendrimer as template.

PubMed

Wan, Haiying; Shi, Shifan; Bai, Litao; Shamsuzzoha, Mohammad; Harrell, J W; Street, Shane C

2010-08-01

We describe an approach to synthesize monodisperse CoPt nanoparticles with dendrimer as template by a simple chemical reduction method in aqueous solution using NaBH4 as reducing agent at room temperature. The as-made CoPt nanoparticles buried in the dendrimer matrix have the chemically disordered fcc structure and can be transformed to the fct phase after annealing at 700 degrees C. This is the first report of dendrimer-mediated room temperature synthesis of monodisperse magnetic nanoparticles in aqueous solution.

Synthesis, investigation of the new derivatives of dihydropyrimidines and determination of their biological activity

NASA Astrophysics Data System (ADS)

Maharramov, A. M.; Ramazanov, M. A.; Guliyeva, G. A.; Huseynzada, A. E.; Hasanova, U. A.; Shikhaliyev, N. G.; Eyvazova, G. M.; Hajiyeva, S. F.; Mamedov, I. G.; Aghayev, M. M.

2017-08-01

We reported of synthesis and investigation of the new biologically active derivatives of dihydropyrimidines 2 and 3. The investigation of structures of compounds by various experiments of NMR spectroscopy revealed the splitting of the signals to doublets and multiplets that confirms the presence of diastereomers in solution of compound 2 and the presence of diastereomers and tautomers in solution of compound 3. The individual diastereomer of compound 3 has been isolated. Biological activity of the synthesized compounds was studied on various species of genus Aspergillus fungi.

Solid-phase synthesis and chemical space analysis of a 190-membered alkaloid/terpenoid-like library

PubMed Central

Moura-Letts, Gustavo; DiBlasi, Christine M.; Bauer, Renato A.; Tan, Derek S.

2011-01-01

Alkaloid and terpenoid natural products display an extensive array of chemical frameworks and biological activities. However such scaffolds remain underrepresented in current screening collections and are, thus, attractive targets for the synthesis of natural product-based libraries that access underexploited regions of chemical space. Recently, we reported a systematic approach to the stereoselective synthesis of multiple alkaloid/terpenoid-like scaffolds using transition metal-mediated cycloaddition and cyclization reactions of enyne and diyne substrates assembled on a tert-butylsulfinamide lynchpin. We report herein the synthesis of a 190-membered library of alkaloid/terpenoid-like molecules using this synthetic approach. Translation to solid-phase synthesis was facilitated by the use of a tert-butyldiarylsilyl (TBDAS) linker that closely mimics the tert-butyldiphenysilyl protecting group used in the original solution-phase route development work. Unexpected differences in stereoselectivity and regioselectivity were observed in some reactions when carried out on solid support. Further, the sulfinamide moiety could be hydrolyzed or oxidized efficiently without compromising the TBDAS linker to provide additional amine and sulfonamide functionalities. Principal component analysis of the structural and physicochemical properties of these molecules confirmed that they access regions of chemical space that overlap with bona fide natural products and are distinct from areas addressed by conventional synthetic drugs and drug-like molecules. The influences of scaffolds and substituents were also evaluated, with both found to have significant impacts on location in chemical space and three-dimensional shape. Broad biological evaluation of this library will provide valuable insights into the abilities of natural product-based libraries to access similarly underexploited regions of biological space. PMID:21451137

Analyzing locomotion synthesis with feature-based motion graphs.

PubMed

Mahmudi, Mentar; Kallmann, Marcelo

2013-05-01

We propose feature-based motion graphs for realistic locomotion synthesis among obstacles. Among several advantages, feature-based motion graphs achieve improved results in search queries, eliminate the need of postprocessing for foot skating removal, and reduce the computational requirements in comparison to traditional motion graphs. Our contributions are threefold. First, we show that choosing transitions based on relevant features significantly reduces graph construction time and leads to improved search performances. Second, we employ a fast channel search method that confines the motion graph search to a free channel with guaranteed clearance among obstacles, achieving faster and improved results that avoid expensive collision checking. Lastly, we present a motion deformation model based on Inverse Kinematics applied over the transitions of a solution branch. Each transition is assigned a continuous deformation range that does not exceed the original transition cost threshold specified by the user for the graph construction. The obtained deformation improves the reachability of the feature-based motion graph and in turn also reduces the time spent during search. The results obtained by the proposed methods are evaluated and quantified, and they demonstrate significant improvements in comparison to traditional motion graph techniques.

Synthesis of highly elastic biocompatible polyurethanes based on bio-based isosorbide and poly(tetramethylene glycol) and their properties

PubMed Central

Kim, Hyo-Jin; Kang, Min-Sil; Knowles, Jonathan C

2014-01-01

Bio-based high elastic polyurethanes were prepared from hexamethylene diisocyanate and various ratios of isosorbide to poly(tetramethylene glycol) as a diol by a simple one-shot bulk polymerization without a catalyst. Successful synthesis of the polyurethanes was confirmed by Fourier transform-infrared spectroscopy and 1H nuclear magnetic resonance. Thermal properties were determined by differential scanning calorimetry and thermogravimetric analysis. The glass transition temperature was −47.8℃. The test results showed that the poly(tetramethylene glycol)/isosorbide-based elastomer exhibited not only excellent stress–strain properties but also superior resilience to the existing polyether-based polyurethane elastomers. The static and dynamic properties of the polyether/isosorbide-based thermoplastic elastomer were more suitable for dynamic applications. Moreover, such rigid diols impart biocompatible and bioactive properties to thermoplastic polyurethane elastomers. Degradation tests performed at 37℃ in phosphate buffer solution showed a mass loss of 4–9% after 8 weeks, except for the polyurethane with the lowest isosorbide content, which showed an initial rapid weight loss. These polyurethanes offer significant promise due to soft, flexible and biocompatible properties for soft tissue augmentation and regeneration. PMID:24812276

One-pot synthesis of SnO{sub 2}/reduced graphene oxide nanocomposite in ionic liquid-based solution and its application for lithium ion batteries

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

Gu, Changdong, E-mail: cdgu@zju.edu.cn; Zhang, Heng; Wang, Xiuli

2013-10-15

Graphical abstract: - Highlights: • A facile and low-temperature method is developed for SnO{sub 2}/graphene composite. • Synthesis performed in a choline chloride-based ionic liquid. • The composite shows an enhanced cycling stability as anode for Li-ion batteries. • 4 nm SnO{sub 2} nanoparticles mono-dispersed on the surface of reduced graphene oxide. - Abstract: A facile and low-temperature method is developed for SnO{sub 2}/graphene composite which involves an ultrasonic-assistant oxidation–reduction reaction between Sn{sup 2+} and graphene oxide in a choline chloride–ethylene glycol based ionic liquid under ambient conditions. The reaction solution is non-corrosive and environmental-friendly. Moreover, the proposed technique doesmore » not require complicated infrastructures and heat treatment. The SnO{sub 2}/graphene composite consists of about 4 nm sized SnO{sub 2} nanoparticles with cassiterite structure mono-dispersed on the surface of reduced graphene oxide. As anode for lithium-ion batteries, the SnO{sub 2}/graphene composite shows a satisfying cycling stability (535 mAh g{sup −1} after 50 cycles @100 mA g{sup −1}), which is significantly prior to the bare 4 nm sized SnO{sub 2} nanocrsytals. The graphene sheets in the hybrid nanostructure could provide a segmentation effect to alleviate the volume expansion of the SnO{sub 2} and restrain the small and active Sn-based particles aggregating into larger and inactive clusters during cycling.« less

Coaxial Lithography

NASA Astrophysics Data System (ADS)

Ozel, Tuncay

The optical and electrical properties of heterogeneous nanowires are profoundly related to their composition and nanoscale architecture. However, the intrinsic constraints of conventional synthetic and lithographic techniques have limited the types of multi-compositional nanowires that can be realized and studied in the laboratory. This thesis focuses on bridging templated electrochemical synthesis and lithography for expanding current synthetic capabilities with respect to materials generality and the ability to tailor two-dimensional growth in the formation of core-shell structures for the rational design and preparation of nanowires with very complex architectures that cannot be made by any other techniques. Chapter 1 introduces plasmonics, templated electrochemical synthesis, and on-wire lithography concepts and their significances within chemistry and materials science. Chapter 2 details a powerful technique for the deposition of metals and semiconductors with nanometer resolution in segment and gap lengths using on-wire lithography, which serves as a new platform to explore plasmon-exciton interactions in the form of long-range optical nanoscale rulers. Chapter 3 highlights an approach for the electrochemical synthesis of solution dispersible core-shell polymeric and inorganic semiconductor nanowires with metallic leads. A photodetector based on a single core-shell semiconductor nanowire is presented to demonstrate the functionality of the nanowires produced using this approach. Chapter 4 describes a new materials general technique, termed coaxial lithography (COAL), bridging templated electrochemical synthesis and lithography for generating coaxial nanowires in a parallel fashion with sub-10 nanometer resolution in both axial and radial dimensions. Combinations of coaxial nanowires composed of metals, metal oxides, metal chalcogenides, conjugated polymers, and a core/shell semiconductor nanowire with an embedded plasmonic nanoring are presented to demonstrate the possibilities afforded by COAL. Chapter 5 addresses the use of COAL for the synthesis of solution dispersible metal nanorings and nanotubes with exceptional architectural tailorability of inner diameter, outer diameter, and length leading to precise spectral control over the resulting plasmonic fields ranging from visible to the near-IR. Chapter 6 is an outlook on templated electrochemical synthesis using coaxial lithography and highlights a few promising applications from nanoparticle assembly to light-matter interactions.

Combinatorial synthesis of phosphors using arc-imaging furnace

PubMed Central

Ishigaki, Tadashi; Toda, Kenji; Yoshimura, Masahiro; Uematsu, Kazuyoshi; Sato, Mineo

2011-01-01

We have applied a novel ‘melt synthesis technique’ rather than a conventional solid-state reaction to rapidly synthesize phosphor materials. During a synthesis, the mixture of oxides or their precursors is melted by light pulses (10–60 s) in an arc-imaging furnace on a water-cooled copper hearth to form a globule of 1–5 mm diameter, which is then rapidly cooled by turning off the light. Using this method, we synthesized several phosphor compounds including Y3Al5O12:Ce(YAG) and SrAl2O4:Eu,Dy. Complex phosphor oxides are difficult to produce by conventional solid-state reaction techniques because of the slow reaction rates among solid oxides; as a result, the oxides form homogeneous compounds or solid solutions. On the other hand, melt reactions are very fast (10–60 s) and result in homogeneous compounds owing to rapid diffusion and mixing in the liquid phase. Therefore, melt synthesis techniques are suitable for preparing multi component homogeneous compounds and solid solutions. PMID:27877432

Combinatorial synthesis of phosphors using arc-imaging furnace

NASA Astrophysics Data System (ADS)

Ishigaki, Tadashi; Toda, Kenji; Yoshimura, Masahiro; Uematsu, Kazuyoshi; Sato, Mineo

2011-10-01

We have applied a novel 'melt synthesis technique' rather than a conventional solid-state reaction to rapidly synthesize phosphor materials. During a synthesis, the mixture of oxides or their precursors is melted by light pulses (10-60 s) in an arc-imaging furnace on a water-cooled copper hearth to form a globule of 1-5 mm diameter, which is then rapidly cooled by turning off the light. Using this method, we synthesized several phosphor compounds including Y3Al5O12:Ce(YAG) and SrAl2O4:Eu,Dy. Complex phosphor oxides are difficult to produce by conventional solid-state reaction techniques because of the slow reaction rates among solid oxides; as a result, the oxides form homogeneous compounds or solid solutions. On the other hand, melt reactions are very fast (10-60 s) and result in homogeneous compounds owing to rapid diffusion and mixing in the liquid phase. Therefore, melt synthesis techniques are suitable for preparing multi component homogeneous compounds and solid solutions.

Synthesis and Oxidation of Silver Nano-particles

DTIC Science & Technology

2011-01-01

solution (20%wt propyl alcohol, 5%wt hydrochloric acid and 5%wt stannous chloride in water). Scheme 1b and c illustrate the sensitization and silver... Synthesis and Oxidation of Silver Nano-particles Hua Qi*, D. A. Alexson, O.J. Glembocki and S. M. Prokes* Electronics Science and Technology...energy dispersive x-ray (EDX) techniques. The results Quantum Dots and Nanostructures: Synthesis , Characterization, and Modeling VIII, edited by Kurt

Synthesis of ultrathin nitrogen-doped graphitic carbon nanocages as advanced electrode materials for supercapacitor.

PubMed

Tan, Yueming; Xu, Chaofa; Chen, Guangxu; Liu, Zhaohui; Ma, Ming; Xie, Qingji; Zheng, Nanfeng; Yao, Shouzhuo

2013-03-01

Synthesis of nitrogen-doped carbons with large surface area, high conductivity, and suitable pore size distribution is highly desirable for high-performance supercapacitor applications. Here, we report a novel protocol for template synthesis of ultrathin nitrogen-doped graphitic carbon nanocages (CNCs) derived from polyaniline (PANI) and their excellent capacitive properties. The synthesis of CNCs involves one-pot hydrothermal synthesis of Mn3O4@PANI core-shell nanoparticles, carbonization to produce carbon coated MnO nanoparticles, and then removal of the MnO cores by acidic treatment. The CNCs prepared at an optimum carbonization temperature of 800 °C (CNCs-800) have regular frameworks, moderate graphitization, high specific surface area, good mesoporosity, and appropriate N doping. The CNCs-800 show high specific capacitance (248 F g(-1) at 1.0 A g(-1)), excellent rate capability (88% and 76% capacitance retention at 10 and 100 A g(-1), respectively), and outstanding cycling stability (~95% capacitance retention after 5000 cycles) in 6 M KOH aqueous solution. The CNCs-800 can also exhibit great pseudocapacitance in 0.5 M H2SO4 aqueous solution besides the large electrochemical double-layer capacitance. The excellent capacitance performance coupled with the facile synthesis of ultrathin nitrogen-doped graphitic CNCs indicates their great application potential in supercapacitors.

Synthesis of positively charged hybrid PHMB-stabilized silver nanoparticles: the search for a new type of active substances used in plant protection products

NASA Astrophysics Data System (ADS)

Krutyakov, Yurii A.; Kudrinsky, Alexey A.; Gusev, Alexander A.; Zakharova, Olga V.; Klimov, Alexey I.; Yapryntsev, Alexey D.; Zherebin, Pavel M.; Shapoval, Olga A.; Lisichkin, Georgii V.

2017-07-01

Modern agriculture calls for a decrease in pesticide application, particularly in order to decrease the negative impact on the environment. Therefore the development of new active substances and plant protection products (PPP) to minimize the chemical load on ecosystems is a very important problem. Substances based on silver nanoparticles are a promising solution of this problem because of the fact that in correct doses such products significantly increase yields and decrease crop diseases while displaying low toxicity to humans and animals. In this paper we for the first time propose application of polymeric guanidine compounds with varying chain lengths (from 10 to 130 elementary links) for the design and synthesis of modified silver nanoparticles to be used as the basis of a new generation of PPP. Colloidal solutions of nanocrystalline silver containing 0.5 g l-1 of silver and 0.01-0.4 g l-1 of polyhexamethylene biguanide hydrochloride (PHMB) were obtained by reduction of silver nitrate with sodium borohydride in the presence of PHMB. The field experiment has shown that silver-containing solutions have a positive effect on agronomic properties of potato, wheat and apple. Also the increase in activity of such antioxidant system enzymes as peroxidase and catalase in the tissues of plants treated with nanosilver has been registered.

Synthesis of non-hydrazine solution processed Cu2(ZnSn)S4 thin films for solar cells applications

NASA Astrophysics Data System (ADS)

Gupta, Indu; Gupta, Preeti; Mohanty, Bhaskar Chandra

2017-05-01

Solution processing provides a versatile and inexpensive means to prepare Cu2ZnSnS4 (CZTS) thin films for photovoltaic applications. Differently with the reported growth of CZTS films from hydrazine based toxic solutions, we demonstrate a simple non-toxic ethanol based solution approach to synthesize the films. Using the chemical bath deposition (CBD) method, the CZTS thin films were grown from metal salts (copper chloride, zinc chloride, and tin chloride) in ethanol and monoethanol amine (MEA) and thioacetamide in ethanol as sulfur source in a single dip followed by sulfurization. The structure, composition, morphology and optical properties of the CZTS film were studied by X-ray diffraction, scanning electron microscopy and UV-vis spectroscopy. The results revealed that a post-deposition sulfurization is necessary to the phase formation and among all, sulfurization at 450°C for 60 min yielded phase pure CZTS films having kesterite structure, relatively compact morphology and an optical band gap of ˜1.52 eV indicating its suitability for solar cell applications. The results clearly validate the CBD method as a potential scalable route of preparation of CZTS thin films.

Facile synthesis of Fe3O4@C hollow nanospheres and their application in polluted water treatment

NASA Astrophysics Data System (ADS)

Zhang, Yuanguang; Xu, Shihao; Xia, Hongyu; Zheng, Fangcai

2016-11-01

Nanostructured carbon-based materials, such as carbon nanotube arrays have shown respectable removal ability for heavy metal ions and organic dyes in aqueous solution. Although the carbon-based materials exhibited excellent removal ability, the separation of them from the aqueous solution is difficult and time-consuming. Here we demonstrated a novel and facile route for the large-scale fabrication of Fe3O4@C hollow nanospheres, with using ferrocene as a single reagent and SiO2 as a template. The as-prepared Fe3O4@C hollow nanospheres exhibited adsorption ability for heavy metal ions and organic dyes from aqueous solution, and can be easily separated by an external magnet. When the as-prepared Fe3O4@C hollow nanospheres were mixed with the aqueous solution of Hg2+ within 15 min, the removal efficiency was 90.3%. The as-prepared Fe3O4@C hollow nanospheres were also exhibited a high adsorption capacity (100%) as the adsorbent for methylene blue (MB). In addition, the as-prepared Fe3O4@C hollow nanospheres can be used as the recyclable sorbent for water treatment via a simple magnetic separation.

CO2 as a smart gelator for Pluronic aqueous solutions.

PubMed

Liu, Chengcheng; Mei, Qingqing; Zhang, Jianling; Kang, Xinchen; Peng, Li; Han, Buxing; Xue, Zhimin; Sang, Xinxin; Yang, Xiaogan; Wu, Zhonghua; Li, Zhihong; Mo, Guang

2014-11-25

It was found that CO2 could induce the gelation of Pluronic aqueous solutions, during which the microstructure of the solution transforms from randomly dispersed spherical micelles to cubic close packed micelles. The gelation switched by compressed CO2 has many advantages and can be applied in the synthesis of porous materials.

Synthesis of nanoparticles through x-ray radiolysis using synchrotron radiation

NASA Astrophysics Data System (ADS)

Yamaguchi, A.; Okada, I.; Fukuoka, T.; Ishihara, M.; Sakurai, I.; Utsumi, Y.

2016-09-01

The synthesis and deposition of nanoparticles consisting of Cu and Au in a CuSO4 solution with some kinds of alcohol and electroplating solution containing gold (I) trisodium disulphite under synchrotron X-ray radiation was investigated. The functional group of alcohol plays an important in nucleation, growth and aggregation process of copper and cupric oxide particles. We found that the laboratory X-ray source also enables us to synthesize the NPs from the metallic solution. As increasing X-ray exposure time, the full length at half width of particle size distribution is broader and higher-order nanostructure containing NPs clusters is formed. The surface-enhanced Raman scattering (SERS) of 4, 4'-bipyridine (4bpy) in aqueous solution was measured using higher-order nanostructure immobilized on silicon substrates under systematically-varied X-ray exposure. This demonstration provide a clue to develop a three-dimensional printing and sensor for environmental analyses and molecular detection through simple SERS measurements.

Controller Synthesis for Periodically Forced Chaotic Systems

NASA Astrophysics Data System (ADS)

Basso, Michele; Genesio, Roberto; Giovanardi, Lorenzo

Delayed feedback controllers are an appealing tool for stabilization of periodic orbits in chaotic systems. Despite their conceptual simplicity, specific and reliable design procedures are difficult to obtain, partly also because of their inherent infinite-dimensional structure. This chapter considers the use of finite dimensional linear time invariant controllers for stabilization of periodic solutions in a general class of sinusoidally forced nonlinear systems. For such controllers — which can be interpreted as rational approximations of the delayed ones — we provide a computationally attractive synthesis technique based on Linear Matrix Inequalities (LMIs), by mixing results concerning absolute stability of nonlinear systems and robustness of uncertain linear systems. The resulting controllers prove to be effective for chaos suppression in electronic circuits and systems, as shown by two different application examples.

N-silyl oxyketene imines are underused yet highly versatile reagents for catalytic asymmetric synthesis

NASA Astrophysics Data System (ADS)

Denmark, Scott E.; Wilson, Tyler W.

2010-11-01

The reactions of acyl anion equivalents (d1 synthons) with carbonyl electrophiles allow for the construction of a wide range of molecules useful for the synthesis of biologically active compounds, natural products and chiral ligands. Despite their utility, significant challenges still exist for developing catalytic, enantioselective variants of these reactions. For example, the asymmetric benzoin process, arguably the most characteristic reaction of d synthetic equivalents, finds no general solution for reactions involving aliphatic acyl anions. In this Article, we introduce a new class of stable, isolable silyl ketene imines derived from protected cyanohydrins. These nucleophiles serve as acyl anion equivalents in Lewis base catalysed aldol addition reactions and allow for the preparation of cross-benzoin and glycolate-aldol products in high yield and with exceptional diastereo- and enantioselectivities.

Microwave-assisted one-step synthesis of white light-emitting carbon dot suspensions

NASA Astrophysics Data System (ADS)

Vanessa, Hinterberger; Wenshuo, Wang; Cornelia, Damm; Simon, Wawra; Martin, Thoma; Wolfgang, Peukert

2018-06-01

In this contribution, we demonstrate that an aqueous solution with adjustable fluorescent color, including white light emission, can be achieved by a rapid one-step microwave synthesis method resulting in a mixture of blue-emitting carbon dots (CDs) and the yellow-emitting 2,3-diaminophenazine (DAP). Aqueous mixtures of o-phenylene-diamine (oPD) and citric acid (CA) are used as precursors. The resulting product structures are analyzed by FT-IR and NMR spectroscopy and the size of the resulting CDs is determined by atomic force microscopy to be 1.1 ± 0.3 nm. The synthesized solution exhibits two fluorescence emission peaks at 430 and 560 nm, which were found to originate from the CDs and DAP, respectively. The intensity ratio of both fluorescence peaks depends on pH, which is driven by the protonation state of DAP. In consequence, the fluorescence emission color of the CD solution can be tuned precisely and reproducibly from blue to white to yellow by careful control of the pH. Finally, at a pH level of 5.4, at which there is equal blue and yellow emission intensity, a white light emitting solution can be successfully produced in a very fast and simple synthesis procedure.

Nonaqueous solution synthesis process for preparing oxide powders of lead zirconate titanate and related materials

DOEpatents

Voigt, J.A.; Sipola, D.L.; Tuttle, B.A.; Anderson, M.T.

1999-06-01

A process is disclosed for producing powders of perovskite-type compounds which comprises mixing a metal alkoxide solution with a lead acetate solution to form a homogeneous, clear metal solution, adding an oxalic acid/n-propanol solution to this metal solution to form an easily filterable, free-flowing precursor powder and then calcining this powder. This process provides fine perovskite-phase powders with ferroelectric properties which are particularly useful in a variety of electronic applications. 4 figs.

Nonaqueous solution synthesis process for preparing oxide powders of lead zirconate titanate and related materials

DOEpatents

Voigt, James A.; Sipola, Diana L.; Tuttle, Bruce A.; Anderson, Mark T.

1999-01-01

A process for producing powders of perovskite-type compounds which comprises mixing a metal alkoxide solution with a lead acetate solution to form a homogeneous, clear metal solution, adding an oxalic acid/n-propanol solution to this metal solution to form an easily filterable, free-flowing precursor powder and then calcining this powder. This process provides fine perovskite-phase powders with ferroelectric properties which are particularly useful in a variety of electronic applications.

Excited state properties of naphtho-homologated xxDNA bases and effect of methanol solution, deoxyribose, and base pairing.

PubMed

Zhang, Laibin; Ren, Tingqi; Tian, Jianxiang; Yang, Xiuqin; Zhou, Liuzhu; Li, Xiaoming

2013-04-18

Design and synthesis of fluorescent nucleobase analogues for studying structures and dynamics of nucleic acids have attracted much attention in recent years. In the present work, a comprehensive theoretical study of electronic transitions of naphtho-homologated base analogues, namely, xxC, xxT, xxA, and xxG, was performed. The nature of the low-lying excited states was discussed, and the results were compared with those of x-bases. Geometrical characteristics of the lowest excited singlet ππ* states were explored using the CIS method. The calculated excitation maxima are 423, 397, 383, and 357 nm for xxA, xxG, xxC, and xxT, respectively, and they are greatly red-shifted compared with x-bases and natural bases, allowing them to be selectively excited in the presence of the natural bases. In the gas phase, the fluorescence from them would be expected to occur around 497, 461, 457, and 417 nm, respectively. The effects of methanol solution, deoxyribose, and base paring with their complementary natural bases on the relevant absorption and emission spectra of these modified bases were also examined.

The promise of solution-processed Fe 2GeS 4 thin films in iron chalcogenide photovoltaics

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

Liu, Mimi; Berg, Dominik M.; Hwang, Po-Yu

The olivine Fe 2GeS 4, featuring non-toxic elements, cost-effective synthesis, and suitable optoelectronic properties, recently emerged as a promising light-absorbing candidate. Fe 2GeS 4 precursor powders obtained via a simple solution-based process were converted to highly crystalline Fe 2GeS 4 powders upon a thermal treatment in controlled atmosphere. Thin films fabricated by dip coating in the Fe 2GeS 4 precursor dispersion and subjected to the same thermal treatment render high-purity Fe 2GeS 4 thin films with a band gap of 1.4 eV, measured by room-temperature photoluminescence. Using Fe 2GeS 4 thin films as the sole absorber in a solution-based solarmore » cell, open-circuit voltages of 361 mV are observed, while the use of the Fe 2GeS 4 films as counter electrodes in dye-sensitized solar cell constructs enhances the overall power conversion efficiency of the cell by a factor of five. Finally, this is the first report of a photovoltaic device based onFe 2GeS 4.« less

Random lasing actions in self-assembled perovskite nanoparticles

NASA Astrophysics Data System (ADS)

Liu, Shuai; Sun, Wenzhao; Li, Jiankai; Gu, Zhiyuan; Wang, Kaiyang; Xiao, Shumin; Song, Qinghai

2016-05-01

Solution-based perovskite nanoparticles have been intensively studied in the past few years due to their applications in both photovoltaic and optoelectronic devices. Here, based on the common ground between solution-based perovskite and random lasers, we have studied the mirrorless lasing actions in self-assembled perovskite nanoparticles. After synthesis from a solution, discrete lasing peaks have been observed from optically pumped perovskites without any well-defined cavity boundaries. We have demonstrated that the origin of the random lasing emissions is the scattering between the nanostructures in the perovskite microplates. The obtained quality (Q) factors and thresholds of random lasers are around 500 and 60 μJ/cm2, respectively. Both values are comparable to the conventional perovskite microdisk lasers with polygon-shaped cavity boundaries. From the corresponding studies on laser spectra and fluorescence microscope images, the lasing actions are considered random lasers that are generated by strong multiple scattering in random gain media. In additional to conventional single-photon excitation, due to the strong nonlinear effects of perovskites, two-photon pumped random lasers have also been demonstrated for the first time. We believe this research will find its potential applications in low-cost coherent light sources and biomedical detection.

The promise of solution-processed Fe 2GeS 4 thin films in iron chalcogenide photovoltaics

DOE PAGES

Liu, Mimi; Berg, Dominik M.; Hwang, Po-Yu; ...

2018-02-06

The olivine Fe 2GeS 4, featuring non-toxic elements, cost-effective synthesis, and suitable optoelectronic properties, recently emerged as a promising light-absorbing candidate. Fe 2GeS 4 precursor powders obtained via a simple solution-based process were converted to highly crystalline Fe 2GeS 4 powders upon a thermal treatment in controlled atmosphere. Thin films fabricated by dip coating in the Fe 2GeS 4 precursor dispersion and subjected to the same thermal treatment render high-purity Fe 2GeS 4 thin films with a band gap of 1.4 eV, measured by room-temperature photoluminescence. Using Fe 2GeS 4 thin films as the sole absorber in a solution-based solarmore » cell, open-circuit voltages of 361 mV are observed, while the use of the Fe 2GeS 4 films as counter electrodes in dye-sensitized solar cell constructs enhances the overall power conversion efficiency of the cell by a factor of five. Finally, this is the first report of a photovoltaic device based onFe 2GeS 4.« less

In vitro mitochondrial test to assess haemodialyser biocompatibility.

PubMed

Tabouy, L J; Chauvet-Monges, A M; Brunet, P J; Braguer, D L; García, P A; Berland, Y F; Crevat, A D

1997-08-01

This paper describes an in vitro mitochondrial test to assess the biocompatibility of haemodialysers. We tested on isolated liver mitochondria the effect of solutions obtained by an aqueous rinse of different haemodialysers (cuprophane, cellulose acetate, Hemophan, polyacrylonitrile, polymethylmethacrylate, polysulphone, polyamide). Moreover, to determine the penetration into the cell and the cytotoxicity of these solutions from haemodialysers, we examined the effect of rinse solutions on HT29-D4 cells. Our results showed that rinse solutions from haemodialysers decrease the mitochondrial ATP synthesis. Cuprophane has the most marked effect, and the synthetic membranes exhibited only mild effects. Rinse solutions penetrated the cell and were cytotoxic by acting on mitochondria in the cell. In this respect, cellulosic membranes were the most toxic. Taken together our findings lead to a classification of haemodialyser membranes which is identical to one based on criteria such as activation of complement (cuprophane > other cellulosics > synthetics). Moreover isolated mitochondria make it possible to differentiate among the synthetic membranes. Isolated mitochondria thus appear to be a good in vitro test to assess the biocompatibility of haemodialysers.

A naphthodithiophene-diketopyrrolopyrrole donor molecule for efficient solution-processed solar cells.

PubMed

Loser, Stephen; Bruns, Carson J; Miyauchi, Hiroyuki; Ortiz, Rocío Ponce; Facchetti, Antonio; Stupp, Samuel I; Marks, Tobin J

2011-06-01

We report the synthesis, characterization, and first implementation of a naphtho[2,3-b:6,7-b']dithiophene (NDT)-based donor molecule in highly efficient organic photovoltaics (OPVs). When NDT(TDPP)(2) (TDPP = thiophene-capped diketopyrrolopyrrole) is combined with the electron acceptor PC(61)BM, a power conversion efficiency (PCE) of 4.06 ± 0.06% is achieved-a record for a PC(61)BM-based small-molecule OPV. The substantial PCE is attributed to the broad, high oscillator strength visible absorption, the ordered molecular packing, and an exceptional hole mobility of NDT(TDPP)(2). © 2011 American Chemical Society

Synthesis and self-assembly behavior of a biodegradable and sustainable soybean oil-based copolymer nanomicelle

NASA Astrophysics Data System (ADS)

Bao, Lixia; Bian, Longchun; Zhao, Mimi; Lei, Jingxin; Wang, Jiliang

2014-08-01

Herein, we report a novel amphiphilic biodegradable and sustainable soybean oil-based copolymer (SBC) prepared by grafting hydrophilic and biocompatible hydroxyethyl acrylate (HEA) polymeric segments onto the natural hydrophobic soybean oil chains. FTIR, H1-NMR, and GPC measurements have been used to investigate the molecular structure of the obtained SBC macromolecules. Self-assembly behaviors of the prepared SBC in aqueous solution have also been extensively evaluated by fluorescence spectroscopy and transmission electron microscopy. The prepared SBC nanocarrier with the size range of 40 to 80 nm has a potential application in the biomedical field.

MPA-11: Materials Synthesis and Integrated Devices; Overview of an Applied Energy Group

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

Dattelbaum, Andrew Martin

Our mission is to provide innovative and creative chemical synthesis and materials science solutions to solve materials problems across the LANL missions. Our group conducts basic and applied research in areas related to energy security as well as problems relevant to the Weapons Program.

MICROWAVE-ASSISTED SHAPE-CONTROLLED BULK SYNTHESIS OF NOBLE NANOCRYSTALS AND THEIR CATALYTIC PROPERTIES

EPA Science Inventory

Bulk and shape-controlled synthesis of gold (Au) nanostructures with various shapes such as prisms, cubes and hexagons is described that occurs via microwave-assisted spontaneous reduction of noble metal salts using an aqueous solution of α-D-glucose, sucrose and maltose. The exp...

ROOM TEMPERATURE BULK SYNTHESIS OF SILVER NANOCABLES WRAPPED WITH POLYPYRROLE

EPA Science Inventory

Wet chemical synthesis of silver cables wrapped with polypyrrole is reported in aqueous media without use of any surfactant/capping agent and/or template. The method employs direct polymerization of pyrrole of an aqueous solution with AgNO3 as an oxidizing agent. The four probe c...

Glass-ionomer cement formulations. II. The synthesis of novel polycarobxylic acids.

PubMed

Crisp, S; Kent, B E; Lewis, B G; Ferner, A J; Wilson, A D

1980-06-01

The synthesis of many polycarboxylic acids is reported. An account is given of their stability in aqueous solution and the properties of cements formed by their reaction with ion-leachable glasses. A copolymer of acrylic and itaconic acids was found to combine several favorable characteristics.

Strategies of Successful Synthesis Solutions: Mapping, Mechanisms, and More

ERIC Educational Resources Information Center

Bodé, Nicholas E.; Flynn, Alison B.

2016-01-01

Organic synthesis problems require the solver to integrate knowledge and skills from many parts of their courses. Without a well-defined, systematic method for approaching them, even the strongest students can experience difficulties. Our research goal was to identify the most successful problem-solving strategies and develop associated teaching…

Synthesis, characterization and reactivity of 3-mercaptopyruvic acid.

PubMed

Galardon, Erwan; Lec, Jean-Chrstophe

2018-05-20

A synthesis of the sulfur metabolic compound 3-mercaptopyruvic acid (3-MPH) is reported and allowed its isolation and characterization for the first time. Detailed kinetic, thermodynamic and spectroscopic studies of its complex behaviour in solution are discussed. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Synthesis and Characterization of Three Dimensional Nanostructures Based on Interconnected Carbon Nanomaterials

NASA Astrophysics Data System (ADS)

Koizumi, Ryota

This thesis addresses various types of synthetic methods for novel three dimensional nanomaterials and nanostructures based on interconnected carbon nanomaterials using solution chemistry and chemical vapor deposition (CVD) methods. Carbon nanotube (CNT) spheres with porous and scaffold structures consisting of interconnected CNTs were synthesized by solution chemistry followed by freeze-drying, which have high elasticity under nano-indentation tests. This allows the CNT spheres to be potentially applied to mechanical dampers. CNTs were also grown on two dimensional materials--such as reduced graphene oxide (rGO) and hexagonal boron nitride (h-BN)--by CVD methods, which are chemically interconnected. CNTs on rGO and h-BN interconnected structures performed well as electrodes for supercapacitors. Furthermore, unique interconnected flake structures of alpha-phase molybdenum carbide were developed by a CVD method. The molybdenum carbide can be used for a catalyst of hydrogen evolution reaction activity as well as an electrode for supercapacitors.

Synthesis, spectroscopic characterization and a comparative study of the corrosion inhibitive efficiency of an α-aminophosphonate and Schiff base derivatives: Experimental and theoretical investigations

NASA Astrophysics Data System (ADS)

Benbouguerra, Khalissa; Chafaa, Salah; Chafai, Nadjib; Mehri, Mouna; Moumeni, Ouahiba; Hellal, Abdelkader

2018-04-01

New α-aminophosphonate (α-APD) and Schiff base (E-NDPIMA) derivatives have been prepared and their structures ware proved by IR, UV-Vis, 1H, 13C and 31P NMR spectroscopy. Their inhibitive capacities on the XC48 carbon steel corrosion in 0.5 mol L-1 H2SO4 solution were explored by weight loss, Tafel polarization, electrochemical impedance spectroscopy (EIS) and atomic force microscope (AFM). Experimental results illustrate that the synthesized compounds are an effectives inhibitors and the adsorption of inhibitors molecules on the carbon steel surface obeys Langmuir adsorption isotherm. In addition, quantum chemical calculations performed with density function theory (DFT) method have been used to correlate the inhibition efficiency established experimentally. Also, the molecular dynamics simulations have been utilized to simulate the interactions between the inhibitors molecules and Fe (100) surface in aqueous solution.

Formation of crystalline InGaO₃(ZnO)n nanowires via the solid-phase diffusion process using a solution-based precursor.

PubMed

Guo, Yujie; Van Bilzen, Bart; Locquet, Jean Pierre; Seo, Jin Won

2015-12-11

One-dimensional single crystalline InGaO3(ZnO)n (IGZO) nanostructures have great potential for various electrical and optical applications. This paper demonstrates for the first time, to our knowledge, a non-vacuum route for the synthesis of IGZO nanowires by annealing ZnO nanowires covered with solution-based IGZO precursor. This method results in nanowires with highly periodic IGZO superlattice structure. The phase transition of IGZO precursor during thermal treatment was systematically studied. Transmission electron microscopy studies reveal that the formation of the IGZO structure is driven by anisotropic inter-diffusion of In, Ga, and Zn atoms, and also by the crystallization of the IGZO precursor. Optical measurements using cathodoluminescence and UV-vis spectroscopy confirm that the nanowires consist of the IGZO compound with wide optical band gap and suppressed luminescence.

Advanced Design Methodology for Robust Aircraft Sizing and Synthesis

NASA Technical Reports Server (NTRS)

Mavris, Dimitri N.

1997-01-01

Contract efforts are focused on refining the Robust Design Methodology for Conceptual Aircraft Design. Robust Design Simulation (RDS) was developed earlier as a potential solution to the need to do rapid trade-offs while accounting for risk, conflict, and uncertainty. The core of the simulation revolved around Response Surface Equations as approximations of bounded design spaces. An ongoing investigation is concerned with the advantages of using Neural Networks in conceptual design. Thought was also given to the development of systematic way to choose or create a baseline configuration based on specific mission requirements. Expert system was developed, which selects aerodynamics, performance and weights model from several configurations based on the user's mission requirements for subsonic civil transport. The research has also resulted in a step-by-step illustration on how to use the AMV method for distribution generation and the search for robust design solutions to multivariate constrained problems.

Selective Chemical Conversion of Sugars in Aqueous Solutions without Alkali to Lactic Acid Over a Zn-Sn-Beta Lewis Acid-Base Catalyst

NASA Astrophysics Data System (ADS)

Dong, Wenjie; Shen, Zheng; Peng, Boyu; Gu, Minyan; Zhou, Xuefei; Xiang, Bo; Zhang, Yalei

2016-05-01

Lactic acid is an important platform molecule in the synthesis of a wide range of chemicals. However, in aqueous solutions without alkali, its efficient preparation via the direct catalysis of sugars is hindered by a side dehydration reaction to 5-hydroxymethylfurfural due to Brønsted acid, which originates from organic acids. Herein, we report that a previously unappreciated combination of common two metal mixed catalyst (Zn-Sn-Beta) prepared via solid-state ion exchange synergistically promoted this reaction. In water without a base, a conversion exceeding 99% for sucrose with a lactic acid yield of 54% was achieved within 2 hours at 190 °C under ambient air pressure. Studies of the acid and base properties of the Zn-Sn-Beta zeolite suggest that the introduction of Zn into the Sn-Beta zeolite sequentially enhanced both the Lewis acid and base sites, and the base sites inhibited a series of side reactions related to fructose dehydration to 5-hydroxymethylfurfural and its subsequent decomposition.

Selective Chemical Conversion of Sugars in Aqueous Solutions without Alkali to Lactic Acid Over a Zn-Sn-Beta Lewis Acid-Base Catalyst

PubMed Central

Dong, Wenjie; Shen, Zheng; Peng, Boyu; Gu, Minyan; Zhou, Xuefei; Xiang, Bo; Zhang, Yalei

2016-01-01

Lactic acid is an important platform molecule in the synthesis of a wide range of chemicals. However, in aqueous solutions without alkali, its efficient preparation via the direct catalysis of sugars is hindered by a side dehydration reaction to 5-hydroxymethylfurfural due to Brønsted acid, which originates from organic acids. Herein, we report that a previously unappreciated combination of common two metal mixed catalyst (Zn-Sn-Beta) prepared via solid-state ion exchange synergistically promoted this reaction. In water without a base, a conversion exceeding 99% for sucrose with a lactic acid yield of 54% was achieved within 2 hours at 190 °C under ambient air pressure. Studies of the acid and base properties of the Zn-Sn-Beta zeolite suggest that the introduction of Zn into the Sn-Beta zeolite sequentially enhanced both the Lewis acid and base sites, and the base sites inhibited a series of side reactions related to fructose dehydration to 5-hydroxymethylfurfural and its subsequent decomposition. PMID:27222322

Facile synthesis of layered V2O5/ZnV2O6 heterostructures with enhanced sensing performance

NASA Astrophysics Data System (ADS)

Xiao, Bingxin; Huang, Hao; Yu, Xiantong; Song, Jun; Qu, Junle

2018-07-01

A low-cost and environment-friendly hydrothermal approach was used for the synthesis of layered V2O5/ZnV2O6 hybrid nanobelts. Characterization results indicate that the V2O5/ZnV2O6 nanobelts are composed of several thin layers. Additionally, it is illustrated that the chemical formation process of V2O5/ZnV2O6 occurred in the solution. The synthesized V2O5/ZnV2O6 heterostructures were subjected to detailed ethanol sensing tests. Results demonstrate that V2O5/ZnV2O6 based sensor shows about 4.3 of response to 100 ppm of ethanol gases, reveals relatively high sensitivity at relatively low optimal operating temperature of 240 °C, as well as relatively good selectivity and stability. The performance of the sensor is better than most of reported vanadium based sensing devices. Thus this work offers a new insight into the rational regulation of vanadium based sensing devices.

Genetic GIScience: Toward a Place-Based Synthesis of the Genome, Exposome, and Behavome

PubMed Central

Jacquez, Geoffrey M.; Sabel, Clive E.; Shi, Chen

2015-01-01

The exposome, defined as the totality of an individual’s exposures over the life course, is a seminal concept in the environmental health sciences. Although inherently geographic, the exposome as yet is unfamiliar to many geographers. This article proposes a place-based synthesis, genetic geographic information science (Genetic GISc) that is founded on the exposome, genome+ and behavome. It provides an improved understanding of human health in relation to biology (the genome+), environmental exposures (the exposome), and their social, societal and behavioral determinants (the behavome). Genetic GISc poses three key needs: First, a mathematical foundation for emergent theory; Second, process-based models that bridge biological and geographic scales; Third, biologically plausible estimates of space-time disease lags. Compartmental models are a possible solution; this article develops two models using pancreatic cancer as an exemplar. The first models carcinogenesis based on the cascade of mutations and cellular changes that lead to metastatic cancer. The second models cancer stages by diagnostic criteria. These provide empirical estimates of the distribution of latencies in cellular states and disease stages, and maps of the burden of yet to be diagnosed disease. This approach links our emerging knowledge of genomics to cancer progression at the cellular level, to individuals and their cancer stage at diagnosis, to geographic distributions of cancer in extant populations. These methodological developments and exemplar provide the basis for a new synthesis in health geography: genetic geographic information science. PMID:26339073

Synthesis and properties of mecoprop-intercalated layered double hydroxide

NASA Astrophysics Data System (ADS)

Ahmed Khan, Modabber; Choi, Choong-Lyeal; Lee, Dong-Hoon; Park, Man; Lim, Bu-Kug; Lee, Jong-Yoon; Choi, Jyung

2007-08-01

This study carried out to elucidate the synthesis of MCPP LDH hybrid, release pattern of MCPP from MCPP LDH hybrid and their properties. MCPP LDH hybrid was synthesized from MCPP and Mg Al complex. Release pattern of MCPP from MCPP LDH hybrid was slower in distilled water and soil solution but it was slower in distilled water than soil solution. MCPP LDH hybrid has shown more stable condition than CO32- form of LDH in thermal and acidic condition. Therefore, MCPP LDH hybrid would lead as functional and benign pesticide to minimize the harmful effects on soil environment by bulk herbicides.

Synthesis of TiO2 by solution combustion technique by mixed fuel approach for wLED applications

NASA Astrophysics Data System (ADS)

Venkatesha Babu K., R.; Renuka C., G.

2018-05-01

Synthesis of Ce3+ (0.25-0.75 mol %) doped TiO2 nanophosphors was done by solution combustion route using combination of fuels. The structural characterization of the nanophosphor was performed by PXRD, SEM and TEM. The estimated crystallite sizes are in the nano meter scale range. The Eg of pure and doped TiO2 were 3.10 and 3.23 eV respectively were estimated from DRS data. The CIE and CCT data reveals that the nanophosphor emits pale green and is useful for wLED at a temperature 4474K.

Ultrasonic-assisted synthesis of monodisperse single-crystalline silver nanoplates and gold nanorings.

PubMed

Jiang, Li-Ping; Xu, Shu; Zhu, Jian-Min; Zhang, Jian-Rong; Zhu, Jun-Jie; Chen, Hong-Yuan

2004-09-20

A simple sonochemical route was developed for the crystal growth of uniform silver nanoplates and ringlike gold nanocrystals in a N,N-dimethylformamide solution. The platelike structures were generated from the selective growth on different crystal planes in the presence of poly(vinylpyrrolidone) and the ultrasonic-assisted Ostwald ripening processes. The silver nanoplates in solution served as the templates for the synthesis of ringlike gold crystals via a displacement reaction. Both the silver nanoplates and gold nanorings were highly oriented single crystals with (111) planes as the basal planes. Copyright 2004 American Chemical Society

Parallel-vector computation for linear structural analysis and non-linear unconstrained optimization problems

NASA Technical Reports Server (NTRS)

Nguyen, D. T.; Al-Nasra, M.; Zhang, Y.; Baddourah, M. A.; Agarwal, T. K.; Storaasli, O. O.; Carmona, E. A.

1991-01-01

Several parallel-vector computational improvements to the unconstrained optimization procedure are described which speed up the structural analysis-synthesis process. A fast parallel-vector Choleski-based equation solver, pvsolve, is incorporated into the well-known SAP-4 general-purpose finite-element code. The new code, denoted PV-SAP, is tested for static structural analysis. Initial results on a four processor CRAY 2 show that using pvsolve reduces the equation solution time by a factor of 14-16 over the original SAP-4 code. In addition, parallel-vector procedures for the Golden Block Search technique and the BFGS method are developed and tested for nonlinear unconstrained optimization. A parallel version of an iterative solver and the pvsolve direct solver are incorporated into the BFGS method. Preliminary results on nonlinear unconstrained optimization test problems, using pvsolve in the analysis, show excellent parallel-vector performance indicating that these parallel-vector algorithms can be used in a new generation of finite-element based structural design/analysis-synthesis codes.

Enzyme-Catalyzed Synthesis of Unsaturated Aliphatic Polyesters Based on Green Monomers from Renewable Resources

PubMed Central

Jiang, Yi; Woortman, Albert J.J.; Alberda van Ekenstein, Gert O.R.; Loos, Katja

2013-01-01

Bio-based commercially available succinate, itaconate and 1,4-butanediol are enzymatically co-polymerized in solution via a two-stage method, using Candida antarctica Lipase B (CALB, in immobilized form as Novozyme® 435) as the biocatalyst. The chemical structures of the obtained products, poly(butylene succinate) (PBS) and poly(butylene succinate-co-itaconate) (PBSI), are confirmed by 1H- and 13C-NMR. The effects of the reaction conditions on the CALB-catalyzed synthesis of PBSI are fully investigated, and the optimal polymerization conditions are obtained. With the established method, PBSI with tunable compositions and satisfying reaction yields is produced. The 1H-NMR results confirm that carbon-carbon double bonds are well preserved in PBSI. The differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA) results indicate that the amount of itaconate in the co-polyesters has no obvious effects on the glass-transition temperature and the thermal stability of PBS and PBSI, but has significant effects on the melting temperature. PMID:24970176

Synthesis of Ammonia-Assisted Porous Nickel Ferrite (NiFe₂O₄) Nanostructures as an Electrode Material for Supercapacitors.

PubMed

Bhojane, Prateek; Sharma, Alfa; Pusty, Manojit; Kumar, Yogendra; Sen, Somaditya; Shirage, Parasharam

2017-02-01

In this work, we report a low cost, facile synthesis method for Nickel ferrite (NiFe₂O₄) nanostructures obtained by chemical bath deposition method for alternate transition metal oxide electrode material as a solution for clean energy. We developed a template free ammonia assisted method for obtaining porous structure which offering better supercapacitive performance of NiFe₂O₄ electrode material than previously reported for pure NiFe₂O₄. Here we explore the physical characterizations X-ray diffraction, FESEM, HRTEM performed to under-stand its crystal structure and morphology as well as the electrochemical measurements was performed to understand the electrochemical behaviour of the material. Here ammonia plays an important role in governing the structure/morphology of the material and enhances the electrochemical performance. The specific capacitance of 541 Fg⁻¹ is achieved at 2 mVs⁻¹ scan rate which is highest for the pure NiFe₂O₄ electrode material without using any addition of carbon based material, heterostructure or template based method.

The Complex Sol-Gel Process for producing small ThO2 microspheres

NASA Astrophysics Data System (ADS)

Brykala, Marcin; Rogowski, Marcin

2016-05-01

Thorium based fuels offer several benefits compared to uranium based fuels thus they might be an attractive alternative to conventional fuel types. This study is devoted to the synthesis and the characterization of small thorium dioxide microspheres (Ø <50 μm). Their application involves using powder-free process, called the Complex Sol-Gel Process. The source sols used for the processes were prepared by the method where in the starting ascorbic acid solution the solid thorium nitrate was dissolved and partially neutralized by aqueous ammonia under pH control. The microspheres of thorium-ascorbate gel were obtained using the ICHTJ Process (INCT in English). Studies allowed to determine an optimal heat treatment with calcination temperature of 700 °C and temperature rate not higher than 2 °C/min which enabled us to obtain a crack-free surface of microspheres. The main parameters which have a strong influence on the synthesis method and features of the spherical particles of thorium dioxide are described in this article.

Room Temperature Co-Precipitation Synthesis of Magnetite Nanoparticles in a Large pH Window with Different Bases.

PubMed

Mascolo, Maria Cristina; Pei, Yongbing; Ring, Terry A

2013-11-28

Magnetite nanoparticles (Fe₃O₄) represent the most promising materials in medical applications. To favor high-drug or enzyme loading on the nanoparticles, they are incorporated into mesoporous materials to form a hybrid support with the consequent reduction of magnetization saturation. The direct synthesis of mesoporous structures appears to be of interest. To this end, magnetite nanoparticles have been synthesized using a one pot co-precipitation reaction at room temperature in the presence of different bases, such as NaOH, KOH or (C₂H₅)₄NOH. Magnetite shows characteristics of superparamagnetism at room temperature and a saturation magnetization (Ms) value depending on both the crystal size and the degree of agglomeration of individual nanoparticles. Such agglomeration appears to be responsible for the formation of mesoporous structures, which are affected by the pH, the nature of alkali, the slow or fast addition of alkaline solution and the drying modality of synthesized powders.

Finite-horizon control-constrained nonlinear optimal control using single network adaptive critics.

PubMed

Heydari, Ali; Balakrishnan, Sivasubramanya N

2013-01-01

To synthesize fixed-final-time control-constrained optimal controllers for discrete-time nonlinear control-affine systems, a single neural network (NN)-based controller called the Finite-horizon Single Network Adaptive Critic is developed in this paper. Inputs to the NN are the current system states and the time-to-go, and the network outputs are the costates that are used to compute optimal feedback control. Control constraints are handled through a nonquadratic cost function. Convergence proofs of: 1) the reinforcement learning-based training method to the optimal solution; 2) the training error; and 3) the network weights are provided. The resulting controller is shown to solve the associated time-varying Hamilton-Jacobi-Bellman equation and provide the fixed-final-time optimal solution. Performance of the new synthesis technique is demonstrated through different examples including an attitude control problem wherein a rigid spacecraft performs a finite-time attitude maneuver subject to control bounds. The new formulation has great potential for implementation since it consists of only one NN with single set of weights and it provides comprehensive feedback solutions online, though it is trained offline.

Engineering calculations for communications satellite systems planning

NASA Technical Reports Server (NTRS)

Reilly, C. H.; Levis, C. A.; Mount-Campbell, C.; Gonsalvez, D. J.; Wang, C. W.; Yamamura, Y.

1985-01-01

Computer-based techniques for optimizing communications-satellite orbit and frequency assignments are discussed. A gradient-search code was tested against a BSS scenario derived from the RARC-83 data. Improvement was obtained, but each iteration requires about 50 minutes of IBM-3081 CPU time. Gradient-search experiments on a small FSS test problem, consisting of a single service area served by 8 satellites, showed quickest convergence when the satellites were all initially placed near the center of the available orbital arc with moderate spacing. A transformation technique is proposed for investigating the surface topography of the objective function used in the gradient-search method. A new synthesis approach is based on transforming single-entry interference constraints into corresponding constraints on satellite spacings. These constraints are used with linear objective functions to formulate the co-channel orbital assignment task as a linear-programming (LP) problem or mixed integer programming (MIP) problem. Globally optimal solutions are always found with the MIP problems, but not necessarily with the LP problems. The MIP solutions can be used to evaluate the quality of the LP solutions. The initial results are very encouraging.

Synthesis of Environmentally Friendly Highly Dispersed Magnetite Nanoparticles Based on Rosin Cationic Surfactants as Thin Film Coatings of Steel

PubMed Central

Atta, Ayman M.; El-Mahdy, Gamal A.; Al-Lohedan, Hamad A.; Al-Hussain, Sami A.

2014-01-01

This work presents a new method to prepare monodisperse magnetite nanoparticles capping with new cationic surfactants based on rosin. Core/shell type magnetite nanoparticles were synthesized using bis-N-(3-levopimaric maleic acid adduct-2-hydroxy) propyl-triethyl ammonium chloride (LPMQA) as capping agent. Fourier transform infrared spectroscopy (FTIR) was employed to characterize the nanoparticles chemical structure. Transmittance electron microscopies (TEM) and X-ray powder diffraction (XRD) were used to examine the morphology of the modified magnetite nanoparticles. The magnetite dispersed aqueous acid solution was evaluated as an effective anticorrosion behavior of a hydrophobic surface on steel. The inhibition effect of magnetite nanoparticles on steel corrosion in 1 M HCl solution was investigated using potentiodynamic polarization curves and electrochemical impedance spectroscopy (EIS). Results obtained from both potentiodynamic polarisation and EIS measurements reveal that the magnetite nanoparticle is an effective inhibitor for the corrosion of steel in 1.0 M HCl solution. Polarization data show that magnetite nanoparticles behave as a mixed type inhibitor. The inhibition efficiencies obtained from potentiodynamic polarization and EIS methods are in good agreement. PMID:24758936

Synthesis of environmentally friendly highly dispersed magnetite nanoparticles based on rosin cationic surfactants as thin film coatings of steel.

PubMed

Atta, Ayman M; El-Mahdy, Gamal A; Al-Lohedan, Hamad A; Al-Hussain, Sami A

2014-04-22

This work presents a new method to prepare monodisperse magnetite nanoparticles capping with new cationic surfactants based on rosin. Core/shell type magnetite nanoparticles were synthesized using bis-N-(3-levopimaric maleic acid adduct-2-hydroxy) propyl-triethyl ammonium chloride (LPMQA) as capping agent. Fourier transform infrared spectroscopy (FTIR) was employed to characterize the nanoparticles chemical structure. Transmittance electron microscopies (TEM) and X-ray powder diffraction (XRD) were used to examine the morphology of the modified magnetite nanoparticles. The magnetite dispersed aqueous acid solution was evaluated as an effective anticorrosion behavior of a hydrophobic surface on steel. The inhibition effect of magnetite nanoparticles on steel corrosion in 1 M HCl solution was investigated using potentiodynamic polarization curves and electrochemical impedance spectroscopy (EIS). Results obtained from both potentiodynamic polarisation and EIS measurements reveal that the magnetite nanoparticle is an effective inhibitor for the corrosion of steel in 1.0 M HCl solution. Polarization data show that magnetite nanoparticles behave as a mixed type inhibitor. The inhibition efficiencies obtained from potentiodynamic polarization and EIS methods are in good agreement.

Developing upconversion nanoparticle-based smart substrates for remote temperature sensing

NASA Astrophysics Data System (ADS)

Coker, Zachary; Marble, Kassie; Alkahtani, Masfer; Hemmer, Philip; Yakovlev, Vladislav V.

2018-02-01

Recent developments in understanding of nanomaterial behaviors and synthesis have led to their application across a wide range of commercial and scientific applications. Recent investigations span from applications in nanomedicine and the development of novel drug delivery systems to nanoelectronics and biosensors. In this study, we propose the application of a newly engineered temperature sensitive water-based bio-compatible core/shell up-conversion nanoparticle (UCNP) in the development of a smart substrate for remote temperature sensing. We developed this smart substrate by dispersing functionalized nanoparticles into a polymer solution and then spin-coating the solution onto one side of a microscope slide to form a thin film substrate layer of evenly dispersed nanoparticles. By using spin-coating to deposit the particle solution we both create a uniform surface for the substrate while simultaneously avoid undesired particle agglomeration. Through this investigation, we have determined the sensitivity and capabilities of this smart substrate and conclude that further development can lead to a greater range of applications for this type smart substrate and use in remote temperature sensing in conjunction with other microscopy and spectroscopy investigations.

Optimal synthesis and design of the number of cycles in the leaching process for surimi production.

PubMed

Reinheimer, M Agustina; Scenna, Nicolás J; Mussati, Sergio F

2016-12-01

Water consumption required during the leaching stage in the surimi manufacturing process strongly depends on the design and the number and size of stages connected in series for the soluble protein extraction target, and it is considered as the main contributor to the operating costs. Therefore, the optimal synthesis and design of the leaching stage is essential to minimize the total annual cost. In this study, a mathematical optimization model for the optimal design of the leaching operation is presented. Precisely, a detailed Mixed Integer Nonlinear Programming (MINLP) model including operating and geometric constraints was developed based on our previous optimization model (NLP model). Aspects about quality, water consumption and main operating parameters were considered. The minimization of total annual costs, which considered a trade-off between investment and operating costs, led to an optimal solution with lesser number of stages (2 instead of 3 stages) and higher volumes of the leaching tanks comparing with previous results. An analysis was performed in order to investigate how the optimal solution was influenced by the variations of the unitary cost of fresh water, waste treatment and capital investment.

Type synthesis and preliminary design of devices supporting lower limb's rehabilitation.

PubMed

Olinski, Michał; Lewandowski, Bogusz; Gronowicz, Antoni

2015-01-01

Based on the analysis of existing solutions, biomechanics of human lower limbs and anticipated applications, results of con- siderations concerning the necessary number of degrees of freedom for the designed device supporting rehabilitation of lower extremities are presented. An analysis was carried out in order to determine the innovative kinematic structure of the device, ensuring sufficient mobility and functionality while minimizing the number of degrees of freedom. With the aid of appropriate formalised meth- ods, for instance, type synthesis, a complete variety of solutions for leg joints were obtained in the form of basic and kinematic schemes, having the potential to find application in devices supporting lower limb rehabilitation. A 3D model of ankle joint module was built in Autodesk Inventor System, then imported to Adams and assembled into a moving numerical model of a mechanism. Several conducted simulations resulted in finding the required maximum stroke of the cylinders. A comparison of the angular ranges of ankle joint and similar devices with the ones achieved by the designed device indicated a sufficient reserve allowing not only movements typical of gait, but approximately achieving the passive range of motion for the ankle joint.

Graphene Nanocomposites with High Molecular Weight Poly(ε-caprolactone) Grafts: Controlled Synthesis and Accelerated Crystallization

DOE PAGES

Mondal, Titash; Ashkar, Rana; Butler, Paul; ...

2016-02-08

Grafting of high molecular weight polymers to graphitic nanoplatelets is a critical step toward the development of high performance graphene nanocomposites. However, designing such a grafting route has remained a major impediment. Herein, we report a "grafting to" synthetic pathway by which high molecular weight polymer, poly(e-caprolactone) (PCL), is tethered, at high grafting density, to highly anisotropic graphitic nanoplatelets. The efficacy of this tethering route and the resultant structural arrangements within the composite are confirmed by neutron and X-ray scattering measurements in the melt and solution phase. In the semicrystalline state, Xray analysis indicates that chain tethering onto the graphiticmore » nanoplatelets results in conformational changes of the polymer chains, which enhance the nucleation process and aid formation of PCL crystallites. This is corroborated by the superior thermal properties of the composite, manifested in accelerated crystallization kinetics and a significant increase in the thermal degradation temperature. Lastly, in principle, this synthesis route can be extended to a variety of high molecular weight polymers, which can open new avenues to solution-based processing of graphitic nanomaterials and the fabrication of complex 3D patterned graphitic nanocomposites.« less

Electrocatalysts for Hydrogen Evolution in Alkaline Electrolytes: Mechanisms, Challenges, and Prospective Solutions.

PubMed

Mahmood, Nasir; Yao, Yunduo; Zhang, Jing-Wen; Pan, Lun; Zhang, Xiangwen; Zou, Ji-Jun

2018-02-01

Hydrogen evolution reaction (HER) in alkaline medium is currently a point of focus for sustainable development of hydrogen as an alternative clean fuel for various energy systems, but suffers from sluggish reaction kinetics due to additional water dissociation step. So, the state-of-the-art catalysts performing well in acidic media lose considerable catalytic performance in alkaline media. This review summarizes the recent developments to overcome the kinetics issues of alkaline HER, synthesis of materials with modified morphologies, and electronic structures to tune the active sites and their applications as efficient catalysts for HER. It first explains the fundamentals and electrochemistry of HER and then outlines the requirements for an efficient and stable catalyst in alkaline medium. The challenges with alkaline HER and limitation with the electrocatalysts along with prospective solutions are then highlighted. It further describes the synthesis methods of advanced nanostructures based on carbon, noble, and inexpensive metals and their heterogeneous structures. These heterogeneous structures provide some ideal systems for analyzing the role of structure and synergy on alkaline HER catalysis. At the end, it provides the concluding remarks and future perspectives that can be helpful for tuning the catalysts active-sites with improved electrochemical efficiencies in future.

Electrocatalysts for Hydrogen Evolution in Alkaline Electrolytes: Mechanisms, Challenges, and Prospective Solutions

PubMed Central

Mahmood, Nasir; Yao, Yunduo; Zhang, Jing‐Wen; Pan, Lun; Zhang, Xiangwen

2017-01-01

Abstract Hydrogen evolution reaction (HER) in alkaline medium is currently a point of focus for sustainable development of hydrogen as an alternative clean fuel for various energy systems, but suffers from sluggish reaction kinetics due to additional water dissociation step. So, the state‐of‐the‐art catalysts performing well in acidic media lose considerable catalytic performance in alkaline media. This review summarizes the recent developments to overcome the kinetics issues of alkaline HER, synthesis of materials with modified morphologies, and electronic structures to tune the active sites and their applications as efficient catalysts for HER. It first explains the fundamentals and electrochemistry of HER and then outlines the requirements for an efficient and stable catalyst in alkaline medium. The challenges with alkaline HER and limitation with the electrocatalysts along with prospective solutions are then highlighted. It further describes the synthesis methods of advanced nanostructures based on carbon, noble, and inexpensive metals and their heterogeneous structures. These heterogeneous structures provide some ideal systems for analyzing the role of structure and synergy on alkaline HER catalysis. At the end, it provides the concluding remarks and future perspectives that can be helpful for tuning the catalysts active‐sites with improved electrochemical efficiencies in future. PMID:29610722

Growth of single crystals of organic salts with large second-order optical nonlinearities by solution processes for devices

NASA Technical Reports Server (NTRS)

Leslie, Thomas M.

1995-01-01

Data obtained from the electric field induced second harmonic generation (EFISH) and Kurtz Powder Methods will be provided to MSFC for further refinement of their method. A theoretical model for predicting the second-order nonlinearities of organic salts is being worked on. Another task is the synthesis of a number of salts with various counterions. Several salts with promising SHG activities and new salts will be tested for the presence of two crystalline forms. The materials will be recrystallized from dry and wet solvents and compared for SHG efficiency. Salts that have a high SHG efficiency and no tendency to form hydrates will be documented. The synthesis of these materials are included in this report. A third task involves method to aid in the growth of large, high quality single crystals by solution processes. These crystals will be characterized for their applicability in the fabrication of devices that will be incorporated into optical computers in future programs. Single crystals of optimum quality may be obtained by crystal growth in low-gravity. The final task is the design of a temperature lowering single crystal growth apparatus for ground based work. At least one prototype will be built.

The Scaevola frutescen (Mill.) Krause dried-leaves extract as a potential natural reduction system for synthesis of gold nanoparticles and their evaluation for antibacterial of Eschericia coli

NASA Astrophysics Data System (ADS)

Salprima Yudha, S.; Angasa, Eka; Suharto, Totok Eka; Nishina, Yuta; Mardlia, Zulfikri Achid; Sipriyadi

2016-02-01

Many reports recently show that some plant and animal extracts were useful to prepare some desired materials. In line with the statement, this report will present a bioresources candidate that can be used for green preparation of gold nanoparticles. The Scaevola fruteschen (Mill.) Krause was obtained from Enggano island, Bengkulu Province, Indonesia. The current research include synthesis, characterization and application study of the obtained nanoparticles in their original medium/reduction system as antibacterial agent of Escherichia coli. Besides that, the interaction study of the nanoparticles solution with Pb2+ ions was also studied. The results, shows that the present reduction system (aqueous extract of the plant leaves) successfully reduced gold (III) ions to gold metals as shown by new peak at 544 nm in spectrophotometry analysis. The average nanopartiles size was 96 nm based on Particles Size Analyzer (PSA) result. The stability study revealed that the nanoparticles solution was not stable in the persence of Pb(OAc)2 at high concentration. The nanoparticles were effective enough toward E. coli as shown by inhibition zone that indicates the degree of sensitivity of bacteria to nanoparticles.

β-Dicalcium silicate-based cement: synthesis, characterization and in vitro bioactivity and biocompatibility studies.

PubMed

Correa, Daniel; Almirall, Amisel; García-Carrodeguas, Raúl; dos Santos, Luis Alberto; De Aza, Antonio H; Parra, Juan; Delgado, José Ángel

2014-10-01

β-dicalcium silicate (β-Ca₂ SiO₄, β-C₂ S) is one of the main constituents in Portland cement clinker and many refractory materials, itself is a hydraulic cement that reacts with water or aqueous solution at room/body temperature to form a hydrated phase (C-S-H), which provides mechanical strength to the end product. In the present investigation, β-C₂ S was synthesized by sol-gel process and it was used as powder to cement preparation, named CSiC. In vitro bioactivity and biocompatibility studies were assessed by soaking the cement samples in simulated body fluid solutions and human osteoblast cell cultures for various time periods, respectively. The results showed that the sol-gel process is an available synthesis method in order to obtain a pure powder of β-C₂ S at relatively low temperatures without chemical stabilizers. A bone-like apatite layer covered the material surface after soaking in SBF and its compressive strength (CSiC cement) was comparable with that of the human trabecular bone. The extracts of this cement were not cytotoxic and the cell growth and relative cell viability were comparable to negative control. © 2013 Wiley Periodicals, Inc.

Composition characteristics and regularities of dissolving of hydroxyapatite materials obtained in water solutions with varied content of silicate ions

NASA Astrophysics Data System (ADS)

Solonenko, A. P.

2018-01-01

Research aimed at developing new bioactive materials for the repair of defects in bone tissues, do not lose relevance due to the strengthening of the regenerative approach in medicine. From this point of view, materials based on calcium phosphates, including silicate ions, consider as one of the most promising group of substances. Methods of synthesis and properties of hydroxyapatite doped with various amounts of SiO4 4- ions are described in literature. In the present work synthesis of a solid phase in the systems Ca(NO3)2 - (NH4)2HPO4 - Na2SiO3 - NH4OH - H2O (Cca/CP = 1.70) performed with a wide range of sodium silicate additive concentration (y = CSi/CP = 0 ÷ 5). It is established that under the studied conditions at y ≥ 0.3 highly dispersed poorly crystallized apatite containing isomorphic impurities of CO3 2- and SiO4 4- precipitates in a mixture with calcium hydrosilicate and SiO2. It is shown that the resulting composites can gradually dissolve in physiological solution and initiate passive formation of the mineral component of hard tissues.

Synthesis, Rietveld refinements, Infrared and Raman spectroscopy studies of the sodium diphosphate NaCryFe1-yP2O7 (0 ≤ y ≤ 1)

NASA Astrophysics Data System (ADS)

Bih, H.; Saadoune, I.; Bih, L.; Mansori, M.; ToufiK, H.; Fuess, H.; Ehrenberg, H.

2016-01-01

In the present study we report on the synthesis and crystal structure studies of NaCryFe1-yP2O7 sodium diphosphate solid solution (0 ≤ y ≤ 1). The X-ray diffraction shows that these compounds are isostructural with NaFeP2O7 and NaCrP2O7 (space group P21/c (C2h5) Z = 4). The Rietveld refinements based on the XRD patterns show the existence of a continuous solid solution over the whole composition range (0 ≤ y ≤ 1). A continuous evolution of the monoclinic unit cell parameters was obtained. The transition metal ions (Cr3+ and/or Fe3+) connect the diphosphate anions forming a three-dimensional network with cages filled by Na+ cations. IR and Raman spectra have been interpreted using factor group analysis. A small shift of the band frequencies is observed when Fe is substituted by Cr. The POP bridge angles are determined from Lazarev's relation and agree well with those deduced from the crystal structure refinement.

Synthesis and Performance of a Biomimetic Indicator for Alkylating Agents.

PubMed

Provencher, Philip A; Love, Jennifer A

2015-10-02

4-(4-Nitrobenzyl)pyridine (NBP) is a colorimetric indicator compound for many types of carcinogenic alkylating agents. Because of the similar reactivity of NBP and guanine in DNA, NBP serves as a DNA model. NBP assays are used in the toxicological screening of pharmaceutical compounds, detection of chemical warfare agents, environmental hygiene technology, preliminary toxicology tests, mutagenicity of medicinal compounds, and other chemical analyses. Nevertheless, the use of NBP as a DNA model suffers from the compound's low water solubility, its lack of reactive oxygen sites, and dissimilar steric encumbrance compared to DNA. We report herein the design and synthesis of NBP derivatives that address some of these issues. These derivatives have been tested in solution and found to be superior in the colorimetric assay of the alkylating anticancer drug cyclophosphamide. The derivatives have also been integrated into a polymeric silica material which changes color upon the exposure to dangerous alkylating agents, such as iodomethane vapor, without the need for an exogenous base. This material modernizes the NBP assay from a time-consuming laboratory analysis to a real-time solid state sensor, which requires neither solvent nor additional reagents and can detect both gas- and solution-phase alkylating agents.

High degree of polymerization in a fullerene-containing supramolecular polymer.

PubMed

Isla, Helena; Pérez, Emilio M; Martín, Nazario

2014-05-26

Supramolecular polymers based on dispersion forces typically show lower molecular weights (MW) than those based on hydrogen bonding or metal-ligand coordination. We present the synthesis and self-assembling properties of a monomer featuring two complementary units, a C60 derivative and an exTTF-based macrocycle, that interact mainly through π-π, charge-transfer, and van der Waals interactions. Thanks to the preorganization in the host part, a remarkable log K(a)=5.1±0.5 in CHCl3 at room temperature is determined for the host-guest couple. In accordance with the large binding constant, the monomer self-assembles in the gas phase, in solution, and in the solid state to form linear supramolecular polymers with a very high degree of polymerization. A MW above 150 kDa has been found experimentally in solution, while in the solid state the monomer forms extraordinarily long, straight, and uniform fibers with lengths reaching several microns. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Synthesis and characterization of zeolite from coal fly ash

NASA Astrophysics Data System (ADS)

Liu, Yong; Luo, Qiong; Wang, Guodong; Li, Xianlong; Na, Ping

2018-05-01

Fly ash (FA) from coal-based thermal power plant was used to synthesize zeolite in NaOH solution with hydrothermal method in this work. Firstly, the effects of calcination and acid treatment on the removal of impurities in fly ash were studied. Then based on the pretreated FA, the effects of alkali concentration, reaction temperature and Si/Al ratio on the synthesis of zeolite were studied in detail. The mineralogy, morphology, thermal behavior, infrared spectrum and specific surface for the synthetic sample were investigated. The results indicated that calcination at 750 °C for 1.5 h can basically remove unburned carbon from FA, and 4 M hydrochloric acid treatment of calcined FA at 90 °C for 2 h will reduce the quality of about 34.3%wt, which are mainly iron, calcium and sulfur elements. The concentration of NaOH, reaction temperature and Si/Al ratio have important effect on the synthesis of zeolite. In this study, 0.5 M NaOH cannot obtain any zeolite. High temperature is beneficial to zeolite synthesis from FA, but easily lead to a variety of zeolites. The synthetic sample contains three kinds of zeolites such as zeolite P, sodalite and zeolite X, when the reaction conditions are 2 M NaOH and 120 °C for 24 h. In this research, quartz always exists in the synthetic sample, but will reduce with the increase of temperature. The synthetic zeolite has the specific surface area of about 42 m2 g‑1 and better thermal stability.

Greener Route for Synthesis of aryl and alkyl-14H-dibenzo [a.j] xanthenes using Graphene Oxide-Copper Ferrite Nanocomposite as a Recyclable Heterogeneous Catalyst

NASA Astrophysics Data System (ADS)

Kumar, Aniket; Rout, Lipeeka; Achary, Lakkoji Satish Kumar; Dhaka, Rajendra. S.; Dash, Priyabrat

2017-02-01

A facile, efficient and environmentally-friendly protocol for the synthesis of xanthenes by graphene oxide based nanocomposite (GO-CuFe2O4) has been developed by one-pot condensation route. The nanocomposite was designed by decorating copper ferrite nanoparticles on graphene oxide (GO) surface via a solution combustion route without the use of template. The as-synthesized GO-CuFe2O4 composite was comprehensively characterized by XRD, FTIR, Raman, SEM, EDX, HRTEM with EDS mapping, XPS, N2 adsorption-desorption and ICP-OES techniques. This nanocomposite was then used in an operationally simple, cost effective, efficient and environmentally benign synthesis of 14H-dibenzo xanthene under solvent free condition. The present approach offers several advantages such as short reaction times, high yields, easy purification, a cleaner reaction, ease of recovery and reusability of the catalyst by a magnetic field. Based upon various controlled reaction results, a possible mechanism for xanthene synthesis over GO-CuFe2O4 catalyst was proposed. The superior catalytic activity of the GO-CuFe2O4 nanocomposite can be attributed to the synergistic interaction between GO and CuFe2O4 nanoparticles, high surface area and presence of small sized CuFe2O4 NPs. This versatile GO-CuFe2O4 nanocomposite synthesized via combustion method holds great promise for applications in wide range of industrially important catalytic reactions.

Single step synthesis and organization of gold colloids assisted by copolymer templates

NASA Astrophysics Data System (ADS)

Sarrazin, Aurélien; Gontier, Arthur; Plaud, Alexandre; Béal, Jérémie; Yockell-Lelièvre, Hélène; Bijeon, Jean-Louis; Plain, Jérôme; Adam, Pierre-Michel; Maurer, Thomas

2014-06-01

We report here an original single-step process for the synthesis and self-organization of gold colloids by simply incorporating gold salts into a solution prepared using polystyrene (PS)-polymethylmethacrylate copolymer and thiolated PS with propylene glycol methyl ether acetate as a solvent. The spin-coating and annealing of this solution then allows the formation of PS domains. Depending on the polymer concentration of the as-prepared solution, there can be either one or several gold nanoparticles (Au NPs) per PS domain. For high concentrations of Au NPs in PS domains, the coupling between plasmonic NPs leads to the observation of a second peak in the optical extinction spectrum. Such a collective effect could be relevant for the development of optical strain sensors in the near future.

Salt-assistant combustion synthesis of nanocrystalline Nd{sub 2}(Zr{sub 1-x}Sn{sub x}){sub 2}O{sub 7} (0 {<=} x {<=} 1) solid solutions

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

Tong Yuping, E-mail: huabeitong@yahoo.cn; Wang Yanping

2009-11-15

Nanocrystalline Nd{sub 2}(Zr{sub 1-x}Sn{sub x}){sub 2}O{sub 7} series solid solutions were prepared by a convenient salt-assisted combustion process using glycine as fuel. The samples were characterized by X-ray diffraction, Fourier transform infrared spectroscopy, Raman spectroscopy, transmission electron microscopy and high-resolution transmission electron microscopy. The results showed the Zr ion can be partially replaced by Sn ion. The partial substituted products were still single-phase solid solutions and the crystal form remained unchanged. TEM images reveal that the products are composed of well-dispersed square-shaped nanocrystals. The method provides a convenient and low-cost route for the synthesis of nanostructures of oxide materials.

Effect of mint solution concentration on the absorption spectra of silver nanoparticles in thulium ions presence

NASA Astrophysics Data System (ADS)

Rasmagin, S. I.; Krasovskii, V. I.; Apresyan, L. A.; Novikov, I. K.; Krystob, V. I.; Kazaryan, M. A.

2018-04-01

By the method of green synthesis, silver nanoparticles were obtained in colloidal solutions. The solutions were modified with thulium ions. Using the method of electron microscopy and optical method, the properties of silver nanoparticles obtained are studied. The influence of change in concentration of the solution of mint and thulium ions on the properties of colloidal silver nanoparticles was studied.

Precipitation method for barium metaborate (BaB2O4) synthesis from borax solution

NASA Astrophysics Data System (ADS)

Akşener, Eymen; Figen, Aysel Kantürk; Pişkin, Sabriye

2013-12-01

In this study, barium metaborate (BaB2O4, BMB) synthesis from the borax solution was carried out. BMB currently is used in production of ceramic glazes, luminophors, oxide cathodes as well as additives to pigments for aqueous emulsion paints and also β-BaB2O4 single crystals are the best candidate for fabrication of solid-state UV lasers operating at a wavelength of 200 nm due to excellent nonlinear optical properties. In the present study, synthesis was carried out from the borax solution (Na2B4O7ṡ10H2O, BDH) and barium chloride (BaCI2ṡ2H2O, Ba) in the glass-batch reactor with stirring. The effect of, times (5-15 min), molar ratio [stoich.ration (1.0:2.0), 1.25:2.0, 1.5:2.0, 2.5:2:0, 3.0:2.0, 3.5:2.0,4.0:2.0, 5.0:2.0] and also crystallization time (2-6 hour) on the BMB yield (%) was investigated at 80 °C reaction temperature. It is found that, BMB precipitation synthesis with 90 % yield can be performed from 0.50 molar ration (BDH:Ba), under 80 °C, 15 minute, and 6 hours crystallization time. The structural properties of BMB powders were characterized by using XRD, FT-IR and DTA-TG instrumental analysis technique.

A Cross-Lingual Mobile Medical Communication System Prototype for Foreigners and Subjects with Speech, Hearing, and Mental Disabilities Based on Pictograms

PubMed Central

Wołk, Agnieszka; Glinkowski, Wojciech

2017-01-01

People with speech, hearing, or mental impairment require special communication assistance, especially for medical purposes. Automatic solutions for speech recognition and voice synthesis from text are poor fits for communication in the medical domain because they are dependent on error-prone statistical models. Systems dependent on manual text input are insufficient. Recently introduced systems for automatic sign language recognition are dependent on statistical models as well as on image and gesture quality. Such systems remain in early development and are based mostly on minimal hand gestures unsuitable for medical purposes. Furthermore, solutions that rely on the Internet cannot be used after disasters that require humanitarian aid. We propose a high-speed, intuitive, Internet-free, voice-free, and text-free tool suited for emergency medical communication. Our solution is a pictogram-based application that provides easy communication for individuals who have speech or hearing impairment or mental health issues that impair communication, as well as foreigners who do not speak the local language. It provides support and clarification in communication by using intuitive icons and interactive symbols that are easy to use on a mobile device. Such pictogram-based communication can be quite effective and ultimately make people's lives happier, easier, and safer. PMID:29230254

A Cross-Lingual Mobile Medical Communication System Prototype for Foreigners and Subjects with Speech, Hearing, and Mental Disabilities Based on Pictograms.

PubMed

Wołk, Krzysztof; Wołk, Agnieszka; Glinkowski, Wojciech

2017-01-01

People with speech, hearing, or mental impairment require special communication assistance, especially for medical purposes. Automatic solutions for speech recognition and voice synthesis from text are poor fits for communication in the medical domain because they are dependent on error-prone statistical models. Systems dependent on manual text input are insufficient. Recently introduced systems for automatic sign language recognition are dependent on statistical models as well as on image and gesture quality. Such systems remain in early development and are based mostly on minimal hand gestures unsuitable for medical purposes. Furthermore, solutions that rely on the Internet cannot be used after disasters that require humanitarian aid. We propose a high-speed, intuitive, Internet-free, voice-free, and text-free tool suited for emergency medical communication. Our solution is a pictogram-based application that provides easy communication for individuals who have speech or hearing impairment or mental health issues that impair communication, as well as foreigners who do not speak the local language. It provides support and clarification in communication by using intuitive icons and interactive symbols that are easy to use on a mobile device. Such pictogram-based communication can be quite effective and ultimately make people's lives happier, easier, and safer.

Gas-phase synthesis of singly and multiply charged polyoxovanadate anions employing electrospray ionization and collision induced dissociation.

PubMed

Al Hasan, Naila M; Johnson, Grant E; Laskin, Julia

2013-09-01

Electrospray ionization mass spectrometry (ESI-MS) combined with in-source fragmentation and tandem mass spectrometry (MS/MS) experiments were used to generate a wide range of singly and multiply charged vanadium oxide cluster anions including VxOy(n-) and VxOyCl(n-) ions (x = 1-14, y = 2-36, n = 1-3), protonated clusters, and ligand-bound polyoxovanadate anions. The cluster anions were produced by electrospraying a solution of tetradecavanadate, V14O36Cl(L)5 (L = Et4N(+), tetraethylammonium), in acetonitrile. Under mild source conditions, ESI-MS generates a distribution of doubly and triply charged VxOyCl(n-) and VxOyCl(L)((n-1)-) clusters predominantly containing 14 vanadium atoms as well as their protonated analogs. Accurate mass measurement using a high-resolution LTQ/Orbitrap mass spectrometer (m/Δm = 60,000 at m/z 410) enabled unambiguous assignment of the elemental composition of the majority of peaks in the ESI-MS spectrum. In addition, high-sensitivity mass spectrometry allowed the charge state of the cluster ions to be assigned based on the separation of the major from the much less abundant minor isotope of vanadium. In-source fragmentation resulted in facile formation of smaller VxOyCl((1-2)-) and VxOy ((1-2)-) anions. Collision-induced dissociation (CID) experiments enabled systematic study of the gas-phase fragmentation pathways of the cluster anions originating from solution and from in-source CID. Surprisingly simple fragmentation patterns were obtained for all singly and doubly charged VxOyCl and VxOy species generated through multiple MS/MS experiments. In contrast, cluster anions originating directly from solution produced comparatively complex CID spectra. These results are consistent with the formation of more stable structures of VxOyCl and VxOy anions through low-energy CID. Furthermore, our results demonstrate that solution-phase synthesis of one precursor cluster anion combined with gas-phase CID is an efficient approach for the top-down synthesis of a wide range of singly and multiply charged gas-phase metal oxide cluster anions for subsequent investigations of structure and reactivity using mass spectrometry and ion spectroscopy techniques.

Gas-Phase Synthesis of Singly and Multiply Charged Polyoxovanadate Anions Employing Electrospray Ionization and Collision Induced Dissociation

NASA Astrophysics Data System (ADS)

Al Hasan, Naila M.; Johnson, Grant E.; Laskin, Julia

2013-09-01

Electrospray ionization mass spectrometry (ESI-MS) combined with in-source fragmentation and tandem mass spectrometry (MS/MS) experiments were used to generate a wide range of singly and multiply charged vanadium oxide cluster anions including VxOy n- and VxOyCln- ions (x = 1-14, y = 2-36, n = 1-3), protonated clusters, and ligand-bound polyoxovanadate anions. The cluster anions were produced by electrospraying a solution of tetradecavanadate, V14O36Cl(L)5 (L = Et4N+, tetraethylammonium), in acetonitrile. Under mild source conditions, ESI-MS generates a distribution of doubly and triply charged VxOyCln- and VxOyCl(L)(n-1)- clusters predominantly containing 14 vanadium atoms as well as their protonated analogs. Accurate mass measurement using a high-resolution LTQ/Orbitrap mass spectrometer (m/Δm = 60,000 at m/z 410) enabled unambiguous assignment of the elemental composition of the majority of peaks in the ESI-MS spectrum. In addition, high-sensitivity mass spectrometry allowed the charge state of the cluster ions to be assigned based on the separation of the major from the much less abundant minor isotope of vanadium. In-source fragmentation resulted in facile formation of smaller VxOyCl(1-2)- and VxOy (1-2)- anions. Collision-induced dissociation (CID) experiments enabled systematic study of the gas-phase fragmentation pathways of the cluster anions originating from solution and from in-source CID. Surprisingly simple fragmentation patterns were obtained for all singly and doubly charged VxOyCl and VxOy species generated through multiple MS/MS experiments. In contrast, cluster anions originating directly from solution produced comparatively complex CID spectra. These results are consistent with the formation of more stable structures of VxOyCl and VxOy anions through low-energy CID. Furthermore, our results demonstrate that solution-phase synthesis of one precursor cluster anion combined with gas-phase CID is an efficient approach for the top-down synthesis of a wide range of singly and multiply charged gas-phase metal oxide cluster anions for subsequent investigations of structure and reactivity using mass spectrometry and ion spectroscopy techniques.

Facile synthesis of stable superhydrophobic nanocomposite based on multi-walled carbon nanotubes

NASA Astrophysics Data System (ADS)

Mokarian, Zahra; Rasuli, Reza; Abedini, Yousefali

2016-04-01

A facile approach to fabricate a stable superhydrophobic composite comprising multi-walled carbon nanotubes and silicone rubber has been reported. Contact angle of de-ionized water droplets on the prepared surface was measured with the value of near 159°; while water droplets easily rolled off and bounced on it. Surface free energy of the superhydrophobic coating was examined by three methods about 26 mJ/m2. The prepared film shows good stability under high stress conditions such as ultraviolet exposure, heating, pencil hardness test, attacking with different pH value and ionic-strength solutions. In addition, remarkable stability of the coating was observed after soaking in condensed hydrochloric acid, 5 wt.% NaCl aqueous solution, boiling water and tape test.

Synthesis of porous Cu from Al-Cu-Co decagonal quasicrystalline alloys

NASA Astrophysics Data System (ADS)

Kalai Vani, V.; Kwon, O. J.; Hong, S. M.; Fleury, E.

2011-07-01

The formation of a porous Cu structure from cast Al-Cu-Co decagonal quasicrystalline alloys has been studied using a selective corrosion technique. Two alkaline solutions were selected based on the electrochemical properties of the constituent elements. Selective corrosion of Al and Co was achieved by chemical immersion of the cast Al-Cu-Co alloy in both 5 M NaOH and 0.5 M Na2CO3 solutions; values for BET surface-to-weight ratio of up to 30 m2/g could be reached. Microstructural analyses indicated that the architecture of the resulting porous structures was composed of a needle-type phase, remaining from the decagonal phase, in addition to Cu and Cu-Co phases.

A hybrid nonlinear programming method for design optimization

NASA Technical Reports Server (NTRS)

Rajan, S. D.

1986-01-01

Solutions to engineering design problems formulated as nonlinear programming (NLP) problems usually require the use of more than one optimization technique. Moreover, the interaction between the user (analysis/synthesis) program and the NLP system can lead to interface, scaling, or convergence problems. An NLP solution system is presented that seeks to solve these problems by providing a programming system to ease the user-system interface. A simple set of rules is used to select an optimization technique or to switch from one technique to another in an attempt to detect, diagnose, and solve some potential problems. Numerical examples involving finite element based optimal design of space trusses and rotor bearing systems are used to illustrate the applicability of the proposed methodology.

Niobium oxide synthesized via etching agent - assisted hydrothermal process: A films with low reflectance properties

NASA Astrophysics Data System (ADS)

Rani, Rozina Abdul; Zoolfakar, Ahmad Sabirin; Alrokayan, Salman; Khan, Haseeb; Rusop, M.

2018-05-01

In this paper, synthesis of the hydrothermal based etching process of niobium oxide (Nb2O5) films and their reflectance properties are presented. The concentration of etching agent, which is ammonium fluoride (NH4F) in the hydrothermal solution as well as the grain size and the annealing condition have significantly affected the reflectance properties of Nb2O5 films. Films that synthesized in 1.65M of NH4F solution showed the lowest percentage of reflectance value of 3.22% at 222 nm. The obtained reflectance results have shown that this kind of Nb2O5 films is very suitable for anti-reflective coating layer and UV sensor application.

Strategies to initiate and control the nucleation behavior of bimetallic nanoparticles.

PubMed

Krishnan, Gopi; de Graaf, Sytze; Ten Brink, Gert H; Persson, Per O Å; Kooi, Bart J; Palasantzas, George

2017-06-22

In this work we report strategies to nucleate bimetallic nanoparticles (NPs) made by gas phase synthesis of elements showing difficulty in homogeneous nucleation. It is shown that the nucleation assisted problem of bimetallic NP synthesis can be solved via the following pathways: (i) selecting an element which can itself nucleate and act as a nucleation center for the synthesis of bimetallic NPs; (ii) introducing H 2 or CH 4 as an impurity/trace gas to initiate nucleation during the synthesis of bimetallic NPs. The latter can solve the problem if none of the elements in a bimetallic NP can initiate nucleation. We illustrate the abovementioned strategies for the case of Mg based bimetallic NPs, which are interesting as hydrogen storage materials and exhibit both nucleation and oxidation issues even under ultra-high vacuum conditions. In particular, it is shown that adding H 2 in small proportions favors the formation of a solid solution/alloy structure even in the case of immiscible Mg and Ti, where normally phase separation occurs during synthesis. In addition, we illustrate the possibility of improving the nucleation rate, and controlling the structure and size distribution of bimetallic NPs using H 2 /CH 4 as a reactive/nucleating gas. This is shown to be associated with the dimer bond energies of the various formed species and the vapor pressures of the metals, which are key factors for NP nucleation.

Improvements in Block-Krylov Ritz Vectors and the Boundary Flexibility Method of Component Synthesis

NASA Technical Reports Server (NTRS)

Carney, Kelly Scott

1997-01-01

A method of dynamic substructuring is presented which utilizes a set of static Ritz vectors as a replacement for normal eigenvectors in component mode synthesis. This set of Ritz vectors is generated in a recurrence relationship, proposed by Wilson, which has the form of a block-Krylov subspace. The initial seed to the recurrence algorithm is based upon the boundary flexibility vectors of the component. Improvements have been made in the formulation of the initial seed to the Krylov sequence, through the use of block-filtering. A method to shift the Krylov sequence to create Ritz vectors that will represent the dynamic behavior of the component at target frequencies, the target frequency being determined by the applied forcing functions, has been developed. A method to terminate the Krylov sequence has also been developed. Various orthonormalization schemes have been developed and evaluated, including the Cholesky/QR method. Several auxiliary theorems and proofs which illustrate issues in component mode synthesis and loss of orthogonality in the Krylov sequence have also been presented. The resulting methodology is applicable to both fixed and free- interface boundary components, and results in a general component model appropriate for any type of dynamic analysis. The accuracy is found to be comparable to that of component synthesis based upon normal modes, using fewer generalized coordinates. In addition, the block-Krylov recurrence algorithm is a series of static solutions and so requires significantly less computation than solving the normal eigenspace problem. The requirement for less vectors to form the component, coupled with the lower computational expense of calculating these Ritz vectors, combine to create a method more efficient than traditional component mode synthesis.

[Quantitative determination of 7-phenoxyacetamidodesacetoxycephalosporanic acid].

PubMed

Dzegilenko, N B; Riabova, N M; Zinchenko, E Ia; Korchagin, V B

1976-11-01

7-Phenoxyacetamidodesacetoxycephalosporanic acid, an intermediate product in synthesis of cephalexin, was prepared by oxydation of phenoxymethylpenicillin into the respective sulphoxide and transformation of the latter. The UV-spectra of the reaction products were studied. A quantitative method is proposed for determination of 7-phenoxyacetamidodesacetoxycephalosporanic acid in the finished products based on estimation os the coefficient of specific extinction of the ethanol solutions at a wave length of 268 um in the UV-spectrum region in combination with semiquantitative estimation of the admixtures with the method of thin-layer chromatography.

Approximation algorithms for the min-power symmetric connectivity problem

NASA Astrophysics Data System (ADS)

Plotnikov, Roman; Erzin, Adil; Mladenovic, Nenad

2016-10-01

We consider the NP-hard problem of synthesis of optimal spanning communication subgraph in a given arbitrary simple edge-weighted graph. This problem occurs in the wireless networks while minimizing the total transmission power consumptions. We propose several new heuristics based on the variable neighborhood search metaheuristic for the approximation solution of the problem. We have performed a numerical experiment where all proposed algorithms have been executed on the randomly generated test samples. For these instances, on average, our algorithms outperform the previously known heuristics.

Synthesis and studies of polypeptide materials: Enantioselective polymerization of gamma-benzyl glutamate-N-carboxyanhydride and synthesis of optically active poly(beta-peptides)

NASA Astrophysics Data System (ADS)

Cheng, Jianjun

A class of zero-valent transition metal complexes have been developed by Deming et al for the controlled polymerization of alpha-aminoacid-N-carboxyanhydrides (alpha-NCAs). This discovery provided a superior starting point for the development of enantioselective polymerizations of racemic alpha-NCAs. Bidentate chiral ligands were synthesized and tested for their abilities to induce enantioselective polymerization of gamma-benzyl-glutamate NCA (Glu NCA) when they were coordinated to zero-valent nickel complexes. When optically active 2-pyridinyl oxazoline ligands were mixed with bis(1,5-cyclooctadiene)nickel in THF, chiral nickel complexes were formed that selectively polymerized one enantiomer of Glu NCA over the other. The highest selectivity was observed with the nickel complex of (S)-4-tert-butyl-2-pyridinyl oxazoline, which gave a ratio of enantiomeric polymerization rate constants (kD/kL) of 5.2. It was found that subtle modification of this ligand by incorporation of additional substituents had a substantial impact on initiator enantioselectivities. In separate efforts, methodology was developed for the general synthesis of optically active beta-aminoacid-N-carboxyanhydrides (beta-NCAs) via cyclization of Nbeta-Boc- or Nbeta-Cbz-beta-amino acids using phosphorus tribromide. The beta-NCA molecules could be polymerized in good yields using strong bases or transition metal complexes to give optically active poly(beta-peptides) bearing proteinogenic side chains. The resulting poly(beta-peptides), which have moderate molecular weights, adopt stable helical conformations in solution. Poly(beta-homoglutamate and poly(beta-homolysine), the side-chain deprotected polymers, were found to display pH dependent helix-coil conformation transitions in aqueous solution, similar to their alpha-analogs. A novel method for poly(beta-aspartate) synthesis was developed via the polymerization of L-aspartate alkyl ester beta lactams using metal-amido complexes. Poly(beta-aspartates) bearing short ethylene glycol side chains were obtained with controlled molecular weights and narrow molecular weight distributions when Sc(N(TMS)2)3 was used as initiator for the beta-lactam polymerizations. Polymer chain lengths could be controlled by both stoichiometry and monomer conversion, characteristic of a living polymerization system. Di- and tri-block copoly(beta-peptides) with desired chain lengths were also synthesized using this method. It was found that these techniques were generally applicable for the synthesis of poly(beta-peptides), bearing other proteinogetic side chains. Synthesis and studies of polypeptide materials were extended to unexplored areas by incorporation of both alpha- and beta-amino acid residues into single polymer chains. Two sequence specific polypeptides bearing alternating beta-alpha, or beta-alpha-alpha amino acid residues were synthesized. Both polymers were found to adopt unprecedented stable conformations in solution.

GAP Peptide Synthesis via Design of New GAP Protecting Group: An Fmoc/tBu Synthesis of Thymopentin Free from Polymers, Chromatography and Recrystallization

PubMed Central

Seifert, Cole W.; Paniagua, Armando; White, Gabrielle A.; Cai, Lucy

2016-01-01

A novel method for Fmoc/tBu solution-phase peptide synthesis and the development of a new benzyl-type GAP protecting group is reported. This new GAP protecting group is utilized in place of a polymer support, facilitating C→N Fmoc peptide synthesis without chromatography, recrystallization, or polymer supports. The GAP group can be added and removed in high yield, and was used to synthesize over 1 gram of the immunostimulant, thymopentin, in high overall yield (83%) and purity (99%). PMID:28663711

The solusphere-its inferences and study

USGS Publications Warehouse

Rainwater, F.H.; White, W.F.

1958-01-01

Water is a fundamental geologic agent active in rock decomposition, erosion, and synthesis. Solutes in water are of particular interest to geochemists as sources of raw material for synthesis or as products of decomposition. When geochemical studies move from the laboratory into natural environment many variables relating to solute hydrology must be considered. As a focal point there has been designed a graphical representation of solute hydrology, the solusphere, which embodies the concepts of land-water occurrence and movement on which are superimposed geologic, biologic, physical, chemical, and cultural processes affecting solutes. The solusphere is demonstrated by passing an imaginary plane through the centre of the earth. This plane intercepts concentric zones designated as rock flowage, saturation, aeration, surface activity, and atmosphere. Transport processes carry solutes within and between zones without alteration or conversion. However, whether stationary or in motion, the water's solute character is constantly subject to (1) alteration processes that change concentration by addition or subtraction of solutes or solvent without loss of solute identities, and (2) conversion processes that change the chemical state and form of solutes. The geochemist is concerned with specific conversion processes, but he also must consider transport, alteration, and other conversion processes that are continually modifying the materials with which he is dealing in nature. The solusphere is an attempt to organize processes affecting the chemical quality of land waters into a unified field of science much like the field of marine chemistry. ?? 1958.

alpha-DNA II. Synthesis of unnatural alpha-anomeric oligodeoxyribonucleotides containing the four usual bases and study of their substrate activities for nucleases.

PubMed Central

Morvan, F; Rayner, B; Imbach, J L; Thenet, S; Bertrand, J R; Paoletti, J; Malvy, C; Paoletti, C

1987-01-01

This paper describes for the first time the synthesis of alpha-oligonucleotides containing the four usual bases. Two unnatural hexadeoxyribonucleotides: alpha-[d(CpApTpGpCpG)] and alpha-[d(CpGpCpApTpG)], consisting only of alpha-anomeric nucleotide units, were obtained by an improved phosphotriester method, in solution. Starting material was the four base-protected alpha-deoxyribonucleosides 3a-d. Pyrimidine alpha-deoxynucleosides 3a and 3b were prepared by self-anomerization reactions followed by selective deprotection of sugar hydroxyles, while the two purine alpha-deoxynucleosides 3c and 3d were prepared by glycosylation reactions. In the case of guanine alpha-nucleoside derivative a supplementary base-protecting group: N,N-diphenylcarbamoyl was introduced on O6-position in order to avoid side-reactions during oligonucleotide assembling. The hexadeoxynucleotide alpha-[d(CpApTpGpCpG)] was tested as substrate of selected endo- and exonucleases. In conditions where the natural corresponding beta-hexamer was completely degradated by nuclease S1 and calf spleen phosphodiesterase, the alpha-oligonucleotide remained almost intact. PMID:3575096

BULK SYNTHESIS OF SILVER NANORODS IN POLY(ETHYLENE GLYCOL) USING MICROWAVE IRRADIATION

EPA Science Inventory

Microwave-assisted (MW), surfactantless, greener approach to bulk synthesis of silver nanorods employing poly (ethylene glycol) (PEG) is described. An aqueous solution of silver nitrate (AgNO-3,- 0.1 M, 4 mL) and 4 mL of PEG (molecular weight 300) were mixed at room temperature t...

A rapid room temperature chemical route for the synthesis of graphene: metal-mediated reduction of graphene oxide.

PubMed

Dey, Ramendra Sundar; Hajra, Saumen; Sahu, Ranjan K; Raj, C Retna; Panigrahi, M K

2012-02-07

A rapid and facile route for the synthesis of reduced graphene oxide sheets (rGOs) at room temperature by the chemical reduction of graphene oxide using Zn/acid in aqueous solution is demonstrated. This journal is © The Royal Society of Chemistry 2012

An efficient microwave-assisted synthesis method for the production of water soluble amine-terminated Si nanoparticles.

PubMed

Atkins, Tonya M; Louie, Angelique Y; Kauzlarich, Susan M

2012-07-27

Silicon nanoparticles can be considered a green material, especially when prepared via a microwave-assisted method without the use of highly reactive reducing agents or hydrofluoric acid. A simple solution synthesis of hydrogen-terminated Si- and Mn-doped Si nanoparticles via microwave-assisted synthesis is demonstrated. The reaction of the Zintl salt, Na(4)Si(4), or Mn-doped Na(4)Si(4), Na(4)Si(4(Mn)), with ammonium bromide, NH(4)Br, produces small dispersible nanoparticles along with larger particles that precipitate. Allylamine and 1-amino-10-undecene were reacted with the hydrogen-terminated Si nanoparticles to provide water solubility and stability. A one-pot, single-reaction process and a one-pot, two-step reaction process were investigated. Details of the microwave-assisted process are provided, with the optimal synthesis being the one-pot, two-step reaction procedure and a total time of about 15 min. The nanoparticles were characterized by transmission electron microscopy (TEM), x-ray diffraction, and fluorescence spectroscopies. The microwave-assisted method reliably produces a narrow size distribution of Si nanoparticles in solution.

A comparative study of the properties of five-layered Aurivillius oxides A2Bi4Ti5O18 (A = Ba, Pb, and Sr) synthesized by different wet chemical routes

NASA Astrophysics Data System (ADS)

Dubey, Shivangi; Subohi, Oroosa; Kurchania, Rajnish

2018-07-01

This paper reports the detailed study of the effect of different wet chemical synthesis routes (solution combustion, co-precipitation, and sol-gel route) on the microstructure, phase formation, dielectric, electrical, and ferroelectric properties of five-layered Aurivillius oxides: A2Bi4Ti5O18 (A = Ba, Pb, and Sr). Different synthesis parameters like the precursors used, synthesis temperature, and reaction time affects the morphology of the ceramics. Microstructure in turn influences the dielectric and ferroelectric properties. It was observed that the sol-gel-synthesized ceramics possess higher dielectric constant and remanent polarization, low dielectric loss due to lower conductivity in these samples as a result of higher density in these compounds as compared to those synthesized by other wet chemical synthesis routes such as solution combustion route and co-precipitation technique. The XRD data are used for phase analysis and surface morphology is studied using SEM images. Dielectric and electrical properties are investigated as a function of frequency and temperature.

Solution combustion synthesis of metal oxide nanomaterials for energy storage and conversion.

PubMed

Li, Fa-tang; Ran, Jingrun; Jaroniec, Mietek; Qiao, Shi Zhang

2015-11-14

The design and synthesis of metal oxide nanomaterials is one of the key steps for achieving highly efficient energy conversion and storage on an industrial scale. Solution combustion synthesis (SCS) is a time- and energy-saving method as compared with other routes, especially for the preparation of complex oxides which can be easily adapted for scale-up applications. This review summarizes the synthesis of various metal oxide nanomaterials and their applications for energy conversion and storage, including lithium-ion batteries, supercapacitors, hydrogen and methane production, fuel cells and solar cells. In particular, some novel concepts such as reverse support combustion, self-combustion of ionic liquids, and creation of oxygen vacancies are presented. SCS has some unique advantages such as its capability for in situ doping of oxides and construction of heterojunctions. The well-developed porosity and large specific surface area caused by gas evolution during the combustion process endow the resulting materials with exceptional properties. The relationship between the structural properties of the metal oxides studied and their performance is discussed. Finally, the conclusions and perspectives are briefly presented.

Solution combustion synthesis of metal oxide nanomaterials for energy storage and conversion

NASA Astrophysics Data System (ADS)

Li, Fa-Tang; Ran, Jingrun; Jaroniec, Mietek; Qiao, Shi Zhang

2015-10-01

The design and synthesis of metal oxide nanomaterials is one of the key steps for achieving highly efficient energy conversion and storage on an industrial scale. Solution combustion synthesis (SCS) is a time- and energy-saving method as compared with other routes, especially for the preparation of complex oxides which can be easily adapted for scale-up applications. This review summarizes the synthesis of various metal oxide nanomaterials and their applications for energy conversion and storage, including lithium-ion batteries, supercapacitors, hydrogen and methane production, fuel cells and solar cells. In particular, some novel concepts such as reverse support combustion, self-combustion of ionic liquids, and creation of oxygen vacancies are presented. SCS has some unique advantages such as its capability for in situ doping of oxides and construction of heterojunctions. The well-developed porosity and large specific surface area caused by gas evolution during the combustion process endow the resulting materials with exceptional properties. The relationship between the structural properties of the metal oxides studied and their performance is discussed. Finally, the conclusions and perspectives are briefly presented.

Synthesis of Silver Nanoparticles from Microbial Source-A Green Synthesis Approach, and Evaluation of its Antimicrobial Activity against Escherichia coli

NASA Astrophysics Data System (ADS)

Behera, S. S.; Jha, S.; Arakha, M.; Panigrahi, T. K.

2012-03-01

TRACT Nanoparticles synthesis by biological methods using various microorganisms, plants, and plant extracts and enzymes have attracted a great attention as these are cost effective, nontoxic, eco-friendly and an alternative to physical and chemical methods. In this research, Silver nanoparticles (Ag-NPs) were synthesized from AgNO3 solution by green synthesis process with the assistance of microbial source only. The detailed characterization of the Ag NPs were carried out using UV-visible spectroscopy, Scanning electron microscopy (SEM), Energy dispersive X-ray Spectroscopy (EDS), Dynamic light scattering (DLS) analysis, and their antimicrobial evaluation was done against Escherichia coli. The UV-visible spectroscopy analysis showed the surface plasmon resonance property of nanoparticles. The DLS analysis showed the particle distribution of synthesized silver nanoparticles in solution, and SEM analysis showed the morphology of nanoparticles. The elemental composition of synthesized sample was confirmed by EDS analysis. Antibacterial assay of synthesized Ag NP was carried out in solid (Nutrient Agar) growth medium against E.coli. The presence of zone of inhibition clearly indicated the antibacterial activity of silver nanoparticles.

Gold nanocrystals with DNA-directed morphologies.

PubMed

Ma, Xingyi; Huh, June; Park, Wounjhang; Lee, Luke P; Kwon, Young Jik; Sim, Sang Jun

2016-09-16

Precise control over the structure of metal nanomaterials is important for developing advanced nanobiotechnology. Assembly methods of nanoparticles into structured blocks have been widely demonstrated recently. However, synthesis of nanocrystals with controlled, three-dimensional structures remains challenging. Here we show a directed crystallization of gold by a single DNA molecular regulator in a sequence-independent manner and its applications in three-dimensional topological controls of crystalline nanostructures. We anchor DNA onto gold nanoseed with various alignments to form gold nanocrystals with defined topologies. Some topologies are asymmetric including pushpin-, star- and biconcave disk-like structures, as well as more complex jellyfish- and flower-like structures. The approach of employing DNA enables the solution-based synthesis of nanocrystals with controlled, three-dimensional structures in a desired direction, and expands the current tools available for designing and synthesizing feature-rich nanomaterials for future translational biotechnology.

Gold nanocrystals with DNA-directed morphologies

NASA Astrophysics Data System (ADS)

Ma, Xingyi; Huh, June; Park, Wounjhang; Lee, Luke P.; Kwon, Young Jik; Sim, Sang Jun

2016-09-01

Precise control over the structure of metal nanomaterials is important for developing advanced nanobiotechnology. Assembly methods of nanoparticles into structured blocks have been widely demonstrated recently. However, synthesis of nanocrystals with controlled, three-dimensional structures remains challenging. Here we show a directed crystallization of gold by a single DNA molecular regulator in a sequence-independent manner and its applications in three-dimensional topological controls of crystalline nanostructures. We anchor DNA onto gold nanoseed with various alignments to form gold nanocrystals with defined topologies. Some topologies are asymmetric including pushpin-, star- and biconcave disk-like structures, as well as more complex jellyfish- and flower-like structures. The approach of employing DNA enables the solution-based synthesis of nanocrystals with controlled, three-dimensional structures in a desired direction, and expands the current tools available for designing and synthesizing feature-rich nanomaterials for future translational biotechnology.

The Role of Ontologies in Schema-based Program Synthesis

NASA Technical Reports Server (NTRS)

Bures, Tomas; Denney, Ewen; Fischer, Bernd; Nistor, Eugen C.

2004-01-01

Program synthesis is the process of automatically deriving executable code from (non-executable) high-level specifications. It is more flexible and powerful than conventional code generation techniques that simply translate algorithmic specifications into lower-level code or only create code skeletons from structural specifications (such as UML class diagrams). Key to building a successful synthesis system is specializing to an appropriate application domain. The AUTOBAYES and AUTOFILTER systems, under development at NASA Ames, operate in the two domains of data analysis and state estimation, respectively. The central concept of both systems is the schema, a representation of reusable computational knowledge. This can take various forms, including high-level algorithm templates, code optimizations, datatype refinements, or architectural information. A schema also contains applicability conditions that are used to determine when it can be applied safely. These conditions can refer to the initial specification, to intermediate results, or to elements of the partially-instantiated code. Schema-based synthesis uses AI technology to recursively apply schemas to gradually refine a specification into executable code. This process proceeds in two main phases. A front-end gradually transforms the problem specification into a program represented in an abstract intermediate code. A backend then compiles this further down into a concrete target programming language of choice. A core engine applies schemas on the initial problem specification, then uses the output of those schemas as the input for other schemas, until the full implementation is generated. Since there might be different schemas that implement different solutions to the same problem this process can generate an entire solution tree. AUTOBAYES and AUTOFILTER have reached the level of maturity where they enable users to solve interesting application problems, e.g., the analysis of Hubble Space Telescope images. They are large (in total around 100kLoC Prolog), knowledge intensive systems that employ complex symbolic reasoning to generate a wide range of non-trivial programs for complex application do- mains. Their schemas can have complex interactions, which make it hard to change them in isolation or even understand what an existing schema actually does. Adding more capabilities by increasing the number of schemas will only worsen this situation, ultimately leading to the entropy death of the synthesis system. The root came of this problem is that the domain knowledge is scattered throughout the entire system and only represented implicitly in the schema implementations. In our current work, we are addressing this problem by making explicit the knowledge from Merent parts of the synthesis system. Here; we discuss how Gruber's definition of an ontology as an explicit specification of a conceptualization matches our efforts in identifying and explicating the domain-specific concepts. We outline the dual role ontologies play in schema-based synthesis and argue that they address different audiences and serve different purposes. Their first role is descriptive: they serve as explicit documentation, and help to understand the internal structure of the system. Their second role is prescriptive: they provide the formal basis against which the other parts of the system (e.g., schemas) can be checked. Their final role is referential: ontologies also provide semantically meaningful "hooks" which allow schemas and tools to access the internal state of the program derivation process (e.g., fragments of the generated code) in domain-specific rather than language-specific terms, and thus to modify it in a controlled fashion. For discussion purposes we use AUTOLINEAR, a small synthesis system we are currently experimenting with, which can generate code for solving a system of linear equations, Az = b.

Synthesis of highly elastic biocompatible polyurethanes based on bio-based isosorbide and poly(tetramethylene glycol) and their properties.

PubMed

Kim, Hyo-Jin; Kang, Min-Sil; Knowles, Jonathan C; Gong, Myoung-Seon

2014-09-01

Bio-based high elastic polyurethanes were prepared from hexamethylene diisocyanate and various ratios of isosorbide to poly(tetramethylene glycol) as a diol by a simple one-shot bulk polymerization without a catalyst. Successful synthesis of the polyurethanes was confirmed by Fourier transform-infrared spectroscopy and (1)H nuclear magnetic resonance. Thermal properties were determined by differential scanning calorimetry and thermogravimetric analysis. The glass transition temperature was -47.8℃. The test results showed that the poly(tetramethylene glycol)/isosorbide-based elastomer exhibited not only excellent stress-strain properties but also superior resilience to the existing polyether-based polyurethane elastomers. The static and dynamic properties of the polyether/isosorbide-based thermoplastic elastomer were more suitable for dynamic applications. Moreover, such rigid diols impart biocompatible and bioactive properties to thermoplastic polyurethane elastomers. Degradation tests performed at 37℃ in phosphate buffer solution showed a mass loss of 4-9% after 8 weeks, except for the polyurethane with the lowest isosorbide content, which showed an initial rapid weight loss. These polyurethanes offer significant promise due to soft, flexible and biocompatible properties for soft tissue augmentation and regeneration. © The Author(s) 2014 Reprints and permissions: sagepub.co.uk/journalsPermissions.nav.

Green Synthesis of Silver Nanoparticles using Extract of Pinus merkusii Jungh & De Vriese Cone Flower

NASA Astrophysics Data System (ADS)

Azkiya, N. I.; Masruri, M.; Ulfa, S. M.

2018-01-01

The paper studies recent application of cone flower waste from Pinus merkusii Jungh & De Vriese for an environmentally unclear method for synthesis silver nanoparticle. Phytochemical characterization using iron trichloride solution showed the extract of Pinus merkusii cone flower contains of phenolic group of secondary metabolite. This group acts as both reducing and stabilizing agents. For the synthesis of silver nanoparticle, solution of silver nitrate is added to the extract at 60°C. The effect of extract concentration (5-20%) and time reaction (15-60 min) is investigated. The formation of silver nanoparticle is confirmed by the color change from yellowish to brown. Meanwhile, UV-Vis characterization of silver nanoparticle in extract 20% and 60 min reaction showed surface plasmon resonance (SPR) at 431 nm, and transmission electron microscope (TEM) revealed the particle size range in between 8 and 23 nm with a spherical in shape.

Solution-phase synthesis of nanomaterials at low temperature

NASA Astrophysics Data System (ADS)

Zhu, Yongchun; Qian, Yitai

2009-01-01

This paper reviews the solution-phase synthesis of nanoparticles via some routes at low temperatures, such as room temperature route, wave-assisted synthesis (γ-irradiation route and sonochemical route), directly heating at low temperatures, and hydrothermal/solvothermal methods. A number of strategies were developed to control the shape, the size, as well as the dispersion of nanostructures. Using diethylamine or n-butylamine as solvent, semiconductor nanorods were yielded. By the hydrothermal treatment of amorphous colloids, Bi2S3 nanorods and Se nanowires were obtained. CdS nanowires were prepared in the presence of polyacrylamide. ZnS nanowires were obtained using liquid crystal. The polymer poly (vinyl acetate) tubule acted as both nanoreactor and template for the CdSe nanowire growth. Assisted by the surfactant of sodium dodecyl benzenesulfonate (SDBS), nickel nanobelts were synthesized. In addition, Ag nanowires, Te nanotubes and ZnO nanorod arrays could be prepared without adding any additives or templates.

Sparse Image Reconstruction on the Sphere: Analysis and Synthesis.

PubMed

Wallis, Christopher G R; Wiaux, Yves; McEwen, Jason D

2017-11-01

We develop techniques to solve ill-posed inverse problems on the sphere by sparse regularization, exploiting sparsity in both axisymmetric and directional scale-discretized wavelet space. Denoising, inpainting, and deconvolution problems and combinations thereof, are considered as examples. Inverse problems are solved in both the analysis and synthesis settings, with a number of different sampling schemes. The most effective approach is that with the most restricted solution-space, which depends on the interplay between the adopted sampling scheme, the selection of the analysis/synthesis problem, and any weighting of the l 1 norm appearing in the regularization problem. More efficient sampling schemes on the sphere improve reconstruction fidelity by restricting the solution-space and also by improving sparsity in wavelet space. We apply the technique to denoise Planck 353-GHz observations, improving the ability to extract the structure of Galactic dust emission, which is important for studying Galactic magnetism.

Size controlled hydroxyapatite and calcium carbonate particles: synthesis and their application as templates for SERS platform.

PubMed

Parakhonskiy, B V; Svenskaya, Yu I; Yashchenok, A М; Fattah, H A; Inozemtseva, O A; Tessarolo, F; Antolini, R; Gorin, D A

2014-06-01

An elegant route for hydroxyapatite (HA) particle synthesis via ionic exchange reaction is reported. Calcium carbonate particles (CaCO3) were recrystallized into HA beads in water solution with phosphate ions. The size of initial CaCO3 particles was controlled upon the synthesis by varying the amount of ethylene glycol (EG) in aqueous solution. The average size of HA beads ranged from 0.6±0.1 to 4.3±1.1μm. Silver nanoparticles were deposited on the surface of HA and CaCO3 particles via silver mirror reaction. Surface enhanced Raman scattering of silver functionalized beads was demonstrated by detecting Rhodamine B. CaCO3 and HA particles have a great potential for design of carrier which can provide diagnostic and therapeutic functions. Copyright © 2014 Elsevier B.V. All rights reserved.

Efficient One-Pot Synthesis of Colloidal Zirconium Oxide Nanoparticles for High-Refractive-Index Nanocomposites.

PubMed

Liu, Chao; Hajagos, Tibor Jacob; Chen, Dustin; Chen, Yi; Kishpaugh, David; Pei, Qibing

2016-02-01

Zirconium oxide nanoparticles are promising candidates for optical engineering, photocatalysis, and high-κ dielectrics. However, reported synthetic methods for the colloidal zirconium oxide nanoparticles use unstable alkoxide precursors and have various other drawbacks, limiting their wide application. Here, we report a facile one-pot method for the synthesis of colloidally stable zirconium oxide nanoparticles. Using a simple solution of zirconium trifluoroacetate in oleylamine, highly stable zirconium oxide nanoparticles have been synthesized with high yield, following a proposed amidization-assisted sol-gel mechanism. The nanoparticles can be readily dispersed in nonpolar solvents, forming a long-term stable transparent solution, which can be further used to fabricate high-refractive-index nanocomposites in both monolith and thin-film forms. In addition, the same method has also been extended to the synthesis of titanium oxide nanoparticles, demonstrating its general applicability to all group IVB metal oxide nanoparticles.

Facile and one-pot solution synthesis of several kinds of 3D hierarchical flower-like α-Bi2O3 microspheres

NASA Astrophysics Data System (ADS)

Wang, Yajun; Li, Zexue; Yu, Haiyang; Feng, Changgen

2016-09-01

Several kinds of three-dimensional (3D) hierarchical constructed flower-like α-Bi2O3 microspheres were prepared successfully via a simple solution precipitation synthesis at 95∘C and ambient atmospheric pressure in 1h. The synthesis process was operated in ethanol-water system as solvent with the assistance of glycerin and oleic acid as capping agents. These flower-like α-Bi2O3 architectures with diameter of several micrometers were 3D self-assembled from nanorods or nanocubes step by step. By adjusting the concentration of the capping agents, various flower-like α-Bi2O3 microspheres were obtained. The formation of the flower-like superstructures was attributed to the modification of nucleation and growth kinetics, and the guidance of self-assembly approach by capping agents. The formation mechanism of these microstructures was discussed briefly.

Application of chiral critical clusters to assymetric synthesis

DOEpatents

Ferrieri, Richard A.

2002-01-01

Disclosed is a composition, a method of making and a method of using critical clusters for asymmetric synthesis using substantially optically-pure chiral solvent molecules in a supercritical fluid. The solvent molecules are capable of forming a multipoint hydrogen bonded solvate as they encage at least one solute molecule. The encaged solute molecule is capable of reacting to form an optically active chiral center. In another aspect, there is disclosed a method of directing the position of bonding between a solute molecule and a ligand involving encaging the solute molecule and the ligand with polar solvent molecules in a supercritical fluid under conditions of temperature and pressure sufficient to change electric charge distribution in the solute molecule. In yet another aspect, disclosed is a method of making pharmaceutical compounds involving encaging a solute molecule, which is capable of forming a chiral center, and a ligand with polar solvent molecules in a supercritical fluid under conditions of temperature and pressure sufficient to change electric charge distribution of the solute molecule. The solute molecule and ligand are then reacted whereby the ligand bonds to the solute molecule forming a chiral center. Also disclosed is a method for racemic resolution using critical clusters involving encaging racemic mixtures of solute molecules with substantially optically-pure chiral solvent molecules in a supercritical fluid under conditions of temperature and pressure sufficient to form critical clusters. The solvent molecules are capable of multipoint hydrogen bonding with the solute molecules. The encaged solute molecules are then nonenzymatically reacted to enhance the optical purity of the solute molecules.

Synthesis and characterization of ion containing polymers

NASA Astrophysics Data System (ADS)

Dou, Shichen

Two types of ion-containing polymers are included in this dissertation. The first was focused on the rheology, solvation, and correlation length of polyelectrolyte solutions in terms of charge density, solvent dielectric constant, and solvent quality. The second was focused on the PEO-based polyester ionomers as single ion conductors. A series of polyelectrolytes with varied charge density (0.03 < alpha < 0.6) and counterions (Cl- and I-) were investigated in good solvent (EG, NMF, and GC) and poor solvent (DW and F). The concentration dependence of the specific viscosity and relaxation time of polyelectrolytes in solution agrees with Dobrynin's theoretical predictions at c < c**. Effective charge density greatly impacts the viscosity of polyelectrolyte semidilute solutions, while residual salt significantly reduces the viscosity of polyelectrolyte solutions at concentrations c < 2cs/f. For polyelectrolyte solutions with less condensed counterions, the correlation length obtained from SAXS and rheology perfectly matches and agrees with de Gennes prediction. Dobrynin scaling model successfully predicts the rheology of polyelectrolyte solutions in all cases: without salt, with low residual salt, and with high residual salt concentration. PEO-based polyester ionomers were synthesized by melt polycondensation. Mn was determined using the 1H NMR of ionomers. No ion-cluster was observed from the DSC, SAXS, and rheology measurements. Ionic conductivity greatly depends on the Tg, T-T g and ion content of the ionomers. PEG600-PTMO650 (z)-Li copolyester ionomers show microphase separation and much lower ionic conductivity, compared to that of PE600-Li. PTMO650-Li shows nonconductor behavior.

Mutation Testing for Effective Verification of Digital Components of Physical Systems

NASA Astrophysics Data System (ADS)

Kushik, N. G.; Evtushenko, N. V.; Torgaev, S. N.

2015-12-01

Digital components of modern physical systems are often designed applying circuitry solutions based on the field programmable gate array technology (FPGA). Such (embedded) digital components should be carefully tested. In this paper, an approach for the verification of digital physical system components based on mutation testing is proposed. The reference description of the behavior of a digital component in the hardware description language (HDL) is mutated by introducing into it the most probable errors and, unlike mutants in high-level programming languages, the corresponding test case is effectively derived based on a comparison of special scalable representations of the specification and the constructed mutant using various logic synthesis and verification systems.

Kinematic synthesis of adjustable robotic mechanisms

NASA Astrophysics Data System (ADS)

Chuenchom, Thatchai

1993-01-01

Conventional hard automation, such as a linkage-based or a cam-driven system, provides high speed capability and repeatability but not the flexibility required in many industrial applications. The conventional mechanisms, that are typically single-degree-of-freedom systems, are being increasingly replaced by multi-degree-of-freedom multi-actuators driven by logic controllers. Although this new trend in sophistication provides greatly enhanced flexibility, there are many instances where the flexibility needs are exaggerated and the associated complexity is unnecessary. Traditional mechanism-based hard automation, on the other hand, neither can fulfill multi-task requirements nor are cost-effective mainly due to lack of methods and tools to design-in flexibility. This dissertation attempts to bridge this technological gap by developing Adjustable Robotic Mechanisms (ARM's) or 'programmable mechanisms' as a middle ground between high speed hard automation and expensive serial jointed-arm robots. This research introduces the concept of adjustable robotic mechanisms towards cost-effective manufacturing automation. A generalized analytical synthesis technique has been developed to support the computational design of ARM's that lays the theoretical foundation for synthesis of adjustable mechanisms. The synthesis method developed in this dissertation, called generalized adjustable dyad and triad synthesis, advances the well-known Burmester theory in kinematics to a new level. While this method provides planar solutions, a novel patented scheme is utilized for converting prescribed three-dimensional motion specifications into sets of planar projections. This provides an analytical and a computational tool for designing adjustable mechanisms that satisfy multiple sets of three-dimensional motion specifications. Several design issues were addressed, including adjustable parameter identification, branching defect, and mechanical errors. An efficient mathematical scheme for identification of adjustable member was also developed. The analytical synthesis techniques developed in this dissertation were successfully implemented in a graphic-intensive user-friendly computer program. A physical prototype of a general purpose adjustable robotic mechanism has been constructed to serve as a proof-of-concept model.

Rapid One-step Enzymatic Synthesis and All-aqueous Purification of Trehalose Analogues.

PubMed

Meints, Lisa M; Poston, Anne W; Piligian, Brent F; Olson, Claire D; Badger, Katherine S; Woodruff, Peter J; Swarts, Benjamin M

2017-02-17

Chemically modified versions of trehalose, or trehalose analogues, have applications in biology, biotechnology, and pharmaceutical science, among other fields. For instance, trehalose analogues bearing detectable tags have been used to detect Mycobacterium tuberculosis and may have applications as tuberculosis diagnostic imaging agents. Hydrolytically stable versions of trehalose are also being pursued due to their potential for use as non-caloric sweeteners and bioprotective agents. Despite the appeal of this class of compounds for various applications, their potential remains unfulfilled due to the lack of a robust route for their production. Here, we report a detailed protocol for the rapid and efficient one-step biocatalytic synthesis of trehalose analogues that bypasses the problems associated with chemical synthesis. By utilizing the thermostable trehalose synthase (TreT) enzyme from Thermoproteus tenax, trehalose analogues can be generated in a single step from glucose analogues and uridine diphosphate glucose in high yield (up to quantitative conversion) in 15-60 min. A simple and rapid non-chromatographic purification protocol, which consists of spin dialysis and ion exchange, can deliver many trehalose analogues of known concentration in aqueous solution in as little as 45 min. In cases where unreacted glucose analogue still remains, chromatographic purification of the trehalose analogue product can be performed. Overall, this method provides a "green" biocatalytic platform for the expedited synthesis and purification of trehalose analogues that is efficient and accessible to non-chemists. To exemplify the applicability of this method, we describe a protocol for the synthesis, all-aqueous purification, and administration of a trehalose-based click chemistry probe to mycobacteria, all of which took less than 1 hour and enabled fluorescence detection of mycobacteria. In the future, we envision that, among other applications, this protocol may be applied to the rapid synthesis of trehalose-based probes for tuberculosis diagnostics. For instance, short-lived radionuclide-modified trehalose analogues (e.g., 18 F-modified trehalose) could be used for advanced clinical imaging modalities such as positron emission tomography-computed tomography (PET-CT).

Ultrasonic synthesis of hydroxyapatite in non-cavitation and cavitation modes.

PubMed

Nikolaev, A L; Gopin, A V; Severin, A V; Rudin, V N; Mironov, M A; Dezhkunov, N V

2018-06-01

The size control of materials is of great importance in research and technology because materials of different size and shape have different properties and applications. This paper focuses on the synthesis of hydroxyapatite in ultrasound fields of different frequencies and intensities with the aim to find the conditions which allow control of the particles size. The results are evaluated by X-ray diffraction, Transmission Electron Microscopy, morphological and sedimentation analyses. It is shown that the hydroxyapatite particles synthesized at low intensity non-cavitation regime of ultrasound have smaller size than those prepared at high intensity cavitation regime. The explanation of observed results is based on the idea of formation of vortices at the interface between phosphoric acid and calcium hydroxide solution where the nucleation of hydroxyapatite particles is taken place. Smaller vortices formed at high frequency non-cavitation ultrasound regime provide smaller nucleation sites and smaller resulting particles, compared to vortices and particles obtained without ultrasound. Discovered method has a potential of industrial application of ultrasound for the controlled synthesis of nanoparticles. Copyright © 2018 Elsevier B.V. All rights reserved.

Synthesis and characterization of novel polymers from non-petroleum sources for use in enhanced oil recovery. Progress report, July 1,1981-June 30, 1982. [Starch-g-polyacrylamide; polysaccharides and acrylamides; Schardinger-. beta. -dextrin and acrylamide

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

Butler, G.B.; Hogen-Esch, T.E.

1982-01-01

Annual progress reports are presented for the following tasks: (1) synthesis and structural characterization of polysaccharide-based graft copolymers for use in tertiary oil recovery; (2) determination of physical properties of the polymers and their solutions, and screening of the polymers to determine their utility in oil recovery. Over the past year synthesis and characterization studies have continued in the following five areas: (1) starch-g-polyacrylamide (ST-g-PAM) copolymers; (2) graft copolymers of other polysaccharides (gum arabic, yellow dextrin, pectin, okra polysaccharide, and guar gum) and acrylamides; (3) a naturally occurring polysaccharide extracted from okra (Akro); (4) graft copolymers of Schardinger-..beta..-dextrin and acrylamidemore » (SD-g-PAM); (5) chemical degradation of ST-g-PAM and SD-g-PAM copolymers. For physical properties studies, the following areas were investigated: (1) characterization of copolymers by ultracentrifugation, size exclusion chromatography and nucleophore membrane filtration; (2) rheological studies on copolymers; and (3) statistical analysis of variables in graft copolymerization. (ATT)« less

hcp-Co nanowires grown on metallic foams as catalysts for the Fischer-Tropsch synthesis.

PubMed

Soulantica, Katerina; Harmel, Justine; Peres, Laurent; Estrader, Marta; Berliet, Adrien; Maury, Sylvie; Fécant, Antoine; Chaudret, Bruno; Serp, Philippe

2018-06-12

The possibility to control the structural characteristics of the active phase of supported catalysts offers the opportunity to improve catalyst performance, especially in structure sensitive catalytic reactions. In parallel, heat management is of critical importance for the catalytic performance in highly endo- or exothermic reactions. The Fisher-Tropsch synthesis (FTS) is a structure sensitive exothermic reaction, which enables catalytic transformation of syngas to high quality liquid fuels. We have elaborated monolithic cobalt based heterogeneous catalysts through a wet chemistry approach that allows control over nanocrystal shape and crystallographic phase, while at the same time enables heat management. Copper and nickel foams have been employed as supports for the epitaxial growth of hcp-Co nanowires, directly from a solution containing a coordination compound of cobalt and stabilizing ligands. The Co/Cufoam catalyst has been tested for the Fischer-Tropsch synthesis in fixed bed reactor, showing stability, and significantly superior activity and selectivity towards C5+ compared to a Co/SiO2-Al2O3 reference catalyst under the same conditions. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Conformation-Based Design and Synthesis of Apratoxin A Mimetics Modified at the α,β-Unsaturated Thiazoline Moiety.

PubMed

Onda, Yuichi; Masuda, Yuichi; Yoshida, Masahito; Doi, Takayuki

2017-08-10

We have demonstrated design, synthesis, and biological evaluation of apratoxin A mimetics. In the first generation, the moCys moiety was replaced with seven simple amino acids as their 3D structures can be similar to that of apratoxin A. Apratoxins M1-M7 were synthesized using solid-phase peptide synthesis and solution-phase macrolactamization. Apratoxin M7, which contains a piperidinecarboxylic acid moiety, exhibited potent cytotoxicity against HCT-116 cells. In the second generation, substitution of each amino acid residue in the tripeptide Tyr(Me)-MeAla-MeIle moiety in apratoxin M7 led to the development of the highly potent apratoxin M16 possessing biphenylalanine (Bph) instead of Tyr(Me), which exhibited an IC 50 value of 1.1 nM against HCT-116 cells. Moreover, compared to apratoxin A, apratoxin M16 exhibited a similarly high level of growth inhibitory activity against various cancer cell lines. The results indicate that apratoxin M16 could be a potential candidate as an anticancer agent.

Formation of sodium bismuth titanate-barium titanate during solid-state synthesis

DOE PAGES

Hou, Dong; Aksel, Elena; Fancher, Chris M.; ...

2017-01-12

Phase formation of sodium bismuth titanate (Na 0.5Bi 0.5TiO 3 or NBT) and its solid solution with barium titanate (BaTiO 3 or BT) during the calcination process is studied using in situ high-temperature diffraction. The reactant powders were mixed and heated to 1000°C, while X-ray diffraction patterns were recorded continuously. Phase evolutions from starting materials to final perovskite products are observed, and different transient phases are identified. The formation mechanism of NBT and NBT–xBT perovskite structures is discussed, and a reaction sequence is suggested based on the observations. The in situ study leads to a new processing approach, which ismore » the use of nano-TiO 2, and gives insights to the particle size effect for solid-state synthesis products. Lastly, it was found that the use of nano-TiO 2 as reactant powder accelerates the synthesis process, decreases the formation of transient phases, and helps to obtain phase-pure products using a lower thermal budget.« less

MgO-based adsorbents for CO2 adsorption: Influence of structural and textural properties on the CO2 adsorption performance.

PubMed

Elvira, Gutiérrez-Bonilla; Francisco, Granados-Correa; Víctor, Sánchez-Mendieta; Alberto, Morales-Luckie Raúl

2017-07-01

A series of MgO-based adsorbents were prepared through solution-combustion synthesis and ball-milling process. The prepared MgO-based powders were characterized using X-ray diffraction, scanning electron microscopy, N 2 physisorption measurements, and employed as potential adsorbents for CO 2 adsorption. The influence of structural and textural properties of these adsorbents over the CO 2 adsorption behaviour was also investigated. The results showed that MgO-based products prepared by solution-combustion and ball-milling processes, were highly porous, fluffy, nanocrystalline structures in nature, which are unique physico-chemical properties that significantly contribute to enhance their CO 2 adsorption. It was found that the MgO synthesized by solution combustion process, using a molar ratio of urea to magnesium nitrate (2:1), and treated by ball-milling during 2.5hr (MgO-BM2.5h), exhibited the maximum CO 2 adsorption capacity of 1.611mmol/g at 25°C and 1atm, mainly via chemisorption. The CO 2 adsorption behaviour on the MgO-based adsorbents was correlated to their improved specific surface area, total pore volume, pore size distribution and crystallinity. The reusability of synthesized MgO-BM2.5h was confirmed by five consecutive CO 2 adsorption-desorption times, without any significant loss of performance, that supports the potential of MgO-based adsorbent. The results confirmed that the special features of MgO prepared by solution-combustion and treated by ball-milling during 2.5hr are favorable to be used as effective MgO-based adsorbent in post-combustion CO 2 capture technologies. Copyright © 2016. Published by Elsevier B.V.

Improved production and processing of ⁸⁹Zr using a solution target.

PubMed

Pandey, Mukesh K; Bansal, Aditya; Engelbrecht, Hendrik P; Byrne, John F; Packard, Alan B; DeGrado, Timothy R

2016-01-01

The objectives of the present work were to improve the cyclotron production yield of (89)Zr using a solution target, develop a practical synthesis of the hydroxamate resin used to process the target, and develop a biocompatible medium for (89)Zr elution from the hydroxamate resin. A new solution target (BMLT-2) with enhanced heat dissipation capabilities was designed by using helium-cooled dual foils (0.2 mm Al and 25 μ Havar) and an enhanced water-cooled, elongated solution cavity in the target insert. Irradiations were performed with 14 MeV protons on a 2M solution of yttrium nitrate in 1.25 M nitric acid at 40-μA beam current for 2 h in a closed system. Zirconium-89 was separated from Y by use of a hydroxamate resin. A one-pot synthesis of hydroxamate resin was accomplished by activating the carboxylate groups on a carboxymethyl cation exchange resin using methyl chloroformate followed by reaction with hydroxylamine hydrochloride. After trapping of (89)Zr on hydroxamate resin and rinsing the resin with HCl and water to release Y, (89)Zr was eluted with 1.2 M K2HPO4/KH2PO4 buffer (pH3.5). ICP-MS was used to measure metal contaminants in the final (89)Zr solution. The BMLT-2 target produced 349±49 MBq (9.4±1.2 mCi) of (89)Zr at the end of irradiation with a specific activity of 1.18±0.79 GBq/μg. The hydroxamate resin prepared using the new synthesis method showed a trapping efficiency of 93% with a 75 mg resin bed and 96-97% with a 100-120 mg resin bed. The elution efficiency of (89)Zr with 1.2M K2HPO4/KH2PO4 solution was found to be 91.7±3.7%, compared to >95% for 1 M oxalic acid. Elution with phosphate buffer gave very small levels of metal contaminants: Al=0.40-0.86 μg (n=2), Fe=1.22±0.71 μg (n=3), Y=0.29 μg (n=1). The BMLT-2 target allowed doubling of the beam current for production of (89)Zr, resulting in a greater than 2-fold increase in production yield in comparison with a conventional liquid target. The new one-pot synthesis of hydroxamate resin provides a simpler synthesis method for the (89)Zr trapping resin. Finally, phosphate buffer elutes the (89)Zrfrom the hydroxamate resin in high efficiency while at the same time providing a more biocompatible medium for subsequent use of (89)Zr. Copyright © 2015 Elsevier Inc. All rights reserved.

Synthesis and properties of nickel cobalt boron nanoparticles

NASA Astrophysics Data System (ADS)

Patel, J.; Pankhurst, Q. A.; Parkin, I. P.

2005-01-01

Amorphous cobalt nickel boride nanoparticles were synthesised by chemical reduction synthesis in aqueous solution. Careful control of synthesis conditions and post reaction oxidation enabled the nanoparticles to be converted into a core-shell structure comprising of an amorphous Co-Ni-B core and an outer metal oxide sheet. These particles had interesting magnetic properties including saturation magnetisations and coercivities of the order of 80 emu/g and 170 Oe respectively, making them suitable for a potential use as an exchange-pinned magnetic material.

Parallel-vector computation for structural analysis and nonlinear unconstrained optimization problems

NASA Technical Reports Server (NTRS)

Nguyen, Duc T.

1990-01-01

Practical engineering application can often be formulated in the form of a constrained optimization problem. There are several solution algorithms for solving a constrained optimization problem. One approach is to convert a constrained problem into a series of unconstrained problems. Furthermore, unconstrained solution algorithms can be used as part of the constrained solution algorithms. Structural optimization is an iterative process where one starts with an initial design, a finite element structure analysis is then performed to calculate the response of the system (such as displacements, stresses, eigenvalues, etc.). Based upon the sensitivity information on the objective and constraint functions, an optimizer such as ADS or IDESIGN, can be used to find the new, improved design. For the structural analysis phase, the equation solver for the system of simultaneous, linear equations plays a key role since it is needed for either static, or eigenvalue, or dynamic analysis. For practical, large-scale structural analysis-synthesis applications, computational time can be excessively large. Thus, it is necessary to have a new structural analysis-synthesis code which employs new solution algorithms to exploit both parallel and vector capabilities offered by modern, high performance computers such as the Convex, Cray-2 and Cray-YMP computers. The objective of this research project is, therefore, to incorporate the latest development in the parallel-vector equation solver, PVSOLVE into the widely popular finite-element production code, such as the SAP-4. Furthermore, several nonlinear unconstrained optimization subroutines have also been developed and tested under a parallel computer environment. The unconstrained optimization subroutines are not only useful in their own right, but they can also be incorporated into a more popular constrained optimization code, such as ADS.

Poly(imide-siloxane) segmented copolymer structural adhesives prepared by bulk and solution thermal imidization

NASA Technical Reports Server (NTRS)

Bott, R. H.; Summers, J. D.; Arnold, C. A.; Blankenship, C. P., Jr.; Taylor, L. T.

1988-01-01

The improved properties that have been demonstrated through thermal solution imidization in the case of polyimides and poly(imide-siloxane) segmented copolymers suggests significant potential for application of these new materials. Specifically, the enhancement in solubility, moisture reduction, and processability observed through this solution technique is quite dramatic. Previous work has shown that the presence of low amounts of siloxane does not detract significantly from the lap shear strength of these materials to titanium in the case of bulk thermal imidization synthesis. In addition, the siloxane incorporation results in the added advantage of resistance to hot, wet environments. This added durability is presumably due to the hydrophobic siloxane segments preventing the uptake of water at the critical interphase between the adhesive and the adherend. This paper discusses the extension of this work to the solution imidization synthesis technique recently developed in our laboratory. Results dealing with the absolute bond strengths as well as durability and failure surface analysis will be presented.

Prebiotic chemistry in eutectic solutions at the water-ice matrix.

PubMed

Menor-Salván, César; Marín-Yaseli, Margarita R

2012-08-21

A crystalline ice matrix at subzero temperatures can maintain a liquid phase where organic solutes and salts concentrate to form eutectic solutions. This concentration effect converts the confined reactant solutions in the ice matrix, sometimes making condensation and polymerisation reactions occur more favourably. These reactions occur at significantly high rates from a prebiotic chemistry standpoint, and the labile products can be protected from degradation. The experimental study of the synthesis of nitrogen heterocycles at the ice-water system showed the efficiency of this scenario and could explain the origin of nucleobases in the inner Solar System bodies, including meteorites and extra-terrestrial ices, and on the early Earth. The same conditions can also favour the condensation of monomers to form ribonucleic acid and peptides. Together with the synthesis of these monomers, the ice world (i.e., the chemical evolution in the range between the freezing point of water and the limit of stability of liquid brines, 273 to 210 K) is an under-explored experimental model in prebiotic chemistry.

Hydrothermal synthesis of pollucite, analcime and their solid solutions and analysis of their properties

NASA Astrophysics Data System (ADS)

Jing, Zhenzi; Cai, Kunchuan; Li, Yan; Fan, Junjie; Zhang, Yi; Miao, Jiajun; Chen, Yuqian; Jin, Fangming

2017-05-01

Pollucite, as a perfect long-term potential host for radioactive Cs immobilization, barely exists in pure form naturally but in an isomorphism form between pollucite and analcime due to coexistence of Cs and Na. Pollucite could be hydrothermally synthesized with Cs-polluted soil or clay minerals which contain Cs and Na, and it is necessary to study the properties of the synthesis if Cs and Na contained. Pure pollucite, analcime and their solid solutions were hydrothermally synthesized with chemicals, and it was found that the most formed pollucite analcime solid solutions with Cs/(Cs + Na) ratios of 2/6-5/6 had very similar properties in mineral composition, morphology and size, structural water (Cs cations) and coordination environment to pollucite. This also suggests that even coexistence of Cs and Na in nature, pollucite favors to form due to site preference for Cs over Na, which leads to the property and the structure of the most solid solutions similar to that of pollucite.

Green synthesis of silver nanoparticles mediated by Pulicaria glutinosa extract

PubMed Central

Khan, Mujeeb; Khan, Merajuddin; Adil, Syed Farooq; Tahir, Muhammad Nawaz; Tremel, Wolfgang; Alkhathlan, Hamad Z; Al-Warthan, Abdulrahman; Siddiqui, Mohammed Rafiq H

2013-01-01

The green synthesis of metallic nanoparticles (NPs) has attracted tremendous attention in recent years because these protocols are low cost and more environmentally friendly than standard methods of synthesis. In this article, we report a simple and eco-friendly method for the synthesis of silver NPs using an aqueous solution of Pulicaria glutinosa plant extract as a bioreductant. The as-prepared silver NPs were characterized using ultraviolet–visible spectroscopy, powder X-ray diffraction, transmission electron microscopy, energy-dispersive X-ray spectroscopy, and Fourier-transform infrared spectroscopy. Moreover, the effects of the concentration of the reductant (plant extract) and precursor solution (silver nitrate), the temperature on the morphology, and the kinetics of reaction were investigated. The results indicate that the size of the silver NPs varied as the plant extract concentration increased. The as-synthesized silver NPs were phase pure and well crystalline with a face-centered cubic structure. Further, Fourier-transform infrared spectroscopy analysis confirmed that the plant extract not only acted as a bioreductant but also functionalized the NPs’ surfaces to act as a capping ligand to stabilize them in the solvent. The developed eco-friendly method for the synthesis of NPs could prove a better substitute for the physical and chemical methods currently used to prepare metallic NPs commonly used in cosmetics, foods, and medicines. PMID:23620666

Oxidative acylation using thioacids

NASA Technical Reports Server (NTRS)

Liu, R.; Orgel, L. E.

1997-01-01

Several important prebiotic reactions, including the coupling of amino acids into polypeptides by the formation of amide linkages, involve acylation. Theae reactions present a challenge to the understanding of prebiotic synthesis. Condensation reactions relying on dehydrating agents are either inefficient in aqueous solution or require strongly acidic conditions and high temperatures. Activated amino acids such as thioester derivatives have therefore been suggested as likely substrates for prebiotic peptide synthesis. Here we propose a closely related route to amide bond formation involving oxidative acylation by thioacids. We find that phenylalanine, leucine and phenylphosphate are acylated efficiently in aqueous solution by thioacetic acid and an oxidizing agent. From a prebiotic point of view, oxidative acylation has the advantage of proceeding efficiently in solution and under mild conditions. We anticipate that oxidative acylation should prove to be a general method for activating carboxylic acids, including amino acids.

Efficacy of a solution-based approach for making sodalite waste forms for an oxide reduction salt utilized in the reprocessing of used uranium oxide fuel

DOE PAGES

Riley, Brian J.; Pierce, David A.; Frank, Steven M.; ...

2015-04-01

This paper describes the various approaches attempted to make solution-derived sodalite with a LiCl-Li 2O oxide reduction salt used to dissolve used uranium oxide fuel so the uranium can be recovered and recycled. The approaches include modified sol-gel and solutionbased synthesis processes. As-made products were mixed with 5 and 10 mass% of a Na 2O-B 2O 3- SiO 2 glass binder and these, along with product without a binder, were heated using either a cold-press-and-sinter method or hot uniaxial pressing. The results demonstrate the limitation of sodalite yield due to the fast intermediate reactions between Na+ and Cl- to formmore » halite in solution and Li 2O and SiO 2 to form lithium silicates (e.g., Li 2SiO 3 or Li 2Si 2O 5) in the calcined and sintered pellets. The results show that pellets can be made with high sodalite fractions in the crystalline product (~92 mass%) and low porosities using a solution-based approach and this LiCl-Li 2O salt but that the incorporation of Li into the sodalite is low.« less

Some VTOL head-up display drive-law problems and solutions

NASA Technical Reports Server (NTRS)

Merrick, Vernon K.

1993-01-01

A piloted simulation test was conducted on the Ames Research Center's vertical motion simulator (VMS) in support of the Phase 2A flight test of NASA's V/STOL systems research aircraft (VSRA). During the simulation several problems were found with the head-up display (HUD) symbol drive laws and the flightpath synthesis. These problems and the solutions devised to solve them are described. Most of the resulting HUD drive-law changes were implemented during the simulation and their effectiveness was verified. Subsequently both the HUD symbol drive-law and flightpath-synthesis changes were implemented in the VSRA and tested successfully in the Phase 2A flight tests.

Synthesis of calcium vanadate minerals and related compounds

USGS Publications Warehouse

Marvin, Richard F.

1956-01-01

Synthesis of natural vanadates shows that most of them are stable in an acid environment. Phase studies of a portion of the system CaO-V2O5-H2O indicate that calcium vanadates are an indicator of environmental pH conditions. Some minerals, such as pascoute, indicate rapid evaporation of vanadite solutions; other minerals, such as hewettite, show that slow evaporation took place. Cursory examination of systems K2O-UO2-(NO3)2-V2O5 and CaO-UO2(NO3)2-V2O5, both in aqueous solution, has yielded information on the relationships among carnotite, tyuyamunite, and rauvite.

Responsive copolymers for enhanced petroleum recovery. Annual report

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

McCormick, C.; Hester, R.

1994-08-01

A coordinated research program involving synthesis, characterization, and rheology has been undertaken to develop advanced polymer system which should be significantly more efficient than polymers presently used for mobility control and conformance. Unlike the relatively inefficient, traditional EOR polymers, these advanced polymer systems possess microstructural features responsive to temperature, electrolyte concentration, and shear conditions. Contents of this report include the following chapters. (1) First annual report responsive copolymers for enhanced oil recovery. (2) Copolymers of acrylamide and sodium 3-acrylamido-3-methylbutanoate. (3) Terpolymers of NaAMB, Am, and n-decylacrylamide. (4) Synthesis and characterization of electrolyte responsive terpolymers of acrylamide, N-(4-butyl)phenylacrylamide, and sodium acrylate,more » sodium-2-acrylamido-2-methylpropanesulphonate or sodium-3-acrylamido-3-methylbutanoate. (5) Synthesis and solution properties of associative acrylamido copolymers with pyrensulfonamide fluorescence labels. (6) Photophysical studies of the solution behavior of associative pyrenesulfonamide-labeled polyacrylamides. (7) Ampholytic copolymers of sodium 2-(acrylamido)-2-methylpropanesulfonate with [2-(acrylamido)-2-methypropyl]trimethylammonium chloride. (8) Ampholytic terpolymers of acrylamide with sodium 2-acrylamido-2-methylpropanesulphoante and 2-acrylamido-2-methylpropanetrimethyl-ammonium chloride and (9) Polymer solution extensional behavior in porous media.« less

Synthesis and characterization of guar-alginate hybrid bead templated mercury sorbing titania spheres.

PubMed

Singh, Vandana; Preeti; Singh, Angela; Singh, Devendra; Singh, Yadveer; Pandey, Arvind Kumar

2015-01-01

Present communication reports on the synthesis and characterization of Hg(II) sorbing millimeter sized porous titania spheres (TSP). The synthesis utilizes guar gum-alginate hybrid beads as sacrificial template to polymerize titanium(IV) isopropoxide. The hybrid beads are crafted by pouring guar-alginate mixed solution to calcium bath. The mechanical strength of the beads depended on guar to alginate ratio in the mixed solution. The equal weight ratio of the two polysaccharides is appropriate for adequate mechanical strength beads. The unique performance of the templating beads is attributed to the synergistic interaction between guar gum and sodium alginate. FTIR, BET, SEM, TEM, XRD, TGA, and DTG analyses have been used for the characterization of the optimum performance TSP (TSPAG2). TSPAG2 is a mesoporous material that has higher surface area and narrower pore size distribution than pure alginate derived titania spheres (TSPA). TEM study demonstrated that TSPAG2 spheres are constituted of aggregated TiO2 nanoparticles of ∼ 10 nm size. TSPAG2 is able to capture >95% Hg(II) from synthetic Hg(II) solution in 10h at pH 5 as opposed to only 68% removal by TSPA. Copyright © 2014 Elsevier B.V. All rights reserved.

Hydrothermal synthesis of a photovoltaic material based on CuIn0.5Ga0.5Se2

NASA Astrophysics Data System (ADS)

Castellanos Báez, Y. T.; Fuquen Peña, D. A.; Gómez-Cuaspud, J. A.; Vera-López, E.; Pineda-Triana, Y.

2017-12-01

The present work report, the synthesis and characterization of the CuIn0.5Ga0.5Se2 system (abbreviated CIGS), by the implementation of a hydrothermal route, in order to obtain a solid with appropriate properties in terms of surface, morphological and texture properties for potential applications in the design of photovoltaic cells. The synthesis was carried out using the corresponding stoichiometric quantities (Cu:In:Ga:Se 1:0.5:0.5:2), which were mixed in a Teflon vessel under stirring conditions. The homogeneous solution was treated in a steel autoclave at 300°C for 72 hours at the end of which the resulting material was characterized by X-Ray Diffraction (XRD) and Rietveld refinement. The results of the structural characterization allowed to confirm the obtaining of a chalcopyrite type structure, with a I-42 d (122) structure and cell parameters a=0.570, b=0.570, c=1.140nm, α=90, β=90, γ=90° oriented along (1 0 4) facet, detecting the presence of a secondary phases, related with CuInSe and CuIn metallic selenides, derived from synthesis process. The structural refinement allowing to validate the obtaining of a nanometric crystalline material (10-20nm) for potential applications in field of photovoltaic technology.

An efficient synthesis of tetramic acid derivatives with extended conjugation from L-Ascorbic Acid

PubMed Central

Singh, Biswajit K; Bisht, Surendra S; Tripathi, Rama P

2006-01-01

Background Tetramic acids with polyenyl substituents are an important class of compounds in medicinal chemistry. Both solid and solution phase syntheses of such molecules have been reported recently. Thiolactomycin, a clinical candidate for treatment of tuberculosis has led to further explorations in this class. We have recently developed an efficient synthesis of tetramic acids derivatives from L- ascorbic acid. In continuation of this work, we have synthesised dienyl tetramic acid derivatives. Results 5,6-O-Isopropylidene-ascorbic acid on reaction with DBU led to the formation of tetronolactonyl allyl alcohol, which on oxidation with pyridinium chlorochromate gave the respective tetranolactonyl allylic aldehydes. Wittig olefination followed by reaction of the resulting tetranolactonyl dienyl esters with different amines resulted in the respective 5-hydroxy lactams. Subsequent dehydration of the hydroxy lactams with p-toluene sulphonic acid afforded the dienyl tetramic acid derivatives. All reactions were performed at ambient temperature and the yields are good. Conclusion An efficient and practical method for the synthesis of dienyl tetramic acid derivatives from inexpensive and easily accessible ascorbic acid has been developed. The compounds bear structural similarities to the tetramic acid based polyenic antibiotics and thus this method offers a new and short route for the synthesis of tetramic acid derivatives of biological significance. PMID:17147830