CATALYST-FREE REACTIONS UNDER SOLVENT-FEE CONDITIONS: MICROWAVE-ASSISTED SYNTHESIS OF HETEROCYCLIC HYDRAZONES BELOW THE MELTING POINT OF NEAT REACTANTS

EPA Science Inventory

The reaction of neat 5- or 8-oxobenzopyran-2(1H)-ones with a variety of aromatic and heteroaromatic hydrazines are remarkable accelerated upon irradiation in a household microwave oven in the absence of any catalyst, solid support or solvent thus providing an environmentally frie...

Microwave synthesis and electrochemical properties of lithium manganese borate as cathode for lithium ion batteries

NASA Astrophysics Data System (ADS)

Ma, Ting; Muslim, Arzugul; Su, Zhi

2015-05-01

Nano structured LiMnBO3/C cathode materials are synthesized by a fast microwave solid-state reaction method using MnCO3, Li2CO3, H3BO3 and glucose as starting materials for the first time. The crystal structure, morphology and electrochemical properties of LiMnBO3/C composites are characterized by X-ray diffraction (XRD), raman spectroscopy (Ramon), scanning electron microscopy (SEM), transmission electron microscopy (TEM), cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS) and charge-discharge tests. The result shows that not only monoclinic LiMnBO3/C but also hexagonal LiMnBO3/C cathode materials can be successfully synthesized by microwave solid-state method with power of 240 W in different time. Compared with h-LiMnBO3/C and mixed phase LiMnBO3/C, m-LiMnBO3/C displays lower charge-transfer resistance and the Warburg impedance, so it reveals a higher first discharge capacity of 156.3 mAh g-1 at 0.05 C within 1.8V-4.6 V, The value increases up to 173.2 mAh g-1 caused by the activation process. Even after 50 cycles, the discharge capacity of m-LiMnBO3/C still remains at 148.2 mAh g-1.

Satellite Power Systems (SPS) Concept Definition Study (Exhibit D). Solid-State Amplifier Investigation

NASA Technical Reports Server (NTRS)

Hanley, G. M.

1981-01-01

Data resulting from a continuing effort to provide system/subsystem definition data to aid in the evaluation of the SPS program concept is presented. The specific data described relate to the proposed use of solid state devices as microwave power amplifiers in the satellite microwave power transmission subsystem.

Flash microwave synthesis and sintering of nanosized La{sub 0.75}Sr{sub 0.25}Cr{sub 0.93}Ru{sub 0.07}o{sub 3-{delta}} for fuel cell application

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

Combemale, L., E-mail: lionel.combemale@u-bourgogne.f; Caboche, G.; Stuerga, D.

2009-10-15

Perovskite-oxide nanocrystals of La{sub 0.75}Sr{sub 0.25}Cr{sub 0.93}Ru{sub 0.07}O{sub 3-{delta}} with a mean size around 10 nm were prepared by microwave flash synthesis. This reaction was performed in alcoholic solution using metallic salts, sodium ethoxide and microwave autoclave. The obtained powder was characterised after purification by energy dispersive X-ray analysis (EDX), X-ray powder diffraction (XRD), BET adsorption technique, photon correlation spectroscopy (PCS) and transmission electron microscopy (TEM). The results show that integrated perovskite-type phase and uniform particle size were obtained in the microwave treated samples. At last the synthesised powder was directly used in a sintering process. A porous solid, inmore » accordance with the expected applications, was then obtained at low sintering temperature (1000 deg. C) without use of pore forming agent. - Graphical abstract: TEM photograph of La{sub 0.75}Sr{sub 0.25}Cr{sub 0.93}Ru{sub 0.07}O{sub 3-{delta}} obtained by microwave flash synthesis. This picture confirms the nanometric size of the ceramic particles.« less

Microwave-assisted synthesis of triple-helical, collagen-mimetic lipopeptides

PubMed Central

Banerjee, Jayati; Hanson, Andrea J; Muhonen, Wallace W; Shabb, John B; Mallik, Sanku

2018-01-01

Collagen-mimetic peptides and lipopeptides are widely used as substrates for matrix degrading enzymes, as new biomaterials for tissue engineering, as drug delivery systems and so on. However, the preparation and subsequent purification of these peptides and their fatty-acid conjugates are really challenging. Herein, we report a rapid microwave-assisted, solid-phase synthetic protocol to prepare the fatty-acid conjugated, triple-helical peptides containing the cleavage site for the enzyme matrix metalloproteinase-9 (MMP-9). We employed a PEG-based resin as the solid support and the amino acids were protected with Fmoc- and tert-butyl groups. The amino acids were coupled at 50 °C (25 W of microwave power) for 5 min. The deprotection reactions were carried out at 75 °C (35 W of microwave power) for 3 min. Using this protocol, a peptide containing 23 amino acids was synthesized and then conjugated to stearic acid in 14 h. PMID:20057380

Microwave plasma enabled synthesis of free standing carbon nanostructures at atmospheric pressure conditions.

PubMed

Bundaleska, N; Tsyganov, D; Dias, A; Felizardo, E; Henriques, J; Dias, F M; Abrashev, M; Kissovski, J; Tatarova, E

2018-05-23

An experimental and theoretical study on microwave (2.45 GHz) plasma enabled assembly of carbon nanostructures, such as multilayer graphene sheets and nanoparticles, was performed. The carbon nanostructures were fabricated at different Ar-CH4 gas mixture composition and flows at atmospheric pressure conditions. The synthesis method is based on decomposition of the carbon-containing precursor (CH4) in the "hot" microwave plasma environment into carbon atoms and molecules, which are further converted into solid carbon nuclei in the "colder" plasma zones. By tailoring of the plasma environment, a controlled synthesis of graphene sheets and diamond-like nanoparticles was achieved. Selective synthesis of graphene flakes was achieved at a microwave power of 1 kW, Ar and methane flow rates of 600 sccm and 2 sccm respectively, while the predominant synthesis of diamond-like nanoparticles was obtained at the same power, but with higher flow rates, i.e. 1000 and 7.5 sccm, respectively. Optical emission spectroscopy was applied to detect the plasma emission related to carbon species from the 'hot' plasma zone and to determine the main plasma parameters. Raman spectroscopy and scanning electron microscopy have been applied to characterize the synthesized nanostructures. A previously developed theoretical model was further updated and employed to understand the mechanism of CH4 decomposition and formation of the main building units, i.e. C and C2, of the carbon nanostructures. An insight into the physical chemistry of carbon nanostructure formation in a high energy density microwave plasma environment is presented.

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.

Innovative processing of dense LSGM electrolytes for IT-SOFC's

NASA Astrophysics Data System (ADS)

Rambabu, B.; Ghosh, Samrat; Zhao, Weichang; Jena, Hrudananda

This paper reports for the first time the attempted synthesis of SrO- and MgO-doped LaGaO 3 (La 1- xSr xGa 1- yMg yO 3-0.5(x+ y), LSGM) perovskite by an aqueous 'regenerative' solution route. This novel technique enabled recycling of the undesired product and subsequently yielded product with much better phase purity and density than that obtained from the solid-state route. La 0.8Sr 0.2Ga 0.85Mg 0.15O 2.825 (LSGM-2015) and LaGaO 3 were prepared using both the regenerative sol-gel (RSG) and conventional solid-state route at 1400 °C. Series of La 0.8Sr 0.2Ga 0.83Mg 0.17O 2.815 (LSGM-2017) pellets were also prepared by the RSG method at different sintering temperature (1200-1500 °C) and time. The effect of conventional and microwave sintering of samples obtained from both solid-state and regenerative route was also investigated. Microwave heating was carried out using SiC as a microwave susceptor. The LSGM pellets prepared by using different synthetic methods were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), electrochemical impedance spectroscopy (EIS) and pellet density was determined by pycnometry. The LSGM-2015 prepared by RSG route exhibited conductivity σ t = 0.066 and 0.029 S cm -1 at 800 and 700 °C, respectively, and activation energy of the bulk, grain-boundary, and total are E b = 0.97 eV, E gb = 1.03 eV and E t = 1.01 eV, respectively. The sintering temperature severely affected the grain size (<0.1-10 μm) and also the grain-boundary resistance (3-175 kΩ). The unique aspect of this RSG technique is that the final product can be recycled which makes the process cost effective and time saving compared to the solid-state ceramic technique and this technique would allow optimization of processing parameters in a cost effective and time saving manner for obtaining well sintered LSGM as an electrolyte for IT-SOFC's.

Greener and rapid access to bio-active heterocycles: one-pot solvent-free synthesis of 1,3,4-oxadiazoles and 1,3,4-thiadiazoles

EPA Science Inventory

A novel one-pot solvent free synthesis of 1,3,4-oxadiazoles and 1,3,4-thiadiazoles by condensation of acid hydrazide and triethyl orthoalkanates under microwave irradiations is reported. This green protocol was catalyzed efficiently by solid supported Nafion®NR50 and phosphorus p...

Analysis of S-band solid-state transmitters for the solar power satellite

NASA Technical Reports Server (NTRS)

Belohoubek, E. F.; Ettenberg, M.; Huang, H. C.; Nowogrodzki, M.; Sechi, F. N.

1979-01-01

The possibility of replacing the Reference System antenna in which thermionic devices are used for the dc-to-microwave conversion, with solid-state elements was explored. System, device, and antenna module tradeoff investigations strongly point toward the desirability of changing the transmitter concept to a distributed array of relatively low power elements, deriving their dc power directly from the solar cell array and whose microwave power outputs are combined in space. The approach eliminates the thermal, weight, and dc-voltage distribution problems of a system in which high power tubes are simply replaced with clusters of solid state amplifiers. The proposed approach retains the important advantages of a solid state system: greatly enhanced reliability and graceful degradation of the system.

MW-assisted synthesis of SVO for ICD primary batteries

NASA Astrophysics Data System (ADS)

Beninati, Sabina; Fantuzzi, Matteo; Mastragostino, Marina; Soavi, Francesca

An Ag 2V 4O 11 (SVO) cathode material prepared by microwave (MW)-assisted solid-state synthesis (MW-SVO) was developed for lithium primary batteries for implantable cardioverter/defibrillators (ICDs). This paper presents the results of physical-chemical and electrochemical characterizations of MW-SVO as well as those of SVO prepared by conventional thermal route (T-SVO). A specific effect of MWs which accelerates the synthesis reaction and contributes to yield a material of different morphology and degree of crystallinity compared with those of T-SVO was observed. The results of pulsed electrochemical tests carried out at 37 °C in operative conditions of ICDs on Li/MW-SVO batteries with cathode mass loading sized for practical use are also reported. These tests demonstrated that MW-SVO can be used for high performing lithium primary battery delivering in few seconds the specific energy values required by ICD application.

Conventional and Microwave Joining of Silicon Carbide Using Displacement Reactions

NASA Technical Reports Server (NTRS)

Kingsley, J.; Yiin, T.; Barmatz, M.

1995-01-01

Microwave heating was used to join Silicon Carbide rods using a thin TiC /Si tape interlayer . Microwaves quickly heated the rods and tape to temperatures where solid-state displacement reactions between TiC and Si occurred.

Workshop on Microwave Power Transmission and Reception. Workshop Paper Summaries

NASA Technical Reports Server (NTRS)

1980-01-01

Microwave systems performance and phase control are discussed. Component design and reliability are highlighted. The power amplifiers, radiating elements, rectennas, and solid state configurations are described. The proper sizing of microwave transmission systems is also discussed.

Effect of microwave-assisted sintering on dielectric properties of CaCu3Ti4O12 ceramic

NASA Astrophysics Data System (ADS)

Rani, Suman; Ahlawat, Neetu; Punia, R.; Kundu, R. S.; Ahlawat, N.

2016-05-01

In this present work, CaCu3Ti4O12 (CCTO) was synthesized by conventional solid-state reaction technique. The synthesis process was carried out in two phases; by conventional process (calcination and sintering at 1080°C for 10 hours) and phase II involves the micro assisted pre sintering of conventionally calcined CCTO for very short soaking time of 30 min at 1080°C in a microwave furnace followed by sintering at 1080°C for 10 hours in conventional furnace. X-ray diffraction (XRD) patterns confirmed the formation of single phase ceramic. Dielectric properties were studied over the frequency range from 50Hz -5MHz at temperatures (273K-343K). It was observed that pre- microwave sintering enhance the dielectric constant values from 10900 to 11893 and respectively reduces the dielectric loss values from 0.49 to 0.34 at room temperature(1 KHz). CCTO ceramics which are found desirable for many technological applications. The effect is more pronounced at low frequencies of applied electric field.

Ultra-stable microwave generation with a diode-pumped solid-state laser in the 1.5-μm range

NASA Astrophysics Data System (ADS)

Dolgovskiy, Vladimir; Schilt, Stéphane; Bucalovic, Nikola; Di Domenico, Gianni; Grop, Serge; Dubois, Benoît; Giordano, Vincent; Südmeyer, Thomas

2014-09-01

We demonstrate the first ultra-stable microwave generation based on a 1.5-μm diode-pumped solid-state laser (DPSSL) frequency comb. Our system relies on optical-to-microwave frequency division from a planar-waveguide external cavity laser referenced to an ultra-stable Fabry-Perot cavity. The evaluation of the microwave signal at ~10 GHz uses the transportable ultra-low-instability signal source ULISS®, which employs a cryo-cooled sapphire oscillator. With the DPSSL comb, we measured -125 dBc/Hz phase noise at 1 kHz offset frequency, likely limited by the photo-detection shot-noise or by the noise floor of the reference cryo-cooled sapphire oscillator. For comparison, we also generated low-noise microwave using a commercial Er:fiber comb stabilized in similar conditions and observed >20 dB lower phase noise in the microwave generated from the DPSSL comb. Our results confirm the high potential of the DPSSL technology for low-noise comb applications.

Beyond the Compositional Threshold of Nanoparticle-Based Materials.

PubMed

Portehault, David; Delacroix, Simon; Gouget, Guillaume; Grosjean, Rémi; Chan-Chang, Tsou-Hsi-Camille

2018-04-17

The design of inorganic nanoparticles relies strongly on the knowledge from solid-state chemistry not only for characterization techniques, but also and primarily for choosing the systems that will yield the desired properties. The range of inorganic solids reported and studied as nanoparticles is however strikingly narrow when compared to the solid-state chemistry portfolio of bulk materials. Efforts to enlarge the collection of inorganic particles are becoming increasingly important for three reasons. First, they can yield materials more performing than current ones for a range of fields including biomedicine, optics, catalysis, and energy. Second, looking outside the box of common compositions is a way to target original properties or to discover genuinely new behaviors. The third reason lies in the path followed to reach these novel nano-objects: exploration and setup of new synthetic approaches. Indeed, willingness to access original nanoparticles faces a synthetic challenge: how to reach nanoparticles of solids that originally belong to the realm of solid-state chemistry and its typical protocols at high temperature? To answer this question, alternative reaction pathways must be sought, which may in turn provide tracks for new, untargeted materials. The corresponding strategies require limiting particle growth by confinement at high temperatures or by decreasing the synthesis temperature. Both approaches, especially the latter, provide a nice playground to discover metastable solids never reported before. The aim of this Account is to raise attention to the topic of the design of new inorganic nanoparticles. To do so, we take the perspective of our own work in the field, by first describing synthetic challenges and how they are addressed by current protocols. We then use our achievements to highlight the possibilities offered by new nanomaterials and to introduce synthetic approaches that are not in the focus of recent literature but hold, in our opinion, great promise. We will span methods of low temperature "chimie douce" aqueous synthesis coupled to microwave heating, sol-gel chemistry and processing coupled to solid state reactions, and then molten salt synthesis. These protocols pave the way to metastable low valence oxyhydroxides, vanadates, perovskite oxides, boron carbon nitrides, and metal borides, all obtained at the nanoscale with structural and morphological features differing from "usual" nanomaterials. These nano-objects show original properties, from sensing, thermoelectricity, charge and spin transports, photoluminescence, and catalysis, which require advanced characterization of surface states. We then identify future trends of synthetic methodologies that will merit further attention in this burgeoning field, by emphasizing the importance of unveiling reaction mechanisms and coupling experiments with modeling.

Solar Power Satellite Microwave Transmission and Reception

NASA Technical Reports Server (NTRS)

Dietz, R. H.

1980-01-01

Numerous analytical and experimental investigations related to SPS microwave power transmission and reception are reported. Aspects discussed include system performance, phase control, power amplifiers, radiating elements, rectenna, solid state configurations, and planned program activities.

Synthesis and evaluation of nitroxide-based oligoradicals for low-temperature dynamic nuclear polarization in solid state NMR

PubMed Central

Yau, Wai-Ming; Thurber, Kent R.; Tycko, Robert

2014-01-01

We describe the synthesis of new nitroxide-based biradical, triradical, and tetraradical compounds and the evaluation of their performance as paramagnetic dopants in dynamic nuclear polarization (DNP) experiments in solid state nuclear magnetic resonance (NMR) spectroscopy with magic-angle spinning (MAS). Under our experimental conditions, which include temperatures in the 25–30 K range, a 9.4 T magnetic field, MAS frequencies of 6.2–6.8 kHz, and microwave irradiation at 264.0 GHz from a 800 mW extended interaction oscillator source, the most effective compounds are triradicals that are related to the previously-described compound DOTOPA-TEMPO (see Thurber et al., 2010), but have improved solubility in glycerol/water solvent near neutral pH. Using these compounds at 30 mM total nitroxide concentration, we observe DNP enhancement factors of 92–128 for cross-polarized 13C NMR signals from 15N,13C-labeled melittin in partially protonated glycerol/water, and build-up times of 2.6–3.8 s for 1H spin polarizations. Net sensitivity enhancements with biradical and tetraradical dopants, taking into account absolute 13C NMR signal amplitudes and build-up times, are approximately 2–4 times lower than with the best triradicals. PMID:24887201

Synthesis and evaluation of nitroxide-based oligoradicals for low-temperature dynamic nuclear polarization in solid state NMR

NASA Astrophysics Data System (ADS)

Yau, Wai-Ming; Thurber, Kent R.; Tycko, Robert

2014-07-01

We describe the synthesis of new nitroxide-based biradical, triradical, and tetraradical compounds and the evaluation of their performance as paramagnetic dopants in dynamic nuclear polarization (DNP) experiments in solid state nuclear magnetic resonance (NMR) spectroscopy with magic-angle spinning (MAS). Under our experimental conditions, which include temperatures in the 25-30 K range, a 9.4 T magnetic field, MAS frequencies of 6.2-6.8 kHz, and microwave irradiation at 264.0 GHz from a 800 mW extended interaction oscillator source, the most effective compounds are triradicals that are related to the previously-described compound DOTOPA-TEMPO (see Thurber et al., 2010), but have improved solubility in glycerol/water solvent near neutral pH. Using these compounds at 30 mM total nitroxide concentration, we observe DNP enhancement factors of 92-128 for cross-polarized 13C NMR signals from 15N,13C-labeled melittin in partially protonated glycerol/water, and build-up times of 2.6-3.8 s for 1H spin polarizations. Net sensitivity enhancements with biradical and tetraradical dopants, taking into account absolute 13C NMR signal amplitudes and build-up times, are approximately 2-4 times lower than with the best triradicals.

Synthesis and evaluation of nitroxide-based oligoradicals for low-temperature dynamic nuclear polarization in solid state NMR.

PubMed

Yau, Wai-Ming; Thurber, Kent R; Tycko, Robert

2014-07-01

We describe the synthesis of new nitroxide-based biradical, triradical, and tetraradical compounds and the evaluation of their performance as paramagnetic dopants in dynamic nuclear polarization (DNP) experiments in solid state nuclear magnetic resonance (NMR) spectroscopy with magic-angle spinning (MAS). Under our experimental conditions, which include temperatures in the 25-30 K range, a 9.4 T magnetic field, MAS frequencies of 6.2-6.8 kHz, and microwave irradiation at 264.0 GHz from a 800 mW extended interaction oscillator source, the most effective compounds are triradicals that are related to the previously-described compound DOTOPA-TEMPO (see Thurber et al., 2010), but have improved solubility in glycerol/water solvent near neutral pH. Using these compounds at 30 mM total nitroxide concentration, we observe DNP enhancement factors of 92-128 for cross-polarized (13)C NMR signals from (15)N,(13)C-labeled melittin in partially protonated glycerol/water, and build-up times of 2.6-3.8s for (1)H spin polarizations. Net sensitivity enhancements with biradical and tetraradical dopants, taking into account absolute (13)C NMR signal amplitudes and build-up times, are approximately 2-4 times lower than with the best triradicals. Published by Elsevier Inc.

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

Wildfire, Christina; Sabolsky, Edward M.; Spencer, Michael J.

The rapid synthesis of yttrium aluminum garnet (Y 3Al 15O 12, YAG) powder was investigated through the use of microwave irradiation of the oxide precursor system. For this investigation, an external hybrid heating source was not used. Instead, the rapid heating of the precursor materials (yttria and alumina powders, which are typically transparent to 2.45 GHz microwaves) was initiated by mixing an intrinsic absorbing material (carbon) into the original oxide precursors. The effect of the carbon characteristics, such as carbon source, concentration, particle size, and agglomerate microstructure were evaluated on the efficiency of coupling and resultant oxide reaction. The microwavemore » power was varied to optimize the YAG conversion and eliminate intermediate phase formation. Interactions between the conductive carbon particles and the dielectric oxides within the microwave exposure produced local arching and micro-plasma formation within the powder bed, resulting in the rapid formation of the refractory YAG composition. This optimal conduction led to temperatures of 1000°C that could be achieved in less than 5 min resulting in the formation of > 90 vol% YAG. The understanding of a conductor/dielectric particulate system here, provided insight into possible application of similar systems where microwave irradiation could be used for enhanced solid-state formation, local melting events, and gas phase reactions with a composite powder media.« less

Microwave spectroscopic observation of multiple phase transitions in the bilayer electron solid in wide quantum wells

NASA Astrophysics Data System (ADS)

Hatke, Anthony; Engel, Lloyd; Liu, Yang; Shayegan, Mansour; Pfeiffer, Loren; West, Ken; Baldwin, Kirk

2015-03-01

The termination of the low Landau filling factor (ν) fractional quantum Hall series for a single layer two dimensional system results in the formation of a pinned Wigner solid for ν < 1 / 5. In a wide quantum well the system can support a bilayer state in which interlayer and intralayer interactions become comparable, which is measured in traditional transport as an insulating state for ν < 1 / 2. We perform microwave spectroscopic studies of this bilayer state and observe that this insulator exhibits a resonance, a signature of a solid phase. Additionally, we find that as we increase the density of the well at fixed ν this bilayer solid exhibits multiple sharp reductions in the resonance amplitude vs ν. This behavior is characteristic of multiple phase transitions, which remain hidden from dc transport measurements.

Microwave-assisted solid-phase peptide synthesis of the 60-110 domain of human pleiotrophin on 2-chlorotrityl resin.

PubMed

Friligou, Irene; Papadimitriou, Evangelia; Gatos, Dimitrios; Matsoukas, John; Tselios, Theodore

2011-05-01

A fast and efficient microwave-assisted solid phase peptide synthesis (MW-SPPS) of a 51mer peptide, the main heparin-binding site (60-110) of human pleiotrophin (hPTN), using 2-chlorotrityl chloride resin (CLTR-Cl) following the 9-fluorenylmethyloxycarbonyl/tert-butyl (Fmoc/tBu) methodology and with the standard N,N'-diisopropylcarbodiimide/1-hydroxybenzotriazole (DIC/HOBt) coupling reagents, is described. An MW-SPPS protocol was for the first time successfully applied to the acid labile CLTR-Cl for the faster synthesis of long peptides (51mer peptide) and with an enhanced purity in comparison to conventional SPPS protocols. The synthesis of such long peptides is not trivial and it is generally achieved by recombinant techniques. The desired linear peptide was obtained in only 30 h of total processing time and in 51% crude yield, in which 60% was the purified product obtained with 99.4% purity. The synthesized peptide was purified by reversed phase high performance liquid chromatography (RP-HPLC) and identified by electrospray ionization mass spectrometry (ESI-MS). Then, the regioselective formation of the two disulfide bridges of hPTN 60-110 was successfully achieved by a two-step procedure, involving an oxidative folding step in dimethylsulfoxide (DMSO) to form the Cys(77)-Cys(109) bond, followed by iodine oxidation to form the Cys(67)-Cys(99) bond.

Microwave assisted transformation of N,N-diphenylamine as precursors of organic light emitting diodes (OLED)

NASA Astrophysics Data System (ADS)

Jefri, Wahyuningrum, Deana

2015-09-01

In this research, study on the transformation of N,N-diphenylamine (DPA) using iodine (I2) utilizing solid state Microwave Assisted Organic Synthesis (MAOS) method has been carried out. The reaction was performed by variations of three parameters namely the mole of reagents, the amount and type of solid support (alumina/Al2O3), and the reaction conditions. Experimental results showed that neutral-alumina was a better solid support than basic-alumina. The optimum temperature for the reaction was approximately at 125-133 °C with reaction time of 15 minutes and microwave reactor power at 500-600 W. The separation of the yellowish green product solution with preparative Thin Layer Chromatography (TLC) method using n-hexane:ethyl acetate = 4:1 (v/v) as eluent yielded two fractions (I and II) and both fractions can undergo fluorescence under 365 nm UV light. Based on the LC chromatogram with methanol:water = 95:5 (v/v) as eluent and its corresponding mass spectra (ESI+), fraction I contained three compounds, which were tetracarbazole A, triphenylamine, and impurities in the form of plasticizer such as bis(2-ethylhexyl) phthalate. Fraction II also contained three compounds, which were tetracarbazole C, tetraphenylhydrazine, and plasticizer such as bis(2-ethylhexyl) phthalate. Both FT-IR (KBr disks) and NMR (500 MHz, CDCl3) spectra of fraction I and II confirmed the aromatic amine groups in those compounds. The observed fluorescence colors of fraction I and II were violet and violet-blue, respectively. Based on their structures and fluorescence characters, the compounds in fraction I and II have the potential to be used as Organic Light Emitting Diode (OLED) compound precursors.

Microwave assisted transformation of N,N-diphenylamine as precursors of organic light emitting diodes (OLED)

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

Jefri,; Wahyuningrum, Deana, E-mail: deana@chem.itb.ac.id

2015-09-30

In this research, study on the transformation of N,N-diphenylamine (DPA) using iodine (I2) utilizing solid state Microwave Assisted Organic Synthesis (MAOS) method has been carried out. The reaction was performed by variations of three parameters namely the mole of reagents, the amount and type of solid support (alumina/Al2O3), and the reaction conditions. Experimental results showed that neutral-alumina was a better solid support than basic-alumina. The optimum temperature for the reaction was approximately at 125-133 °C with reaction time of 15 minutes and microwave reactor power at 500-600 W. The separation of the yellowish green product solution with preparative Thin Layer Chromatographymore » (TLC) method using n-hexane:ethyl acetate = 4:1 (v/v) as eluent yielded two fractions (I and II) and both fractions can undergo fluorescence under 365 nm UV light. Based on the LC chromatogram with methanol:water = 95:5 (v/v) as eluent and its corresponding mass spectra (ESI+), fraction I contained three compounds, which were tetracarbazole A, triphenylamine, and impurities in the form of plasticizer such as bis(2-ethylhexyl) phthalate. Fraction II also contained three compounds, which were tetracarbazole C, tetraphenylhydrazine, and plasticizer such as bis(2-ethylhexyl) phthalate. Both FT-IR (KBr disks) and NMR (500 MHz, CDCl{sub 3}) spectra of fraction I and II confirmed the aromatic amine groups in those compounds. The observed fluorescence colors of fraction I and II were violet and violet-blue, respectively. Based on their structures and fluorescence characters, the compounds in fraction I and II have the potential to be used as Organic Light Emitting Diode (OLED) compound precursors.« less

Light fluorous-tagged traceless one-pot synthesis of benzimidazoles facilitated by microwave irradiation.

PubMed

Tseng, Chih-Chung; Tasi, Cheng-Hsun; Sun, Chung-Ming

2012-06-01

A novel protocol for rapid assemble of benzimidazole framework has been demonstrated. This method incorporated with light fluorous-tag provides a convenient method for diversification of benzimidazoles and for easy purification via fluorous solid-phase extraction (F-SPE) in a parallel manner. The key transformation of this study involves in situ reduction of aromatic nitro compound, amide formation, cyclization and aromatization promoted by microwave irradiation in a one-pot fashion. The strategy is envisaged to be applied for the establishment of drug-like small molecule libraries for high throughput screening.

Establishment of quality, reliability and design standards for low, medium, and high power microwave hybrid microcircuits

NASA Technical Reports Server (NTRS)

Robinson, E. A.

1973-01-01

Quality, reliability, and design standards for microwave hybrid microcircuits were established. The MSFC Standard 85M03926 for hybrid microcircuits was reviewed and modifications were generated for use with microwave hybrid microcircuits. The results for reliability tests of microwave thin film capacitors, transistors, and microwave circuits are presented. Twenty-two microwave receivers were tested for 13,500 unit hours. The result of 111,121 module burn-in and operating hours for an integrated solid state transceiver module is reported.

Military microwaves '84; Proceedings of the Conference, London, England, October 24-26, 1984

NASA Astrophysics Data System (ADS)

The present conference on microwave frequency electronic warfare and military sensor equipment developments consider radar warning receivers, optical frequency spread spectrum systems, mobile digital communications troposcatter effects, wideband bulk encryption, long range air defense radars (such as the AR320, W-2000 and Martello), multistatic radars, and multimode airborne and interceptor radars. IR system and subsystem component topics encompass thermal imaging and active IR countermeasures, class 1 modules, and diamond coatings, while additional radar-related topics include radar clutter in airborne maritime reconnaissance systems, microstrip antennas with dual polarization capability, the synthesis of shaped beam antenna patterns, planar phased arrays, radar signal processing, radar cross section measurement techniques, and radar imaging and pattern analysis. Attention is also given to optical control and signal processing, mm-wave control technology and EW systems, W-band operations, planar mm-wave arrays, mm-wave monolithic solid state components, mm-wave sensor technology, GaAs monolithic ICs, and dielectric resonator and wideband tunable oscillators.

Effect of microwave-assisted sintering on dielectric properties of CaCu{sub 3}Ti{sub 4}O{sub 12} ceramic

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

Rani, Suman, E-mail: sumanranigju@gmail.com; Ahlawat, Neetu; Punia, R.

2016-05-23

In this present work, CaCu{sub 3}Ti{sub 4}O{sub 12} (CCTO) was synthesized by conventional solid-state reaction technique. The synthesis process was carried out in two phases; by conventional process (calcination and sintering at 1080°C for 10 hours) and phase II involves the micro assisted pre sintering of conventionally calcined CCTO for very short soaking time of 30 min at 1080°C in a microwave furnace followed by sintering at 1080°C for 10 hours in conventional furnace. X-ray diffraction (XRD) patterns confirmed the formation of single phase ceramic. Dielectric properties were studied over the frequency range from 50Hz -5MHz at temperatures (273K-343K). It wasmore » observed that pre- microwave sintering enhance the dielectric constant values from 10900 to 11893 and respectively reduces the dielectric loss values from 0.49 to 0.34 at room temperature(1 KHz). CCTO ceramics which are found desirable for many technological applications. The effect is more pronounced at low frequencies of applied electric field.« less

Solid State Technology Branch of NASA Lewis Research Center

NASA Technical Reports Server (NTRS)

1992-01-01

A collection of papers written by the members of the Solid State Technology Branch of NASA LeRC from Jun. 1991 - Jun. 1992 is presented. A range of topics relating to superconductivity, Monolithic Microwave Circuits (MMIC's), coplanar waveguides, and material characterization is covered.

Microwave generated solid dispersions containing Ibuprofen.

PubMed

Moneghini, Mariarosa; Bellich, Barbara; Baxa, Pietro; Princivalle, Francesco

2008-09-01

The purpose of this study was to apply the attractive technique of the microwaves irradiation (MW) for the preparation of solvent-free solid dispersions (SD). In particular, the microwave technology has been considered in order to prepare an enhanced release dosage form for the poorly soluble drug Ibuprofen (IBU), employing PVP/VA 60/40 (PVP/VA 64) and hydroxypropyl-beta-cyclodextrin (HP-beta-CD) as hydrophilic carriers. Their physico-chemical characteristics and dissolution properties were compared to the corresponding physical mixtures and the drug alone. The results of physico-chemical characterization attested a correspondence of the solid state of the drug before and after irradiation treatment and that an amorphous form of the drug was obtained. This result, together with the presence of the hydrophilic polymers determined a remarkable enhancement of the in vitro dissolution rate of the drug suggesting that the microwave technique could be considered as a new and interesting method to prepare drug-polymer systems.

Accomplishment of highly porous-lithium lanthanum titanate through microwave treatment

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

Lakshmi, D.; Nalini, B., E-mail: jyothsnalalin99@gmail.com; Abhilash, K. P.

Perovskite structured (ABO{sub 3}) lithium lanthanum titanate (LLTO) is a successful electrolyte reported by several scientists in the recent past. It is believed that intercalation and de-intercalation of Li ions inside solid electrolyte can be improved by increasing the porosity of the material. Hence in this research work, an attempt is made to increase the porosity of the LLTO electrolyte by rapid-microwave synthesis route. The microwave prepared LLTO is compared with the sol-gel synthesized LLTO. The prepared samples are analyzed with XRD, SEM, PL and cyclic Voltammetry studies. Morphological analysis proves that microwave synthesized LLTO contains much pores compared tomore » the Sol-gel LLTO. A remarkable difference in its electrochemical property is also demonstrated and analysed with cyclic voltammetric studies and the results are presented.« less

Energy issues in microwave food processing: A review of developments and the enabling potentials of solid-state power delivery.

PubMed

Atuonwu, J C; Tassou, S A

2018-01-23

The enormous magnitude and variety of microwave applications in household, commercial and industrial food processing creates a strong motivation for improving the energy efficiency and hence, sustainability of the process. This review critically assesses key energy issues associated with microwave food processing, focusing on previous energy performance studies, energy performance metrics, standards and regulations. Factors affecting energy-efficiency are categorised into source, load and source-load matching factors. This highlights the need for highly-flexible and controllable power sources capable of receiving real-time feedback on load properties, and effecting rapid control actions to minimise reflections, heating non-uniformities and other imperfections that lead to energy losses. A case is made for the use of solid-state amplifiers as alternatives to conventional power sources, magnetrons. By a full-scale techno-economic analysis, including energy aspects, it is shown that the use of solid-state amplifiers as replacements to magnetrons is promising, not only from an energy and overall technical perspective, but also in terms of economics.

Microwave Crystallization of Lithium Aluminum Germanium Phosphate Solid-State Electrolyte.

PubMed

Mahmoud, Morsi M; Cui, Yuantao; Rohde, Magnus; Ziebert, Carlos; Link, Guido; Seifert, Hans Juergen

2016-06-23

Lithium aluminum germanium phosphate (LAGP) glass-ceramics are considered as promising solid-state electrolytes for Li-ion batteries. LAGP glass was prepared via the regular conventional melt-quenching method. Thermal, chemical analyses and X-ray diffraction (XRD) were performed to characterize the prepared glass. The crystallization of the prepared LAGP glass was done using conventional heating and high frequency microwave (MW) processing. Thirty GHz microwave (MW) processing setup were used to convert the prepared LAGP glass into glass-ceramics and compared with the conventionally crystallized LAGP glass-ceramics that were heat-treated in an electric conventional furnace. The ionic conductivities of the LAGP samples obtained from the two different routes were measured using impedance spectroscopy. These samples were also characterized using XRD and scanning electron microscopy (SEM). Microwave processing was successfully used to crystallize LAGP glass into glass-ceramic without the aid of susceptors. The MW treated sample showed higher total, grains and grain boundary ionic conductivities values, lower activation energy and relatively larger-grained microstructure with less porosity compared to the corresponding conventionally treated sample at the same optimized heat-treatment conditions. The enhanced total, grains and grain boundary ionic conductivities values along with the reduced activation energy that were observed in the MW treated sample was considered as an experimental evidence for the existence of the microwave effect in LAGP crystallization process. MW processing is a promising candidate technology for the production of solid-state electrolytes for Li-ion battery.

Effective utilizations of palm oil mill fly ash for synthetic amorphous silica and carbon zeolite composite synthesis

NASA Astrophysics Data System (ADS)

Utama, P. S.; Saputra, E.; Khairat

2018-04-01

Palm Oil Mill Fly Ash (POMFA) the solid waste of palm oil industry was used as a raw material for synthetic amorphous silica and carbon zeolite composite synthesis in order to minimize the wastes of palm oil industry. The alkaline extraction combine with the sol-gel precipitation and mechanical fragmentation was applied to produce synthetic amorphous silica. The byproduct, extracted POMFA was rich in carbon and silica content in a significant amount. The microwave heated hydrothermal process used to synthesize carbon zeolite composite from the byproduct. The obtained silica had chemical composition, specific surface area and the micrograph similar to commercial precipitated silica for rubber filler. The microwave heated hydrothermal process has a great potential for synthesizing carbon zeolite composite. The process only needs one-step and shorter time compare to conventional hydrothermal process.

QUARTERLY PROGRESS REPORT NO. 83,

DTIC Science & Technology

Topics included are: microwave spectroscopy; radio astronomy; solid-state microwave electronics; optical and infrared spectroscopy; physical electronics and surface physics; physical acoustics; plasma physics; gaseous electronics; plasmas and controlled nuclear fusion ; energy conversion research; statistical communication theory; linguistics; cognitive information processing; communications biophysics; neurophysiology; computation research.

Solid State Technology Branch of NASA Lewis Research Center: Fifth Annual Digest

NASA Technical Reports Server (NTRS)

1993-01-01

The digest is a collection of papers written by the members of the Solid State Technology Branch of NASA Lewis Research Center from June 1992-June 1993. The papers cover a range of topics relating to superconductivity, monolithic microwave integrated circuits (MMIC's), coplanar waveguide, and material characterization.

Synthesis and characterization of natural and modified antifreeze glycopeptides: glycosylated foldamers.

PubMed

Nagel, Lilly; Plattner, Carolin; Budke, Carsten; Majer, Zsuzsanna; DeVries, Arthur L; Berkemeier, Thomas; Koop, Thomas; Sewald, Norbert

2011-08-01

In Arctic and Antarctic marine regions, where the temperature declines below the colligative freezing point of physiological fluids, efficient biological antifreeze agents are crucial for the survival of polar fish. One group of such agents is classified as antifreeze glycoproteins (AFGP) that usually consist of a varying number (n = 4-55) of [AAT]( n )-repeating units. The threonine side chain of each unit is glycosidically linked to β-D: -galactosyl-(1 → 3)-α-N-acetyl-D: -galactosamine. These biopolymers can be considered as biological antifreeze foldamers. A preparative route for stepwise synthesis of AFGP allows for efficient synthesis. The diglycosylated threonine building block was introduced into the peptide using microwave-enhanced solid phase synthesis. By this versatile solid phase approach, glycosylated peptides of varying sequences and lengths could be obtained. Conformational studies of the synthetic AFGP analogs were performed by circular dichroism experiments (CD). Furthermore, the foldamers were analysed microphysically according to their inhibiting effect on ice recrystallization and influence on the crystal habit.

Innovative microwave design leads to smart, small EW systems

NASA Astrophysics Data System (ADS)

Niehenke, Edward C.

1988-02-01

An account is given of the state-of-the-art in microwave component and system design for EW systems, whose size and weight has been progressively reduced in recent years as a result of continuing design innovation in microwave circuitry. Typically, AI-function computers are employed to control microwave functions in a way that allows rapid RAM or ROM software modification to meet new performance requirements, thereby obviating hardware modifications. Attention is given to high-isolation GaAs MMIC filters, switches and amplifiers, frequency converters, instantaneous frequency measurement systems, frequency translators, digital RF memories, and high effective radiated power solid-state active antenna arrays.

Gigahertz dual-comb modelocked diode-pumped semiconductor and solid-state lasers

NASA Astrophysics Data System (ADS)

Link, S. M.; Mangold, M.; Golling, M.; Klenner, A.; Keller, U.

2016-03-01

We present a simple approach to generate simultaneously two gigahertz mode-locked pulse trains from a single gain element. A bi-refringent crystal in the laser cavity splits the one cavity beam into two cross-polarized and spatially separated beams. This polarization-duplexing is successfully demonstrated for both a semiconductor disk laser (i.e. MIXSEL) and a diode-pumped solid-state Nd:YAG laser. The beat between the two beams results in a microwave frequency comb, which represents a direct link between the terahertz optical frequencies and the electronically accessible microwave regime. This dual-output technique enables compact and cost-efficient dual-comb lasers for spectroscopy applications.

Determination of solid-propellant transient regression rates using a microwave Doppler shift technique

NASA Technical Reports Server (NTRS)

Strand, L. D.; Schultz, A. L.; Reedy, G. K.

1972-01-01

A microwave Doppler shift system, with increased resolution over earlier microwave techniques, was developed for the purpose of measuring the regression rates of solid propellants during rapid pressure transients. A continuous microwave beam is transmitted to the base of a burning propellant sample cast in a metal waveguide tube. A portion of the wave is reflected from the regressing propellant-flame zone interface. The phase angle difference between the incident and reflected signals and its time differential are continuously measured using a high resolution microwave network analyzer and related instrumentation. The apparent propellant regression rate is directly proportional to this latter differential measurement. Experiments were conducted to verify the (1) spatial and time resolution of the system, (2) effect of propellant surface irregularities and compressibility on the measurements, and (3) accuracy of the system for quasi-steady-state regression rate measurements. The microwave system was also used in two different transient combustion experiments: in a rapid depressurization bomb, and in the high-frequency acoustic pressure environment of a T-burner.

Synthesis, physico-chemical properties and complexing abilities of new amphiphilic ligands from D-galacturonic acid.

PubMed

Allam, Anas; Behr, Jean-Bernard; Dupont, Laurent; Nardello-Rataj, Véronique; Plantier-Royon, Richard

2010-04-19

This paper describes a convenient and efficient synthesis of new complexing surfactants from d-galacturonic acid and n-octanol as renewable raw materials in a two-step sequence. In the first step, simultaneous O-glycosidation-esterification under Fischer conditions was achieved. The anomeric ratio of the products was studied based on the main experimental parameters and the activation mode (thermal or microwave). In the second step, aminolysis of the n-octyl ester was achieved with various functionalized primary amines under standard thermal or microwave activation. The physico-chemical properties of these new amphiphilic ligands were measured and these compounds were found to exhibit interesting surface properties. Complexing abilities of one uronamide ligand functionalized with a pyridine moiety toward Cu(II) ions was investigated in solution by EPR titrations. A solid compound was also synthesized and characterized, its relative structure was deduced from spectroscopic data. Copyright (c) 2010 Elsevier Ltd. All rights reserved.

Antifreeze glycopeptide analogues: microwave-enhanced synthesis and functional studies.

PubMed

Heggemann, Carolin; Budke, Carsten; Schomburg, Benjamin; Majer, Zsuzsa; Wissbrock, Marco; Koop, Thomas; Sewald, Norbert

2010-01-01

Antifreeze glycoproteins enable life at temperatures below the freezing point of physiological solutions. They usually consist of the repetitive tripeptide unit (-Ala-Ala-Thr-) with the disaccharide alpha-D-galactosyl-(1-3)-beta-N-acetyl-D-galactosamine attached to each hydroxyl group of threonine. Monoglycosylated analogues have been synthesized from the corresponding monoglycosylated threonine building block by microwave-assisted solid phase peptide synthesis. This method allows the preparation of analogues containing sequence variations which are not accessible by other synthetic methods. As antifreeze glycoproteins consist of numerous isoforms they are difficult to obtain in pure form from natural sources. The synthetic peptides have been structurally analyzed by CD and NMR spectroscopy in proton exchange experiments revealing a structure as flexible as reported for the native peptides. Microphysical recrystallization tests show an ice structuring influence and ice growth inhibition depending on the concentration, chain length and sequence of the peptides.

C-shaped diastereomers containing cofacial thiophene-substituted quinoxaline rings: synthesis, photophysical properties, and X-ray crystallography.

PubMed

DeBlase, Catherine R; Finke, Ryan T; Porras, Jonathan A; Tanski, Joseph M; Nadeau, Jocelyn M

2014-05-16

Synthesis and characterization of two diastereomeric C-shaped molecules containing cofacial thiophene-substituted quinoxaline rings are described. A previously known bis-α-diketone was condensed with an excess of 4-bromo-1,2-diaminobenzene in the presence of zinc acetate to give a mixture of two C-shaped diastereomers with cofacial bromine-substituted quinoxaline rings. After chromatographic separation, thiophene rings were installed by a microwave-assisted Suzuki coupling reaction, resulting in highly emissive diastereomeric compounds that were studied by UV-vis, fluorescence, and NMR spectroscopy, as well as X-ray crystallography. The unique symmetry of each diastereomer was confirmed by NMR spectroscopy. NMR data indicated that the syn isomer has restricted rotation about the bond connecting the thiophene and quinoxaline rings, which was also observed in the solid state. The spectroscopic properties of the C-shaped diastereomers were compared to a model compound containing only a single thiophene-substituted quinoxaline ring. Ground state intramolecular π-π interactions in solution were detected by NMR and UV-vis spectroscopy. Red-shifted emission bands, band broadening, and large Stokes shifts were observed, which collectively suggest excited state π-π interactions that produce excimer-like emissions, as well as a remarkable positive emission solvatochromism, indicating charge-transfer character in the excited state.

A Novel Oscillating Rectenna for Wireless Microwave Power Transmission

NASA Technical Reports Server (NTRS)

McSpadden, J. O.; Dickinson, R. M.; Fan, L.; Chang, K.

1998-01-01

A new concept for solid state wireless microwave power transmission is presented. A 2.45 GHz rectenna element that was designed for over 85% RF to dc power conversion efficiency has been used to oscillate at 3.3 GHz with an approximate 1% dc to RF conversion efficiency.

High-power microwave bipolar transistor modeling

NASA Astrophysics Data System (ADS)

Asensio, Alberto; Perez, Felix

1992-01-01

This article introduces a model for high-power microwave bipolar transistors and its associated parameter-measuring strategy, whose inclusion of thermal phenomena in the dc characterization allows a good estimate of the device's thermal resistance to be obtained. This type of model provides important capabilities for solid-state radar transmitter design.

Solid-phase synthesis of graphene quantum dots from the food additive citric acid under microwave irradiation and their use in live-cell imaging.

PubMed

Zhuang, Qianfen; Wang, Yong; Ni, Yongnian

2016-05-01

The work demonstrated that solid citric acid, one of the most common food additives, can be converted to graphene quantum dots (GQDs) under microwave heating. The as-prepared GQDs were further characterized by various analytical techniques like transmission electron microscopy, atomic force microscopy, X-ray diffraction, X-ray photoelectron spectroscopy, Fourier transform infrared spectroscopy, fluorescence and UV-visible spectroscopy. Cytotoxicity of the GQDs was evaluated using HeLa cells. The result showed that the GQDs almost did not exhibit cytotoxicity at concentrations as high as 1000 µg mL(-1). In addition, it was found that the GQDs showed good solubility, excellent photostability, and excitation-dependent multicolor photoluminescence. Subsequently, the multicolor GQDs were successfully used as a fluorescence light-up probe for live-cell imaging. Copyright © 2015 John Wiley & Sons, Ltd.

Low Temperature Graphene Synthesis from Poly(methyl methacrylate) Using Microwave Plasma Treatment

NASA Astrophysics Data System (ADS)

Yamada, Takatoshi; Ishihara, Masatou; Hasegawa, Masataka

2013-11-01

A graphene film having low sheet resistance (600 Ω/sq.) was synthesized at low temperatures of 280 °C. Utilizing microwave plasma treatment, graphene films were synthesized from a solid phase on a copper surface. The full width at half maximum of the 2D-band in the Raman spectrum indicated that a high quality graphene film was formed. Cross-sectional transmission electron microscopy observation revealed that the deposited graphene films consisted of single- or double-layer graphene flakes of nanometer order on the Cu surface, which agrees with the estimated number of layers from an average optical transmittance of 96%.

MW-assisted synthesis of LiFePO 4 for high power applications

NASA Astrophysics Data System (ADS)

Beninati, Sabina; Damen, Libero; Mastragostino, Marina

LiFePO 4/C was prepared by solid-state reaction from Li 3PO 4, Fe 3(PO 4) 2·8H 2O, carbon and glucose in a few minutes in a scientific MW (microwave) oven with temperature and power control. The material was characterized by X-ray diffraction, scanning electron microscopy and by TGA analysis to evaluate carbon content. The electrochemical characterization as positive electrode in EC (ethylene carbonate)-DMC (dimethylcarbonate) 1 M LiPF 6 was performed by galvanostatic charge-discharge cycles at C/10 to evaluate specific capacity and by sequences of 10 s discharge-charge pulses, at different high C-rates (5-45C) to evaluate pulse-specific power in simulate operative conditions for full-HEV application. The maximum pulse-specific power and, particularly, pulse efficiency values are quite high and make MW synthesis a very promising route for mass production of LiFePO 4/C for full-HEV batteries at low energy costs.

Hybrid microwave/conventionally heated calorimeter

NASA Astrophysics Data System (ADS)

Binner, Jon G. P.; Price, Duncan M.; Reading, Mike; Vaidhyanathan, Bala

2005-06-01

The design and construction of a calorimeter in which the specimen may be heated by microwave radiation and/or hot air is described. The apparatus was used to examine the effect of microwave radiation on the melting of benzil (89°C) and the solid-state phase transition of silver iodide (147°C). Reproducibility of transition temperature determinations were within ±1°C. No changes were observed for benzil but silver iodide exhibited an apparent reduction in transition temperature to around 120°C in the presence of microwaves, which increased with the level of microwave irradiation.

Microwave spectroscopic observation of distinct electron solid phases in wide quantum wells

NASA Astrophysics Data System (ADS)

Hatke, A. T.; Liu, Yang; Magill, B. A.; Moon, B. H.; Engel, L. W.; Shayegan, M.; Pfeiffer, L. N.; West, K. W.; Baldwin, K. W.

2014-06-01

In high magnetic fields, two-dimensional electron systems can form a number of phases in which interelectron repulsion plays the central role, since the kinetic energy is frozen out by Landau quantization. These phases include the well-known liquids of the fractional quantum Hall effect, as well as solid phases with broken spatial symmetry and crystalline order. Solids can occur at the low Landau-filling termination of the fractional quantum Hall effect series but also within integer quantum Hall effects. Here we present microwave spectroscopy studies of wide quantum wells that clearly reveal two distinct solid phases, hidden within what in d.c. transport would be the zero diagonal conductivity of an integer quantum-Hall-effect state. Explanation of these solids is not possible with the simple picture of a Wigner solid of ordinary (quasi) electrons or holes.

Microwave-assisted reactive sintering and lithium ion conductivity of Li1.3Al0.3Ti1.7(PO4)3 solid electrolyte

NASA Astrophysics Data System (ADS)

Hallopeau, Leopold; Bregiroux, Damien; Rousse, Gwenaëlle; Portehault, David; Stevens, Philippe; Toussaint, Gwenaëlle; Laberty-Robert, Christel

2018-02-01

Li1.3Al0.3Ti1.7(PO4)3 (LATP) materials are made of a three-dimensional framework of TiO6 octahedra and PO4 tetrahedra, which provides several positions for Li+ ions. The resulting high ionic conductivity is promising to yield electrolytes for all-solid-state Li-ion batteries. In order to elaborate dense ceramics, conventional sintering methods often use high temperature (≥1000 °C) with long dwelling times (several hours) to achieve high relative density (∼90%). In this work, an innovative synthesis and processing approach is proposed. A fast and easy processing technique called microwave-assisted reactive sintering is used to both synthesize and sinter LATP ceramics with suitable properties in one single step. Pure and crystalline LATP ceramics can be achieved in only 10 min at 890 °C starting from amorphous, compacted LATP's precursors powders. Despite a relative density of 88%, the ionic conductivity measured at ambient temperature (3.15 × 10-4 S cm-1) is among the best reported so far. The study of the activation energy for Li+ conduction confirms the high quality of the ceramic (purity and crystallinity) achieved by using this new approach, thus emphasizing its interest for making ion-conducting ceramics in a simple and fast way.

Morphological evolution of Bi2Se3 nanocrystalline materials synthesized by microwave assisted solvothermal method

NASA Astrophysics Data System (ADS)

Bera, Sumit; Behera, P.; Mishra, A. K.; Krishnan, M.; Patidar, M. M.; Singh, D.; Gangrade, M.; Venkatesh, R.; Deshpande, U. P.; Phase, D. M.; Ganesan, V.

2018-04-01

Structural, morphological and spectroscopic properties of Bi2Se3 nanoparticles synthesized by microwave assisted solvothermal method were investigated systematically. A controlled synthesis of different morphologies by a small variation in synthesis procedure is demonstrated. Powder X-ray diffraction (XRD) confirmed the formation of single phase. Crystallite and particle size reductions were studied with XRD and AFM (Atomic Force Microscopy). Different morphologies such as hexagonal nanoflakes with cross section of around˜6µm, nanoflower and octahedral agglomerated crystals of nearly ˜60 nm size have been observed in scanning electron microscope while varying the microwave assisted synthesis procedures. A significant blue shift observed in diffuse reflectance spectroscopy evidences the energy gap tuning as a result of morphological evolution. The difference in morphology observed in this three fast, facile and scalable synthesis is advantageous for tuning the thermoelectric figure of merit and for probing the surface states of these topological insulators. Low temperature resistivity remains similar for all three variants depicting a 2D character as evidenced by a -lnT term of localization.

1990 MTT-S International Microwave Symposium and Exhibition and Microwave and Millimeter-Wave Monolithic IC Symposium, Dallas, TX, May 7-10, 1990, Proceedings

NASA Astrophysics Data System (ADS)

McQuiddy, David N., Jr.; Sokolov, Vladimir

1990-12-01

The present conference discusses microwave filters, lightwave technology for microwave antennas, planar and quasi-planar guides, mixers and VCOs, cavity filters, discontinuity and coupling effects, control circuits, power dividers and phase shifters, microwave ICs, biological effects and medical applications, CAD and modeling for MMICs, directional couplers, MMIC design trends, microwave packaging and manufacturing, monolithic ICs, and solid-state devices and circuits. Also discussed are microwave and mm-wave superconducting technology, MICs for communication systems, the merging of optical and microwave technologies, microwave power transistors, ferrite devices, network measurements, advanced transmission-line structures, FET devices and circuits, field theory of IC discontinuities, active quasi-optical techniques, phased-array techniques and circuits, nonlinear CAD, sub-mm wave devices, and high power devices.

Comparison of Conventional and Microwave-assisted Synthesis of Benzimidazole Derivative from Citronellal in Kaffir lime oil (Citrus hystrix DC.)

NASA Astrophysics Data System (ADS)

Warsito, W.; Noorhamdani, A. S.; Suratmo; Dwi Sapri, R.; Alkaroma, D.; Azhar, A. Z.

2018-04-01

Simple method has been used for the synthesis of benzimidazole derivative from citronellal in kaffir lime oil under microwave irradiation. These compounds were synthesized also by conventional heating for comparison. In addtion, microwave-assited synthesis was also compared between using to dichloromethane and methanol solvents with variation of reaction time for 30 to 70 minutes and 4 to 12 h for conventional heating. The 2-citronellyl benzimidazole compound synthesized were characterised by FT-IR, GC-MS, 1H and 13C NMR spectroscopy. Comparison between conventional and microwave-assisted synthesis was done by comparing between correlation of reaction time and percentage yield. The time optimum of microwave-assisted and conventional synthesis using dichloromethane solvent respectively at 60 minutes (yield 19.23%) and 8 hours (yield 11.54%). In addition, microwave-assited synthesis increasing 157.81 times compared by conventional heating. While using methanol solvent tends to increase linearly however the percentage of yield only 0.77 times of synthesis using dichloromethane solvent.

Solvent-free, microwave-assisted synthesis of thiophene oligomers via Suzuki coupling.

PubMed

Melucci, Manuela; Barbarella, Giovanna; Sotgiu, Giovanna

2002-12-13

The purpose of this study was to obtain a rapid, efficient, and environmentally friendly methodology for the synthesis of highly pure thiophene oligomers. The solvent-free, microwave-assisted coupling of thienyl boronic acids and esters with thienyl bromides, using aluminum oxide as the solid support, allowed us to rapidly check the reaction trends on changing times, temperature, catalyst, and base and easily optimize the experimental conditions to obtain the targeted product in fair amounts. This procedure offers a novel, general, and very rapid route to the preparation of soluble thiophene oligomers. Thus, for example, quaterthiophene was obtained in 6 min by reaction of 2-bromo-2,2'-bithiophene with bis(pinacolato)diboron (isolated yield 65%), whereas quinquethiophene was obtained in 11 min by reaction of dibromoterthiophene with thienylboronic acid (isolated yield 74%). The synthesis of new chiral 2,2'-bithiophenes is reported. The detailed analysis of the byproducts of some reactions allowed us to elucidate a few aspects of reaction mechanisms. While the use of microwaves proved to be very convenient for the coupling between conventional thienyl moieties, the same was not true for the coupling of thienyl rings to thienyl-S,S-dioxide moieties. Indeed, in this case, the targeted product was obtained in low yields because of the competitive, accelerated, Diels-Alder reaction that affords a variety of condensation products.

Chemo-enzymatic synthesis of furfuralcohol from chestnut shell hydrolysate by a sequential acid-catalyzed dehydration under microwave and Escherichia coli CCZU-Y10 whole-cells conversion.

PubMed

Di, Junhua; Ma, Cuiluan; Qian, Jianghao; Liao, Xiaolong; Peng, Bo; He, Yucai

2018-08-01

In this study, chemo-enzymatic synthesis of furfuralcohol from biomass-derived xylose was successfully demonstrated by a sequential acid-catalyzed dehydration under microwave and whole-cells reduction. After dry dewaxed chestnut shells (CNS, 75 g/L) was acid-hydrolyzed with dilute oxalic acid (0.5 wt%) at 140 °C for 40 min, the obtained CNS-derived xylose (17.9 g/L xylose) could be converted to furfural at 78.8% yield with solid acid SO 4 2- /SnO 2 -Attapulgite (2.0 wt% catalyst loading) in the dibutyl phthalate-water (1:1, v:v) under microwave (600 W) at 180 °C for 10 min. In the dibutyl phthalate-water (1:1, v/v) media at 30 °C and pH 6.5, the furfural liquor (47.0 mM furfural) was biologically converted to furfuralcohol by recombinant Escherichia coli CCZU-Y10 whole-cells harboring an NADH-dependent reductase (PgCR) without extra addition of NAD + and glucose, and furfural was completely converted to furfuralcohol after 2.5 h. Clearly, this one-pot synthesis strategy can be effectively used for furfuralcohol production. Copyright © 2018 Elsevier Ltd. All rights reserved.

Solid State Technology Branch of NASA Lewis Research Center: Fifth Annual Digest

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

Not Available

1993-08-01

The digest is a collection of papers written by the members of the Solid State Technology Branch of NASA Lewis Research Center from June 1992-June 1993. The papers cover a range of topics relating to superconductivity, monolithic microwave integrated circuits (MMIC`s), coplanar waveguide, and material characterization. Individual papers are abstracted separately on the data base.

Solid state sandwich concept: Designs, considerations and issues. [solar power satellite transmission

NASA Technical Reports Server (NTRS)

Maynard, O. E.

1980-01-01

Progress in analysis and design of solid state approaches to the solar power satellite microwave power transmission system is reviewed with special emphasis on the Sandwich concept and the issues of maintenance of low junction temperatures for amplifiers to assure acceptable lifetime. Ten specific issues or considerations are discussed and their resolution or status is presented.

Microwave surface resistance of bulk YBa2Cu3O6+x material

NASA Astrophysics Data System (ADS)

Fathy, A.; Kalokitis, D.; Belohoubek, E.; Sundar, H. G. K.; Safari, A.

1988-10-01

Superconducting Y-Ba-Cu-O samples were prepared by conventional solid-state reaction. The microwave surface resistance of 1:2:3 compound superconductor material was measured in a special disk resonator structure at 10 GHz. At liquid-nitrogen temperatures the microwave surface resistance is comparable to that of Au. At lower temperature (~10 K) the surface resistance is an order of magnitude lower than that of Au at the same temperature.

Rapid solid-phase microwave synthesis of highly photoluminescent nitrogen-doped carbon dots for Fe3+ detection and cellular bioimaging

NASA Astrophysics Data System (ADS)

He, Guili; Xu, Minghan; Shu, Mengjun; Li, Xiaolin; Yang, Zhi; Zhang, Liling; Su, Yanjie; Hu, Nantao; Zhang, Yafei

2016-09-01

Recently, carbon dots (CDs) have been playing an increasingly important role in industrial production and biomedical field because of their excellent properties. As such, finding an efficient method to quickly synthesize a large scale of relatively high purity CDs is of great interest. Herein, a facile and novel microwave method has been applied to prepare nitrogen doped CDs (N-doped CDs) within 8 min using L-glutamic acid as the sole reaction precursor in the solid phase condition. The as-prepared N-doped CDs with an average size of 1.64 nm are well dispersed in aqueous solution. The photoluminescence of N-doped CDs is pH-sensitive and excitation-dependent. The N-doped CDs show a strong blue fluorescence with relatively high fluorescent quantum yield of 41.2%, which remains stable even under high ionic strength. Since the surface is rich in oxygen-containing functional groups, N-doped CDs can be applied to selectively detect Fe3+ with the limit of detection of 10-5 M. In addition, they are also used for cellular bioimaging because of their high fluorescent intensity and nearly zero cytotoxicity. The solid-phase microwave method seems to be an effective strategy to rapidly obtain high quality N-doped CDs and expands their applications in ion detection and cellular bioimaging.

Development of Nonelectronic Part Cyclic Failure Rates

DTIC Science & Technology

1977-12-01

Schilling, W. A., "The User-Oriented Connector," Microwave Journal, Octcber 1976 40. Schneider, C., "Military Relay Reliability," Bell Telephone...polyimide B Diallyl phthalate, melamine , -55 to 200 fluorosilicone, silicone rubber, polysulfone, epoxy resin C Polytetrafluoroethylene (teflon) -55 to 125...propagation, solid state sciences, microwave physics and electronic reliability, maintainabilitg andcompatibility. .,% -UT104, , 8. g z

Solid State Technology Branch of NASA Lewis Research Center

NASA Technical Reports Server (NTRS)

1991-01-01

Reprints of one year's production of research publications (June 1990 to June 1991) are presented. These are organized into three major sections: microwave circuits, both hybrid and monolithic microwave integrated circuits (MMICs); materials and device work; and superconductivity. The included papers also cover more specific topics involving waveguides, phase array antennas, dielectrics, and high temperature superconductors.

77 FR 1017 - Export and Reexport License Requirements for Certain Microwave and Millimeter Wave Electronic...

Federal Register 2010, 2011, 2012, 2013, 2014

2012-01-09

... * * * * * Related Controls: * * * (3) See ECCN 3A982.a for discrete microwave transistors not controlled by...) power amplifiers other than those controlled by this entry. (2) See ECCN 3A001.b.3 for discrete... mobility transistors that are solid state semiconductor switches, diodes or modules rather than discrete...

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.

Entanglement transfer from microwaves to diamond NV centers

NASA Astrophysics Data System (ADS)

Gomez, Angela V.; Rodriguez, Ferney J.; Quiroga, Luis

2014-03-01

Strong candidates to create quantum entangled states in solid-state environments are the nitrogen-vacancy (NV) defect centers in diamond. By the combination of radiation from different wavelength (optical, microwave and radio-frequency), several protocols have been proposed to create entangled states of different NVs. Recently, experimental sources of non-classical microwave radiation have been successfully realized. Here, we consider the entanglement transfer from spatially separated two-mode microwave squeezed (entangled) photons to a pair of NV centers by exploiting the fact that the spin triplet ground state of a NV has a natural splitting with a frequency on the order of GHz (microwave range). We first demonstrate that the transfer process in the simplest case of a single pair of spatially separated NVs is feasible. Moreover, we proceed to extend the previous results to more realistic scenarios where 13C nuclear spin baths surrounding each NV are included, quantifying the degradation of the entanglement transfer by the dephasing/dissipation effects produced by the nuclear baths. Finally, we address the issue of assessing the possibility of entanglement transfer from the squeezed microwave light to two nuclear spins closely linked to different NV center electrons. Facultad de Ciencias Uniandes.

Synthesis and synergistic, additive inhibitory effects of novel spiro derivatives against ringworm infections.

PubMed

Sharma, Gajanand; Sharma, Richa; Dandia, Anshu; Bansal, Preeti

2013-01-01

An environmentally benign solvent free synthesis of various spiro-1,4-dihydropyridines (1,4-DHPs) incorporating 2-oxindole/piperidines is performed in 5-8 min with reasonable purity in 80-90% yield under microwave irradiation using montmorillonite KSF as an inorganic solid support. The reaction is found to be general with respect to various cyclic carbonyl compounds, e.g. cyclohexanone, substituted indole-2,3-dione, and piperidinone derivatives. In our study, these compounds were also found effective against dermatophytes and other fungal organisms. Our results suggest that novel spiro derivatives can be used for the treatment of dermatophytosis or ringworm infections.

Microwave-Assisted Rapid Enzymatic Synthesis of Nucleic Acids.

PubMed

Hari Das, Rakha; Ahirwar, Rajesh; Kumar, Saroj; Nahar, Pradip

2016-07-02

Herein we report microwave-induced enhancement of the reactions catalyzed by Escherichia coli DNA polymerase I and avian myeloblastosis virus-reverse transcriptase. The reactions induced by microwaves result in a highly selective synthesis of nucleic acids in 10-50 seconds. In contrast, same reactions failed to give desired reaction products when carried out in the same time periods, but without microwave irradiation. Each of the reactions was carried out for different duration of microwave exposure time to find the optimum reaction time. The products produced by the respective enzyme upon microwave irradiation of the reaction mixtures were identical to that produced by the conventional procedures. As the microwave-assisted reactions are rapid, microwave could be a useful alternative to the conventional and time consuming procedures of enzymatic synthesis of nucleic acids.

Microwave frequency effect in the formation of Au nanocolloids in polar and non-polar solvents

NASA Astrophysics Data System (ADS)

Horikoshi, Satoshi; Abe, Hideki; Sumi, Takuya; Torigoe, Kanjiro; Sakai, Hideki; Serpone, Nick; Abe, Masahiko

2011-04-01

Given earlier observations that microwave frequencies can have a substantial effect on the photoactivity of a well-known photocatalyst (TiO2), in the synthesis of 3,6-diphenyl-4-n-butylpyridazine through a Diels-Alder process, and in the one-pot solvent-free synthesis of a room-temperature ionic liquid, we proceeded to examine the frequency effects of the 5.8 and 2.45 GHz microwave (MW) radiation in the synthesis of gold nanoparticles in non-polar media, such as oleylamine, which have a low dielectric constant (ε'), and we further examine differences in shape and size under otherwise identical temperature conditions when the synthesis of the gold nanoparticles was carried out in an ethylene glycol polar medium in the presence of polyvinylpyrrolidone. Whereas a change in microwave frequency from 2.45 to 5.8 GHz at equal microwave power levels led to the synthesis of gold nanoparticles in the non-polar media, a change in the microwave frequency had no effect on the size and shape of the gold nanoparticles synthesized in polar media for identical microwave power levels.

Microwave frequency effect in the formation of Au nanocolloids in polar and non-polar solvents.

PubMed

Horikoshi, Satoshi; Abe, Hideki; Sumi, Takuya; Torigoe, Kanjiro; Sakai, Hideki; Serpone, Nick; Abe, Masahiko

2011-04-01

Given earlier observations that microwave frequencies can have a substantial effect on the photoactivity of a well-known photocatalyst (TiO(2)), in the synthesis of 3,6-diphenyl-4-n-butylpyridazine through a Diels-Alder process, and in the one-pot solvent-free synthesis of a room-temperature ionic liquid, we proceeded to examine the frequency effects of the 5.8 and 2.45 GHz microwave (MW) radiation in the synthesis of gold nanoparticles in non-polar media, such as oleylamine, which have a low dielectric constant (ε'), and we further examine differences in shape and size under otherwise identical temperature conditions when the synthesis of the gold nanoparticles was carried out in an ethylene glycol polar medium in the presence of polyvinylpyrrolidone. Whereas a change in microwave frequency from 2.45 to 5.8 GHz at equal microwave power levels led to the synthesis of gold nanoparticles in the non-polar media, a change in the microwave frequency had no effect on the size and shape of the gold nanoparticles synthesized in polar media for identical microwave power levels.

Facile and rapid one-pot microwave-assisted synthesis of Pd-Ni magnetic nanoalloys confined in mesoporous carbons

NASA Astrophysics Data System (ADS)

Martínez de Yuso, Alicia; Le Meins, Jean-Marc; Oumellal, Yassine; Paul-Boncour, Valérie; Zlotea, Claudia; Matei Ghimbeu, Camelia

2016-12-01

An easy and rapid one-pot microwave-assisted soft-template synthesis method for the preparation of Pd-Ni nanoalloys confined in mesoporous carbon is reported. This approach allows the formation of mesoporous carbon and the growth of the particles at the same time, under short microwave irradiation (4 h) compared to the several days spent for the classical approach. In addition, the synthesis steps are diminished and no thermopolymerization step or reduction treatment being required. The influence of the Pd-Ni composition on the particle size and on the carbon characteristics was investigated. Pd-Ni solid solutions in the whole composition range could be obtained, and the metallic composition proved to have an important effect on the nanoparticle size but low influence on carbon textural properties. Small and uniformly distributed nanoparticles were confined in mesoporous carbon with uniform pore size distribution, and dependence between the nanoparticle size and the nanoalloy composition was observed, i.e., increase of the particle size with increasing the Ni content (from 5 to 14 nm). The magnetic properties of the materials showed a strong nanoparticle size and/or composition effect. The blocking temperature of Pd-Ni nanoalloys increases with the increase of Ni amount and therefore of particle size. The magnetization values are smaller than the bulk counterpart particularly for the Ni-rich compositions due to the formed graphitic shells surrounding the particles inducing a dead magnetic layer.

Extended papers selected from ESSDERC 2015

NASA Astrophysics Data System (ADS)

Grasser, Tibor; Schmitz, Jurriaan; Lemme, Max C.

2016-11-01

This special issue of Solid State Electronics includes 28 papers which have been carefully selected from the best presentations given at the 45th European Solid-State Device Research Conference (ESSDERC 2015) held from September 14-18, 2015 in Graz, Austria. These papers cover a wide range of topics related to the research on solid-state devices. These topics are used also to organize the conference submissions and presentations into 7 tracks: CMOS Processes, Devices and Integration; Opto-, Power- and Microwave Devices; Modeling & Simulation; Characterization, Reliability & Yield; Advanced & Emerging Memories; MEMS, Sensors & Display Technologies; Emerging Non-CMOS Devices & Technologies.

Rapid syntheses of a metal-organic framework material Cu3(BTC)2(H2O)3 under microwave: a quantitative analysis of accelerated syntheses.

PubMed

Khan, Nazmul Abedin; Haque, Enamul; Jhung, Sung Hwa

2010-03-20

A typical MOF material, Cu-BTC has been synthesized with microwave and conventional electric heating in various conditions to elucidate, for the first time, the quantitative acceleration in the synthesis of a MOF by microwaves. The acceleration by microwaves is mainly due to rapid nucleation rather than rapid crystal growth, even though both stages are accelerated. The acceleration in the nucleation stage by microwaves is due to the very large pre-exponential factor (about 1.4 x 10(10) times that of conventional synthesis) in the Arrhenius plot. However, the activation energy for the nucleation in the case of microwave synthesis is higher than the activation energy of conventional synthesis. The large acceleration in the nucleation, compared with that in the crystal growth, is observed once again by the syntheses in two-steps (changing heating methods from microwave into conventional heating or from conventional heating into microwave heating just after the nucleation is completed). The crystal size of Cu-BTC obtained by microwave-nucleation is generally smaller than the Cu-BTC made by conventional-nucleation, probably due to rapid nucleation and the small size of nuclei with microwave-nucleation.

Three Short Stories about Hexaarylbenzene-Porphyrin Scaffolds.

PubMed

Lungerich, Dominik; Hitzenberger, Jakob F; Donaubauer, Wolfgang; Drewello, Thomas; Jux, Norbert

2016-11-14

A feasible two-step synthesis and characterization of a full series of hexaarylbenzene (HAB) substituted porphyrins and tetrabenzoporphyrins is presented. Key steps represent the microwave-assisted porphyrin condensation and the statistical Diels-Alder reaction to the desired HAB-porphyrins. Regarding their applications, they proved to be easily accessible and effective high molecular mass calibrants for (MA)LDI mass spectrometry. The free-base and zinc(II) porphyrin systems, as well as the respective tetrabenzoporphyrins, demonstrate in solid state experiments strong red- and near-infrared-light emission and are potentially interesting for the application in "truly organic" light-emitting devices. Lastly, they represent facile precursors to large polycyclic aromatic hydrocarbon (PAH) substituted porphyrins. We prepared the first tetra-hexa-peri-hexabenzocoronene substituted porphyrin, which represents the largest prepared PAH-porphyrin conjugate to date. © 2016 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

An electron-deficient small molecule accessible from sustainable synthesis and building blocks for use as a fullerene alternative in organic photovoltaics.

PubMed

McAfee, Seth M; Topple, Jessica M; Payne, Abby-Jo; Sun, Jon-Paul; Hill, Ian G; Welch, Gregory C

2015-04-27

An electron-deficient small molecule accessible from sustainable isoindigo and phthalimide building blocks was synthesized via optimized synthetic procedures that incorporate microwave-assisted synthesis and a heterogeneous catalyst for Suzuki coupling, and direct heteroarylation carbon-carbon bond forming reactions. The material was designed as a non-fullerene acceptor with the help of DFT calculations and characterized by optical, electronic, and thermal analysis. Further investigation of the material revealed a differing solid-state morphology with the use of three well-known processing conditions: thermal annealing, solvent vapor annealing and small volume fractions of 1,8-diiodooctane (DIO) additive. These unique morphologies persist in the active layer blends and have demonstrated a distinct influence on device performance. Organic photovoltaic-bulk heterojunction (OPV-BHJ) devices show an inherently high open circuit voltage (Voc ) with the best power conversion efficiency (PCE) cells reaching 1.0 V with 0.4 v/v % DIO as a processing additive. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Synthesis of POSS-based ionic conductors with low glass transition temperatures for efficient solid-state dye-sensitized solar cells.

PubMed

Zhang, Wei; Wang, Zhong-Sheng

2014-07-09

Replacing liquid-state electrolytes with solid-state electrolytes has been proven to be an effective way to improve the durability of dye-sensitized solar cells (DSSCs). We report herein the synthesis of amorphous ionic conductors based on polyhedral oligomeric silsesquioxane (POSS) with low glass transition temperatures for solid-state DSSCs. As the ionic conductor is amorphous and in the elastomeric state at the operating temperature of DSSCs, good pore filling in the TiO2 film and good interfacial contact between the solid-state electrolyte and the TiO2 film can be guaranteed. When the POSS-based ionic conductor containing an allyl group is doped with only iodine as the solid-state electrolyte without any other additives, power conversion efficiency of 6.29% has been achieved with good long-term stability under one-sun soaking for 1000 h.

All solid-state high power microwave source with high repetition frequency.

PubMed

Bragg, J-W B; Sullivan, W W; Mauch, D; Neuber, A A; Dickens, J C

2013-05-01

An all solid-state, megawatt-class high power microwave system featuring a silicon carbide (SiC) photoconductive semiconductor switch (PCSS) and a ferrimagnetic-based, coaxial nonlinear transmission line (NLTL) is presented. A 1.62 cm(2), 50 kV 4H-SiC PCSS is hard-switched to produce electrical pulses with 7 ns full width-half max (FWHM) pulse widths at 2 ns risetimes in single shot and burst-mode operation. The PCSS resistance drops to sub-ohm when illuminated with approximately 3 mJ of laser energy at 355 nm (tripled Nd:YAG) in a single pulse. Utilizing a fiber optic based optical delivery system, a laser pulse train of four 7 ns (FWHM) signals was generated at 65 MHz repetition frequency. The resulting electrical pulse train from the PCSS closely follows the optical input and is utilized to feed the NLTL generating microwave pulses with a base microwave-frequency of about 2.1 GHz at 65 MHz pulse repetition frequency (prf). Under typical experimental conditions, the NLTL produces sharpened output risetimes of 120 ps and microwave oscillations at 2-4 GHz that are generated due to damped gyromagnetic precession of the ferrimagnetic material's axially pre-biased magnetic moments. The complete system is discussed in detail with its output matched into 50 Ω, and results covering MHz-prf in burst-mode operation as well as frequency agility in single shot operation are discussed.

Coherent quantum dynamics of a superconducting flux qubit.

PubMed

Chiorescu, I; Nakamura, Y; Harmans, C J P M; Mooij, J E

2003-03-21

We have observed coherent time evolution between two quantum states of a superconducting flux qubit comprising three Josephson junctions in a loop. The superposition of the two states carrying opposite macroscopic persistent currents is manipulated by resonant microwave pulses. Readout by means of switching-event measurement with an attached superconducting quantum interference device revealed quantum-state oscillations with high fidelity. Under strong microwave driving, it was possible to induce hundreds of coherent oscillations. Pulsed operations on this first sample yielded a relaxation time of 900 nanoseconds and a free-induction dephasing time of 20 nanoseconds. These results are promising for future solid-state quantum computing.

A Novel Method of Preparation of Inorganic Glasses by Microwave Irradiation

NASA Astrophysics Data System (ADS)

Vaidhyanathan, B.; Ganguli, Munia; Rao, K. J.

1994-12-01

Microwave heating is shown to provide an extremely facile and automatically temperature-controlled route to the synthesis of glasses. Glass-forming compositions of several traditional and novel glasses were melted in a kitchen microwave oven, typically within 5 min and quenched into glasses. This is only a fraction of the time required in normal glass preparation methods. The rapidity of melting minimizes undesirable features such as loss of components of the glass, variation of oxidation states of metal ions, and oxygen loss leading to reduced products in the glass such as metal particles. This novel procedure of preparation is applicable when at least one of the components of the glass-forming mixture absorbs microwaves.

Facile synthesis and microwave absorbability of C@Ni–NiO core–shell hybrid solid sphere and multi-shelled NiO hollow sphere

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

Wu, Hongjing, E-mail: wuhongjing@mail.nwpu.edu.cn; Wu, Guanglei, E-mail: wuguanglei@mail.xjtu.edu.cn; Wu, Qiaofeng

2014-11-15

We reported the preparation of C@Ni–NiO core–shell hybrid solid spheres or multi-shelled NiO hollow spheres by combining a facile hydrothermal route with a calcination process in H{sub 2} or air atmosphere, respectively. The synthesized C@Ni–NiO core–shell solid spheres with diameters of approximately 2–6 μm were in fact built from dense NiO nanoparticles coated by random two-dimensional metal Ni nanosheets without any visible pores. The multi-shelled NiO hollow spheres were built from particle-like ligaments and there are a lot of pores with size of several nanometers on the surface. Combined Raman spectra with X-ray photoelectron spectra (XPS), it suggested that themore » defects in the samples play a limited role in the dielectric loss. Compared with the other samples, the permeability of the samples calcined in H{sub 2} and air was increased slightly and the natural resonance frequency shifted to higher frequency (7, 11 and 14 GHz, respectively), leading to an enhancement of microwave absorption property. For the sample calcined in H{sub 2}, an optimal reflection loss less than − 10 was obtained at 7 GHz with a matching thickness of 5.0 mm. Our study demonstrated the potential application of C@Ni–NiO core–shell hybrid solid sphere or multi-shelled NiO hollow sphere as a more efficient electromagnetic (EM) wave absorber. - Highlights: • C@Ni–NiO core–shell hybrid solid sphere was synthesized by a facile method. • Multi-shelled NiO hollow sphere was synthesized by a facile method. • It suggested that the defects in the samples play a limited role in dielectric loss. • The permeability of the samples calcined in H{sub 2} and air was increased. • Microwave absorbability of C@Ni–NiO core–shell hybrid solid sphere was investigated.« less

Rapid microwave-assisted synthesis of polydextrose and identification of structure and function.

PubMed

Wang, Haisong; Shi, Yonghui; Le, Guowei

2014-11-26

Microwave irradiation is a rapid and efficient method to synthesize oligomers and can be employed in polysaccharides production. As an artificial polysaccharide, polydextrose is known for its solid performance in food processing and its additional health benefits. This study was aimed at producing polydextrose by microwave irradiation using glucose and sorbitol as substrates; water and phosphoric acid as initiator and catalyst. The actual maximum yield was 99%. Synthetic polydextrose were purified by ethanol elution and Sepherdex G-25 column chromatography. Its purity was demonstrated by the high-performance gel-permeation chromatography as a single symmetrical sharp peak, additionally the average molecular weight was calculated to be 2.131 kDa. FT-IR spectra showed that the synthesized polydextrose has the structural feature similar to Polydextrose-Litesse(®). In vitro fermentation revealed that polydextrose possesses the biological function similar to Polydextrose-Litesse(®) in increasing the concentration of short chain fatty acid and decreasing pH. This research demonstrated the feasibility of a rapid and efficient microwave mediated method to synthesize polydextrose and potentially other value added carbohydrate polymers. Copyright © 2014 Elsevier Ltd. All rights reserved.

Rapid microwave assisted synthesis of YIn1-xMnxO3 blue pigments: Synthesis, microstructure and optical properties

NASA Astrophysics Data System (ADS)

Zhou, Yuncheng; Jiang, Peng; Kuang, Jianlei; Yang, Xueshan; Cao, Wenbin

2018-07-01

The YIn1-xMnxO3 (0.1 ≤x ≤ 0.5) blue pigment samples are successfully prepared through a sol-gel process followed by microwave assisted sintering process. All the samples are shown single phases in the X-ray diffraction results. In the morphology study from scanning electronic microscope, the samples are composed of loosely connected small particles. The oxidation state of Mn is confirmed to be 3 + from the results of X-ray photonelectronic scan. The optical properties are characterized by UV-Visible spectrum and UV-visible-NIR spectrum. The samples exhibit intense blue color and they show small absorption in infrared region.

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.

MICROWAVES IN ORGANIC SYNTHESIS

EPA Science Inventory

The effect of microwaves, a non-ionizing radiation, on organic reactions is described both in polar solvents and under solvent-free conditions. The special applications are highlighted in the context of solventless organic synthesis which involve microwave (MW) exposure of neat r...

CHEMICAL SYNTHESIS & TRANSFORMATIONS USING MICROWAVES

EPA Science Inventory

A historical account of the utility of microwaves in a variety of chemical synthesis applications will be presented, including a solvent-free strategy that involves microwave (MW) exposure of neat reactants (undiluted) catalyzed by the surfaces of recyclable mineral supports such...

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.

One Step Combustion Synthesis Of YAG:Ce Phosphor For Solid State Lighting

NASA Astrophysics Data System (ADS)

Yadav, Pooja; Gupta, K. Vijay Kumar; Muley, Aarti; Joshi, C. P.; Moharil, S. V.

2011-10-01

YAG:Ce is an important phosphor having applications in various fields ranging from solid state lighting to scintillation detectors. YAG phosphors doped with activators are mainly synthesized by solid state reaction techniques that require high sintering temperatures (above 1500°C) to eliminate YAM and YAP phases. Though several soft chemical routes have been explored for synthesis of YAG, most of these methods are complex and phase pure materials are not obtained in one step, but prolonged annealing at temperatures around 1000 C or above becomes necessary. One step combustion synthesis of YAG:Ce3+ and related phosphors carried out at 500 C furnace temperature is reported here. Activation with Ce3+ could be achieved during the synthesis without taking recourse to any post-combustion thermal treatment. LEDs prepared from the combustion synthesized YAG:Ce3+, exhibited properties comparable to those produced from the commercial phosphor.

Modern Microwave and Millimeter-Wave Power Electronics

NASA Astrophysics Data System (ADS)

Barker, Robert J.; Luhmann, Neville C.; Booske, John H.; Nusinovich, Gregory S.

2005-04-01

A comprehensive study of microwave vacuum electronic devices and their current and future applications While both vacuum and solid-state electronics continue to evolve and provide unique solutions, emerging commercial and military applications that call for higher power and higher frequencies to accommodate massive volumes of transmitted data are the natural domain of vacuum electronics technology. Modern Microwave and Millimeter-Wave Power Electronics provides systems designers, engineers, and researchers-especially those with primarily solid-state training-with a thoroughly up-to-date survey of the rich field of microwave vacuum electronic device (MVED) technology. This book familiarizes the R&D and academic communities with the capabilities and limitations of MVED and highlights the exciting scientific breakthroughs of the past decade that are dramatically increasing the compactness, efficiency, cost-effectiveness, and reliability of this entire class of devices. This comprehensive text explores a wide range of topics: * Traveling-wave tubes, which form the backbone of satellite and airborne communications, as well as of military electronic countermeasures systems * Microfabricated MVEDs and advanced electron beam sources * Klystrons, gyro-amplifiers, and crossed-field devices * "Virtual prototyping" of MVEDs via advanced 3-D computational models * High-Power Microwave (HPM) sources * Next-generation microwave structures and circuits * How to achieve linear amplification * Advanced materials technologies for MVEDs * A Web site appendix providing a step-by-step walk-through of a typical MVED design process Concluding with an in-depth examination of emerging applications and future possibilities for MVEDs, Modern Microwave and Millimeter-Wave Power Electronics ensures that systems designers and engineers understand and utilize the significant potential of this mature, yet continually developing technology. SPECIAL NOTE: All of the editors' royalties realized from the sale of this book will fund the future research and publication activities of graduate students in the vacuum electronics field.

GREENER SYNTHESIS OF HETEROCYCLIC COMPOUNDS USING MICROWAVE IRRADIATION

EPA Science Inventory

An introduction of our interest in the microwave-assisted greener synthesis of a variety of heterocyclic compounds will be presented. It involves microwave (MW) exposure of neat reactants (undiluted) catalyzed by the surfaces of recyclable mineral supports, such as alumina, sili...

Solid state nuclear magnetic resonance with magic-angle spinning and dynamic nuclear polarization below 25 K

PubMed Central

Thurber, Kent R.; Potapov, Alexey; Yau, Wai-Ming; Tycko, Robert

2012-01-01

We describe an apparatus for solid state nuclear magnetic resonance (NMR) with dynamic nuclear polarization (DNP) and magic-angle spinning (MAS) at 20–25 K and 9.4 Tesla. The MAS NMR probe uses helium to cool the sample space and nitrogen gas for MAS drive and bearings, as described earlier (Thurber et al., J. Magn. Reson. 2008) [1], but also includes a corrugated waveguide for transmission of microwaves from below the probe to the sample. With a 30 mW circularly polarized microwave source at 264 GHz, MAS at 6.8 kHz, and 21 K sample temperature, greater than 25-fold enhancements of cross-polarized 13C NMR signals are observed in spectra of frozen glycerol/water solutions containing the triradical dopant DOTOPA-TEMPO when microwaves are applied. As demonstrations, we present DNP-enhanced one-dimensional and two-dimensional 13C MAS NMR spectra of frozen solutions of uniformly 13C-labeled L-alanine and melittin, a 26-residue helical peptide that we have synthesized with four uniformly 13C-labeled amino acids. PMID:23238592

Solid state nuclear magnetic resonance with magic-angle spinning and dynamic nuclear polarization below 25 K.

PubMed

Thurber, Kent R; Potapov, Alexey; Yau, Wai-Ming; Tycko, Robert

2013-01-01

We describe an apparatus for solid state nuclear magnetic resonance (NMR) with dynamic nuclear polarization (DNP) and magic-angle spinning (MAS) at 20-25 K and 9.4 Tesla. The MAS NMR probe uses helium to cool the sample space and nitrogen gas for MAS drive and bearings, as described earlier, but also includes a corrugated waveguide for transmission of microwaves from below the probe to the sample. With a 30 mW circularly polarized microwave source at 264 GHz, MAS at 6.8 kHz, and 21 K sample temperature, greater than 25-fold enhancements of cross-polarized (13)C NMR signals are observed in spectra of frozen glycerol/water solutions containing the triradical dopant DOTOPA-TEMPO when microwaves are applied. As demonstrations, we present DNP-enhanced one-dimensional and two-dimensional (13)C MAS NMR spectra of frozen solutions of uniformly (13)C-labeled l-alanine and melittin, a 26-residue helical peptide that we have synthesized with four uniformly (13)C-labeled amino acids. Published by Elsevier Inc.

Materials research at Stanford University

NASA Technical Reports Server (NTRS)

1976-01-01

Information briefly describing the total research activity related to the science of materials is reported. Emphasis is placed on physical and mechanical properties of composite materials, energy transportation, superconductors, microwave electronics, and solid state electrochemistry.

Electrical and electronic devices and components: A compilation

NASA Technical Reports Server (NTRS)

1975-01-01

Components and techniques which may be useful in the electronics industry are described. Topics discussed include transducer technology, printed-circuit technology, solid state devices, MOS transistors, Gunn device, microwave antennas, and position indicators.

Characterization of biomass waste torrefaction under conventional and microwave heating.

PubMed

Ho, Shih-Hsin; Zhang, Congyu; Chen, Wei-Hsin; Shen, Ying; Chang, Jo-Shu

2018-05-13

To evaluate the potential of microwave heating for biomass torrefaction, the torrefaction performances and energy utilization of coffee grounds and microalga residue, under conventional and microwave heating were investigated and compared with each other. For the two biomass samples, the dehydrogenation of the coffee grounds was more sensitive to torrefaction severity, whereas the microalga residue consumed more energy under the same torrefaction conditions. Microwave heating under lower torrefaction severity had a higher energy efficiency. As regard to the lower solid yields or higher torrefaction severity, the energy efficiency of microwave heating was close to that of conventional heating, irrespective of the feedstocks. This revealed the comparable energy consumption state between the two heating modes. Accordingly, it is concluded that microwave torrefaction is more efficient for biomass upgrading and densification than conventional torrefaction. Copyright © 2018 Elsevier Ltd. All rights reserved.

Solar power satellite system definition study, volume 4, phase 2

NASA Technical Reports Server (NTRS)

1979-01-01

Results of an overall evaluation of the solar power satellite concept are reported. Specific topics covered include: solid state sandwich configuration; parametric development of reliability design; power distribution system for solid state solar power satellites; multibeam transmission; GEO base system configuration; suppression of the heavy lift launch vehicle trajectory; conceptual design of an offshore space center facility; solar power satellite development and operations scenario; and microwave power transmission technology, advancement, development, and facility requirements.

Solid State Research

DTIC Science & Technology

1999-02-23

pumped at frequencies up to 5.5 kHz (with 10-W pumping). At high pulse repetition rates the radius of the beam waist decreases to ~60 jum, owing to...1998) A 1.3-GHz SOI CMOS Test Chip for R. Berger Low-Power High -Speed Pulse W. G. Lyons Processing A. M. Soares IEEE J. Solid-State Circuits...Goodhue D. E. Mull J. M. Rossler Y. Royter C.G.Fonstad* /. Vac. Sei. Technol. Modeling the Microwave Impedance of High -Tc Long Josephson

Path Entanglement of Continuous-Variable Quantum Microwaves

NASA Astrophysics Data System (ADS)

Menzel, E. P.; Deppe, F.; Eder, P.; Zhong, L.; Haeberlein, M.; Baust, A.; Hoffmann, E.; Marx, A.; Gross, R.; di Candia, R.; Solano, E.; Ballester, D.; Ihmig, M.; Inomata, K.; Yamamoto, T.; Nakamura, Y.

2013-03-01

Entanglement is a quantum mechanical phenomenon playing a key role in quantum communication and information processing protocols. Here, we report on frequency-degenerate entanglement between continuous-variable quantum microwaves propagating along two separated paths. In our experiment, we combine a squeezed and a vacuum state via a beam splitter. Overcoming the challenges imposed by the low photon energies in the microwave regime, we reconstruct the squeezed state and, independently from this, detect and quantify the produced entanglement via correlation measurements (E. P. Menzel et al., arXiv:1210.4413). Our work paves the way towards quantum communication and teleportation with continuous variables in the microwave regime. This work is supported by SFB 631, German Excellence Initiative via NIM, EU projects SOLID, CCQED and PROMISCE, MEXT Kakenhi ``Quantum Cybernetics'', JSPS FIRST Program, the NICT Commissioned Research, EPSRC EP/H050434/1, Basque Government IT472-10, and Spanish MICINN FIS2009-12773-C02-01.

Lifetime of excess electrons in Cu–Zn–Sn–Se powders

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

Novikov, G. F., E-mail: ngf@icp.ac.ru; Gapanovich, M. V.; Gremenok, V. F.

2017-01-15

The method of time-resolved microwave photoconductivity at a frequency of 36 GHz in the range of temperatures of 200–300 K is used to study the kinetics of the annihilation of charge carriers in Cu–Zn–Sn–Se powders obtained by the solid-phase method of synthesis in cells. The lifetime of excess electrons at room temperature is found to be shorter than 5 ns. The activation energy for the process of recombination amounted to E{sub a} ~ 0.054 eV.

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

Biasotto, G.; Simoes, A.Z., E-mail: alezipo@yahoo.com; Foschini, C.R.

Highlights: Black-Right-Pointing-Pointer BiFeO{sub 3} (BFO) nanoparticles were grown by hydrothermal microwave method (HTMW). Black-Right-Pointing-Pointer The soaking time is effective in improving phase formation. Black-Right-Pointing-Pointer Rietveld refinement reveals an orthorhombic structure. Black-Right-Pointing-Pointer The observed magnetism of the BFO crystallites is a consequence of particle size. Black-Right-Pointing-Pointer The HTMW is a genuine technique for low temperatures and short times of synthesis. -- Abstract: Hydrothermal microwave method (HTMW) was used to synthesize crystalline bismuth ferrite (BiFeO{sub 3}) nanoparticles (BFO) in the temperature of 180 Degree-Sign C with times ranging from 5 min to 1 h. BFO nanoparticles were characterized by means of X-raymore » analyses, FT-IR, Raman spectroscopy, TG-DTA and FE-SEM. X-ray diffraction results indicated that longer soaking time was benefit to refraining the formation of any impurity phases and growing BFO crystallites into almost single-phase perovskites. Typical FT-IR spectra for BFO nanoparticles presented well defined bands, indicating a substantial short-range order in the system. TG-DTA analyses confirmed the presence of lattice OH{sup -} groups, commonly found in materials obtained by HTMW process. Compared with the conventional solid-state reaction process, submicron BFO crystallites with better homogeneity could be produced at the temperature as low as 180 Degree-Sign C. These results show that the HTMW synthesis route is rapid, cost effective, and could be used as an alternative to obtain BFO nanoparticles in the temperature of 180 Degree-Sign C for 1 h.« less

Investigation of Local Structures in Cation-ordered Microwave Dielectric A Solid-state NMR and First Principle Calculation Study

NASA Astrophysics Data System (ADS)

Kalfarisi, Rony G.

Solid-state Nuclear Magnetic Resonance (ssNMR) spectroscopy has proven to be a powerful method to probe the local structure and dynamics of a system. In powdered solids, the nuclear spins experience various anisotropic interactions which depend on the molecular orientation. These anisotropic interactions make ssNMR very useful as they give a specific appearance to the resonance lines of the spectra. The position and shape of these resonance lines can be related to local structure and dynamics of the system under study. My research interest has focused around studying local structures and dynamics of quadrupolar nuclei in materials using ssNMR spectroscopy. 7Li and 93Nb ssNMR magic angle spinning (MAS) spectra, acquired at 17.6 and 7.06 T, have been used to evaluate the structural and dynamical properties of cation-ordered microwave dielectric materials. Microwave dielectric materials are essential in the application of wireless telecommunication, biomedical engineering, and other scientific and industrial implementations that use radio and microwave signals. The study of the local environment with respect to average structure, such as X-ray diffraction study, is essential for the better understanding of the correlations between structures and properties of these materials. The investigation for short and medium range can be performed with the use of ssNMR techniques. Even though XRD results show cationic ordering at the B-site (third coordination sphere), NMR spectra show a presence of disorder materials. This was indicated by the observation of a distribution in NMR parameters derived from experimental . {93}Nb NMR spectraand supported by theoretical calculations.

MICROWAVE-ASSISTED SYNTHESIS OF NOBLE NANOSTRUCTURES USING BIODEGRADABLE POLYMER CARBOXYMETHYL CELLULOSE

EPA Science Inventory

Microwave-assisted synthesis of noble nanostructures (Au, Pt, and Pd) using biodegradable polymer carboxymethyl cellulose (CMC) under microwave irradiation (MW) at 100 0C is reported. The reaction occurs within a few minutes, whereas at room temperature the reaction does not pro...

Direct Synthesis of Microwave Waveforms for Quantum Computing

NASA Astrophysics Data System (ADS)

Raftery, James; Vrajitoarea, Andrei; Zhang, Gengyan; Leng, Zhaoqi; Srinivasan, Srikanth; Houck, Andrew

Current state of the art quantum computing experiments in the microwave regime use control pulses generated by modulating microwave tones with baseband signals generated by an arbitrary waveform generator (AWG). Recent advances in digital analog conversion technology have made it possible to directly synthesize arbitrary microwave pulses with sampling rates of 65 gigasamples per second (GSa/s) or higher. These new ultra-wide bandwidth AWG's could dramatically simplify the classical control chain for quantum computing experiments, presenting potential cost savings and reducing the number of components that need to be carefully calibrated. Here we use a Keysight M8195A AWG to study the viability of such a simplified scheme, demonstrating randomized benchmarking of a superconducting qubit with high fidelity.

Catalytic and atmospheric effects on microwave pyrolysis of corn stover.

PubMed

Huang, Yu-Fong; Kuan, Wen-Hui; Chang, Chi-Cheng; Tzou, Yu-Min

2013-03-01

Corn stover, which is one of the most abundant agricultural residues around the world, could be converted into valuable biofuels and bio based products by means of microwave pyrolysis. After the reaction at the microwave power level of 500W for the processing time of 30min, the reaction performance under N2 atmosphere was generally better than under CO2 atmosphere. This may be due to the better heat absorbability of CO2 molecules to reduce the heat for stover pyrolysis. Most of the metal-oxide catalysts effectively increased the maximum temperature and mass reduction ratio but lowered the calorific values of solid residues. The gas most produced was CO under N2 atmosphere but CO2 under CO2 atmosphere. Catalyst addition lowered the formation of PAHs and thus made liquid products less toxic. More liquid products and less gas products were generated when using the catalysts possibly due to the existence of the Fischer-Tropsch synthesis. Copyright © 2013 Elsevier Ltd. All rights reserved.

Synthesis, magnetic and ethanol gas sensing properties of semiconducting magnetite nanoparticles

NASA Astrophysics Data System (ADS)

Al-Ghamdi, Ahmed A.; Al-Hazmi, Faten; Al-Tuwirqi, R. M.; Alnowaiser, F.; Al-Hartomy, Omar A.; El-Tantawy, Farid; Yakuphanoglu, F.

2013-05-01

The superparamagnetic magnetite (Fe3O4) nanoparticles with an average size of 7 nm were synthesized using a rapid and facile microwave hydrothermal technique. The structure of the magnetite nanoparticles was characterized by X-ray diffraction (X-ray), field effect scanning electron microscopy (FESEM), energy dispersive X-ray spectroscopy (EDS), and transmission electron microscopy (TEM). The prepared Fe3O4 was shown to have a cubic phase of pure magnetite. Magnetization hysteresis loop shows that the synthesized magnetite exhibits no hysteretic features with a superparamagnetic behavior. The ethanol gas sensing properties of the synthesized magnetite were investigated, and it was found that the responsibility time is less than 10 s with good reproducibility for ethanol sensor. Accordingly, it is evaluated that the magnetite nanoparticles can be effectively used as a solid state ethanol sensor in industrial commercial product applications.

Seeing through walls at the nanoscale: Microwave microscopy of enclosed objects and processes in liquids

DOE PAGES

Velmurugan, Jeyavel; Kalinin, Sergei V.; Kolmakov, Andrei; ...

2016-02-11

Here, noninvasive in situ nanoscale imaging in liquid environments is a current imperative in the analysis of delicate biomedical objects and electrochemical processes at reactive liquid–solid interfaces. Microwaves of a few gigahertz frequencies offer photons with energies of ≈10 μeV, which can affect neither electronic states nor chemical bonds in condensed matter. Here, we describe an implementation of scanning near-field microwave microscopy for imaging in liquids using ultrathin molecular impermeable membranes separating scanning probes from samples enclosed in environmental cells. We imaged a model electroplating reaction as well as individual live cells. Through a side-by-side comparison of the microwave imagingmore » with scanning electron microscopy, we demonstrate the advantage of microwaves for artifact-free imaging.« less

RF Testing Of Microwave Integrated Circuits

NASA Technical Reports Server (NTRS)

Romanofsky, R. R.; Ponchak, G. E.; Shalkhauser, K. A.; Bhasin, K. B.

1988-01-01

Fixtures and techniques are undergoing development. Four test fixtures and two advanced techniques developed in continuing efforts to improve RF characterization of MMIC's. Finline/waveguide test fixture developed to test submodules of 30-GHz monolithic receiver. Universal commercially-manufactured coaxial test fixture modified to enable characterization of various microwave solid-state devices in frequency range of 26.5 to 40 GHz. Probe/waveguide fixture is compact, simple, and designed for non destructive testing of large number of MMIC's. Nondestructive-testing fixture includes cosine-tapered ridge, to match impedance wavequide to microstrip. Advanced technique is microwave-wafer probing. Second advanced technique is electro-optical sampling.

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

Teka, S.; Gaied, A.; Jaballah, N.

Highlights: • Microwave-assisted synthesis of rotaxane based on anthracene and β-cyclodextrin. • Morphological and optical characterization of thin solid film. • Elaboration of impedimetric gold/rotaxane sensor. • Investigation of the membrane sensitivity towards Hg{sup 2+}, Cu{sup 2+} and Pb{sup 2+} cations. - Abstract: An impedimetric sensor based on a new semi-conducting rotaxane has been described for detection of toxic cations. The rotaxane, consists on a π-conjugated material encapsulated into β-cyclodextrin (β-CD); it has been synthesized via the Williamson reaction under microwaves irradiation. The supramolecular structure of the compound was confirmed by NMR and FT-IR spectroscopies. A thin solid film ofmore » the rotaxane was deposited by spin-coating to develop a new electrochemical sensor. The morphological properties of the organic membrane were evaluated using contact angle measurements and atomic force microscopy. The gold/rotaxane/solution interfaces were investigated by electrochemical impedance spectroscopy and the obtained data were fitted using an equivalent electrical circuit. The response of the gold/rotaxane membrane towards Hg{sup 2+}, Cu{sup 2+} and Pb{sup 2+} cations was studied and the results showed a good sensitivity to the mercury cations.« less

Solid effect in magic angle spinning dynamic nuclear polarization

NASA Astrophysics Data System (ADS)

Corzilius, Björn; Smith, Albert A.; Griffin, Robert G.

2012-08-01

For over five decades, the solid effect (SE) has been heavily utilized as a mechanism for performing dynamic nuclear polarization (DNP). Nevertheless, it has not found widespread application in contemporary, high magnetic field DNP experiments because SE enhancements display an ω _0 ^{ - 2} field dependence. In particular, for nominally forbidden zero and double quantum SE transitions to be partially allowed, it is necessary for mixing of adjacent nuclear spin states to occur, and this leads to the observed field dependence. However, recently we have improved our instrumentation and report here an enhancement of ɛ = 91 obtained with the organic radical trityl (OX063) in magic angle spinning experiments performed at 5 T and 80 K. This is a factor of 6-7 higher than previous values in the literature under similar conditions. Because the solid effect depends strongly on the microwave field strength, we attribute this large enhancement to larger microwave field strengths inside the sample volume, achieved with more efficient coupling of the gyrotron to the sample chamber. In addition, we develop a theoretical model to explain the dependence of the buildup rate of enhanced nuclear polarization and the steady-state enhancement on the microwave power. Buildup times and enhancements were measured as a function of 1H concentration for both trityl and Gd-DOTA. Comparison of the results indicates that for trityl the initial polarization step is the slower, rate-determining step. However, for Gd-DOTA the spread of nuclear polarization via homonuclear 1H spin diffusion is rate-limiting. Finally, we discuss the applicability of the solid effect at fields > 5 T and the requirements to address the unfavorable field dependence of the solid effect.

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

Wang, Hui; Chen, Yan; Hood, Zachary D.

All-solid-state sodium batteries, using abundant sodium resources and solid electrolyte, hold much promise for safe, low cost, large-scale energy storage. To realize the practical applications of all solid Na-ion batteries at ambient temperature, the solid electrolytes are required to have high ionic conductivity, chemical stability, and ideally, easy preparation. Ceramic electrolytes show higher ionic conductivity than polymers, but they often require extremely stringent synthesis conditions, either high sintering temperature above 1000 C or long-time, low-energy ball milling. Herein, we report a new synthesis route for Na 3SbS 4, a novel Na superionic conductor that needs much lower processing temperature belowmore » 200 C and easy operation. This new solid electrolyte exhibits a remarkable ionic conductivity of 1.05 mS cm -1 at 25 °C and is chemically stable under ambient atmosphere. In conclusion, this synthesis process provides unique insight into the current state-of-the-art solid electrolyte preparation and opens new possibilities for the design of similar materials.« less

Microwave plasma chemical synthesis of nanocrystalline carbon film structures and study their properties

NASA Astrophysics Data System (ADS)

Bushuev, N.; Yafarov, R.; Timoshenkov, V.; Orlov, S.; Starykh, D.

2015-08-01

The self-organization effect of diamond nanocrystals in polymer-graphite and carbon films is detected. The carbon materials deposition was carried from ethanol vapors out at low pressure using a highly non-equilibrium microwave plasma. Deposition processes of carbon film structures (diamond, graphite, graphene) is defined. Deposition processes of nanocrystalline structures containing diamond and graphite phases in different volume ratios is identified. The solid film was obtained under different conditions of microwave plasma chemical synthesis. We investigated the electrical properties of the nanocrystalline carbon films and identified it's from various factors. Influence of diamond-graphite film deposition mode in non-equilibrium microwave plasma at low pressure on emission characteristics was established. This effect is justified using the cluster model of the structure of amorphous carbon. It was shown that the reduction of bound hydrogen in carbon structures leads to a decrease in the threshold electric field of emission from 20-30 V/m to 5 V/m. Reducing the operating voltage field emission can improve mechanical stability of the synthesized film diamond-graphite emitters. Current density emission at least 20 A/cm2 was obtained. Nanocrystalline carbon film materials can be used to create a variety of functional elements in micro- and nanoelectronics and photonics such as cold electron source for emission in vacuum devices, photonic devices, cathodoluminescent flat display, highly efficient white light sources. The obtained graphene carbon net structure (with a net size about 6 μm) may be used for the manufacture of large-area transparent electrode for solar cells and cathodoluminescent light sources

Microwave-Assisted Synthesis of "N"-Phenylsuccinimide

ERIC Educational Resources Information Center

Shell, Thomas A.; Shell, Jennifer R.; Poole, Kathleen A.; Guetzloff, Thomas F.

2011-01-01

A microwave-assisted synthesis of "N"-phenylsuccinimide has been developed for the second-semester organic teaching laboratory. Utilizing this procedure, "N"-phenylsuccinimide can be synthesized in moderate yields (40-60%) by heating a mixture of aniline and succinic anhydride in a domestic microwave oven for four minutes. This technique reduces…

Determining the microwave coupling and operational efficiencies of a microwave plasma assisted chemical vapor deposition reactor under high pressure diamond synthesis operating conditions

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

Nad, Shreya; Department of Physics and Astronomy, Michigan State University, East Lansing, Michigan 48824; Gu, Yajun

2015-07-15

The microwave coupling efficiency of the 2.45 GHz, microwave plasma assisted diamond synthesis process is investigated by experimentally measuring the performance of a specific single mode excited, internally tuned microwave plasma reactor. Plasma reactor coupling efficiencies (η) > 90% are achieved over the entire 100–260 Torr pressure range and 1.5–2.4 kW input power diamond synthesis regime. When operating at a specific experimental operating condition, small additional internal tuning adjustments can be made to achieve η > 98%. When the plasma reactor has low empty cavity losses, i.e., the empty cavity quality factor is >1500, then overall microwave discharge coupling efficienciesmore » (η{sub coup}) of >94% can be achieved. A large, safe, and efficient experimental operating regime is identified. Both substrate hot spots and the formation of microwave plasmoids are eliminated when operating within this regime. This investigation suggests that both the reactor design and the reactor process operation must be considered when attempting to lower diamond synthesis electrical energy costs while still enabling a very versatile and flexible operation performance.« less

Synthesis of azines in solid state: reactivity of solid hydrazine with aldehydes and ketones.

PubMed

Lee, Byeongno; Lee, Kyu Hyung; Cho, Jaeheung; Nam, Wonwoo; Hur, Nam Hwi

2011-12-16

Highly conjugated azines were prepared by solid state grinding of solid hydrazine and carbonyl compounds such as aldehydes and ketones, using a mortar and a pestle. Complete conversion to the azine product is generally achieved at room temperature within 24 h, without using solvents or additives. The solid-state reactions afford azines as the sole products with greater than 97% yield, producing only water and carbon dioxide as waste.

Rapid determination of the volatile components in tobacco by ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction with gas chromatography-mass spectrometry.

PubMed

Yang, Yanqin; Chu, Guohai; Zhou, Guojun; Jiang, Jian; Yuan, Kailong; Pan, Yuanjiang; Song, Zhiyu; Li, Zuguang; Xia, Qian; Lu, Xinbo; Xiao, Weiqiang

2016-03-01

An ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction was first employed to determine the volatile components in tobacco samples. The method combined the advantages of ultrasound, microwave, and headspace solid-phase microextraction. The extraction, separation, and enrichment were performed in a single step, which could greatly simplify the operation and reduce the whole pretreatment time. In the developed method, several experimental parameters, such as fiber type, ultrasound power, and irradiation time, were optimized to improve sampling efficiency. Under the optimal conditions, there were 37, 36, 34, and 36 components identified in tobacco from Guizhou, Hunan, Yunnan, and Zimbabwe, respectively, including esters, heterocycles, alkanes, ketones, terpenoids, acids, phenols, and alcohols. The compound types were roughly the same while the contents were varied from different origins due to the disparity of their growing conditions, such as soil, water, and climate. In addition, the ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction method was compared with the microwave-assisted extraction coupled to headspace solid-phase microextraction and headspace solid-phase microextraction methods. More types of volatile components were obtained by using the ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction method, moreover, the contents were high. The results indicated that the ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction technique was a simple, time-saving and highly efficient approach, which was especially suitable for analysis of the volatile components in tobacco. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Effect of Microwave Radiation Power on the Size of Aggregates of ZnO NPs Prepared Using Microwave Solvothermal Synthesis

PubMed Central

Chudoba, Tadeusz; Gierlotka, Stanisław; Lojkowski, Witold

2018-01-01

This paper reports the possibility of changing the size of zinc oxide nanoparticles (ZnO NPs) aggregates through a change of synthesis parameters. The effect of the changed power of microwave heating on the properties of ZnO NPs obtained by the microwave solvothermal synthesis from zinc acetate dissolved in ethylene glycol was tested for the first time. It was found that the size of ZnO aggregates ranged from 60 to 120 nm depending on the power of microwave radiation used in the synthesis of ZnO NPs. The increase in the microwave radiation power resulted in the reduction of the total synthesis time with simultaneous preservation of the constant size and shape of single ZnO NPs, which were synthesized at a pressure of 4 bar. All the obtained ZnO NPs samples were composed of homogeneous spherical particles that were single crystals with an average size of 27 ± 3 nm with a developed specific surface area of 40 m2/g and the skeleton density of 5.18 ± 0.03 g/cm3. A model of a mechanism explaining the correlation between the size of aggregates and the power of microwaves was proposed. This method of controlling the average size of ZnO NPs aggregates is presented for the first time and similar investigations are not found in the literature. PMID:29783651

Facile solid-state synthesis of oxidation-resistant metal nanoparticles at ambient conditions

NASA Astrophysics Data System (ADS)

Lee, Kyu Hyung; Jung, Hyuk Joon; Lee, Ju Hee; Kim, Kyungtae; Lee, Byeongno; Nam, Dohyun; Kim, Chung Man; Jung, Myung-Hwa; Hur, Nam Hwi

2018-05-01

A simple and scalable method for the synthesis of metal nanoparticles in the solid-state was developed, which can produce nanoparticles in the absence of solvents. Nanoparticles of coinage metals were synthesized by grinding solid hydrazine and the metal precursors in their acetates and oxides at 25 °C. The silver and gold acetates converted completely within 6 min into Ag and Au nanoparticles, respectively, while complete conversion of the copper acetate to the Cu sub-micrometer particles took about 2 h. Metal oxide precursors were also converted into metal nanoparticles by grinding alone. The resulting particles exhibit distinctive crystalline lattice fringes, indicating the formation of highly crystalline phases. The Cu sub-micrometer particles are better resistant to oxidation and exhibit higher conductivity compared to conventional Cu nanoparticles. This solid-state method was also applied for the synthesis of platinum group metals and intermetallic Cu3Au, which can be further extended to synthesize other metal nanoparticles.

Microwave synthesis of molybdenum doped LiFePO4/C and its electrochemical studies.

PubMed

Naik, Amol; P, Sajan C

2016-05-10

A Mo-doped LiFePO4 composite was prepared successfully from an iron carbonyl complex by adopting a facile and rapid microwave assisted solid state method. The evolution of gases from the iron precursor produces a highly porous product. The formation and substitution of Mo in LiFePO4 were confirmed by X-ray diffraction; surface analysis was carried out by scanning electron microscopy, field emission scanning electron microscopy, and transmission electron microscopy. The electrochemical properties of the substituted LiFePO4 were examined by cyclic voltammetry, electrochemical impedance spectroscopy and by recording charge-discharge cycles. It was observed that the as prepared composites consisted of a single phase orthorhombic olivine-type structure, where Mo(6+) was successfully introduced into the M2(Fe) sites. Incorporation of supervalent Mo(6+) introduced Li(+) ion vacancies in LiFePO4. The synthesized material facilitated lithium ion diffusion during charging/discharging due to the charge compensation effect and porosity. The battery performance studies showed that LiMo0.05Fe0.095PO4 exhibited a maximum capacity of 169.7 mA h g(-1) at 0.1 C current density, with admirable stability retention. Even at higher current densities, the retention of the specific capacity was exceptional.

High-power microwave LDMOS transistors for wireless data transmission technologies (Review)

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

Kuznetsov, E. V., E-mail: E.Kouzntsov@tcen.ru; Shemyakin, A. V.

The fields of the application, structure, fabrication, and packaging technology of high-power microwave LDMOS transistors and the main advantages of these devices were analyzed. Basic physical parameters and some technology factors were matched for optimum device operation. Solid-state microwave electronics has been actively developed for the last 10-15 years. Simultaneously with improvement of old devices, new devices and structures are actively being adopted and developed and new semiconductor materials are being commercialized. Microwave LDMOS technology is in demand in such fields as avionics, civil and military radars, repeaters, base stations of cellular communication systems, television and broadcasting transmitters, and transceiversmore » for high-speed wireless computer networks (promising Wi-Fi and Wi-Max standards).« less

Microwave-Mediated Synthesis of Lophine: Developing a Mechanism to Explain a Product

ERIC Educational Resources Information Center

Crouch, R. David; Howard, Jessica L.; Zile, Jennifer L.; Barker, Kathryn H.

2006-01-01

The microwave-mediated preparation of lophine (2,4,5-triphenylimidazole) is described. This experiment allows for an introduction to the emerging technology of microwave-assisted organic synthesis while providing an opportunity for students to employ the principles of carbonyl chemistry in devising a mechanism to explain the formation of the…

Microwave-assisted liquid-liquid microextraction based on solidification of ionic liquid for the determination of sulfonamides in environmental water samples.

PubMed

Song, Ying; Wu, Lijie; Lu, Chunmei; Li, Na; Hu, Mingzhu; Wang, Ziming

2014-12-01

An easy, quick, and green method, microwave-assisted liquid-liquid microextraction based on solidification of ionic liquid, was first developed and applied to the extraction of sulfonamides in environmental water samples. 1-Ethy-3-methylimidazolium hexafluorophosphate, which is a solid-state ionic liquid at room temperature, was used as extraction solvent in the present method. After microwave irradiation for 90 s, the solid-state ionic liquid was melted into liquid phase and used to finish the extraction of the analytes. The ionic liquid and sample matrix can be separated by freezing and centrifuging. Several experimental parameters, including amount of extraction solvent, microwave power and irradiation time, pH of sample solution, and ionic strength, were investigated and optimized. Under the optimum experimental conditions, good linearity was observed in the range of 2.00-400.00 μg/L with the correlation coefficients ranging from 0.9995 to 0.9999. The limits of detection for sulfathiazole, sulfachlorpyridazine, sulfamethoxazole, and sulfaphenazole were 0.39, 0.33, 0.62, and 0.85 μg/L, respectively. When the present method was applied to the analysis of environmental water samples, the recoveries of the analytes ranged from 75.09 to 115.78% and relative standard deviations were lower than 11.89%. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Solid solutions of gadolinium doped zinc oxide nanorods by combined microwave-ultrasonic irradiation assisted crystallization

NASA Astrophysics Data System (ADS)

Kiani, Armin; Dastafkan, Kamran; Obeydavi, Ali; Rahimi, Mohammad

2017-12-01

Nanocrystalline solid solutions consisting of un-doped and gadolinium doped zinc oxide nanorods were fabricated by a modified sol-gel process utilizing combined ultrasonic-microwave irradiations. Polyvinylpyrrolidone, diethylene glycol, and triethylenetetramine respectively as capping, structure directing, and complexing agents were used under ultrasound dynamic aging and microwave heating to obtain crystalline nanorods. Crystalline phase monitoring, lattice parameters and variation, morphology and shape, elemental analysis, functional groups, reducibility, and the oxidation state of emerged species were examined by PXRD, FESEM, TEM, EDX, FTIR, micro Raman, H2-TPR, and EPR techniques. Results have verified that irradiation mechanism of gelation and crystallization reduces the reaction time, augments the crystal quality, and formation of hexagonal close pack structure of Wurtzite morphology. Besides, dissolution of gadolinium within host lattice involves lattice deformation, unit cell distortion, and angular position variation. Structure related shape and growth along with compositional purity were observed through microscopic and spectroscopic surveys. Furthermore, TPR and EPR studies elucidated more detailed behavior upon exposure to the exerted irradiations and subsequent air-annealing including the formed oxidation states and electron trapping centers, presence of gadolinium, zinc, and oxygen disarrays and defects, as well as alteration in the host unit cell via gadolinium addition.

Purchase of Microwave Reactors for Implementation of Small-scale Microwave-accelerated Organic Chemistry Laboratory Program in Undergraduate Curriculum and Synthetic Chemistry Research at HU

DTIC Science & Technology

2015-05-16

synthesis of iron magnetic nanoparticles is being investigated (Appendix A; Scheme IV). In the first step, precursor iron(III) chloride nanoparticles...and other methods. Currently, we are developing a two-step scheme for the synthesis of esters that will require distillation and/or column...recognize the link between them. We are developing for the above purpose, the microwave-assisted, two-step synthesis of high boiling point esters. The

Sr 2Fe 1.5Mo 0.5O 6- δ as a regenerative anode for solid oxide fuel cells

NASA Astrophysics Data System (ADS)

Liu, Qiang; Bugaris, Daniel E.; Xiao, Guoliang; Chmara, Maxwell; Ma, Shuguo; zur Loye, Hans-Conrad; Amiridis, Michael D.; Chen, Fanglin

Sr 2Fe 1.5Mo 0.5O 6- δ (SFM) was prepared using a microwave-assisted combustion synthesis method. Rietveld refinement of powder X-ray diffraction data reveals that SFM crystallizes in the simple cubic perovskite structure with iron and molybdenum disordered on the B-site. No structure transition was observed by variable temperature powder X-ray diffraction measurements in the temperature range of 25-800 °C. XPS results show that the iron and molybdenum valences change with an increase in temperature, where the mixed oxidation states of both iron and molybdenum are believed to be responsible for the increase in the electrical conductivity with increasing temperature. SFM exhibits excellent redox stability and has been used as both anode and cathode for solid oxide fuel cells. Presence of sulfur species in the fuel or direct utilization of hydrocarbon fuel can result in loss of activity, however, as shown in this paper, the anode performance can be regenerated from sulfur poisoning or coking by treating the anode in an oxidizing atmosphere. Thus, SFM can be used as a regenerating anode for direct oxidation of sulfur-containing hydrocarbon fuels.

Phase Transformation of VO2 Nanoparticles Assisted by Microwave Heating

PubMed Central

Sikong, Lek.

2014-01-01

The microwave assisted synthesis nowadays attracts a great deal of attention. Monoclinic phase VO2 (M) was prepared from NH4VO3 and H2C2O4 · 2H2O by a rapid microwave assisted technique. The synthesis parameters, microwave irradiation time, microwave power, and calcinations temperature were systematically varied and their influences on the structure and morphology were evaluated. The microwave power level has been carried out in range 180–600 W. TEM analysis demonstrated nanosized samples. The structural and morphological properties were measured using XRD, TEM, and thermal analyses. The variations of vanadium phase led to thermochromic properties. PMID:24688438

Microwave-Enhanced Organic Syntheses for the Undergraduate Laboratory: Diels-Alder Cycloaddition, Wittig Reaction, and Williamson Ether Synthesis

ERIC Educational Resources Information Center

Baar, Marsha R.; Falcone, Danielle; Gordon, Christopher

2010-01-01

Microwave heating enhanced the rate of three reactions typically performed in our undergraduate organic chemistry laboratory: a Diels-Alder cycloaddition, a Wittig salt formation, and a Williamson ether synthesis. Ninety-minute refluxes were shortened to 10 min using a laboratory-grade microwave oven. In addition, yields improved for the Wittig…

Mechanism of Formation of Li 7 P 3 S 11 Solid Electrolytes through Liquid Phase Synthesis

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

Wang, Yuxing; Lu, Dongping; Bowden, Mark

Crystalline Li7P3S11 is a promising solid electrolyte for all solid state lithium/lithium ion batteries. A controllable liquid phase synthesis of Li7P3S11 is more desirable compared to conventional mechanochemical synthesis, but recent attempts suffer from reduced ionic conductivities. Here we elucidate the formation mechanism of crystalline Li7P3S11 synthesized in the liquid phase (acetonitrile, or ACN). We conclude that the crystalline Li7P3S11 forms through a two-step reaction: 1) formation of solid Li3PS4∙ACN and amorphous Li2S∙P2S5 phases in the liquid phase; 2) solid-state conversion of the two phases. The implication of this two-step reaction mechanism to the morphology control and the transport propertiesmore » of liquid phase synthesized Li7P3S11 is identified and discussed.« less

The application of microwave digestion in decomposing some refractory ore samples with solid fusion agent.

PubMed

Lu, Yan; Li, Gang; Liu, Wei; Yuan, Hongyan; Xiao, Dan

2018-08-15

It is known that most of the refractory ore are the basis of national economy and widely applied in various fields, however, the complexity of the chemical composition and the diversity of the crystallinity in the mineral phases make the sample pre-treatment of refractory ore still remains a challenge. In this work, the complete decomposition of the refractory ore sample can be achieved just by exposing the solid fusion agent and the refractory ore sample in the microwave irradiation environment for a few minutes, and induced by a drop of water. A digestion time of 15 min for 3.0 g solid fusion agent mixture of sodium peroxide/sodium carbonate (Na 2 O 2 /Na 2 CO 3 ) in a corundum crucible via microwave heating is sufficient to decompose 0.1 g refractory ore sample. An excellent microwave digestion solid agent should meet the following conditions, a good decomposition ability, an outstanding ability of absorbing microwave energy and converting it into heat quickly, a higher melting point than the decomposing temperature of the ore sample. In the research, the induction effect of water plays an important role for the microwave digestion. The energy which is released by the reaction of water and the solid fusion agent (Na 2 O 2 ) is the key to decompose refractory ore samples with solid fusion agent, which replenished the total energy required for the microwave digestion and made the microwave digestion completed successfully. This microwave digestion technique has good reproducibility and precision, RSD % for Mo, Fe, Ti, Cr and W in the refractory ore samples were all better than 6, except RSD % for Be of about 8 because of the influence of matrix-effect. Meanwhile, the analysis results of the elements in the refractory ore samples provided by the microwave digestion technique were all in good agreement with the analysis results provided by the traditional fusion method except for Cr in the mixture ore samples. In the study, the non-linear dependence of the electromagnetic and thermal properties of the solid fusion agent on temperature under microwave irradiation and the selective heating of microwave are fully applied in this simple microwave technique. Comparing to the traditional fusion decomposition method, this microwave digestion technique is a simple, economical, fast and energy-saving sample pre-treatment technique. Copyright © 2018 Elsevier B.V. All rights reserved.

Gold Nanoparticle Microwave Synthesis

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

Krantz, Kelsie E.; Christian, Jonathan H.; Coopersmith, Kaitlin

At the nanometer scale, numerous compounds display different properties than those found in bulk material that can prove useful in areas such as medicinal chemistry. Gold nanoparticles, for example, display promise in newly developed hyperthermia therapies for cancer treatment. Currently, gold nanoparticle synthesis is performed via the hot injection technique which has large variability in final particle size and a longer reaction time. One underdeveloped area by which these particles could be produced is through microwave synthesis. To initiate heating, microwaves agitate polar molecules creating a vibration that gives off the heat energy needed. Previous studies have used microwaves formore » gold nanoparticle synthesis; however, polar solvents were used that partially absorbed incident microwaves, leading to partial thermal heating of the sample rather than taking full advantage of the microwave to solely heat the gold nanoparticle precursors in a non-polar solution. Through this project, microwaves were utilized as the sole heat source, and non-polar solvents were used to explore the effects of microwave heating only as pertains to the precursor material. Our findings show that the use of non-polar solvents allows for more rapid heating as compared to polar solvents, and a reduction in reaction time from 10 minutes to 1 minute; this maximizes the efficiency of the reaction, and allows for reproducibility in the size/shape of the fabricated nanoparticles.« less

Low Loss Substrates for Microwave Applications and Sol-Gel Processing of Superconductors

DTIC Science & Technology

1994-03-31

crystallographic axis normal to solid state technology, in the growth of ferrimagnetic garnets the substrate plane) or. better, in "epitaxial" films (i.e...hay- by liquid phase epitaxy ( LPE ). is from a melt using a para- ing their three crystallographic axes related to those of a magnetic garnet structure...yttrium barium cuprate (YBCO) films and their microwave applications have been carried out. Several promising new hosts such as Sr(All/2Tal/2)03, Sr(Al1

An air-stable Na 3SbS 4 superionic conductor prepared by a rapid and economic synthetic procedure

DOE PAGES

Wang, Hui; Chen, Yan; Hood, Zachary D.; ...

2016-01-01

All-solid-state sodium batteries, using abundant sodium resources and solid electrolyte, hold much promise for safe, low cost, large-scale energy storage. To realize the practical applications of all solid Na-ion batteries at ambient temperature, the solid electrolytes are required to have high ionic conductivity, chemical stability, and ideally, easy preparation. Ceramic electrolytes show higher ionic conductivity than polymers, but they often require extremely stringent synthesis conditions, either high sintering temperature above 1000 C or long-time, low-energy ball milling. Herein, we report a new synthesis route for Na 3SbS 4, a novel Na superionic conductor that needs much lower processing temperature belowmore » 200 C and easy operation. This new solid electrolyte exhibits a remarkable ionic conductivity of 1.05 mS cm -1 at 25 °C and is chemically stable under ambient atmosphere. In conclusion, this synthesis process provides unique insight into the current state-of-the-art solid electrolyte preparation and opens new possibilities for the design of similar materials.« less

A Green Protocol for Synthesis of MAl2O4, [M=Cu and Co] Spinels Under Microwave Irradiation Method

NASA Astrophysics Data System (ADS)

Yuvasravana, R.; George, P. P.

Nanosized metal aluminates MAl2O4, [M=Cu and Co] are synthesized from their nitrates solution by using pomegranate peel extract as fuel in microwave combustion. MAl2O4 [M=Cu and Co] nanoparticles are grown in microwave assisted synthesis followed by annealing at 700∘C. The nanoparticles have been characterized by powder X-ray diffraction (PXRD), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), UV-VIS spectroscopy and photoluminescence (PL) spectroscopy. The PXRD analysis has confirmed their spinel composition. The green protocol and microwave combustion route for spinel synthesis are rapid, simple, without any hazardous chemicals as reducing or stabilizing agents and economical.

Rapid determination of 54 pharmaceutical and personal care products in fish samples using microwave-assisted extraction-Hollow fiber-Liquid/solid phase microextraction.

PubMed

Zhang, Yi; Guo, Wen; Yue, Zhenfeng; Lin, Li; Zhao, Fengjuan; Chen, Peijin; Wu, Weidong; Zhu, Hong; Yang, Bo; Kuang, Yanyun; Wang, Jiong

2017-04-15

In this paper, a simple, rapid, solvent-less and environmental friendliness microextraction method, microwave-assisted extraction-hollow fiber-liquid/solid phase microextraction (MAE-HF-L/SME), was developed for simultaneous extraction and enrichment of 54 trace hydrophilic/lipophilic pharmaceutical and personal care products (PPCPs) from fish samples. A solid-phase extraction material, solid-phase microextraction (SPME) fiber, was synthesized. The SPME fiber had a homogeneous, loose structure and good mechanical properties, and they exhibited a good adsorption capacity for most PPCPs selected. The material formed the basis for the method of MAE-HF-L/SME. A method of liquid chromatography-high resolution mass spectroscopy (LC-HRMS) for analysis of 54 PPCPs. Under optimal synthesis and extraction conditions, the limits of detection (LODs, n=3) and the limits of quantitation (LOQs, n=10) for the 54 PPCPs were between 0.01-0.50μg·kg -1 and 0.052.00μg·kg -1 , respectively. Percent recoveries and the relative standard deviations (RSDs) in spiked fish samples (n=6) were between 56.3%-119.9% and 0.3%-17.1%, respectively. The microextraction process of 54 PPCPs in MAE-HF-L/SME took approximately 12min. The method has a low matrix interference and high enrichment factor and may be applicable for determination of 54 different PPCPs in fish samples. Copyright © 2017 Elsevier B.V. All rights reserved.

Activation of boron and recrystallization in Ge preamorphization implant structure of ultra shallow junctions by microwave annealing

NASA Astrophysics Data System (ADS)

Tsai, Ming Han; Wu, Chi-Ting; Lee, Wen-His

2014-04-01

In this study, high-current and low-energy (400 eV) ion implantation and low-temperature microwave annealing were employed to achieve ultra shallow junctions. To use the characteristic of microwave annealing more effectively, two-step microwave annealing was also employed. In the first step annealing, a high-power (2400 W; ˜500 °C) microwave was used to achieve solid-state epitaxial regrowth (SPER) and enhance microwave absorption. In the second step of annealing, unlike in conventional thermal annealing, which requires a higher energy to activate the dopant, a 600 W (˜250 °C) microwave was used to achieve low sheet resistance. The device subjected to two-step microwave annealing at 2400 W for 300 s + 600 W for 600 s has the lowest Vth. It also has the lowest subthreshold swing (SS), which means that it has the highest cap ability to control sub threshold current. In these three devices, the largest Ion/Ioff ratio is 2.203 × 106, and the smallest Ion/Ioff ratio is 2.024 × 106.

Characterization of resonant tunneling diodes for microwave and millimeter-wave detection

NASA Technical Reports Server (NTRS)

Mehdi, I.; East, J. R.; Haddad, G. I.

1991-01-01

The authors report on the direct detection capabilities of resonant tunneling diodes in the 10-100 GHz range. An open circuit voltage sensitivity of 1750 mV/mW (in Ka-band) was measured. This is higher than the sensitivity of comparatively based commercially available solid-state detectors. The detector properties are a strong function of diode bias and the measured tangential signal sensitivity (-32 dBm at Ka-band with 1-MHz bandwidth) and the dynamic range (25 dB) of the diode are smaller compared to other solid-state detectors.

High-Efficiency Power Module

NASA Technical Reports Server (NTRS)

Simons, Rainee N (Inventor); Wintucky, Edwin G (Inventor)

2013-01-01

One or more embodiments of the present invention pertain to an all solid-state microwave power module. The module includes a plurality of solid-state amplifiers configured to amplify a signal using a low power stage, a medium power stage, and a high power stage. The module also includes a power conditioner configured to activate a voltage sequencer (e.g., bias controller) when power is received from a power source. The voltage sequencer is configured to sequentially apply voltage to a gate of each amplifier and sequentially apply voltage to a drain of each amplifier.

High-Efficiency Power Module

NASA Technical Reports Server (NTRS)

Simons, Rainee N. (Inventor); Wintucky, Edwin G. (Inventor)

2015-01-01

One or more embodiments of the present invention pertain to an all solid-state microwave power module. The module includes a plurality of solid-state amplifiers configured to amplify a signal using a low power stage, a medium power stage, and a high power stage. The module also includes a power conditioner configured to activate a voltage sequencer (e.g., bias controller) when power is received from a power source. The voltage sequencer is configured to sequentially apply voltage to a gate of each amplifier and sequentially apply voltage to a drain of each amplifier.

M ssbauer spectroscopy

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

Hermann, Raphael P

2017-01-01

This most comprehensive and unrivaled compendium in the field provides an up-to-date account of the chemistry of solids, nanoparticles and hybrid materials. Following a valuable introductory chapter reviewing important synthesis techniques, the handbook presents a series of contributions by about 150 international leading experts -- the "Who's Who" of solid state science. Clearly structured, in six volumes it collates the knowledge available on solid state chemistry, starting from the synthesis, and modern methods of structure determination. Understanding and measuring the physical properties of bulk solids and the theoretical basis of modern computational treatments of solids are given ample space, asmore » are such modern trends as nanoparticles, surface properties and heterogeneous catalysis. Emphasis is placed throughout not only on the design and structure of solids but also on practical applications of these novel materials in real chemical situations.« less

"In silico" mechanistic studies as predictive tools in microwave-assisted organic synthesis.

PubMed

Rodriguez, A M; Prieto, P; de la Hoz, A; Díaz-Ortiz, A

2011-04-07

Computational calculations can be used as a predictive tool in Microwave-Assisted Organic Synthesis (MAOS). A DFT study on Intramolecular Diels-Alder reactions (IMDA) indicated that the activation energy of the reaction and the polarity of the stationary points are two fundamental parameters to determine "a priori" if a reaction can be improved by using microwave irradiation.

Microwave-assisted synthesis of organics and nanomaterials

EPA Science Inventory

Microwave-assisted chemistry techniques and greener reaction media are dramatically reducing chemical waste and reaction times in several organic transformations and material synthesis. This presentation summarizes author’s own experience in developing MW-assisted chemical proces...

A comparative study of conventionally sintered and microwave sintered nickel zinc ferrite

NASA Astrophysics Data System (ADS)

Rani, Rekha; Juneja, J. K.; Raina, K. K.; Kotnala, R. K.; Prakash, Chandra

2014-04-01

For the present work, nickel zinc ferrite having compositional formula Ni0.8Zn0.2Fe2O4 was synthesized by conventional solid state method and sintered in conventional and microwave furnaces. Pellets were sintered with very short soaking time of 10 min at 1150 °C in microwave furnace whereas 4 hrs of soaking time was selected for conventional sintering at 1200 °C. Phase formation was confirmed by X-ray diffraction analysis technique. Scanning electron micrographs were taken for microstructural study. Dielectric properties were studied as a function of temperature. To study magnetic behavior, M-H hysteresis loops were recorded for both samples. It is observed that microwave sintered sample could obtain comparable properties to the conventionally sintered one in lesser soaking time at lower sintering temperature.

Solid State Division progress report for period ending March 31, 1992

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

Green, P.H.; Hinton, L.W.

1992-09-01

During this period, the division conducted a broad, interdisciplinary materials research program with emphasis on theoretical solid state physics, superconductivity, neutron scattering, synthesis and characterization of materials, ion beam and laser processing, and the structure of solids and surfaces. The High Flux Isotope Reactor was returned to full operation.

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.

Continuous microwave flow synthesis of mesoporous hydroxyapatite.

PubMed

Akram, Muhammad; Alshemary, Ammar Z; Goh, Yi-Fan; Wan Ibrahim, Wan Aini; Lintang, Hendrik O; Hussain, Rafaqat

2015-11-01

We have successfully used continuous microwave flow synthesis (CMFS) technique for the template free synthesis of mesoporous hydroxyapatite. The continuous microwave flow reactor consisted of a modified 2.45GHz household microwave, peristaltic pumps and a Teflon coil. This cost effective and efficient system was exploited to produce semi-crystalline phase pure nano-sized hydroxyapatite. Effect of microwave power, retention time and the concentration of reactants on the phase purity, degree of crystallinity and surface area of the final product was studied in detail. X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) were used to study the phase purity and composition of the product, while transmission electron microscopy (TEM) was used to study the effect of process parameters on the morphology of hydroxyapatite. The TEM analysis confirmed the formation of spherical particles at low microwave power; however the morphology of the particles changed to mesoporous needle and rod-like structure upon exposing the reaction mixture to higher microwave power and longer retention time inside the microwave. The in-vitro ion dissolution behavior of the as synthesized hydroxyapatite was studied by determining the amount of Ca(2+) ion released in SBF solution. Copyright © 2015 Elsevier B.V. All rights reserved.

Silicon carbide passive heating elements in microwave-assisted organic synthesis.

PubMed

Kremsner, Jennifer M; Kappe, C Oliver

2006-06-09

Microwave-assisted organic synthesis in nonpolar solvents is investigated utilizing cylinders of sintered silicon carbide (SiC)--a chemically inert and strongly microwave absorbing material--as passive heating elements (PHEs). These heating inserts absorb microwave energy and subsequently transfer the generated thermal energy via conduction phenomena to the reaction mixture. The use of passive heating elements allows otherwise microwave transparent or poorly absorbing solvents such as hexane, carbon tetrachloride, tetrahydrofuran, dioxane, or toluene to be effectively heated to temperatures far above their boiling points (200-250 degrees C) under sealed vessel microwave conditions. This opens up the possibility to perform microwave synthesis in unpolar solvent environments as demonstrated successfully for several organic transformations, such as Claisen rearrangements, Diels-Alder reactions, Michael additions, N-alkylations, and Dimroth rearrangements. This noninvasive technique is a particularly valuable tool in cases where other options to increase the microwave absorbance of the reaction medium, such as the addition of ionic liquids as heating aids, are not feasible due to an incompatibility of the ionic liquid with a particular substrate. The SiC heating elements are thermally and chemically resistant to 1500 degrees C and compatible with any solvent or reagent.

Amorphous and nanocrystalline luminescent Si and Ge obtained via a solid-state chemical metathesis synthesis route

NASA Astrophysics Data System (ADS)

McMillan, Paul F.; Gryko, Jan; Bull, Craig; Arledge, Richard; Kenyon, Anthony J.; Cressey, Barbara A.

2005-03-01

A new solid-state metathesis synthesis route was applied to obtain bulk samples of amorphous or microcrystalline Si and Ge. The method involves reaction of Zintl phases such as NaSi or NaGe, with ammonium or metal (e.g., CuCl, CoBr 2) halides. The driving force for the solid-state reaction is provided by the formation of alkali halides and the transition metals or metal silicides, or gaseous ammonia and hydrogen. The semiconductors were purified by washing to remove other solid products. The amorphous semiconductors were obtained in bulk form from reactions carried out at 200-300 °C. Syntheses at higher temperatures gave rise to microcrystalline semiconductors, or to micro-/nanocrystalline particles contained within the amorphous material. Similar crystalline/amorphous composites were obtained after heat treatment of bulk amorphous materials.

Microwave-assisted 'greener' synthesis of organics and nanomaterials

EPA Science Inventory

Microwave selective heating techniques in conjunction with greener reaction media are dramatically reducing chemical waste and reaction times in several organic transformations and material synthesis. This presentation summarizes author’s own experience in developing MW-assisted ...

Enhanced low-temperature lithium storage performance of multilayer graphene made through an improved ionic liquid-assisted synthesis

NASA Astrophysics Data System (ADS)

Raccichini, Rinaldo; Varzi, Alberto; Chakravadhanula, Venkata Sai Kiran; Kübel, Christian; Balducci, Andrea; Passerini, Stefano

2015-05-01

The electrochemical properties of graphene are strongly depending on its synthesis. Between the different methods proposed so far, liquid phase exfoliation turns out to be a promising method for the production of graphene. Unfortunately, the low yield of this technique, in term of solid material obtained, still limit its use to small scale applications. In this article we propose a low cost and environmentally friendly method for producing multilayer crystalline graphene with high yield. Such innovative approach, involving an improved ionic liquid assisted, microwave exfoliation of expanded graphite, allows the production of graphene with advanced lithium ion storage performance, for the first time, at low temperatures (<0 °C), as low as -30 °C, with respect to commercially available graphite.

Theoretical verification of nonthermal microwave effects on intramolecular reactions.

PubMed

Kanno, Manabu; Nakamura, Kosuke; Kanai, Eri; Hoki, Kunihito; Kono, Hirohiko; Tanaka, Motohiko

2012-03-08

There have been a growing number of articles that report dramatic improvements in the experimental performance of chemical reactions by microwave irradiation compared to that under conventional heating conditions. We theoretically examined whether nonthermal microwave effects on intramolecular reactions exist or not, in particular, on Newman-Kwart rearrangements and intramolecular Diels-Alder reactions. The reaction rates of the former calculated by the transition state theory, which consider only the thermal effects of microwaves, agree quantitatively with experimental data, and thus, the increases in reaction rates can be ascribed to dielectric heating of the solvent by microwaves. In contrast, for the latter, the temperature dependence of reaction rates can be explained qualitatively by thermal effects but the possibility of nonthermal effects still remains regardless of whether competitive processes are present or not. The effective intramolecular potential energy surface in the presence of a microwave field suggests that nonthermal effects arising from potential distortion are vanishingly small in intramolecular reactions. It is useful in the elucidation of the reaction mechanisms of microwave synthesis to apply the present theoretical approach with reference to the experiments where thermal and nonthermal effects are separated by screening microwave fields.

Optimization and stabilization of gold nanoparticles by using herbal plant extract with microwave heating

NASA Astrophysics Data System (ADS)

Yasmin, Akbar; Ramesh, Kumaraswamy; Rajeshkumar, Shanmugam

2014-04-01

In this study, we have synthesized the gold nanoparticles by using Hibiscus rosa-sinensis, a medicinal plant. The gold nanoparticles were synthesized rapidly by the involvement of microwave heating. By changing of plant extract concentration, gold solution concentration, microwave heating time and power of microwave heating the optimized condition was identified. The surface Plasmon resonance found at 520 nm confirmed the gold nanoparticles synthesis. The spherical sized nanoparticles in the size range of 16-30 nm were confirmed by Transmission Electron Microscope (TEM). The stability of the nanoparticles is very well proved in the invitro stability tests. The biochemical like alkaloids and flavonoids play a vital role in the nanoparticles synthesis was identified using the Fourier Transform Infrared Spectroscopy (FTIR). Combining the phytochemical and microwave heating, the rapid synthesis of gold nanoparticles is the novel process for the medically applicable gold nanoparticles production.

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.

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...

Synthesis and Characterization of a Perovskite Barium Zirconate (BaZrO[subscript 3]): An Experiment for an Advanced Inorganic Chemistry Laboratory

ERIC Educational Resources Information Center

Thananatthanachon, Todsapon

2016-01-01

In this experiment, the students explore the synthesis of a crystalline solid-state material, barium zirconate (BaZrO3) by two different synthetic methods: (a) the wet chemical method using BaCl[subscript 2]·2H[subscript 2]O and ZrOCl[subscript 2]·8H[subscript 2]O as the precursors, and (b) the solid-state reaction from BaCO[subscript 3] and…

Hybrid quantum processors: molecular ensembles as quantum memory for solid state circuits.

PubMed

Rabl, P; DeMille, D; Doyle, J M; Lukin, M D; Schoelkopf, R J; Zoller, P

2006-07-21

We investigate a hybrid quantum circuit where ensembles of cold polar molecules serve as long-lived quantum memories and optical interfaces for solid state quantum processors. The quantum memory realized by collective spin states (ensemble qubit) is coupled to a high-Q stripline cavity via microwave Raman processes. We show that, for convenient trap-surface distances of a few microm, strong coupling between the cavity and ensemble qubit can be achieved. We discuss basic quantum information protocols, including a swap from the cavity photon bus to the molecular quantum memory, and a deterministic two qubit gate. Finally, we investigate coherence properties of molecular ensemble quantum bits.

Comparison of microwave and conduction-convection heating autohydrolysis pretreatment for bioethanol production.

PubMed

Aguilar-Reynosa, Alejandra; Romaní, Aloia; Rodríguez-Jasso, Rosa M; Aguilar, Cristóbal N; Garrote, Gil; Ruiz, Héctor A

2017-11-01

This work describes the application of two forms of heating for autohydrolysis pretreatment on isothermal regimen: conduction-convection heating and microwave heating processing using corn stover as raw material for bioethanol production. Pretreatments were performed using different operational conditions: residence time (10-50 min) and temperature (160-200°C) for both pretreatments. Subsequently, the susceptibility of pretreated solids was studied using low enzyme loads, and high substrate loads. The highest conversion was 95.1% for microwave pretreated solids. Also solids pretreated by microwave heating processing showed better ethanol conversion in simultaneous saccharification and fermentation process (92% corresponding to 33.8g/L). Therefore, microwave heating processing is a promising technology in the pretreatment of lignocellulosic materials. Copyright © 2017 Elsevier Ltd. All rights reserved.

Microwave-assisted Chemical Transformations

EPA Science Inventory

In recent years, there has been a considerable interest in developing sustainable chemistries utilizing green chemistry principles. Since the first published report in 1986 by Gedye and Giguere on microwave assisted synthesis in household microwave ovens, the use of microwaves as...

Dynamic nuclear polarisation via the integrated solid effect II: experiments on naphthalene-h8 doped with pentacene-d14

NASA Astrophysics Data System (ADS)

Eichhorn, T. R.; van den Brandt, B.; Hautle, P.; Henstra, A.; Wenckebach, W. Th.

2014-07-01

In dynamic nuclear polarisation (DNP), also called hyperpolarisation, a small amount of unpaired electron spins is added to the sample containing the nuclear spins, and the polarisation of these unpaired electron spins is transferred to the nuclear spins by means of a microwave field. Traditional DNP polarises the electron spin of stable paramagnetic centres by cooling down to low temperature and applying a strong magnetic field. Then weak continuous wave microwave fields are used to induce the polarisation transfer. Complicated cryogenic equipment and strong magnets can be avoided using short-lived photo-excited triplet states that are strongly aligned in the optical excitation process. However, a much faster transfer of the electron spin polarisation is needed and pulsed DNP methods like nuclear orientation via electron spin locking (NOVEL) and the integrated solid effect (ISE) are used. To describe the polarisation transfer with the strong microwave fields in NOVEL and ISE, the usual perturbation methods cannot be used anymore. In the previous paper, we presented a theoretical approach to calculate the polarisation transfer in ISE. In the present paper, the theory is applied to the system naphthalene-h8 doped with pentacene-d14 yielding the photo-excited triplet states and compared with experimental results.

DIRECT SYNTHESIS OF TERTIARY AMINES IN WATER USING MICROWAVES

EPA Science Inventory

A direct synthesis of tertiary amines is presented that proceeds expeditiously via N-alkylation of amines using alkyl halides in alkaline aqueous medium. This environmentally benign reaction is accelerated upon exposure to microwave irradiation resulting in shortened reaction tim...

Microwave-Assisted Synthesis – Catalytic Applications in Aqueous Media

EPA Science Inventory

The development of sustainable methods directed towards the synthesis of molecules is due to the heightened awareness and recognition of alternative eco-friendly and economical protocols that have minimum impact on environment. Among others, microwave (MW)-assisted methodology ha...

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

Microwave Assisted Synthesis of Biorelevant Benzazoles.

PubMed

Seth, Kapileswar; Purohit, Priyank; Chakraborti, Asit K

2017-01-01

The benzazole scaffolds are present in various therapeutic agents and have been recognized as the essential pharmacophore for diverse biological activities. These have generated interest and necessity to develop efficient synthetic methods of these privileged classes of compounds to generate new therapeutic leads for various diseases. The biological activities of the benzazoles and efforts towards their synthesis have been summarized in a few review articles. In view of these, the aim of this review is to provide an account of the developments that have taken place in the synthesis of biorelevant benzazoles under microwave irradiation as the application of microwave heating has long been recognized as a green chemistry tool for speedy generation of synthetic targets. Attention has been focused to those literature reports wherein the use of microwave irradiation is the key step in the formation of the heterocyclic ring system or in functionalization of the benzazole ring system to generate the essential pharmacophoric feature. The convenient and economic way to synthesize these privileged class of heterocycles through the use of microwave irradiation that would be beneficial for the drug discovery scientist to synthesize biologically active benzazoles and provide access to wide range of reactions for the synthesis of benzazoles constitute the theme of this review. Examples have been drawn wherein the use of microwave heating offers distinct advantage in terms of improved product yields and reduction of reaction time as compared to those observed for the synthesis under conventional heating. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

The effect of B{sub 2}O{sub 3} flux on growth NLBCO superconductor by solid state reaction and wet-mixing methods

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

Suharta, W. G., E-mail: wgsuharta@gmail.com; Wendri, N.; Ratini, N.

The synthesis of B{sub 2}O{sub 3} flux substituted NLBCO superconductor NdBa{sub 1.75}La{sub 0.25}Cu{sub 3}O{sub 7-∂} has been done using solid state reaction and wet-mixing methods in order to obtain homogeneous crystals and single phase. From DTA/TGA characteritations showed the synthesis process by wet-mixing requires a lower temperature than the solid state reaction in growing the superconductor NdBa{sub 1.75}La{sub 0.25}Cu{sub 3}O{sub 7-∂}. Therefore, in this research NdBa{sub 1.75}La{sub 0.25}Cu{sub 3}O{sub 7-∂} sample calcinated at 650°C for wet-mixing method and 820°C for solid state reaction methods. The all samples was sintered at 950°C for ten hours. Crystallinity of the sample was confirmedmore » using X-ray techniques and generally obtained sharp peaks that indicates the sample already well crystallized. Search match analyses for diffraction data gave weight fractions of impurity phase of the solid state reaction method higher than wet-mixing method. In this research showed decreasing the price of the lattice parameter about 1% with the addition of B{sub 2}O{sub 3} flux for the both synthesis process and 2% of wet mixing process for all samples. Characterization using scanning electron microscopy (SEM) showed the distribution of crystal zise for wet-mixing method more homogeneous than solid state reaction method, with he grain size of samples is around 150–250 nm. The results of vibrating sample magnetometer (VSM) showed the paramagnetic properties for all samples.« less

Amorphous and nanocrystalline luminescent Si and Ge obtained via a solid-state chemical metathesis synthesis route

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

McMillan, Paul F.; Gryko, Jan; Bull, Craig

A new solid-state metathesis synthesis route was applied to obtain bulk samples of amorphous or microcrystalline Si and Ge. The method involves reaction of Zintl phases such as NaSi or NaGe, with ammonium or metal (e.g., CuCl, CoBr{sub 2}) halides. The driving force for the solid-state reaction is provided by the formation of alkali halides and the transition metals or metal silicides, or gaseous ammonia and hydrogen. The semiconductors were purified by washing to remove other solid products. The amorphous semiconductors were obtained in bulk form from reactions carried out at 200-300{sup o}C. Syntheses at higher temperatures gave rise tomore » microcrystalline semiconductors, or to micro-/nanocrystalline particles contained within the amorphous material. Similar crystalline/amorphous composites were obtained after heat treatment of bulk amorphous materials.« less

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).

Photonic microwave signals with zeptosecond-level absolute timing noise

NASA Astrophysics Data System (ADS)

Xie, Xiaopeng; Bouchand, Romain; Nicolodi, Daniele; Giunta, Michele; Hänsel, Wolfgang; Lezius, Matthias; Joshi, Abhay; Datta, Shubhashish; Alexandre, Christophe; Lours, Michel; Tremblin, Pierre-Alain; Santarelli, Giorgio; Holzwarth, Ronald; Le Coq, Yann

2017-01-01

Photonic synthesis of radiofrequency (RF) waveforms revived the quest for unrivalled microwave purity because of its ability to convey the benefits of optics to the microwave world. In this work, we perform a high-fidelity transfer of frequency stability between an optical reference and a microwave signal via a low-noise fibre-based frequency comb and cutting-edge photodetection techniques. We demonstrate the generation of the purest microwave signal with a fractional frequency stability below 6.5 × 10-16 at 1 s and a timing noise floor below 41 zs Hz-1/2 (phase noise below -173 dBc Hz-1 for a 12 GHz carrier). This outperforms existing sources and promises a new era for state-of-the-art microwave generation. The characterization is achieved through a heterodyne cross-correlation scheme with the lowermost detection noise. This unprecedented level of purity can impact domains such as radar systems, telecommunications and time-frequency metrology. The measurement methods developed here can benefit the characterization of a broad range of signals.

Synthesis, microwave spectrum, and dipole moment of allenylisocyanide (H2C═C═CHNC), a compound of potential astrochemical interest.

PubMed

Møllendal, Harald; Samdal, Svein; Matrane, Abdellatif; Guillemin, Jean-Claude

2011-07-14

An improved synthesis of a compound of potential astrochemical interest, allenylisocyanide (H(2)C═C═CHNC), is reported together with its microwave spectrum, which has been investigated in the 8-120 GHz spectral range to facilitate a potential identification in interstellar space. The spectra of the ground vibrational state and of five vibrationally excited states belonging to three different vibrational modes have been assigned for the parent species. A total of 658 transitions with a maximum value of J = 71 were assigned for the ground state and accurate values obtained for the rotational and quartic centrifugal distortion constants. The spectra of five heavy-atom ((13)C and (15)N) isotopologues were also assigned. The dipole moment was determined to be μ(a) = 11.93(16) × 10(-30) C m, μ(b) = 4.393(44) × 10(-30) C m, and μ(tot) = 12.71(16) × 10(-30) C m. The spectroscopic work has been augmented by theoretical calculations at the CCSD/cc-pVTZ and B3LYP/cc-pVTZ levels of theory. The theoretical calculations are generally in good agreement with the experimental results.

Solar power satellite system definition study. Volume 2, part 3: Final briefing, 16 May 1980, phase 3

NASA Technical Reports Server (NTRS)

1980-01-01

Alternatives to the microwave transmission system previously defined Solar Power Satellite Systems were investigated. These were the laser power transmission, transportation systems, and an analysis or solid state power transmission. The advantages of each system are presented.

Microwave-assisted synthesis of sensitive silver substrate for surface-enhanced Raman scattering spectroscopy

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

Xia Lixin; Wang Haibo; Wang Jian

A sensitive silver substrate for surface-enhanced Raman scattering (SERS) spectroscopy is synthesized under multimode microwave irradiation. The microwave-assisted synthesis of the SERS-active substrate was carried out in a modified domestic microwave oven of 2450 MHz, and the reductive reaction was conducted in a polypropylene container under microwave irradiation with a power of 100 W for 5 min. Formaldehyde was employed as both the reductant and microwave absorber in the reductive process. The effects of different heating methods (microwave dielectric and conventional) on the properties of the SERS-active substrates were investigated. Samples obtained with 5 min of microwave irradiation at amore » power of 100 W have more well-defined edges, corners, and sharper surface features, while the samples synthesized with 1 h of conventional heating at 40 deg. C consist primarily of spheroidal nanoparticles. The SERS peak intensity of the {approx}1593 cm{sup -1} band of 4-mercaptobenzoic acid adsorbed on silver nanoparticles synthesized with 5 min of microwave irradiation at a power of 100 W is about 30 times greater than when it is adsorbed on samples synthesized with 1 h of conventional heating at 40 deg. C. The results of quantum chemical calculations are in good agreement with our experimental data. This method is expected to be utilized for the synthesis of other metal nanostructural materials.« less

Energy efficient microwave synthesis of mesoporous Ce 0.5M 0.5O 2 (Ti, Zr, Hf) nanoparticles for low temperature CO oxidation in an ionic liquid – a comparative study

DOE PAGES

Alammar, Tarek; Chow, Ying -Kit; Mudring, Anja -Verena

2014-11-19

Ce 0.5M 0.5O 2 (M = Ti, Zr, Hf) nanoparticles have been successfully synthesized by microwave irradiation in the ionic liquid [C 4mim][Tf 2N] (1-butyl-3-methylimidazolium bis(trifluoromethanesulfonyl)amide). The morphology, crystallinity, and chemical composition of the obtained materials were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), energy dispersive X-ray spectroscopy (EDX), Raman spectroscopy, and N 2–adsorption measurements. XRD and Raman spectroscopy analyses confirmed the formation of solid solutions with cubic fluorite structure. The catalytic activities of the Ce 0.5M 0.5O 2 (M = Ti, Zr, Hf) nanoparticles were investigated in the low-temperature oxidation of CO. Ce 0.5Zr 0.5O 2 nanospheresmore » exhibit the best performance (100% conversion at 350 °C), followed by Ce 0.5Hf 0.5O 2 (55% conversion at 360 °C) and Ce 0.5Ti 0.5O 2 (11% conversion at 350 °C). Heating the as-prepared Ce 0.5Zr 0.5O 2 to 600 °C for extended time leads to a decrease in surface area and, as expected decreased catalytic activity. Depending on the ionic liquid the obtained Ce 0.5Zr 0.5O 2 exhibits different morphologies, varying from nano-spheres in [C 4mim][Tf 2N] and [P 66614][Tf 2N] (P 66614 = trishexyltetradecylphosphonium) to sheet-like assemblies in [C 3mimOH][Tf 2N] (C 3mimOH = 1-(3-hydroxypropyl)-3-methylimidazolium). As a result, the microwave synthesis superiority to other heating methods like sonochemical synthesis and conventional heating was proven by comparative experiments where the catalytic activity of Ce 0.5Zr 0.5O 2 obtained by alternate methods such as conventional heating was found to be poorer than that of the microwave-synthesised material.« less

Synthesis and binding studies of Alzheimer ligands on solid support.

PubMed

Rzepecki, Petra; Geib, Nina; Peifer, Manuel; Biesemeier, Frank; Schrader, Thomas

2007-05-11

Aminopyrazole derivatives constitute the first class of nonpeptidic rationally designed beta-sheet ligands. Here we describe a double solid-phase protocol for both synthesis and affinity testing. The presented solid-phase synthesis of four types of hybrid compounds relies on the Fmoc strategy and circumvents subsequent HPLC purification by precipitating the final product from organic solution in pure form. Hexa- and octapeptide pendants with internal di- and tetrapeptide bridges are now amenable in high yields to combinatorial synthesis of compound libraries for high-throughput screening purposes. Solid-phase peptide synthesis (SPPS) on an acid-resistant PAM allows us, after PMB deprotection, to subject the free aminopyrazole binding sites in an immobilized state to on-bead assays with fluorescence-labeled peptides. From the fluorescence emission intensity decrease, individual binding constants can be calculated via reference curves by simple application of the law of mass action. Gratifyingly, host/guest complexation can be monitored quantitatively even for those ligands, which are almost insoluble in water.

All-Solid-State Mechanochemical Synthesis and Post-Synthetic Transformation of Inorganic Perovskite-type Halides.

PubMed

Pal, Provas; Saha, Sujoy; Banik, Ananya; Sarkar, Arka; Biswas, Kanishka

2018-02-06

All-inorganic and hybrid perovskite type halides are generally synthesized by solution-based methods, with the help of long chain organic capping ligands, complex organometallic precursors, and high boiling organic solvents. Herein, a room temperature, solvent-free, general, and scalable all-solid-state mechanochemical synthesis is demonstrated for different inorganic perovskite type halides, with versatile structural connectivity in three (3D), two (2D), and zero (0D) dimensions. 3D CsPbBr 3 , 2D CsPb 2 Br 5 , 0D Cs 4 PbBr 6 , 3D CsPbCl 3 , 2D CsPb 2 Cl 5 , 0D Cs 4 PbCl 6 , 3D CsPbI 3 , and 3D RbPbI 3 have all been synthesized by this method. The all-solid-state synthesis is materialized through an inorganic retrosynthetic approach, which directs the decision on the solid-state precursors (e.g., CsX and PbX 2 (X=Cl/Br/I) with desired stoichiometric ratios. Moreover, post-synthetic structural transformations from 3D to 2D and 0D perovskite halides were performed by the same mechanochemical synthetic approach at room temperature. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

REVISITING NUCLEOPHILIC SUBSTITUTION REACTIONS: MICROWAVE-ASSISTED SYNTHESIS OF AZIDES, THIOCYANATES AND SULFONES IN AQUEOUS MEDIUM

EPA Science Inventory

A practical, rapid and efficient microwave (MW) promoted synthesis of various azides, thiocyanates and sulfones, is described in aqueous medium. This general and expeditious MW-enhanced nucleophilic substitution approach uses easily accessible starting materials such as halides o...

Nanostructures by ion beams

NASA Astrophysics Data System (ADS)

Schmidt, B.

Ion beam techniques, including conventional broad beam ion implantation, ion beam synthesis and ion irradiation of thin layers, as well as local ion implantation with fine-focused ion beams have been applied in different fields of micro- and nanotechnology. The ion beam synthesis of nanoparticles in high-dose ion-implanted solids is explained as phase separation of nanostructures from a super-saturated solid state through precipitation and Ostwald ripening during subsequent thermal treatment of the ion-implanted samples. A special topic will be addressed to self-organization processes of nanoparticles during ion irradiation of flat and curved solid-state interfaces. As an example of silicon nanocrystal application, the fabrication of silicon nanocrystal non-volatile memories will be described. Finally, the fabrication possibilities of nanostructures, such as nanowires and chains of nanoparticles (e.g. CoSi2), by ion beam synthesis using a focused Co+ ion beam will be demonstrated and possible applications will be mentioned.

Microwave-Assisted Synthesis, Microstructure, and Magnetic Properties of Rare-Earth Cobaltites.

PubMed

Gutiérrez Seijas, Julia; Prado-Gonjal, Jesús; Ávila Brande, David; Terry, Ian; Morán, Emilio; Schmidt, Rainer

2017-01-03

The series of perovskite rare-earth (RE) doped cobaltites (RE)CoO 3 (RE = La-Dy) was prepared by microwave-assisted synthesis. The crystal structure undergoes a change of symmetry depending on the size of the RE cation. LaCoO 3 is rhombohedral, S.G. R3̅c (No. 167), while, for the rest of the RE series (Pr-Dy), the symmetry is orthorhombic, S.G. Pnma (No. 62). The crystal structure obtained by X-ray diffraction was confirmed by high-resolution transmission electron microscopy, which yielded a good match between experimental and simulated images. It is further shown that the well-known magnetism in LaCoO 3 , which involves a thermally induced Co 3+ (d 6 ) low spin to intermediate or high spin state transition, is strongly modified by the RE cation, and a rich variety of magnetic order has been detected across the series.

Improved noise-adding radiometer for microwave receivers

NASA Technical Reports Server (NTRS)

Batelaan, P. D.; Stelzried, C. T.; Goldstein, R. M.

1973-01-01

Use of input switch and noise reference standard is avoided by using noise-adding technique. Excess noise from solid state noise-diode is coupled into receiver through directional coupler and square-wave modulated at low rate. High sensitivity receivers for radioastronomy applications are utilized with greater confidence in stability of radiometer.

Investigation of direct solar-to-microwave energy conversion techniques

NASA Technical Reports Server (NTRS)

Chatterton, N. E.; Mookherji, T. K.; Wunsch, P. K.

1978-01-01

Identification of alternative methods of producing microwave energy from solar radiation for purposes of directing power to the Earth from space is investigated. Specifically, methods of conversion of optical radiation into microwave radiation by the most direct means are investigated. Approaches based on demonstrated device functioning and basic phenomenologies are developed. There is no system concept developed, that is competitive with current baseline concepts. The most direct methods of conversion appear to require an initial step of production of coherent laser radiation. Other methods generally require production of electron streams for use in solid-state or cavity-oscillator systems. Further development is suggested to be worthwhile for suggested devices and on concepts utilizing a free-electron stream for the intraspace station power transport mechanism.

Ferrite film growth on semiconductor substrates towards microwave and millimeter wave integrated circuits

NASA Astrophysics Data System (ADS)

Chen, Z.; Harris, V. G.

2012-10-01

It is widely recognized that as electronic systems' operating frequency shifts to microwave and millimeter wave bands, the integration of ferrite passive devices with semiconductor solid state active devices holds significant advantages in improved miniaturization, bandwidth, speed, power and production costs, among others. Traditionally, ferrites have been employed in discrete bulk form, despite attempts to integrate ferrite as films within microwave integrated circuits. Technical barriers remain centric to the incompatibility between ferrite and semiconductor materials and their processing protocols. In this review, we present past and present efforts at ferrite integration with semiconductor platforms with the aim to identify the most promising paths to realizing the complete integration of on-chip ferrite and semiconductor devices, assemblies and systems.

A Novel Nanoionics-Based Switch for Microwave Applications

NASA Technical Reports Server (NTRS)

Nessel, James A.; Lee, Richard Q.; Mueller, Carl H.; Kozicki, Michael N.; Ren, Minghan; Morse, Jacki

2008-01-01

This paper reports the development and characterization of a novel switching device for use in microwave systems. The device utilizes a switching mechanism based on nanoionics, in which mobile ions within a solid electrolyte undergo an electrochemical process to form and remove a conductive metallic "bridge" to define the change of state. The nanoionics-based switch has demonstrated an insertion loss of approx.0.5dB, isolation of >30dB, low voltage operation (1V), low power (approx. micro-W) and low energy (approx. nJ) consumption, and excellent linearity up to 6 GHz. The switch requires fewer bias operations (due to non-volatile nature) and has a simple planar geometry allowing for novel device structures and easy integration into microwave power distribution circuits.

Advanced 3-V semiconductor technology assessment

NASA Technical Reports Server (NTRS)

Nowogrodzki, M.

1983-01-01

Components required for extensions of currently planned space communications systems are discussed for large antennas, crosslink systems, single sideband systems, Aerostat systems, and digital signal processing. Systems using advanced modulation concepts and new concepts in communications satellites are included. The current status and trends in materials technology are examined with emphasis on bulk growth of semi-insulating GaAs and InP, epitaxial growth, and ion implantation. Microwave solid state discrete active devices, multigigabit rate GaAs digital integrated circuits, microwave integrated circuits, and the exploratory development of GaInAs devices, heterojunction devices, and quasi-ballistic devices is considered. Competing technologies such as RF power generation, filter structures, and microwave circuit fabrication are discussed. The fundamental limits of semiconductor devices and problems in implementation are explored.

Coherent coupling between Vanadyl Phthalocyanine spin ensemble and microwave photons: towards integration of molecular spin qubits into quantum circuits.

PubMed

Bonizzoni, C; Ghirri, A; Atzori, M; Sorace, L; Sessoli, R; Affronte, M

2017-10-12

Electron spins are ideal two-level systems that may couple with microwave photons so that, under specific conditions, coherent spin-photon states can be realized. This represents a fundamental step for the transfer and the manipulation of quantum information. Along with spin impurities in solids, molecular spins in concentrated phases have recently shown coherent dynamics under microwave stimuli. Here we show that it is possible to obtain high cooperativity regime between a molecular Vanadyl Phthalocyanine (VOPc) spin ensemble and a high quality factor superconducting YBa 2 Cu 3 O 7 (YBCO) coplanar resonator at 0.5 K. This demonstrates that molecular spin centers can be successfully integrated in hybrid quantum devices.

One piece microwave container screens for electrodeless lamps

DOEpatents

Turner, Brian; Ury, Michael

1998-01-01

A microwave powered electrodeless lamp includes an improved screen unit having mesh and solid sections with an internal reflector to reflect light into a light-transmitting chamber defined in the lamp microwave cavity by the reflector and the mesh section. A discharge envelope of a bulb is disposed in the light-transmitting chamber. Light emitted from the envelope is prevented by the reflector from entering the cavity portion bounded by the solid section of the screen. Replacing mesh material by solid metal material as part of the screen unit significantly reduces leakage of microwave energy from the lamp. The solid section has multiple compliant fingers defined therein for engaging the periphery of a flange on the waveguide unit so that a hose clamp can easily secure the screen to the assembly. Screen units of this type having different mesh section configurations can be interchanged in the lamp assembly to produce different respective illumination patterns.

DEXTROSE-TEMPLATED MICROWAVE-ASSISTED COMBUSTION SYNTHESIS OF SPONGY METAL OXIDES

EPA Science Inventory

Microwave-assisted combustion synthesis of porous nanocrystalline titania and carbon coated titania is reported using dextrose as template and the product was compared with the one obtained using conventional heating furnace. Out of three compositions viz., 1:1, 1:3, and 1:5 (met...

Sustainable synthesis of chemical entities by microwave heating with nano-catalysis in water

EPA Science Inventory

•Sustainable synthesis of chemical entities by microwave heating with nano-catalysis in water •CRADA’s with the private companies, CEM corporation and VeruTEK Technologies •Green Chemistry principles are accommodated via multi-faceted approach. Learning from nature- using na...

MICROWAVE-ASSISTED SYNTHESIS OF NOBLE NANOSTRUCTURES USING BIODEGRADABLE POLYMER CARBOXYMETHYL CELLULOSE

EPA Science Inventory

Microwave-assisted (MW) synthesis of noble metals such as Au, Pt and Pd is reported using biodegradable polymer carboxymethyl cellulose (CMC) at 100°C within few seconds. The possible reduction entails the coupling of polar hydroxyl units in beta-glucopyranose units with micr...

REVISITING CLASSICAL NUCLEOPHILIC SUBSTITUTIONS IN AQUEOUS MEDIUM: MICROWAVE-ASSISTED SYNTHESIS OF ALKYL AZIDES

EPA Science Inventory

An efficient and clean synthesis of alkyl azides using microwave (MW) radiation is described in aqueous medium by reacting alkyl halides or tosylates with alkali azides. This general and expeditious MW-enhanced approach to nucleophilic substitution reactions is applicable to the ...

Expeditious synthesis of noble metal nanoparticles using Vitamin B12 under microwave irradiation

EPA Science Inventory

A greener synthesis protocol for noble nanometals is developed using vitamin B12 as a reducing and capping agent in conjunction with the use of microwaves. Successful assembly of nanoparticles or microparticles with varied shapes and sizes have been demonstrated. The synthesized ...

Energy-saving approaches to solid state street lighting

NASA Astrophysics Data System (ADS)

Vitta, Pranciškus; Stanikūnas, Rytis; Tuzikas, Arūnas; Reklaitis, Ignas; Stonkus, Andrius; Petrulis, Andrius; Vaitkevičius, Henrikas; Žukauskas, Artūras

2011-10-01

We consider the energy-saving potential of solid-state street lighting due to improved visual performance, weather sensitive luminance control and tracking of pedestrians and vehicles. A psychophysical experiment on the measurement of reaction time with a decision making task was performed under mesopic levels of illumination provided by a highpressure sodium (HPS) lamp and different solid-state light sources, such as daylight and warm-white phosphor converted light-emitting diodes (LEDs) and red-green-blue LED clusters. The results of the experiment imply that photopic luminances of road surface provided by solid-state light sources with an optimized spectral power distribution might be up to twice as low as those provided by the HPS lamp. Dynamical correction of road luminance against road surface conditions typical of Lithuanian climate was estimated to save about 20% of energy in comparison with constant-level illumination. The estimated energy savings due to the tracking of pedestrians and vehicles amount at least 25% with the cumulative effect of intelligent control of at least 40%. A solid-state street lighting system with intelligent control was demonstrated using a 300 m long test ground consisting of 10 solid-state street luminaires, a meteorological station and microwave motion sensor network operated via power line communication.

Synthesis of silver nanoparticles: chemical, physical and biological methods

PubMed Central

Iravani, S.; Korbekandi, H.; Mirmohammadi, S.V.; Zolfaghari, B.

2014-01-01

Silver nanoparticles (NPs) have been the subjects of researchers because of their unique properties (e.g., size and shape depending optical, antimicrobial, and electrical properties). A variety of preparation techniques have been reported for the synthesis of silver NPs; notable examples include, laser ablation, gamma irradiation, electron irradiation, chemical reduction, photochemical methods, microwave processing, and biological synthetic methods. This review presents an overview of silver nanoparticle preparation by physical, chemical, and biological synthesis. The aim of this review article is, therefore, to reflect on the current state and future prospects, especially the potentials and limitations of the above mentioned techniques for industries. PMID:26339255

Novel Routes for Sintering of Ultra-high Temperature Ceramics and their Properties

DTIC Science & Technology

2014-10-31

H. Gocmez, Hydrothermal synthesis and properties of Ce1-xGdxO2-δ solid solutions // Solid State Sciences. – 2002. – Vol. 4. – P. 585-590. 19. E...J. Kilner, Ionic conductivity in the CeO2-Gd2O3 system (0.05≤Gd/Ce≤0.4) prepared by oxalate coprecipitation // Solid State Ionics. - 2002. – Vol

Soliton Microwave Generator

NASA Astrophysics Data System (ADS)

Degrassie, J. S.

1990-12-01

The Soliton Microwave Generator (SMG) represents a truly new concept in the field of high power microwave (HPM) generation. A nonlinear, dispersive transmission line is used to convert an input voltage pulse into an HPM burst at the output. The system is all solid state and projects to be efficient and reliable. Single module peak powers in excess of 1 GW appear feasible, while combining modular units leads to a 10 GW system projection. This project for the DOE has allowed the first steps necessary in experimentally demonstrating the SMG. The project has ended successfully. A relatively high power lumped circuit SMG operating in the uhf band was designed, fabricated, and tested. The maximum peak output RF power was 16 MW from this line approx. 90 cm in length and 2 sq cm in cross section with a peak power efficiency of roughly 20 percent. Additionally a low power continuous strip-line approach demonstrated microwave generation well into L band, at approx. 2 GHz.

Channel Temperature Model for Microwave AlGaN/GaN HEMTs on SiC and Sapphire MMICs in High Power, High Efficiency SSPAs

NASA Technical Reports Server (NTRS)

Freeman, Jon C.

2004-01-01

A key parameter in the design trade-offs made during AlGaN/GaN HEMTs development for microwave power amplifiers is the channel temperature. An accurate determination can, in general, only be found using detailed software; however, a quick estimate is always helpful, as it speeds up the design cycle. This paper gives a simple technique to estimate the channel temperature of a generic microwave AlGaN/GaN HEMT on SiC or Sapphire, while incorporating the temperature dependence of the thermal conductivity. The procedure is validated by comparing its predictions with the experimentally measured temperatures in microwave devices presented in three recently published articles. The model predicts the temperature to within 5 to 10 percent of the true average channel temperature. The calculation strategy is extended to determine device temperature in power combining MMICs for solid-state power amplifiers (SSPAs).

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...

A Student-Centered First-Semester Introductory Organic Laboratory Curriculum Facilitated by Microwave-Assisted Synthesis (MAOS)

ERIC Educational Resources Information Center

Russell, Cianán B.; Mason, Jeremy D.; Bean, Theodore G.; Murphree, S. Shaun

2014-01-01

An instructional laboratory curriculum for a first-semester introductory organic chemistry course has been developed using microwave-assisted organic synthesis (MAOS). Taking advantage of short reaction times, materials were developed to facilitate collaborative experimental design, analysis, and debriefing of results during the normal laboratory…

Microwave assisted total synthesis of a benzothiophene-based new chemical entity (NCE)

EPA Science Inventory

Pharmaceutical scientists are required to generate diverse arrays of complex targets in short span of time, which can now be achieved by microwave-assisted organic synthesis. New chemical entities (NCE) can be built in a fraction of the time using this technique. However, there a...

Green synthesis of α-aminophosphonate derivatives on a solid supported TiO2 -SiO2 catalyst and their anticancer activity.

PubMed

Chinthaparthi, Radha Rani; Bhatnagar, Ira; Gangireddy, Chandra Sekhar Reddy; Syama, Sundar Chereddy; Cirandur, Suresh Reddy

2013-09-01

Syntheses of a new series of biologically potent α-aminophosphonates were accomplished by one-pot Kabachnik-Fields reaction using TiO2-SiO2 as solid supported catalyst under microwave irradiation conditions. The chemical structures of all the newly synthesized compounds were confirmed by analytical and spectral (IR, 1H, 13C, 31P NMR, and mass) data. Their anticancer nature was evaluated by screening the in vitro activity on two human cancer cell lines, HeLa and SK-BR-3. Compounds 4i and 4o showed the best activity on these cancer cells even though the majority of the compounds, and particularly 4l and 4p, have good cytotoxic activity against them. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

MICROWAVE TECHNOLOGY CHEMICAL SYNTHESIS APPLICATIONS

EPA Science Inventory

Microwave-accelerated chemical syntheses in various solvents as well as under solvent-free conditions have witnessed an explosive growth. The technique has found widespread application predominantly exploiting the inexpensive unmodified household microwave (MW) ovens although th...

Solution-phase microwave assisted parallel synthesis, biological evaluation and in silico docking studies of 2-chlorobenzoyl thioureas derivatives

NASA Astrophysics Data System (ADS)

Khan, Muhammad Riaz; Zaib, Sumera; Rauf, Muhammad Khawar; Ebihara, Masahiro; Badshah, Amin; Zahid, Muhammad; Nadeem, Muhammad Arif; Iqbal, Jamshed

2018-07-01

An efficient and facile microwave-assisted solution phase parallel synthesis for a 38-member library of N-aroyl-N‧-aryl thioureas was accomplished successfully. These analogues (1-38) were synthesized under identical set of conditions. It has been observed that the reaction time was drastically reduced from 8 to 12 h for conventional methods to only 10-15 mins. Products obtained were more than 98% pure, as characterized by elemental analysis along with FT-IR and 1H, 13C NMR. The solid-phase structural analysis was accomplished by single crystal XRD analysis. The urease inhibitory potential of synthetic compounds was tested and compounds were found to inhibit urease in moderate to significant manner. Compound 17 was the most potent inhibitor of urease having an IC50 value of 0.17 ± 0.1 μM. To check the cytotoxic profile of the derivatives, lungs cancer cell lines were used. Cytotoxicity analysis revealed remarkable toxicity of the compounds against tested lungs carcinoma and compounds showed variation in inhibition activity due to the substituents attached. The molecular docking studies were carried out to identify the possible binding modes of potent inhibitors in the active site of enzyme. The results suggested that the compounds can be further investigated and used against different cancers.

The microwave-assisted ionic-liquid method: a promising methodology in nanomaterials.

PubMed

Ma, Ming-Guo; Zhu, Jie-Fang; Zhu, Ying-Jie; Sun, Run-Cang

2014-09-01

In recent years, the microwave-assisted ionic-liquid method has been accepted as a promising methodology for the preparation of nanomaterials and cellulose-based nanocomposites. Applications of this method in the preparation of cellulose-based nanocomposites comply with the major principles of green chemistry, that is, they use an environmentally friendly method in environmentally preferable solvents to make use of renewable materials. This minireview focuses on the recent development of the synthesis of nanomaterials and cellulose-based nanocomposites by means of the microwave-assisted ionic-liquid method. We first discuss the preparation of nanomaterials including noble metals, metal oxides, complex metal oxides, metal sulfides, and other nanomaterials by means of this method. Then we provide an overview of the synthesis of cellulose-based nanocomposites by using this method. The emphasis is on the synthesis, microstructure, and properties of nanostructured materials obtained through this methodology. Our recent research on nanomaterials and cellulose-based nanocomposites by this rapid method is summarized. In addition, the formation mechanisms involved in the microwave-assisted ionic-liquid synthesis of nanostructured materials are discussed briefly. Finally, the future perspectives of this methodology in the synthesis of nanostructured materials are proposed. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Synthesis of N-graphene using microwave plasma-based methods

NASA Astrophysics Data System (ADS)

Dias, Ana; Tatarova, Elena; Henriques, Julio; Dias, Francisco; Felizardo, Edgar; Abrashev, Miroslav; Bundaleski, Nenad; Cvelbar, Uros

2016-09-01

In this work a microwave atmospheric plasma driven by surface waves is used to produce free-standing graphene sheets (FSG). Carbonaceous precursors are injected into a microwave plasma environment, where decomposition processes take place. The transport of plasma generated gas-phase carbon atoms and molecules into colder zones of plasma reactor results in carbon nuclei formation. The main part of the solid carbon is gradually carried from the ``hot'' plasma zone into the outlet plasma stream where carbon nanostructures assemble and grow. Subsequently, the graphene sheets have been N-doped using a N2-Ar large-scale remote plasma treatment, which consists on placing the FSG on a substrate in a remote zone of the N2-Ar plasma. The samples were treated with different compositions of N2-Ar gas mixtures, while maintaining 1 mbar pressure in the chamber and a power applied of 600 W. The N-doped graphene sheets were characterized by scanning and by high-resolution transmission electron microscopy, X-ray photoelectron spectroscopy and Raman spectroscopy. Plasma characterization was also performed by optical emission spectroscopy. Work partially funded by Portuguese FCT - Fundacao para a Ciencia e a Tecnologia, under grant SFRH/BD/52413/2013 (PD-F APPLAuSE).

Syngas obtained by microwave pyrolysis of household wastes as feedstock for polyhydroxyalkanoate production in Rhodospirillum rubrum.

PubMed

Revelles, Olga; Beneroso, Daniel; Menéndez, J Angel; Arenillas, Ana; García, J Luis; Prieto, M Auxiliadora

2017-11-01

The massive production of urban and agricultural wastes has promoted a clear need for alternative processes of disposal and waste management. The potential use of municipal solid wastes (MSW) as feedstock for the production of polyhydroxyalkanoates (PHA) by a process known as syngas fermentation is considered herein as an attractive bio-economic strategy to reduce these wastes. In this work, we have evaluated the potential of Rhodospirillum rubrum as microbial cell factory for the synthesis of PHA from syngas produced by microwave pyrolysis of the MSW organic fraction from a European city (Seville). Growth rate, uptake rate, biomass yield and PHA production from syngas in R. rubrum have been analysed. The results revealed the strong robustness of this syngas fermentation where the purity of the syngas is not a critical constraint for PHA production. Microwave-induced pyrolysis is a tangible alternative to standard pyrolysis, because it can reduce cost in terms of energy and time as well as increase syngas production, providing a satisfactory PHA yield. © 2016 The Authors. Microbial Biotechnology published by John Wiley & Sons Ltd and Society for Applied Microbiology.

Continuous-wave room-temperature diamond maser

NASA Astrophysics Data System (ADS)

Breeze, Jonathan D.; Salvadori, Enrico; Sathian, Juna; Alford, Neil Mcn.; Kay, Christopher W. M.

2018-03-01

The maser—the microwave progenitor of the optical laser—has been confined to relative obscurity owing to its reliance on cryogenic refrigeration and high-vacuum systems. Despite this, it has found application in deep-space communications and radio astronomy owing to its unparalleled performance as a low-noise amplifier and oscillator. The recent demonstration of a room-temperature solid-state maser that utilizes polarized electron populations within the triplet states of photo-excited pentacene molecules in a p-terphenyl host paves the way for a new class of maser. However, p-terphenyl has poor thermal and mechanical properties, and the decay rates of the triplet sublevel of pentacene mean that only pulsed maser operation has been observed in this system. Alternative materials are therefore required to achieve continuous emission: inorganic materials that contain spin defects, such as diamond and silicon carbide, have been proposed. Here we report a continuous-wave room-temperature maser oscillator using optically pumped nitrogen–vacancy defect centres in diamond. This demonstration highlights the potential of room-temperature solid-state masers for use in a new generation of microwave devices that could find application in medicine, security, sensing and quantum technologies.

Continuous-wave room-temperature diamond maser.

PubMed

Breeze, Jonathan D; Salvadori, Enrico; Sathian, Juna; Alford, Neil McN; Kay, Christopher W M

2018-03-21

The maser-the microwave progenitor of the optical laser-has been confined to relative obscurity owing to its reliance on cryogenic refrigeration and high-vacuum systems. Despite this, it has found application in deep-space communications and radio astronomy owing to its unparalleled performance as a low-noise amplifier and oscillator. The recent demonstration of a room-temperature solid-state maser that utilizes polarized electron populations within the triplet states of photo-excited pentacene molecules in a p-terphenyl host paves the way for a new class of maser. However, p-terphenyl has poor thermal and mechanical properties, and the decay rates of the triplet sublevel of pentacene mean that only pulsed maser operation has been observed in this system. Alternative materials are therefore required to achieve continuous emission: inorganic materials that contain spin defects, such as diamond and silicon carbide, have been proposed. Here we report a continuous-wave room-temperature maser oscillator using optically pumped nitrogen-vacancy defect centres in diamond. This demonstration highlights the potential of room-temperature solid-state masers for use in a new generation of microwave devices that could find application in medicine, security, sensing and quantum technologies.

Synthesis of (azelaic-co-dodecanedioic) polyanhydride by microwave technique

NASA Astrophysics Data System (ADS)

Gutiérrez, M.; Sierra, C.; Acevedo Morantes, M.; Herrera, A. P.

2016-02-01

A polyanhydride was synthesized through microwave radiation using azelaic acid and dodecanedioic dicarboxylic acid at concentrations of 75:25, 50:50, and 25:75%w/w with acetic anhydride as crosslinking agent. Polymerization was carried out during 3 and 5 minutes. The copolymer with the highest molecular weight was selected using the intrinsic viscometry technique and by Huggin/Kraemer and Solomon/Ciuta methods. Based on these measurements, the 50:50 copolymer was selected with a polymerization time of 3 minutes in the microwave. This sample displayed the highest intrinsic viscosity (41.82cm3/g), demonstrating the relevance of the microwave technique for the synthesis of biopolymers.

Microwave-Assisted Synthesis of a MK2 Inhibitor by Suzuki-Miyaura Coupling for Study in Werner Syndrome Cells.

PubMed

Bagley, Mark C; Baashen, Mohammed; Chuckowree, Irina; Dwyer, Jessica E; Kipling, David; Davis, Terence

2015-06-03

Microwave-assisted Suzuki-Miyaura cross-coupling reactions have been employed towards the synthesis of three different MAPKAPK2 (MK2) inhibitors to study accelerated aging in Werner syndrome (WS) cells, including the cross-coupling of a 2-chloroquinoline with a 3-pyridinylboronic acid, the coupling of an aryl bromide with an indolylboronic acid and the reaction of a 3-amino-4-bromopyrazole with 4-carbamoylphenylboronic acid. In all of these processes, the Suzuki-Miyaura reaction was fast and relatively efficient using a palladium catalyst under microwave irradiation. The process was incorporated into a rapid 3-step microwave-assisted method for the synthesis of a MK2 inhibitor involving 3-aminopyrazole formation, pyrazole C-4 bromination using N-bromosuccinimide (NBS), and Suzuki-Miyaura cross-coupling of the pyrazolyl bromide with 4-carbamoylphenylboronic acid to give the target 4-arylpyrazole in 35% overall yield, suitable for study in WS cells.

A concise synthesis of benzimidazoles via the microwave-assisted one-pot batch reaction of amino acids up to a 10-g scale.

PubMed

Peng, Pai; Xiong, Jin-Feng; Mo, Guang-Zhen; Zheng, Jia-Li; Chen, Ren-Hong; Chen, Xiao-Yun; Wang, Zhao-Yang

2014-10-01

An efficient method for the synthesis of aminomethyl benzimidazoles is developed by using a one-pot batch reaction between amino acids and o-phenylenediamines. This reaction proceeds smoothly in an unmodified household microwave oven, even though scale-up is to 10 g. A desirable method for the quick synthesis of benzimidazoles, which are used as a kind of important intermediates in drug synthesis, is provided by the scale-up utilization of amino acid resource.

Printed Antennas Made Reconfigurable by Use of MEMS Switches

NASA Technical Reports Server (NTRS)

Simons, Rainee N.

2005-01-01

A class of reconfigurable microwave antennas now undergoing development comprise fairly conventional printed-circuit feed elements and radiating patches integrated with novel switches containing actuators of the microelectromechanical systems (MEMS) type. In comparison with solid-state electronic control devices incorporated into some prior printed microwave antennas, the MEMS-based switches in these antennas impose lower insertion losses and consume less power. Because the radio-frequency responses of the MEMS switches are more nearly linear, they introduce less signal distortion. In addition, construction and operation are simplified because only a single DC bias line is needed to control each MEMS actuator.

Green synthesis of noble nanometals (Au, Pt, Pd) using glycerol under microwave irradiation conditions

EPA Science Inventory

A newer application of glycerol in the field of nanomaterials synthesis has been developed from both the economic and environmental points of view. Glycerol can act as a reducing agent for the fabrication of noble nanometals, such as Au, Pt, and Pd, under microwave irradiation. T...

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...

Microwave assisted synthesis of bridgehead alkenes.

PubMed

Cleary, Leah; Yoo, Hoseong; Shea, Kenneth J

2011-04-01

A new, concise method to synthesize triene precursors for the type 2 intramolecular Diels-Alder reaction has been developed. Microwave irradiation of the trienes provides a convenient method for the synthesis of bridgehead alkenes. Higher yields, shorter reaction times, and lower reaction temperatures provide a general and efficient route to this interesting class of molecules.

Microwave Assisted Synthesis of Bridgehead Alkenes

PubMed Central

Cleary, Leah; Yoo, Hoseong; Shea, Kenneth J.

2011-01-01

A new, concise method to synthesize triene precursors for the type 2 intramolecular Diels–Alder reaction has been developed. Microwave irradiation of the trienes provides a convenient method for the synthesis of bridgehead alkenes. Higher yields, shorter reaction times and lower reaction temperatures provide a general and efficient route to this interesting class of molecules. PMID:21384818

Solventless and One-Pot Synthesis of Cu(II) Phthalocyanine Complex: A Green Chemistry Experiment

ERIC Educational Resources Information Center

Sharma, R. K.; Sharma, Chetna; Sidhwani, Indu Tucker

2011-01-01

With the growing awareness of green chemistry, it is increasingly important for students to understand this concept in the context of laboratory experiments. Although microwave-assisted organic synthesis has become a common and invaluable technique in recent years, there have been few procedures published for microwave-assisted inorganic synthesis…

CATALYST-FREE REACTIONS UNDER SOLVENT-FEE CONDITIONS: MICROWAVE-ASSISTED SYNTHESIS OF HETEROCYCLIC HYDRAZONES BELOW THE MELTING POINT OF NEAT REACTANTS: JOURNAL ARTICLE

EPA Science Inventory

NRMRL-CIN-1437 Jeselnik, M., Varma*, R.S., Polanc, S., and Kocevar, M. Catalyst-free Reactions under Solvent-fee Conditions: Microwave-assisted Synthesis of Heterocyclic Hydrazones below the Melting Point of Neat Reactants. Published in: Chemical Communications 18:1716-1717 (200...

Microwave-assisted combustion synthesis of nano iron oxide/iron-coated activated carbon, anthracite, cellulose fiber, and silica, with arsenic adsorption studies

EPA Science Inventory

Combustion synthesis of iron oxide/iron coated carbons such as activated carbon, anthracite, cellulose fiber and silica is described. The reactions were carried out in alumina crucibles using a Panasonic kitchen microwave with inverter technology, and the reaction process was com...

A Survey of Solid-State Microwave Power Devices

DTIC Science & Technology

1977-04-29

from the channel by a thin oxide layer (insulated gate FET or IGFET), it may be a diffused junction at the top of the channel (junction FET or JFET...greater than 100 GHz. YIG-tuned units are finding increasing use as extremely stable sources, whereas varactor tuning is used where tuning speed is

MMIC Amplifier Produces Gain of 10 dB at 235 GHz

NASA Technical Reports Server (NTRS)

Dawson, Douglas; Fung, King Man; Lee, Karen; Samoska, Lorene; Wells, Mary; Gaier, Todd; Kangaslahti, Pekka; Grundbacher, Ronald; Lai, Richard; Raja, Rohit;

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

Ding, Ling; Song, Yu, E-mail: songyu@dlpu.edu.cn; Yang, Wei

Open-framework zinc phosphates were synthesized by microwave-assisted technique, and it was shown that the morphology of as-prepared materials could be easily tailored by changing synthesis temperature, reaction time and pH value. During the synthesis, when the reaction temperature increases from 130 °C to 220 °C, the products transformed from hexagonal prisms to polyhedron along with the disappearance of the hexagonal prisms vertical plane. Simultaneously, both the reaction time and pH value could promote the nucleation and growth of crystal particles. More interestingly, the target products with different morphologies could be obtained by varying the usage of NaOH or NH{sub 3}·H{submore » 2}O at 130 °C during the microwave synthesis process. - Graphical abstract: Zinc phosphates with variable morphologies can be obtained by simply tuning the microwave-heating temperatures. Display Omitted - Highlights: • Synthesis of open-framework Zn{sub 4} (H{sub 3}O) (NH{sub 4}){sub 3}(PO{sub 4}){sub 4} compounds employing microwave technique. • Dependence of morphology on the reaction conditions. • Morphology transformation from hexagonal prisms to polyhedron was observed.« less

A green synthesis of a layered titanate, potassium lithium titanate; lower temperature solid-state reaction and improved materials performance

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

Ogawa, Makoto, E-mail: waseda.ogawa@gmail.com; Department of Earth Sciences, Waseda University, 1-6-1 Nishiwaseda, Shinjuku-ku, Tokyo 169-8050; Morita, Masashi, E-mail: m-masashi@y.akane.waseda.jp

2013-10-15

A layered titanate, potassium lithium titanate, with the size range from 0.1 to 30 µm was prepared to show the effects of the particle size on the materials performance. The potassium lithium titanate was prepared by solid-state reaction as reported previously, where the reaction temperature was varied. The reported temperature for the titanate preparation was higher than 800 °C, though 600 °C is good enough to obtain single-phase potassium lithium titanate. The lower temperature synthesis is cost effective and the product exhibit better performance as photocatalysts due to surface reactivity. - Graphical abstract: Finite particle of a layered titanate, potassiummore » lithium titanate, was prepared by solid-state reaction at lower temperature to show modified materials performance. Display Omitted - Highlights: • Potassium lithium titanate was prepared by solid-state reaction. • Lower temperature reaction resulted in smaller sized particles of titanate. • 600 °C was good enough to obtain single phased potassium lithium titanate. • The product exhibited better performance as photocatalyst.« less

Low temperature probe for dynamic nuclear polarization and multiple-pulse solid-state NMR.

PubMed

Cho, HyungJoon; Baugh, Jonathan; Ryan, Colm A; Cory, David G; Ramanathan, Chandrasekhar

2007-08-01

Here, we describe the design and performance characteristics of a low temperature probe for dynamic nuclear polarization (DNP) experiments, which is compatible with demanding multiple-pulse experiments. The competing goals of a high-Q microwave cavity to achieve large DNP enhancements and a high efficiency NMR circuit for multiple-pulse control lead to inevitable engineering tradeoffs. We have designed two probes-one with a single-resonance RF circuit and a horn-mirror cavity configuration for the microwaves and a second with a double-resonance RF circuit and a double-horn cavity configuration. The advantage of the design is that the sample is in vacuum, the RF circuits are locally tuned, and the microwave resonator has a large internal volume that is compatible with the use of RF and gradient coils.

Satellite Power System (SPS) concept definition study (Exhibit D). Volume 2: Systems/subsystems analyses

NASA Technical Reports Server (NTRS)

Hanley, G. M.

1981-01-01

Modifications to the reference concept were studied and the best approaches defined. The impact of the high efficiency multibandgap solar array on the reference concept design is considered. System trade studies for several solid state concepts, including the sandwich concept and a separate antenna/solar concept, are described. Two solid state concepts were selected and a design definition is presented for each. Magnetrons as an alternative to the reference klystrons for dc/RF conversion are evaluated. System definitions are presented for the preferred klystron and solid state concepts. Supporting systems are analyzed, with major analysis in the microwave, structures, and power distribution areas. Results of studies for thermal control, attitude control, stationkeeping, and details of a multibandgap solar cell study are included. Advanced laser concepts and the meteorological effects of a laser beam power transmission concept are considered.

Eu3+-doped Bi4Si3O12 red phosphor for solid state lighting: microwave synthesis, characterization, photoluminescence properties and thermal quenching mechanisms

PubMed Central

Zhang, Yan; Xu, Jiayue; Cui, Qingzhi; Yang, Bobo

2017-01-01

Europium-doped bismuth silicate (Bi4Si3O12) phosphor has been prepared by microwave irradiation method and its crystal structure is determined using Rietveld method. As-prepared phosphor consists of spherical, monodispersed particles with few agglomeration, high crystallinity, and narrow grain size distribution. The phosphor can be efficiently excited in the wavelength range of 260–400 nm, which matched well with the emission wavelengths of NUV LED chips. The photoluminescence spectra exhibit the highest emission peak at 703 nm originating from 5D0 → 7F4 transition of Eu3+ under NUV excitation. The luminescence lifetime for Bi4Si3O12: 2 at% Eu3+ phosphor decreases from 2.11 to 1.86 ms with increasing temperature from 10 to 498 K. This behavior of decays is discussed in terms of radiative and nonradiative decays dependence on temperature. The thermal quenching mechanism of 5D0 emission of Eu3+ in Bi4Si3O12 phosphor is a crossover process from the 5D0 level of Eu3+ to a ligand-to-europium (O2− → Eu3+) charge transfer state. The quantum efficiency of the phosphor under 393 nm excitation is found to be 14.5%, which is higher than that of the commercial red phosphors Y2O3: Eu3+, Y2O2S: Eu3+. The temperature effect on CIE coordinate was discussed in order to further investigate the potential applications. PMID:28198396

NON-TRADITIONAL 'GREENER' ALTERNATIVES TO SYNTHETIC ORGANIC TRANSFORMATIONS USING MICROWAVES

EPA Science Inventory

Non-traditional 'Greener' Alternatives to synthetic Organic Transformations Using Microwaves

A rapid and environmentally friendlier approach for organic synthesis and transformations is described which involves microwave (MW) exposure of neat reactants (undiluted) often i...

Electronic conductivity studies on oxyhalide glasses containing TMO

NASA Astrophysics Data System (ADS)

Vijayatha, D.; Viswanatha, R.; Sujatha, B.; Narayana Reddy, C.

2016-05-01

Microwave-assisted synthesis is cleaner, more economical and much faster than conventional methods. The development of new routes for the synthesis of solid materials is an integral part of material science and technology. The electronic conductivity studies on xPbCl2 - 60 PbO - (40-x) V2O5 (1 ≥ x ≤ 10) glass system has been carried out over a wide range of composition and temperature (300 K to 423 K). X-ray diffraction study confirms the amorphous nature of the samples. The Scanning electron microscopic studies reveal the formation of cluster like morphology in PbCl2 containing glasses. The d.c conductivity exhibits Arrhenius behaviour and increases with V2O5 concentration. Analysis of the results is interpreted in view Austin-Mott's small polaron model of electron transport. Activation energies calculated using regression analysis exhibit composition dependent trend and the variation is explained in view of the structure of lead-vanadate glass.

TiO{sub 2} synthesized by microwave assisted solvothermal method: Experimental and theoretical evaluation

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

Moura, K.F.; Maul, J.; Albuquerque, A.R.

2014-02-15

In this study, a microwave assisted solvothermal method was used to synthesize TiO{sub 2} with anatase structure. The synthesis was done using Ti (IV) isopropoxide and ethanol without templates or alkalinizing agents. Changes in structural features were observed with increasing time of synthesis and evaluated using periodic quantum chemical calculations. The anatase phase was obtained after only 1 min of reaction besides a small amount of brookite phase. Experimental Raman spectra are in accordance with the theoretical one. Micrometric spheres constituted by nanometric particles were obtained for synthesis from 1 to 30 min, while spheres and sticks were observed aftermore » 60 min. - Graphical abstract: FE-SEM images of anatase obtained with different periods of synthesis associated with the order–disorder degree. Display Omitted - Highlights: • Anatase microspheres were obtained by the microwave assisted hydrothermal method. • Only ethanol and titanium isopropoxide were used as precursors during the synthesis. • Raman spectra and XRD patterns were compared with quantum chemical calculations. • Time of synthesis increased the short-range disorder in one direction and decreased in another.« less

Room temperature synthesis of copper indium diselenide in non-aqueous solution using an organoindium reagent

NASA Technical Reports Server (NTRS)

Hepp, Aloysius F.; Andras, Maria T.; Bailey, Sheila G.; Duraj, Stan A.

1992-01-01

A novel two-phase synthesis of CuInSe2 at 25 C from Cu2Se and Cp3In in 4-methylpyridine has been discovered. Characterization of the material produced shows it to be platelet-shaped crystallites with an average particle size of 10 microns, less than 2 percent C and H, with a small amount of unidentified crystalline impurity. The results demonstrate that it is possible to produce from solution a material that is ordinarily synthesized in bulk or films at much higher temperatures or using extraneous reagents and/or electrons. The use of a solid-state reagent as a starting material which is converted to another solid-state compound by an organometallic reagent has tremendous potential to produce precursors for a wide range of solid-state materials of interest to the electronics, defense, and aerospace communities.

"Cooking the sample": radiofrequency induced heating during solid-state NMR experiments.

PubMed

d'Espinose de Lacaillerie, Jean-Baptiste; Jarry, Benjamin; Pascui, Ovidiu; Reichert, Detlef

2005-09-01

Dissipation of radiofrequency (RF) energy as heat during continuous wave decoupling in solid-state NMR experiment was examined outside the conventional realm of such phenomena. A significant temperature increase could occur while performing dynamic NMR measurements provided the sample contains polar molecules and the sequence calls for relatively long applications of RF power. It was shown that the methyl flip motion in dimethylsulfone (DMS) is activated by the decoupling RF energy conversion to heat during a CODEX pulse sequence. This introduced a significant bias in the correlation time-temperature dependency measurement used to obtain the activation energy of the motion. By investigating the dependency of the temperature increase in hydrated lead nitrate on experimental parameters during high-power decoupling one-pulse experiments, the mechanisms for the RF energy deposition was identified. The samples were heated due to dissipation of the energy absorbed by dielectric losses, a phenomenon commonly known as "microwave" heating. It was thus established that during solid-state NMR experiments at moderate B0 fields, RF heating could lead to the heating of samples containing polar molecules such as hydrated polymers and inorganic solids. In particular, this could result in systematic errors for slow dynamics measurements by solid-state NMR.

Microwave Synthesis of Zinc Hydroxy Sulfate Nanoplates and Zinc Oxide Nanorods in the Classroom

ERIC Educational Resources Information Center

Dziedzic, Rafal M.; Gillian-Daniel, Anne Lynn; Peterson, Greta M.; Martínez-Herna´ndez, Kermin J.

2014-01-01

In this hands-on, inquiry-based lab, high school and undergraduate students learn about nanotechnology by synthesizing their own nanoparticles in a single class period. This simple synthesis of zinc oxide nanorods and zinc hydroxy sulfate nanoplates can be done in 15 min using a household microwave oven. Reagent concentration, reaction…

Synthesis of isoxazolo[5,4-b]pyridines by microwave-assisted multi-component reactions in water.

PubMed

Tu, Shu-Jiang; Zhang, Xiao-Hong; Han, Zheng-Guo; Cao, Xu-Dong; Wu, Shan-Shan; Yan, Shu; Hao, Wen-Juan; Zhang, Ge; Ma, Ning

2009-01-01

A series of new polycyclic-fused isoxazolo[5,4-b]pyridines were obtained by a one-pot tandem reaction under microwave irradiation in water. Without any use of additional reagent or catalyst, the synthetic protocol represents a green one and makes this methodology suitable for library synthesis in drug discovery efforts.

EFFECT OF POLY (ETHYLENE GLYCOL) ON THE FORMATION OF NANOSTRUCTURES: A FACILE SUSTAINABLE APPROACH FOR THE SYNTHESIS OF SILVER NANORODS USING MICROWAVE IRRADIATION

EPA Science Inventory

Bulk synthesis of silver nanorods employing poly (ethylene glycol) (PEG) under microwave irradiation is reported. The formation of nanorods or particulate morphology is dependent on the PEG concentration. This greener method uses no surfactants or reducing agents and employs a b...

Rapid Size- Controlled Synthesis of Dextran-Coated, Copper-Doped Iron Oxide Nanoparticles

NASA Astrophysics Data System (ADS)

Wong, Ray M.

2011-12-01

Development of dual modality probes enabled for magnetic resonance imaging (MRI) and positron emission tomography (PET) has been on the rise in recent years due to the potential for these probes to facilitate combining the complementary high resolution of MRI and the high sensitivity of PET. The efficient synthesis of multimodal probes that include the radiolabels for PET can be hindered due to prolonged reaction times during radioisotope incorporation, and the resulting decay of the radiolabel. Along with a time-efficient synthesis, one also needs an optimal synthesis that yields products in a desirable size range (between 20-100 nm) to increase blood retention time. In this work, we describe a novel, rapid, microwave-based synthesis of dextran-coated iron oxide nanoparticles doped with copper (DIO/Cu). Traditional methods for synthesizing dextran-coated iron oxide particles require refluxing for 2 hours and result in approximately 50 nm particles. We demonstrate that microwave synthesis can produce 50 nm nanoparticles in 5 minutes of heating. We discuss the various parameters used in the microwave synthesis protocol to vary the size distribution of DIO/Cu, and demonstrate the successful incorporation of copper into these particles with the aim of future use for rapid 64Cu incorporation.

Microwave-assisted microemulsion technique for production of miconazole nitrate- and econazole nitrate-loaded solid lipid nanoparticles.

PubMed

Shah, Rohan M; Eldridge, Daniel S; Palombo, Enzo A; Harding, Ian H

2017-08-01

The microwave-assisted production of solid lipid nanoparticles (SLNs) is a novel technique reported recently by our group. The small particle size, solid nature and use of physiologically well-tolerated lipid materials make SLNs an interesting and potentially efficacious drug carrier. The main purpose of this research work was to investigate the suitability of microwave-assisted microemulsion technique to encapsulate selected ionic drug substances such as miconazole nitrate and econazole nitrate. The microwave-produced SLNs had a small size (250-300nm), low polydispersity (<0.20), high encapsulation efficiency (72-87%) and loading capacity (3.6-4.3%). Differential scanning calorimetry (DSC) and X-ray diffraction (XRD) studies suggested reduced crystallinity of stearic acid in SLNs. The release studies demonstrated a slow, sustained but incomplete release of drugs (<60% after 24h) from microwave-produced SLNs. Data fitting of drug release data revealed that the release of both drugs from microwave-produced SLNs was governed by non-Fickian diffusion indicating that drug release was both diffusion- and dissolution- controlled. Anti-fungal efficacy of drug-loaded SLNs was evaluated on C. albicans. The cell viability studies showed that cytotoxicity of SLNs was concentration-dependent. These encouraging results suggest that the microwave-assisted procedure is suitable for encapsulation of ionic drugs and that microwave-produced SLNs can act as potential carriers of antifungal drugs. Copyright © 2017 Elsevier B.V. All rights reserved.

Microwave-Assisted Piloty-Robinson Synthesis of 3,4-Disubstituted Pyrroles

PubMed Central

Milgram, Benjamin C.; Eskildsen, Katrine; Richter, Steven M.; Scheidt, W. Robert; Scheidt, Karl A.

2007-01-01

The synthesis of N-acyl 3,4-disubstituted pyrroles can be accomplished directly from hydrazine and an aldehyde via a Piloty-Robinson pyrrole synthesis. The use of microwave radiation for the cyclization and pyrrole formation greatly reduces the time necessary for this process and facilitates moderate to good yields from hydrazine for the corresponding 3,4-disubstituted products (5–12). By simple hydrolysis, the free N–H pyrroles can be accessed after the Piloty-Robinson reaction and then used directly in the synthesis of octaethylporphyrin (H2OEP, 14) and octaethyltetraphenylporphyrin (H2OETPP, 15). PMID:17432915

Microwave induced plasma for solid fuels and waste processing: A review on affecting factors and performance criteria.

PubMed

Ho, Guan Sem; Faizal, Hasan Mohd; Ani, Farid Nasir

2017-11-01

High temperature thermal plasma has a major drawback which consumes high energy. Therefore, non-thermal plasma which uses comparatively lower energy, for instance, microwave plasma is more attractive to be applied in gasification process. Microwave-induced plasma gasification also carries the advantages in terms of simplicity, compactness, lightweight, uniform heating and the ability to operate under atmospheric pressure that gains attention from researchers. The present paper synthesizes the current knowledge available for microwave plasma gasification on solid fuels and waste, specifically on affecting parameters and their performance. The review starts with a brief outline on microwave plasma setup in general, and followed by the effect of various operating parameters on resulting output. Operating parameters including fuel characteristics, fuel injection position, microwave power, addition of steam, oxygen/fuel ratio and plasma working gas flow rate are discussed along with several performance criteria such as resulting syngas composition, efficiency, carbon conversion, and hydrogen production rate. Based on the present review, fuel retention time is found to be the key parameter that influences the gasification performance. Therefore, emphasis on retention time is necessary in order to improve the performance of microwave plasma gasification of solid fuels and wastes. Copyright © 2017 Elsevier Ltd. All rights reserved.

Recent Advances in the Catalytic One-Pot Synthesis of Flavonoids and Chromones.

PubMed

Mohadeszadeh, Manijeh; Iranshahi, Mehrdad

2017-01-01

Flavonoids and chromones are two important classes of natural products that have various biological properties. During the past 10 years, there has been a significant increase in studies on the one-pot synthesis of flavonoids and chromones as medicinal scaffolds in drug discovery. This review describes the scope, mechanistic properties and regio- and chemo-selectivity features of several recently developed one-pot procedures for the synthesis of substituted chromones and flavonoids that have recently been published. Special importance is placed on the most promising and exciting medicinal applications of flavonoids and chromones. In this review, we discuss the progress on the synthesis of flavonoid and chromone derivatives in the presence of metal catalysts, organocatalysts, solid surfaces, microwave irradiation, acid and base catalysis, etc. For example, flavones can be prepared via the catalytic coordination of palladium complexes in a short time and at a low temperature with a high yield. Additionally, the one-pot synthesis of 2-substituted chromones via metal triflate (Yb(OTf)3) has provided the best result for this type of reaction with a high yield and a high regio and chemoselectivity. Generally, this review proposes the first specific overview of this developing and rapidly expanding field of flavonoid synthesis. We also discuss the mechanisms and advantages and disadvantages of methods for the synthesis of flavonoids and chromones. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

New eco-friendly animal bone meal catalysts for preparation of chalcones and aza-Michael adducts

PubMed Central

2012-01-01

Abstract Two efficient reactions were successfully carried out using Animal Bone Meal (ABM) and potassium fluoride or sodium nitrate doped ABMs as new heterogeneous catalysts under very mild conditions. After preparation and characterization of the catalysts, we first report their use in a simple and convenient synthesis of various chalcones by Claisen–Schmidt condensation and then in an aza-Michael addition involving several synthesized chalcones with aromatic amines. All the reactions were carried out at room temperature in methanol; the chalcone synthesis was also achieved in water environment under microwave irradiation. Doping ABM enhances the rate and yield at each reaction. Catalytic activities are discussed and the ability to re-use the ABM is demonstrated. Results For Claisen–Schmidt the use of ABM alone, yields never exceeded 17%. In each entry, KF/ABM and NaNO3/ABM (79-97%) gave higher yields than using ABM alone under thermic condition. Also the reaction proceeded under microwave irradiation in good yields (72-94% for KF/ABM and 81-97% for NaNO3/ABM) and high purity. For aza-Michael addition the use of ABM doped with KF or NaNO3 increased the catalytic activity remarkably. The very high yields could be noted (84-95% for KF/ABM and 81-94% for NaNO3/ABM). Conclusion The present method is an efficient and selective procedure for the synthesis of chalcones an aza-Michael adducts. The ABM and doped ABMs are a new, inexpensive and attractive solid supports which can contribute to the development of catalytic processes and reduced environmental problems. PMID:22721409

Charge transport in strongly coupled quantum dot solids

NASA Astrophysics Data System (ADS)

Kagan, Cherie R.; Murray, Christopher B.

2015-12-01

The emergence of high-mobility, colloidal semiconductor quantum dot (QD) solids has triggered fundamental studies that map the evolution from carrier hopping through localized quantum-confined states to band-like charge transport in delocalized and hybridized states of strongly coupled QD solids, in analogy with the construction of solids from atoms. Increased coupling in QD solids has led to record-breaking performance in QD devices, such as electronic transistors and circuitry, optoelectronic light-emitting diodes, photovoltaic devices and photodetectors, and thermoelectric devices. Here, we review the advances in synthesis, assembly, ligand treatments and doping that have enabled high-mobility QD solids, as well as the experiments and theory that depict band-like transport in the QD solid state. We also present recent QD devices and discuss future prospects for QD materials and device design.

Charge transport in strongly coupled quantum dot solids.

PubMed

Kagan, Cherie R; Murray, Christopher B

2015-12-01

The emergence of high-mobility, colloidal semiconductor quantum dot (QD) solids has triggered fundamental studies that map the evolution from carrier hopping through localized quantum-confined states to band-like charge transport in delocalized and hybridized states of strongly coupled QD solids, in analogy with the construction of solids from atoms. Increased coupling in QD solids has led to record-breaking performance in QD devices, such as electronic transistors and circuitry, optoelectronic light-emitting diodes, photovoltaic devices and photodetectors, and thermoelectric devices. Here, we review the advances in synthesis, assembly, ligand treatments and doping that have enabled high-mobility QD solids, as well as the experiments and theory that depict band-like transport in the QD solid state. We also present recent QD devices and discuss future prospects for QD materials and device design.

ENVIRONMENTALLY FRIENDLIER ALTERNATIVES TO ORGANIC SYNTHESIS USING MICROWAVES

EPA Science Inventory

Microwave irradiation has been used for a variety of organic transformations wherein chemical reactions are expedited because of selective adsorption of microwave (MW) energy by polar molecules, non-polar molecules being inert to the MW dielectric loss. The MW application under s...

Microwave-Assisted Organic Synthesis and Transformations using Benign Reaction Media

EPA Science Inventory

The nonclassical heating technique using microwaves, termed as 'Bunsen burner of the 21st century, is rapidly becoming popular and is dramatically reducing the reaction times. The significant outcomes of microwave (MW)-assisted green chemistry endeavors are summarized that have r...

Solid state synthesis of layered sodium manganese oxide for sodium-ion battery by in-situ high energy X-ray diffraction and X-ray absorption near edge spectroscopy [Solid state synthesis of layered sodium manganese oxide for sodium-ion battery by in-situ HEXRD and XANES

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

Ma, Tianyuan; Xu, Gui -Liang; Zeng, Xiaoqiao

In situ high energy X-ray diffraction (HEXRD) and in situ X-ray absorption near edge spectroscopy (XANES) were carried out to understand the soild state synthesis of Na xMnO 2, with particular interest on the synthesis of P2 type Na 2/3MnO 2. It was found that there were multi intermediate phases formed before NaMnO 2 appeared at about 600 °C. And the final product after cooling process is a combination of O'3 NaMnO 2 with P2 Na 2/3MnO 2. A P2 type Na 2/3MnO 2 was synthesized at reduced temperature (600 °C). The influence of Na 2CO 3 impurity on themore » electrochemical performance of P2 Na 2/3MnO 2 was thoroughly investigated in our work. It was found that the content of Na 2CO 3 can be reduced by optimizing Na 2CO 3/MnCO 3 ratio during the solid state reaction or other post treatment such as washing with water. Lastly, we expected our results could provide a good guide for future development of high performance cathode materials for sodium-ion batteries.« less

Solid state synthesis of layered sodium manganese oxide for sodium-ion battery by in-situ high energy X-ray diffraction and X-ray absorption near edge spectroscopy [Solid state synthesis of layered sodium manganese oxide for sodium-ion battery by in-situ HEXRD and XANES

DOE PAGES

Ma, Tianyuan; Xu, Gui -Liang; Zeng, Xiaoqiao; ...

2016-12-07

In situ high energy X-ray diffraction (HEXRD) and in situ X-ray absorption near edge spectroscopy (XANES) were carried out to understand the soild state synthesis of Na xMnO 2, with particular interest on the synthesis of P2 type Na 2/3MnO 2. It was found that there were multi intermediate phases formed before NaMnO 2 appeared at about 600 °C. And the final product after cooling process is a combination of O'3 NaMnO 2 with P2 Na 2/3MnO 2. A P2 type Na 2/3MnO 2 was synthesized at reduced temperature (600 °C). The influence of Na 2CO 3 impurity on themore » electrochemical performance of P2 Na 2/3MnO 2 was thoroughly investigated in our work. It was found that the content of Na 2CO 3 can be reduced by optimizing Na 2CO 3/MnCO 3 ratio during the solid state reaction or other post treatment such as washing with water. Lastly, we expected our results could provide a good guide for future development of high performance cathode materials for sodium-ion batteries.« less

A Review of Microwave-Assisted Reactions for Biodiesel Production

PubMed Central

Nomanbhay, Saifuddin; Ong, Mei Yin

2017-01-01

The conversion of biomass into chemicals and biofuels is an active research area as trends move to replace fossil fuels with renewable resources due to society’s increased concern towards sustainability. In this context, microwave processing has emerged as a tool in organic synthesis and plays an important role in developing a more sustainable world. Integration of processing methods with microwave irradiation has resulted in a great reduction in the time required for many processes, while the reaction efficiencies have been increased markedly. Microwave processing produces a higher yield with a cleaner profile in comparison to other methods. The microwave processing is reported to be a better heating method than the conventional methods due to its unique thermal and non-thermal effects. This paper provides an insight into the theoretical aspects of microwave irradiation practices and highlights the importance of microwave processing. The potential of the microwave technology to accomplish superior outcomes over the conventional methods in biodiesel production is presented. A green process for biodiesel production using a non-catalytic method is still new and very costly because of the supercritical condition requirement. Hence, non-catalytic biodiesel conversion under ambient pressure using microwave technology must be developed, as the energy utilization for microwave-based biodiesel synthesis is reported to be lower and cost-effective. PMID:28952536

A Review of Microwave-Assisted Reactions for Biodiesel Production.

PubMed

Nomanbhay, Saifuddin; Ong, Mei Yin

2017-06-15

The conversion of biomass into chemicals and biofuels is an active research area as trends move to replace fossil fuels with renewable resources due to society's increased concern towards sustainability. In this context, microwave processing has emerged as a tool in organic synthesis and plays an important role in developing a more sustainable world. Integration of processing methods with microwave irradiation has resulted in a great reduction in the time required for many processes, while the reaction efficiencies have been increased markedly. Microwave processing produces a higher yield with a cleaner profile in comparison to other methods. The microwave processing is reported to be a better heating method than the conventional methods due to its unique thermal and non-thermal effects. This paper provides an insight into the theoretical aspects of microwave irradiation practices and highlights the importance of microwave processing. The potential of the microwave technology to accomplish superior outcomes over the conventional methods in biodiesel production is presented. A green process for biodiesel production using a non-catalytic method is still new and very costly because of the supercritical condition requirement. Hence, non-catalytic biodiesel conversion under ambient pressure using microwave technology must be developed, as the energy utilization for microwave-based biodiesel synthesis is reported to be lower and cost-effective.

Effects of Microwave Radiation on Oil Recovery

NASA Astrophysics Data System (ADS)

Esmaeili, Abdollah

2011-12-01

A variety of oil recovery methods have been developed and applied to mature and depleted reservoirs in order to improve the efficiency. Microwave radiation oil recovery method is a relatively new method and has been of great interest in the recent years. Crude oil is typically co-mingled with suspended solids and water. To increase oil recovery, it is necessary to remove these components. The separation of oil from water and solids using gravitational settling methods is typically incomplete. Oil-in-water and oil-water-solid emulsions can be demulsified and separated into their individual layers by microwave radiation. The data also show that microwave separation is faster than gravity separation and can be faster than conventional heating at many conditions. After separation of emulsion into water and oil layers, water can be discharged and oil is collected. High-frequency microwave recycling process can recover oil and gases from oil shale, residual oil, drill cuttings, tar sands oil, contaminated dredge/sediments, tires and plastics with significantly greater yields and lower costs than are available utilizing existing known technologies. This process is environmentally friendly, fuel-generating recycler to reduce waste, cut emissions, and save energy. This paper presents a critical review of Microwave radiation method for oil recovery.

Microwave-Assisted Synthesis of a MK2 Inhibitor by Suzuki-Miyaura Coupling for Study in Werner Syndrome Cells

PubMed Central

Bagley, Mark C.; Baashen, Mohammed; Chuckowree, Irina; Dwyer, Jessica E.; Kipling, David; Davis, Terence

2015-01-01

Microwave-assisted Suzuki-Miyaura cross-coupling reactions have been employed towards the synthesis of three different MAPKAPK2 (MK2) inhibitors to study accelerated aging in Werner syndrome (WS) cells, including the cross-coupling of a 2-chloroquinoline with a 3-pyridinylboronic acid, the coupling of an aryl bromide with an indolylboronic acid and the reaction of a 3-amino-4-bromopyrazole with 4-carbamoylphenylboronic acid. In all of these processes, the Suzuki-Miyaura reaction was fast and relatively efficient using a palladium catalyst under microwave irradiation. The process was incorporated into a rapid 3-step microwave-assisted method for the synthesis of a MK2 inhibitor involving 3-aminopyrazole formation, pyrazole C-4 bromination using N-bromosuccinimide (NBS), and Suzuki-Miyaura cross-coupling of the pyrazolyl bromide with 4-carbamoylphenylboronic acid to give the target 4-arylpyrazole in 35% overall yield, suitable for study in WS cells. PMID:26046488

Expeditious organic–free assembly: morphologically controlled synthesis of iron oxides using microwaves

EPA Science Inventory

A microwave hydrothermal method is developed for the synthesis of iron oxides, α-Fe₂O₃, β-FeOOH, and the junction of α-Fe₂O₃–β-FeOOH. This method is absolutely organic-free, and various structures could be obtained simply by changing th...

Bulk Synthesis of Monodisperse Ferrite Nanoparticles at Water-Organic Interfaces under Conventional and Microwave Hydrothermal Treatment and Their Surface Functionalization

EPA Science Inventory

Synthesis of monodisperse MFe2O4 (M=, Ni, Co, Mn) and γ-Fe2O3 nanoparticles at a water-toluene interface under conventional as well as microwave hydrothermal conditions using readily available nitrate or chloride salts and oleic acid as the dispersing agent is described. The ens...

Repercussion of Solid state vs. Liquid state synthesized p-n heterojunction RGO-copper phosphate on proton reduction potential in water.

PubMed

Samal, Alaka; Das, Dipti P; Madras, Giridhar

2018-02-13

The same copper phosphate catalysts were synthesized by obtaining the methods involving solid state as well as liquid state reactions in this work. And then the optimised p-n hybrid junction photocatalysts have been synthesized following the same solid/liquid reaction pathways. The synthesized copper phosphate photocatalyst has unique rod, flower, caramel-treat-like morphology. The Mott-Schottky behavior is in accordance with the expected behavior of n-type semiconductor and the carrier concentration was calculated using the M-S analysis for the photocatalyst. And for the p-n hybrid junction of 8RGO-Cu 3 (PO 4 ) 2 -PA (PA abbreviated for photoassisted synthesis method), 8RGO-Cu 3 (PO 4 ) 2 -EG(EG abbreviated for Ethylene Glycol based synthesis method), 8RGO-Cu 3 (PO 4 ) 2 -PEG (PEG abbreviated for Poly(ethylene glycol)-block-poly(propylene glycol)-block-poly(ethylene glycol based synthesis method)the amount of H 2 synthesized was 7500, 6500 and 4500 µmol/h/g, respectively. The excited electrons resulting after the irradiation of visible light on the CB of p-type reduced graphene oxide (RGO) migrate easily to n-type Cu 3 (PO 4 ) 2 via. the p-n junction interfaces and hence great charge carrier separation was achieved.

The Microwave-Assisted Green Synthesis of TiC Powders.

PubMed

Wang, Hui; Zhu, Wencheng; Liu, Yanchun; Zeng, Lingke; Sun, Luyi

2016-11-08

Titanium carbide (TiC) is an important engineering material and has found widespread applications. Currently, TiC is typically synthesized through carbothermal reduction, requiring a high temperature (ca. 1700-2300 °C) and long reaction time (ca. 10-20 h), which is not eco-friendly. During a conventional reaction path, anatase TiO₂ (A-TiO₂) was first converted to rutile TiO₂ (R-TiO₂), which was subsequently reduced to TiC. Herein, we explored the synthesis of TiC powders with the assistance of microwave heating. In particular, we achieved the conversion of A-TiO₂, which was more reactive than R-TiO₂ for the carbothermal reduction, to TiC, which was directly due to quick microwave heating. As such, the carbothermal reduction started at a much lower temperature of ca. 1200 °C and finished within 30 min when reacting at 1400 °C, leading to significant energy saving. This study shows that microwave-assisted synthesis can be an effective and green process for preparing TiC powders, which is promising for future large-scale production. The influence of the reaction temperature, the reaction duration, and the carbon content on the synthesis of TiC powders was investigated.

Microwave-assisted synthesis of highly fluorescent nanoparticles of a melamine-based porous covalent organic framework for trace-level detection of nitroaromatic explosives.

PubMed

Zhang, Wang; Qiu, Ling-Guang; Yuan, Yu-Peng; Xie, An-Jian; Shen, Yu-Hua; Zhu, Jun-Fa

2012-06-30

Covalent organic frameworks (COFs) are a new generation of porous materials constructed from light elements linked by strong covalent bonds. Herein we present rapid preparation of highly fluorescent nanoparticles of a new type of COF, i.e. melamine-based porous polymeric network SNW-1, by a microwave-assisted synthesis route. Although the synthesis of SNW-1 has to be carried out at 180°C for 3d under conventional reflux conditions, SNW-1 nanoparticles could be obtained in 6h by using such a microwave-assisted method. The results obtained have clearly demonstrated that microwave-assisted synthesis is a simple yet highly efficient approach to nanoscale COFs or other porous polymeric materials. Remarkably, the as-synthesized SNW-1 nanoparticles exhibit extremely high sensitivity and selectivity, as well as fast response to nitroaromatic explosives such as 2,4,6-trinitrotoluene (TNT), 2,4,6-trinitrophenylmethylnitramine (Tetryl) and picric acid (PA) without interference by common organic solvents, which is due to the nanoscaled size and unique hierarchical porosity of such fluorescence-based sensing material. Copyright © 2012 Elsevier B.V. All rights reserved.

Low-temperature synthesis of actinide tetraborides by solid-state metathesis reactions

DOEpatents

Lupinetti, Anthony J [Los Alamos, NM; Garcia, Eduardo [Los Alamos, NM; Abney, Kent D [Los Alamos, NM

2004-12-14

The synthesis of actinide tetraborides including uranium tetraboride (UB.sub.4), plutonium tetraboride (PuB.sub.4) and thorium tetraboride (ThB.sub.4) by a solid-state metathesis reaction are demonstrated. The present method significantly lowers the temperature required to .ltoreq.850.degree. C. As an example, when UCl.sub.4 is reacted with an excess of MgB.sub.2, at 850.degree. C., crystalline UB.sub.4 is formed. Powder X-ray diffraction and ICP-AES data support the reduction of UCl.sub.3 as the initial step in the reaction. The UB.sub.4 product is purified by washing water and drying.

Satellite Power Systems (SPS) concept definition study (exhibit C)

NASA Technical Reports Server (NTRS)

Hanley, G. M.

1978-01-01

A coplanar satellite conceptual approach was defined. This effort included several trade studies related to satellite design and also construction approaches for this satellite. A transportation system, consistent with this concept, was also studied, including an electric orbit transfer vehicle and a parallel-burn heavy lift launch vehicle. Work on a solid state microwave concept continued and several alternative approaches were evaluated. Computer determination of an optimized transistor and circuit design was also continued. Experiment/verification planning resulted in the development of a total solar array and microwave technology development plan, as well as definition of near-term research to evaluate key technology issues.

Solid-state dynamic nuclear polarization at 263 GHz: spectrometer design and experimental results†

PubMed Central

Rosay, Melanie; Tometich, Leo; Pawsey, Shane; Bader, Reto; Schauwecker, Robert; Blank, Monica; Borchard, Philipp M.; Cauffman, Stephen R.; Felch, Kevin L.; Weber, Ralph T.; Temkin, Richard J.; Griffin, Robert G.; Maas, Werner E.

2015-01-01

Dynamic Nuclear Polarization (DNP) experiments transfer polarization from electron spins to nuclear spins with microwave irradiation of the electron spins for enhanced sensitivity in nuclear magnetic resonance (NMR) spectroscopy. Design and testing of a spectrometer for magic angle spinning (MAS) DNP experiments at 263 GHz microwave frequency, 400 MHz 1H frequency is described. Microwaves are generated by a novel continuous-wave gyrotron, transmitted to the NMR probe via a transmission line, and irradiated on a 3.2 mm rotor for MAS DNP experiments. DNP signal enhancements of up to 80 have been measured at 95 K on urea and proline in water–glycerol with the biradical polarizing agent TOTAPOL. We characterize the experimental parameters affecting the DNP efficiency: the magnetic field dependence, temperature dependence and polarization build-up times, microwave power dependence, sample heating effects, and spinning frequency dependence of the DNP signal enhancement. Stable system operation, including DNP performance, is also demonstrated over a 36 h period. PMID:20449524

Parallel and automated library synthesis of 2-long alkyl chain benzoazoles and azole[4,5-b]pyridines under microwave irradiation.

PubMed

Martínez-Palou, Rafael; Zepeda, L Gerardo; Höpfl, Herbert; Montoya, Ascensión; Guzmán-Lucero, Diego J; Guzmán, Javier

2005-01-01

A versatile route to 40-membered library of 2-long alkyl chain substituted benzoazoles (1 and 2) and azole[4,5-b]pyridines (3 and 4) via microwave-assisted combinatorial synthesis was developed. The reactions were carried out in both monomode and multimode microwave oven. With the latter, all reactions were performed in high-throughput experimental settings consisting of an 8 x 5 combinatorial library designed to synthesize 40 compounds. Each step, from the addition of reagents to the recovery of final products, was automated. The microwave-assisted N-long chain alkylation reactions of 2-alkyl-1H-benzimidazole (1) and 2-alkyl-1H-benzimidazole[4,5-b] pyridines (3) were also studied.

Microwave promoted simple, efficient and regioselective synthesis of trisubstituted imidazo[1,2-a]benzimidazoles on soluble support.

PubMed

Chen, Li-Hsun; Hsiao, Ya-Shan; Yellol, Gorakh S; Sun, Chung-Ming

2011-03-14

An efficient microwave-assisted and soluble polymer-supported synthesis of medicinally important imidazole-fused benzimidazoles has been developed. The protocol involves the rapid condensation of polymer-bound amino benzimidazoles with various α-bromoketones and subsequent in situ intramolecular cyclization under microwave irradiation resulting in a one pot synthesis of imidazole interlacing benzimidazole polymer conjugates. The condensed product was obtained with excellent regioselectivity. The biologically interesting imidazo[1,2-a]benzimidazoles was released from polymer support at ambient temperature. Diversity in the triheterocyclic nucleus was achieved by the different substitutions at its 2, 3, and 9 positions. The new protocol has the advantages of short reaction time, easy workup process, excellent yields, reduced environmental impact, wide substrate scope and convenient procedure.

CONTINUOUS FLOW MICROWAVE REACTORS FOR ORGANIC SYNTHESIS: HYDRODECHLORINATION, HETROCYCLIZATION, ISOMERIZATION

EPA Science Inventory

Microwave heating has been sought as a convenient way of enhancing chemical processes. The advantages of microwave heating, such as selective direct heating of materials of a catalytic site, minimized fouling on hot surfaces, process simplicity, rapid startup, as well as the pos...

CONTINUOUS MICROWAVE REACTORS FOR ORGANIC SYNTHESIS: HYDRODECHLORINATION AND HYDROLYSIS

EPA Science Inventory

Microwave heating has been sought as a convenient way of enhancing chemical processes. The advantages of microwave heating, such as selective direct heating of materials of a catalytic site, minimized fouling on hot surfaces, process simplicity, rapid startup, as well as the poss...

Organic Synthesis Using Microwaves and Supported Reagents

EPA Science Inventory

In the electromagnetic radiation region, microwaves (0.3GHz-300GHz) lie between radiowave (Rf) and infrared (IR) frequencies with relatively large wavelengths (1 mm-1 m). Microwaves, non-ionizing radiation incapable of breaking bonds, are a form of energy that manifest as heat t...

Rapid microwave-assisted synthesis of sub-30nm lipid nanoparticles.

PubMed

Dunn, Stuart S; Beckford Vera, Denis R; Benhabbour, S Rahima; Parrott, Matthew C

2017-02-15

Accessing the phase inversion temperature by microwave heating may enable the rapid synthesis of small lipid nanoparticles. Nanoparticle formulations consisted of surfactants Brij 78 and Vitamin E TPGS, and trilaurin, trimyristin, or miglyol 812 as nanoparticle lipid cores. Each formulation was placed in water and heated by microwave irradiation at temperatures ranging from 65°C to 245°C. We observed a phase inversion temperature (PIT) for these formulations based on a dramatic decrease in particle Z-average diameters. Subsequently, nanoparticles were manufactured above and below the PIT and studied for (a) stability toward dilution, (b) stability over time, (c) fabrication as a function of reaction time, and (d) transmittance of lipid nanoparticle dispersions. Lipid-based nanoparticles with distinct sizes down to 20-30nm and low polydispersity could be attained by a simple, one-pot microwave synthesis. This was carried out by accessing the phase inversion temperature using microwave heating. Nanoparticles could be synthesized in just one minute and select compositions demonstrated high stability. The notable stability of these particles may be explained by the combination of van der Waals interactions and steric repulsion. 20-30nm nanoparticles were found to be optically transparent. Published by Elsevier Inc.

Microwave-assisted synthesis and electrochemical evaluation of VO 2 (B) nanostructures

DOE PAGES

Ashton, Thomas E.; Borras, David Hevia; Iadecola, Antonella; ...

2015-12-01

Understanding how intercalation materials change during electrochemical operation is paramount to optimising their behaviour and function and in situ characterisation methods allow us to observe these changes without sample destruction. Here, we first report the improved intercalation properties of bronze phase vanadium dioxide VO2 (B) prepared by a microwave assisted route which exhibits a larger electrochemical capacity (232 mAh g -1) compared to VO 2 (B) prepared by a solvothermal route (197 mAh g -1). These electrochemical differences have also been followed using in situ X-ray absorption spectroscopy allowing us to follow oxidation state changes as they occur during batterymore » operation.« less

Fundamentals handbook of electrical and computer engineering. Volume 1 Circuits fields and electronics

NASA Astrophysics Data System (ADS)

Chang, S. S. L.

State of the art technology in circuits, fields, and electronics is discussed. The principles and applications of these technologies to industry, digital processing, microwave semiconductors, and computer-aided design are explained. Important concepts and methodologies in mathematics and physics are reviewed, and basic engineering sciences and associated design methods are dealt with, including: circuit theory and the design of magnetic circuits and active filter synthesis; digital signal processing, including FIR and IIR digital filter design; transmission lines, electromagnetic wave propagation and surface acoustic wave devices. Also considered are: electronics technologies, including power electronics, microwave semiconductors, GaAs devices, and magnetic bubble memories; digital circuits and logic design.

Investigations on structural and optical properties of starch capped ZnS nanoparticles synthesized by microwave irradiation method

NASA Astrophysics Data System (ADS)

Lalithadevi, B.; Mohan Rao, K.; Ramananda, D.

2018-05-01

Following a green synthesis method, zinc sulfide (ZnS) nanoparticles were prepared by chemical co-precipitation technique using starch as capping agent. Microwave irradiation was used as heating source. X-ray diffraction studies indicated that nanopowders obtained were polycrystalline possessing ZnS simple cubic structure. Transmission electron microscopic studies indicated that starch limits the agglomeration by steric stabilization. Interaction between ZnS and starch was confirmed by Fourier transform infrared spectroscopy as well as Raman scattering studies. Quantum size effects were observed in optical absorption studies while quenching of defect states on nanoparticles was improved with increase in starch addition as indicated by photoluminescence spectra.

Evaluation of microwave oven heating for prediction of drug-excipient compatibilities and accelerated stability studies.

PubMed

Schou-Pedersen, Anne Marie V; Østergaard, Jesper; Cornett, Claus; Hansen, Steen Honoré

2015-05-15

Microwave ovens have been used extensively in organic synthesis in order to accelerate reaction rates. Here, a set up comprising a microwave oven combined with silicon carbide (SiC) plates for the controlled microwave heating of model formulations has been applied in order to investigate, if a microwave oven is applicable for accelerated drug stability testing. Chemical interactions were investigated in three selected model formulations of drug and excipients regarding the formation of ester and amide reaction products. In the accelerated stability studies, a design of experiments (DoE) approach was applied in order to be able to rank excipients regarding reactivity: Study A: cetirizine with PEG 400, sorbitol, glycerol and propylene glycol. Study B: 6-aminocaproic acid with citrate, acetate, tartrate and gluconate. Study C: atenolol with citric, tartaric, malic, glutaric, and sorbic acid. The model formulations were representative for oral solutions (co-solvents), parenteral solutions (buffer species) and solid dosage forms (organic acids applicable for solubility enhancement). The DoE studies showed overall that the same impurities were generated by microwave oven heating leading to temperatures between 150°C and 180°C as compared to accelerated stability studies performed at 40°C and 80°C using a conventional oven. Ranking of the reactivity of the excipients could be made in the DoE studies performed at 150-180°C, which was representative for the ranking obtained after storage at 40°C and 80°C. It was possible to reduce the time needed for drug-excipient compatibility testing of the three model formulations from weeks to less than an hour in the three case studies. The microwave oven is therefore considered to be an interesting alternative to conventional thermal techniques for the investigation of drug-excipient interactions during preformulation. Copyright © 2015 Elsevier B.V. All rights reserved.

Rare earth indates (RE: La-Yb): influence of the synthesis route and heat treatment on the crystal structure.

PubMed

Shukla, Rakesh; Grover, Vinita; Srinivasu, Kancharlapalli; Paul, Barnita; Roy, Anushree; Gupta, Ruma; Tyagi, Avesh Kumar

2018-05-15

Rare earth indates are an interesting class of compounds with rich crystallography. The present study explores the crystallographic phases observed in REInO3 (RE: La-Yb) systems and their dependence on synthesis routes and annealing temperature. All REInO3 compositions were synthesized by a solid state route as well as gel-combustion synthesis (GC) followed by annealing at different temperatures. The systems were well characterized by powder XRD studies and were analysed by Rietveld refinement for the structural parameters. The cell parameters were observed to decrease in accordance with the trend in ionic radii on proceeding from lighter to heavier rare earth ions. Interestingly, the synthesis route and the annealing temperature had a profound bearing on the phase relationships observed in the REInO3 series. The solid state synthesized samples depicted an orthorhombic phase (Pbnm) field for LaInO3 to SmInO3, followed by a hexagonal-type phase (P63cm) for GdInO3 to DyInO3. However, the phase field distribution was greatly influenced upon employing gel-combustion (GC) wherein both single-phasic hexagonal and orthorhombic phase fields were found to shrink. Annealing the GC-synthesized compositions to still higher temperatures (1250 °C) further evolved the phase boundaries. An important outcome of the study is observance of polymorphism in SmInO3 which crystallized in the hexagonal phase when synthesized by GC and orthorhombic phase by solid state synthesis. This reveals the all-important role played by synthesis conditions. The existence and energetics of the two polymorphs have been elucidated and discussed with the aid of theoretical studies.

Broadening microwave absorption via a multi-domain structure

NASA Astrophysics Data System (ADS)

Liu, Zhengwang; Che, Renchao; Wei, Yong; Liu, Yupu; Elzatahry, Ahmed A.; Dahyan, Daifallah Al.; Zhao, Dongyuan

2017-04-01

Materials with a high saturation magnetization have gained increasing attention in the field of microwave absorption; therefore, the magnetization value depends on the magnetic configuration inside them. However, the broad-band absorption in the range of microwave frequency (2-18 GHz) is a great challenge. Herein, the three-dimensional (3D) Fe/C hollow microspheres are constructed by iron nanocrystals permeating inside carbon matrix with a saturation magnetization of 340 emu/g, which is 1.55 times as that of bulk Fe, unexpectedly. Electron tomography, electron holography, and Lorentz transmission electron microscopy imaging provide the powerful testimony about Fe/C interpenetration and multi-domain state constructed by vortex and stripe domains. Benefiting from the unique chemical and magnetic microstructures, the microwave minimum absorption is as strong as -55 dB and the bandwidth (<-10 dB) spans 12.5 GHz ranging from 5.5 to 18 GHz. Morphology and distribution of magnetic nano-domains can be facilely regulated by a controllable reduction sintering under H2/Ar gas and an optimized temperature over 450-850 °C. The findings might shed new light on the synthesis strategies of the materials with the broad-band frequency and understanding the association between multi-domain coupling and microwave absorption performance.

GREENER AND CONTROLLED SYNTHESIS OF NOBLE NANOSTRUCTURES IN AQUEOUS MEDIA USING MICROWAVE IRRADIATION

EPA Science Inventory

Microwave-assisted spontaneous reduction of gold salts is described using sugar solutions such as alpha-D-glucose, sucrose and maltose, etc. The expeditious reactions are conducted in aqueous media using microwave irradiation wherein the reduction occurs within 30 to 60 seconds ...

Microwave-Facilitated SPOT-Synthesis of Antibacterial Dipeptoids.

PubMed

Schneider, Anne C; Fritz, Daniel; Vasquez, Joseph K; Vollrath, Sidonie B L; Blackwell, Helen E; Bräse, Stefan

2017-12-11

With microwave irradiation, the submonomer synthesis of dipeptoids on functionalized cellulose can be accelerated with good yields and purity. Optimization provided a library of 96 dipeptoids. From these, 29 compounds were found with an antibacterial activity against MRSA at a concentration of 25 μM. Large nonpolar residues, such as undecylamine and dehydroabiethylamine, are the key components engendering the observed antibacterial activity of these peptoids.

Microwave assisted tandem reactions for the synthesis of 2-hydrazolyl-4-thiazolidinones

PubMed Central

Saiz, Cecilia; Pizzo, Chiara; Manta, Eduardo; Wipf, Peter; Mahler, S. Graciela

2009-01-01

A tandem method for the synthesis of 2-hydrazolyl-4-thiazolidinones (5) from commercially available materials in a 3 component reaction has been developed. The reaction connects aldehydes, thiosemicarbazides and maleic anhydride, effectively assisted by microwave irradiation. The synthesis of a new type of compound, 2-hydrazolyl-5,5-diphenyl-4-thiazolidinone (7), obtained by treatment of thiosemicarbazone with benzil in basic media is also reported. HOMO/LUMO energies, orbital coefficients and charge distribution were used to explain the proposed reaction mechanism. PMID:19756224

Density Optimization of Lithium Lanthanum Titanate Ceramics for Lightweight Lithium-Air Batteries

DTIC Science & Technology

2014-11-01

Thangadurai V, Weppner W. Lithium lanthanum titanates: a review. Chemistry of Materials. 2003;15:3974–3990. 4. Knauth P. Inorganic solid Li ion conductors...an overview. Solid State Ionics. 2009;180:911–916. 5. Ban CW, Choi GM. The effect of sintering on the grain boundary conductivity of lithium ...lanthanum titanates. Solid State Ionics. 2001;140:285–292. 6. Inada R, Kimura K, Kusakabe K, Tojo T, Sakurai Y. Synthesis and lithium -ion conductivity

Solid State Division progress report for period ending March 31, 1997

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

Green, P.H.; Hinton, L.W.

1997-12-01

This report covers research progress in the Solid State Division from April 1, 1995, through March 31, 1997. During this period, the division conducted a broad, interdisciplinary materials research program in support of Department of Energy science and technology missions. The report includes brief summaries of research activities in condensed matter theory, neutron scattering, synthesis and characterization of materials, ion beam and laser processing, and the structure of solids and surfaces. An addendum includes listings of division publications and professional activities.

MIL-101(Cr)@GO for dispersive micro-solid-phase extraction of pharmaceutical residue in chicken breast used in microwave-assisted coupling with HPLC-MS/MS detection.

PubMed

Wang, Yudan; Dai, Xinpeng; He, Xi; Chen, Lin; Hou, Xiaohong

2017-10-25

In this work, MIL-101(Cr)@GO (Graphite Oxide) was synthesized using a hydrothermal synthesis method and was applied as a dispersive micro-solid-phase extraction (D-μ-SPE) sorbent for the efficient concentration of four residual drugs (metronidazole, MNZ; tinidazole, TNZ; chloramphenicol, CAP; sulfamethoxazole, SMX). Meanwhile, the extraction process was optimized by combining it with microwave-assisted extraction. Factors affecting the D-μ-SPE efficiency, such as selection of sorbent materials, pH of the sample solution, salting-out effect, amount of used material, extraction time, desorption solvent and desorption time, were studied. Under the optimal extraction conditions, the linearity ranged from 10 to 1000ngkg -1 and 1-100ngkg -1 (r 2 ≥0.9928) for the target analytes. The limits of detection were between 0.08 and 1.02ngkg -1 , and the limits of quantitation were between 0.26 and 3.40ngkg -1 . Additionally, the developed method also exhibited good precision (RSD≤2.5%), repeatability (RSD≤4.3%), high recoveries (88.9%-102.3%) and low matrix effects (78.2%-95.1%). The proposed method proved to be an efficient and reliable approach for the determination of the analytes. Finally, we successfully detected the four drugs in chicken breast. Copyright © 2017 Elsevier B.V. All rights reserved.

A broadband chip-scale optical frequency synthesizer at 2.7 × 10−16 relative uncertainty

PubMed Central

Huang, Shu-Wei; Yang, Jinghui; Yu, Mingbin; McGuyer, Bart H.; Kwong, Dim-Lee; Zelevinsky, Tanya; Wong, Chee Wei

2016-01-01

Optical frequency combs—coherent light sources that connect optical frequencies with microwave oscillations—have become the enabling tool for precision spectroscopy, optical clockwork, and attosecond physics over the past decades. Current benchmark systems are self-referenced femtosecond mode-locked lasers, but Kerr nonlinear dynamics in high-Q solid-state microresonators has recently demonstrated promising features as alternative platforms. The advance not only fosters studies of chip-scale frequency metrology but also extends the realm of optical frequency combs. We report the full stabilization of chip-scale optical frequency combs. The microcomb’s two degrees of freedom, one of the comb lines and the native 18-GHz comb spacing, are simultaneously phase-locked to known optical and microwave references. Active comb spacing stabilization improves long-term stability by six orders of magnitude, reaching a record instrument-limited residual instability of 3.6mHz/τ. Comparing 46 nitride frequency comb lines with a fiber laser frequency comb, we demonstrate the unprecedented microcomb tooth-to-tooth relative frequency uncertainty down to 50 mHz and 2.7 × 10−16, heralding novel solid-state applications in precision spectroscopy, coherent communications, and astronomical spectrography. PMID:27152341

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

Microwave assisted solid phase extraction for separation preconcentration sulfamethoxazole in wastewater using tyre based activated carbon as solid phase material prior to spectrophotometric determination

NASA Astrophysics Data System (ADS)

Mogolodi Dimpe, K.; Mpupa, Anele; Nomngongo, Philiswa N.

2018-01-01

This work was chiefly encouraged by the continuous consumption of antibiotics which eventually pose harmful effects on animals and human beings when present in water systems. In this study, the activated carbon (AC) was used as a solid phase material for the removal of sulfamethoxazole (SMX) in wastewater samples. The microwave assisted solid phase extraction (MASPE) as a sample extraction method was employed to better extract SMX in water samples and finally the analysis of SMX was done by the UV-Vis spectrophotometer. The microwave assisted solid phase extraction method was optimized using a two-level fractional factorial design by evaluating parameters such as pH, mass of adsorbent (MA), extraction time (ET), eluent ratio (ER) and microwave power (MP). Under optimized conditions, the limit of detection (LOD) and limit of quantification (LOQ) were 0.5 μg L- 1 and 1.7 μg L- 1, respectively, and intraday and interday precision expressed in terms of relative standard deviation were > 6%.The maximum adsorption capacity was 138 mg g- 1 for SMX and the adsorbent could be reused eight times. Lastly, the MASPE method was applied for the removal of SMX in wastewater samples collected from a domestic wastewater treatment plant (WWTP) and river water.

Short review of high-pressure crystal growth and magnetic and electrical properties of solid-state osmium oxides

NASA Astrophysics Data System (ADS)

Yamaura, Kazunari

2016-04-01

High-pressure crystal growth and synthesis of selected solid-state osmium oxides, many of which are perovskite-related types, are briefly reviewed, and their magnetic and electrical properties are introduced. Crystals of the osmium oxides, including NaOsO3, LiOsO3, and Na2OsO4, were successfully grown under high-pressure and high-temperature conditions at 6 GPa in the presence of an appropriate amount of flux in a belt-type apparatus. The unexpected discovery of a magnetic metal-insulator transition in NaOsO3, a ferroelectric-like transition in LiOsO3, and high-temperature ferrimagnetism driven by a local structural distortion in Ca2FeOsO6 may represent unique features of the osmium oxides. The high-pressure and high-temperature synthesis and crystal growth has played a central role in the development of solid-state osmium oxides and the elucidation of their magnetic and electronic properties toward possible use in multifunctional devices.

Joseph F. Keithley Award For Advances in Measurement Science Talk: Precision Noise Measurements at Microwave and Optical Frequencies

NASA Astrophysics Data System (ADS)

Ivanov, Eugene

2010-03-01

The quest to detect Gravitational Waves resulted in a number of important developments in the fields of oscillator frequency stabilization and precision noise measurements. This was due to the realization of similarities between the principles of high sensitivity measurements of weak mechanical forces and phase/amplitude fluctuations of microwave signals. In both cases interferometric carrier suppression and low-noise amplification of the residual noise sidebands were the main factors behind significant improvements in the resolution of spectral measurements. In particular, microwave frequency discriminators with almost thermal noise limited sensitivity were constructed leading to microwave oscillators with more than 25dB lower phase noise than the previous state-of-the-art. High power solid-state microwave amplifiers offered further opportunity of oscillator phase noise reduction due to the increased energy stored in the high-Q resonator of the frequency discriminator. High power microwave oscillators with the phase noise spectral density close to -160dBc/Hz at 1kHz Fourier frequency have been recently demonstrated. The principles of interferometric signal processing have been applied to the study of noise phenomena in microwave components which were considered to be ``noise free''. This resulted in the first experimental evidence of phase fluctuations in microwave circulators. More efficient use of signal power enabled construction of the ``power recycled'' interferometers with spectral resolution of -200dBc/Hz at 1kHz Fourier frequency. This has been lately superseded by an order of magnitude with a waveguide interferometer due to its higher power recycling factor. A number of opto-electronic measurement systems were developed to characterize the fidelity of frequency transfer from the optical to the microwave domain. This included a new type of a phase detector capable of measuring phase fluctuations of the weak microwave signals extracted from the demodulated femtosecond light pulses with almost thermal noise limited precision. The experiments which followed showed that microwave signals of exceptional spectral purity could be generated from the frequency stabilized lasers

An easy access to 2-Amino-5,6-dihydro-3H-pyrimidin-4-one building blocks: the reaction under conventional and microwave conditions.

PubMed

Ostras, Konstantin S; Gorobets, Nikolay Yu; Desenko, Sergey M; Musatov, Vladimir I

2006-08-01

A new one-stage fast multicomponent synthesis of title compounds leads to products in 21-55% isolated yields under both conventional and microwave conditions. The primary amino group in the building blocks can be easily acylated by various usual electophilic agents that can be utilized in the synthesis of diverse heterocylic compounds libraries.

Synthesis of phenanthridine derivatives by microwave-mediated cyclization of o-furyl(allylamino)arenes.

PubMed

Read, Matthew Lovell; Gundersen, Lise-Lotte

2013-02-01

A novel and efficient synthesis of phenanthridines and aza analogues is reported. The key step is a microwave-mediated intramolecular Diels-Alder cyclization of o-furyl(allylamino)arenes. In the presence of a catalytic amount of acid, the DA-adduct reacts further to give the dihydrophenanthridines, which easily can be oxidized to fully aromatic compounds by air in the presence of UV light or by DDQ.

Traveling-Wave Tubes

NASA Technical Reports Server (NTRS)

Kory, Carol L.

1998-01-01

The traveling-wave tube (TWT) is a vacuum device invented in the early 1940's used for amplification at microwave frequencies. Amplification is attained by surrendering kinetic energy from an electron beam to a radio frequency (RF) electromagnetic wave. The demand for vacuum devices has been decreased largely by the advent of solid-state devices. However, although solid state devices have replaced vacuum devices in many areas, there are still many applications such as radar, electronic countermeasures and satellite communications, that require operating characteristics such as high power (Watts to Megawatts), high frequency (below 1 GHz to over 100 GHz) and large bandwidth that only vacuum devices can provide. Vacuum devices are also deemed irreplaceable in the music industry where musicians treasure their tube-based amplifiers claiming that the solid-state and digital counterparts could never provide the same "warmth" (3). The term traveling-wave tube includes both fast-wave and slow-wave devices. This article will concentrate on slow-wave devices as the vast majority of TWTs in operation fall into this category.

Synthesis and characterization of zinc borophosphates with ANA-zeotype framework by the microwave method

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

Song, Yu, E-mail: songyu@dlpu.edu.cn; Ding, Ling; An, Qingda

2013-06-15

Zinc borophosphate (NH{sub 4}){sub 16}[Zn{sub 16}B{sub 8}P{sub 24}O{sub 96}] (denoted as ZnBP-ANA) with ANA-zeotype structure has been synthesized by employing microwave-assisted solvothermal synthesis in the reaction system ZnCl{sub 2}∙6H{sub 2}O-(NH{sub 4}){sub 2}HPO{sub 4}–H{sub 3}BO{sub 3} using ethylene glycol as a co-solvent. The influences of various experimental parameters, such as reaction temperature, solvent ratio, zinc precursors and reactive power, have been systematically investigated. The products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and thermogravimetric analysis (TGA), and so on. Small and homogeneous ZnBP-ANA single crystal with regular cube morphology are crystallized by using microwave solvothermal synthesis method withinmore » a shorter time, and its grain size decreases with power. - Graphical abstract: Tailor-made ANA zeolites with varied size can be prepared by simply changing the reaction power. - Highlights: • Zinc borophosphate zeolites with ANA-zeotype structures were prepared by microwave technique. • The size of crystals could be controlled by tuning power. • Synthesis period can be significantly reduced by raising reaction temperature.« less

Stabilization of Co{sup 2+} in layered double hydroxides (LDHs) by microwave-assisted ageing

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

Herrero, M.; Benito, P.; Labajos, F.M.

2007-03-15

Co-containing layered double hydroxides at different pH have been prepared, and aged following different routes. The solids prepared have been characterized by element chemical analysis, powder X-ray diffraction, thermogravimetric and differential thermal analyses (both in nitrogen and in oxygen), FT-IR and Vis-UV spectroscopies, temperature-programmed reduction and surface area assessment by nitrogen adsorption at -196 deg. C. The best conditions found to preserve the cobalt species in the divalent oxidation state are preparing the samples at controlled pH, and then submit them to ageing under microwave irradiation. - Graphical abstract: The use of microwave-hydrothermal treatment, controlling both temperature and ageing time,more » permits to synthesize well-crystallized nanomaterials with controlled surface properties. An enhancement in the crystallinity degree and an increase in the particle size are observed when the irradiation time is prolonged.« less

Microwave power amplifiers based on AlGaN/GaN transistors with a two-dimensional electron gas

NASA Astrophysics Data System (ADS)

Vendik, O. G.; Vendik, I. B.; Tural'chuk, P. A.; Parnes, Ya. M.; Parnes, M. D.

2016-11-01

A technique for synthesis of microwave power amplifiers based on transistors with a AlGaN/GaN heterojunction is discussed. Special focus is on the development of a technique for synthesis of transformation circuits of the power amplifier to increase efficiency with a retained high output power. The use of independent matching at the harmonic frequencies and fundamental frequency makes it possible to control the attainable efficiency in a wide frequency band along with the total suppression of harmonics beyond the operational band. Microwave power amplifiers for operation at 4 and 9 GHz have been developed and experimentally investigated.

Microwave assisted facile green synthesis of silver and gold nanocatalysts using the leaf extract of Aerva lanata.

PubMed

Joseph, Siby; Mathew, Beena

2015-02-05

Herein, we report a simple microwave assisted method for the green synthesis of silver and gold nanoparticles by the reduction of aqueous metal salt solutions using leaf extract of the medicinal plant Aerva lanata. UV-vis., FTIR, XRD, and HR-TEM studies were conducted to assure the formation of nanoparticles. XRD studies clearly confirmed the crystalline nature of the synthesized nanoparticles. From the HR-TEM images, the silver nanoparticles (AgNPs) were found to be more or less spherical and gold nanoparticles (AuNPs) were observed to be of different morphology with an average diameter of 18.62nm for silver and 17.97nm for gold nanoparticles. In order to evaluate the effect of microwave heating upon rate of formation, the synthesis was also conducted under ambient condition without the assistance of microwave radiation and the former method was found to be much faster than the later. The synthesized nanoparticles were used as nanocatalysts in the reduction of 4-nitrophenol to 4-aminophenol by NaBH4. Copyright © 2014 Elsevier B.V. All rights reserved.

Hydrothermal Synthesis of Analcime from Kutingkeng Formation Mudstone

NASA Astrophysics Data System (ADS)

Hsiao, Yin-Hsiu; Chen, Kuan-Ting; Ray, Dah-Tong

2015-04-01

In southwest of Taiwan, the foothill located in Tainan-Kaohsiung city is the exposed area of Pliocene strata to early Pleistocene strata. The strata are about a depth of five thousand, named as Kutigkeng Formation. The outcrop of Kutigkeng Formation is typical badlands, specifically called 'Moon World.' It is commonly known as no important economic applications of agricultural land. The mineral compositions of Kutingkeng Formation are quartz, clay minerals and feldspar. The clay minerals consist of illite, clinochlore and swelling clays. To study how the phase and morphology of analcime formed by hydrothermal synthesis were affected, analcime was synthesized from the mudstone of Kutinkeng Formation with microwave hydrothermal reaction was investigated. The parameters of the experiment were the reaction temperature, the concentration of mineralizer, solids/liquid ratio and time. The sodium silicate (Na2SiO3) were used as mineralizer. The results showed that the analcime could be synthesized by hydrothermal reaction above 180° from Kutinkeng Formation mudstone samples. At the highest temperature (240°) of this study, the high purity analcime could be produced. When the concentration of Na2SiO3=3~6M, analcime could be synthesized at 240°. The best solids/liquid ratio was approximate 1 to 5. The hydrothermal reaction almost was completed after 4 hours.

One-step synthesis of pyridines and dihydropyridines in a continuous flow microwave reactor

PubMed Central

Fusillo, Vincenzo; Jenkins, Robert L; Lubinu, M Caterina; Mason, Christopher

2013-01-01

Summary The Bohlmann–Rahtz pyridine synthesis and the Hantzsch dihydropyridine synthesis can be carried out in a microwave flow reactor or using a conductive heating flow platform for the continuous processing of material. In the Bohlmann–Rahtz reaction, the use of a Brønsted acid catalyst allows Michael addition and cyclodehydration to be carried out in a single step without isolation of intermediates to give the corresponding trisubstituted pyridine as a single regioisomer in good yield. Furthermore, 3-substituted propargyl aldehydes undergo Hantzsch dihydropyridine synthesis in preference to Bohlmann–Rahtz reaction in a very high yielding process that is readily transferred to continuous flow processing. PMID:24204407

High-efficiency solid state power amplifier

NASA Technical Reports Server (NTRS)

Wallis, Robert E. (Inventor); Cheng, Sheng (Inventor)

2005-01-01

A high-efficiency solid state power amplifier (SSPA) for specific use in a spacecraft is provided. The SSPA has a mass of less than 850 g and includes two different X-band power amplifier sections, i.e., a lumped power amplifier with a single 11-W output and a distributed power amplifier with eight 2.75-W outputs. These two amplifier sections provide output power that is scalable from 11 to 15 watts without major design changes. Five different hybrid microcircuits, including high-efficiency Heterostructure Field Effect Transistor (HFET) amplifiers and Monolithic Microwave Integrated Circuit (MMIC) phase shifters have been developed for use within the SSPA. A highly efficient packaging approach enables the integration of a large number of hybrid circuits into the SSPA.

Investigation into the use of microwave sensors to monitor particulate manufacturing processes

NASA Astrophysics Data System (ADS)

Austin, John Samuel, III

Knowledge of a material's properties in-line during manufacture is of critical importance to many industries, including the pharmaceutical industry, and can be used for either process or quality control. Different microwave sensor configurations were tested to determine both the moisture content and the bulk density in pharmaceutical powders during processing on-line. Although these parameters can significantly affect a material's flowability, compressibility, and cohesivity, in the presence of blends, the picture is incomplete. Due to the ease with which particulate blends tend to segregate, blend uniformity and chemical composition are two critical parameters in nearly all solids manufacturing industries. The prevailing wisdom has been that microwave sensors are not capable of or sensitive enough to measure the relative concentrations of components in a blend. Consequently, it is common to turn to near infrared sensing to determine material composition on-line. In this study, a novel microwave sensor was designed and utilized to determine, separately, the concentrations of different components in a blend of pharmaceutical powders. This custom microwave sensor was shown to have comparable accuracy to the state-of-the-art for both chemical composition and moisture content determination.

Subcarrier multiplexing with dispersion reduction and direct detection

DOEpatents

Sargis, Paul D.; Haigh, Ronald E.; McCammon, Kent G.

1997-01-01

An SCM system for simultaneously reducing the concomitant problems of receiver complexity and dispersion penalty and without requiring the use of an expensive, high-bandwidth optical detector. The system provides both a dispersion reduction and a direct detection to the receiver, with microwave mixers and lithium niobate external modulators that produce sidebands that are only separated by a few gigahertz from a principal laser optical carrier. Digital data streams are independently impressed upon these sidebands for transmission over an ordinary single-mode fiber. Independent high-speed data streams are upconverted to microwave frequencies. These subcarriers are then combined with a microwave power combiner and amplified with a microwave amplifier. A solid-state 1550-nm laser carrier is modulated by the microwave subcarriers. An erbium-doped fiber amplifier (EDFA) is used just prior to long-distance transmission over ordinary single-mode fiber. The transmitted optical signal may then traverse multiple EDFAs to compensate for long-haul optical fiber losses prior to detection. At a receiving end, the optical signal is split into multiple paths. The subcarrier channels are optically pre-selected using a narrowband optical filter, such as a fiber Fabry-Perot (FFP) filter. An optical detector converts the selected optical signal into a baseband electrical data stream.

TiO2-coated mesoporous carbon: conventional vs. microwave-annealing process.

PubMed

Coromelci-Pastravanu, Cristina; Ignat, Maria; Popovici, Evelini; Harabagiu, Valeria

2014-08-15

The study of coating mesoporous carbon materials with titanium oxide nanoparticles is now becoming a promising and challenging area of research. To optimize the use of carbon materials in various applications, it is necessary to attach functional groups or other nanostructures to their surface. The combination of the distinctive properties of mesoporous carbon materials and titanium oxide is expected to be applied in field emission displays, nanoelectronic devices, novel catalysts, and polymer or ceramic reinforcement. But, their synthesis is still largely based on conventional techniques, such as wet impregnation followed by chemical reduction of the metal nanoparticle precursors, which takes time and money. The thermal heating based techniques are time consuming and often lack control of particle size and morphology. Hence, since there is a growing interest in microwave technology, an alternative way of power input into chemical reactions through dielectric heating is the use of microwaves. This work is focused on the advantages of microwave-assisted synthesis of TiO2-coated mesoporous carbon over conventional thermal heating method. The reviewed studies showed that the microwave-assisted synthesis of such composites allows processes to be completed within a shorter reaction time allowing the nanoparticles formation with superior properties than that obtained by conventional method. Copyright © 2014 Elsevier B.V. All rights reserved.

On the importance of simultaneous infrared/fiber-optic temperature monitoring in the microwave-assisted synthesis of ionic liquids.

PubMed

Obermayer, David; Kappe, C Oliver

2010-01-07

The temperature profiles obtained from both an external infrared and internal fiber-optic sensor were compared for heating and synthesizing the ionic liquid 1-butyl-3-methylimidazolium bromide (bmimBr) under microwave conditions. Utilizing a single-mode microwave reactor that allows simultaneous infrared/fiber-optic temperature measurements, significant differences between the two methods of temperature monitoring were revealed. Due to the strong microwave absorptivity of ionic liquids and the delay experienced in monitoring temperature on the outer surface of a heavy-walled glass vial, external infrared temperature sensors can not be used to accurately control the temperature in the heating of ionic liquids under microwave conditions. The use of internal fiber-optic probes allows the monitoring and control of the heating behavior in a much better way. In order to prevent the strong exotherm in the synthesis of bmimBr under microwave conditions the use of a reaction vessel made out of silicon carbide is the method of choice. Because of the high thermal conductivity and effusivity of silicon carbide, the heat generated during the ionic liquid formation is efficiently exchanged with the comparatively cool air in the microwave cavity via the silicon carbide ceramic.

Beamed microwave power transmitting and receiving subsystems radiation characteristics

NASA Technical Reports Server (NTRS)

Dickinson, R. M.

1980-01-01

Measured characteristics of the spectrum of typical converters and the distribution of radiated Radio Frequency (RF) energy from the terminals (transmitting antenna and rectenna) of a beamed microwave power subsystem are presented for small transmitting and receiving S-band (2.45 GHz) subarrays. Noise and harmonic levels of tube and solid-state RF power amplifiers are shown. The RF patterns and envelope of a 64 element slotted waveguide antenna are given for the fundamental frequency and harmonics through the fifth. Reflected fundamental and harmonic patterns through the fourth for a 42 element rectenna subarray are presented for various dc load and illumination conditions. Bandwidth measurements for the waveguide antenna and rectenna are shown.

Characteristics of a four element gyromagnetic nonlinear transmission line array high power microwave source.

PubMed

Johnson, J M; Reale, D V; Krile, J T; Garcia, R S; Cravey, W H; Neuber, A A; Dickens, J C; Mankowski, J J

2016-05-01

In this paper, a solid-state four element array gyromagnetic nonlinear transmission line high power microwave system is presented as well as a detailed description of its subsystems and general output capabilities. This frequency agile S-band source is easily adjusted from 2-4 GHz by way of a DC driven biasing magnetic field and is capable of generating electric fields of 7.8 kV/m at 10 m correlating to 4.2 MW of RF power with pulse repetition frequencies up to 1 kHz. Beam steering of the array at angles of ±16.7° is also demonstrated, and the associated general radiation pattern is detailed.

Characteristics of a four element gyromagnetic nonlinear transmission line array high power microwave source

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

Johnson, J. M., E-mail: jared.johnson@ttu.edu; Reale, D. V.; Garcia, R. S.

2016-05-15

In this paper, a solid-state four element array gyromagnetic nonlinear transmission line high power microwave system is presented as well as a detailed description of its subsystems and general output capabilities. This frequency agile S-band source is easily adjusted from 2-4 GHz by way of a DC driven biasing magnetic field and is capable of generating electric fields of 7.8 kV/m at 10 m correlating to 4.2 MW of RF power with pulse repetition frequencies up to 1 kHz. Beam steering of the array at angles of ±16.7° is also demonstrated, and the associated general radiation pattern is detailed.

Strong coupling of a single electron in silicon to a microwave photon

NASA Astrophysics Data System (ADS)

Mi, X.; Cady, J. V.; Zajac, D. M.; Deelman, P. W.; Petta, J. R.

2017-01-01

Silicon is vital to the computing industry because of the high quality of its native oxide and well-established doping technologies. Isotopic purification has enabled quantum coherence times on the order of seconds, thereby placing silicon at the forefront of efforts to create a solid-state quantum processor. We demonstrate strong coupling of a single electron in a silicon double quantum dot to the photonic field of a microwave cavity, as shown by the observation of vacuum Rabi splitting. Strong coupling of a quantum dot electron to a cavity photon would allow for long-range qubit coupling and the long-range entanglement of electrons in semiconductor quantum dots.

Applications of microwave-accelerated organic synthesis

NASA Astrophysics Data System (ADS)

Majetich, George; Hicks, Rodgers

1995-04-01

A comparison of microwave vs conventional heating is presented for a variety of Diels-Alder reactions, ortho-Claisen rearrangements, ene reactions, alkyl bromide preparations, Finkelstein reactions, oxidations, esterifications, hydrolyses, Williamson ether syntheses and other common organic transformations. In general, microwave-promoted reactions proceed with significant decreases in reaction times and in comparable chemical yield.

Microwave-Assisted Organic Synthesis in the Organic Teaching Lab: A Simple, Greener Wittig Reaction

ERIC Educational Resources Information Center

Martin, Eric; Kellen-Yuen, Cynthia

2007-01-01

A greener, microwave-assisted Wittig reaction has been developed for the second-semester organic teaching laboratory. Utilizing this microwave technique, a variety of styrene derivatives have been successfully synthesized from aromatic aldehydes in good yields (41-68%). The reaction not only occurs under neat reaction conditions, but also employs…

Conventional and microwave pyrolysis of a macroalgae waste from the Agar-Agar industry. Prospects for bio-fuel production.

PubMed

Ferrera-Lorenzo, N; Fuente, E; Bermúdez, J M; Suárez-Ruiz, I; Ruiz, B

2014-01-01

A comparative study of the pyrolysis of a macroalgae industrial solid waste (algae meal) in an electrical conventional furnace and in a microwave furnace has been carried out. It was found that the chars obtained from both pyrolyses are similar and show good properties for performing as a solid bio-fuel and as a precursor of activated carbon. Bio-oils from conventional pyrolysis have a greater number of phenolic, pyrrole and alkane compounds whereas benzene and pyridine compounds are more predominant in microwave pyrolysis with a major presence of light compounds. The bio-gas fraction from microwave pyrolysis presents a much higher syngas content (H2+CO), and a lower CO2 and CH4 proportion than that obtained by conventional pyrolysis. Yields are similar for both treatments with a slightly higher gas yield in the case of microwave pyrolysis due to the fact that microwave heating favors heterogeneous reactions between the gases and the char. Copyright © 2013 Elsevier Ltd. All rights reserved.

A study on experimental characteristic of microwave-assisted pyrolysis of microalgae.

PubMed

Hu, Zhifeng; Ma, Xiaoqian; Chen, Chunxiang

2012-03-01

The microwave-assisted pyrolysis of Chlorella vulgaris was carried out under different microwave power levels, catalysts and contents of activated carbon and solid residue. The products, pyrolysis temperature and temperature rising rate were analyzed in order to obtain the optimal conditions. The results indicated that the higher the microwave power level was, the higher the maximum temperature rising rate and pyrolysis temperature were. The maximum bio-oil yield (35.83 wt.%) and gas yield (52.37%) were achieved under the microwave power of 1500 W and 2250 W, respectively. And 2250 W was the optimal power to obtain bio-fuel product. High microwave power level and catalyst can enhance the production of gas. Catalysts can promote the pyrolysis of C. vulgaris, and activated carbon was the best among the tested catalysts followed by the solid residue. The optimal content of activated carbon is 5% with the maximum bio-fuel yield of 87.47%. Copyright © 2011 Elsevier Ltd. All rights reserved.

The Synthesis and Characterization of Some Fluoride Perovskites: An Undergraduate Experiment in Solid State Chemistry.

ERIC Educational Resources Information Center

Langley, Richard H.; And Others

1984-01-01

Describes a senior-level experiment dealing with the synthesis and characterization of a perovskite. Since most perovskites are cubic, their characterization by x-ray diffraction is simplified. In addition, magnetic ordering may be observed and the effects of a Jahn-Teller distortion seen. (JN)

Design and synthesis of the superionic conductor Na10SnP2S12

NASA Astrophysics Data System (ADS)

Richards, William D.; Tsujimura, Tomoyuki; Miara, Lincoln J.; Wang, Yan; Kim, Jae Chul; Ong, Shyue Ping; Uechi, Ichiro; Suzuki, Naoki; Ceder, Gerbrand

2016-03-01

Sodium-ion batteries are emerging as candidates for large-scale energy storage due to their low cost and the wide variety of cathode materials available. As battery size and adoption in critical applications increases, safety concerns are resurfacing due to the inherent flammability of organic electrolytes currently in use in both lithium and sodium battery chemistries. Development of solid-state batteries with ionic electrolytes eliminates this concern, while also allowing novel device architectures and potentially improving cycle life. Here we report the computation-assisted discovery and synthesis of a high-performance solid-state electrolyte material: Na10SnP2S12, with room temperature ionic conductivity of 0.4 mS cm-1 rivalling the conductivity of the best sodium sulfide solid electrolytes to date. We also computationally investigate the variants of this compound where tin is substituted by germanium or silicon and find that the latter may achieve even higher conductivity.

Design and synthesis of the superionic conductor Na10SnP2S12.

PubMed

Richards, William D; Tsujimura, Tomoyuki; Miara, Lincoln J; Wang, Yan; Kim, Jae Chul; Ong, Shyue Ping; Uechi, Ichiro; Suzuki, Naoki; Ceder, Gerbrand

2016-03-17

Sodium-ion batteries are emerging as candidates for large-scale energy storage due to their low cost and the wide variety of cathode materials available. As battery size and adoption in critical applications increases, safety concerns are resurfacing due to the inherent flammability of organic electrolytes currently in use in both lithium and sodium battery chemistries. Development of solid-state batteries with ionic electrolytes eliminates this concern, while also allowing novel device architectures and potentially improving cycle life. Here we report the computation-assisted discovery and synthesis of a high-performance solid-state electrolyte material: Na10SnP2S12, with room temperature ionic conductivity of 0.4 mS cm(-1) rivalling the conductivity of the best sodium sulfide solid electrolytes to date. We also computationally investigate the variants of this compound where tin is substituted by germanium or silicon and find that the latter may achieve even higher conductivity.

Ultrasound/microwave-assisted solid-liquid-solid dispersive extraction with high-performance liquid chromatography coupled to tandem mass spectrometry for the determination of neonicotinoid insecticides in Dendrobium officinale.

PubMed

Zheng, Shuilian; Wu, Huizhen; Li, Zuguang; Wang, Jianmei; Zhang, Hu; Qian, Mingrong

2015-01-01

A one-step ultrasound/microwave-assisted solid-liquid-solid dispersive extraction procedure was used for the simultaneous determination of eight neonicotinoids (dinotefuran, nitenpyram, thiamethoxam, clothianidin, imidacloprid, acetamiprid, thiacloprid, imidaclothiz) in dried Dendrobium officinale by liquid chromatography combined with electrospray ionization triple quadrupole tandem mass spectrometry in multiple reaction monitoring mode. The samples were quickly extracted by acetonitrile and cleaned up by the mixed dispersing sorbents including primary secondary amine, C18 , and carbon-GCB. Parameters that could influence the ultrasound/microwave-assisted extraction efficiency such as microwave irradiation power, ultrasound irradiation power, temperature, and solvent were investigated. Recovery studies were performing well (70.4-113.7%) at three examined spiking levels (10, 50, and 100 μg/kg). Meanwhile, the limits of quantification for the neonicotinoids ranged from 0.87 to 1.92 μg/kg. The method showed good linearity in the concentration range of 1-100 μg/L with correlation coefficients >0.99. This quick and useful analytical method could provide a basis for monitoring neonicotinoid insecticide residues in herbs. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Sustainable synthesis of monodispersed spinel nano-ferrites

EPA Science Inventory

A sustainable approach for the synthesis of various monodispersed spinel ferrite nanoparticles has been developed that occurs at water-toluene interface under both conventional and microwave hydrothermal conditions. This general synthesis procedure utilizes readily available and ...

Solid State Division progress report for period ending September 30, 1993

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

Green, P.H.; Hinton, L.W.

1994-08-01

This report covers research progress in the Solid State Division from April 1, 1992, to September 30, 1993. During this period, the division conducted a broad, interdisciplinary materials research program with emphasis on theoretical solid state physics, neutron scattering, synthesis and characterization of materials, ion beam and laser processing, and the structure of solids and surfaces. This research effort was enhanced by new capabilities in atomic-scale materials characterization, new emphasis on the synthesis and processing of materials, and increased partnering with industry and universities. The theoretical effort included a broad range of analytical studies, as well as a new emphasismore » on numerical simulation stimulated by advances in high-performance computing and by strong interest in related division experimental programs. Superconductivity research continued to advance on a broad front from fundamental mechanisms of high-temperature superconductivity to the development of new materials and processing techniques. The Neutron Scattering Program was characterized by a strong scientific user program and growing diversity represented by new initiatives in complex fluids and residual stress. The national emphasis on materials synthesis and processing was mirrored in division research programs in thin-film processing, surface modification, and crystal growth. Research on advanced processing techniques such as laser ablation, ion implantation, and plasma processing was complemented by strong programs in the characterization of materials and surfaces including ultrahigh resolution scanning transmission electron microscopy, atomic-resolution chemical analysis, synchrotron x-ray research, and scanning tunneling microscopy.« less

The synthesis of Cu/Fe/Fe3O4 catalyst through the aqueous solution ball milling method assisted by high-frequency electromagnetic field

NASA Astrophysics Data System (ADS)

Yingzhe, Zhang; Yuxing, He; Qingdong, Qin; Fuchun, Wang; Wankun, Wang; Yongmei, Luo

2018-06-01

In this paper, nano-magnetic Cu/Fe/Fe3O4 catalyst was prepared by a new aqueous solution ball milling method assisted by high-frequency electromagnetic field at room temperature. The products were characterized by means of X-ray diffraction (XRD), high-resolution transmission electron microscope (HRTEM), selected area electron diffraction (SAED), and vibrating sample magnetometer (VSM). Microwave induced catalytic degradation of methylene blue (MB) was carried out in the presence of Cu/Fe/Fe3O4. The concentration of methylene blue was determined by UV-Vis spectrophotometry. The solid catalyst showed high catalytic activity of degrade MB and considerable saturation magnetization, lower remanence and coercivity. It indicate that the catalyst can be effectively separated for reuse by simply applying an external magnetic field and it can greatly promote their potential industrial application to eliminate organic pollutants from waste-water. Finally, we found that it is the non-thermal effect of microwave that activated the catalytic activity of Cu/Fe/Fe3O4 to degrade MB.

Platinum CCC-NHC benzimidazolyl pincer complexes: synthesis, characterization, photostability, and theoretical investigation of a blue-green emitter.

PubMed

Huckaba, Aron J; Cao, Bei; Hollis, T Keith; Valle, Henry U; Kelly, John T; Hammer, Nathan I; Oliver, Allen G; Webster, Charles Edwin

2013-06-28

The recently reported metallation/transmetallation route for the synthesis of CCC-bis(NHC) pincer ligand architectures was extended to 1,3-bis(3'-(trimethylsilylmethyl)-benzimidizol-1'-yl)benzene. The precursor was metallated with Zr(NMe2)4 and transmetallated to Pt using [Pt(COD)Cl2]. This Pt complex was found to resist photobleaching under UV irradiation in ambient conditions. Density functional theory (DFT) computations were used to generate the emission spectrum of the complex and reveal that this spectrum is the result of a transition from the triplet excited state (T1) to the ground state (S0). The Pt complex's molecular structure was determined by X-ray crystallography. The UV-vis absorption and emission spectra in solution and the solid-state emission spectra are reported. The solid-state photostability data and the radiative lifetime is also reported.

RTO Technical Publications: A Quarterly Listing

NASA Technical Reports Server (NTRS)

2004-01-01

This is a listing of recent unclassified RTO technical publications for April 1, 2004 through June 30, 2004, processed by the NASA Center for AeroSpace Information. Topics covered include: heat transfer and cooling in propulsion and power systems; assessment of operator functional state; microwaves; aerodynamics in solid rocket propulsion; command, control, communications and intelligence modeling; personal protective equipment against anti-personnel mine blast; and data fusion and visualization.

Satellite Power Systems (SPS) concept definition study, exhibit C. Volume 6: In-depth element investigation

NASA Technical Reports Server (NTRS)

Hanley, G.

1979-01-01

Computer assisted design of a gallium arsenide solid state dc-to-RF converter with supportive fabrication data was investigated. Specific tasks performed include: computer program checkout; amplifier comparisons; computer design analysis of GaSa solar cells; and GaAs diode evaluation. Results obtained in the design and evaluation of transistors for the microwave space power system are presented.

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.

Solid state synthesis of poly(dichlorophosphazene)

DOEpatents

Allen, Christopher W.; Hneihen, Azzam S.; Peterson, Eric S.

2001-01-01

A method for making poly(dichlorophosphazene) using solid state reactants is disclosed and described. The present invention improves upon previous methods by removing the need for chlorinated hydrocarbon solvents, eliminating complicated equipment and simplifying the overall process by providing a "single pot" two step reaction sequence. This may be accomplished by the condensation reaction of raw materials in the melt phase of the reactants and in the absence of an environmentally damaging solvent.

EXPEDITIOUS SYNTHETIC TRANSFORMATIONS USING MICROWAVES

EPA Science Inventory

Microwave-expedited solvent-free synthetic processes will be described for the synthesis of a variety of industrially significant compounds and intermediates namely, enamines, nitroalkenes, enones, oxidized sulfur compounds and ionic liquids. This solvent-free synthetic methodolo...

Green and microwave synthesis of SrAl2O4 nanoparticles by application of pomegranate juice: study and characterization

NASA Astrophysics Data System (ADS)

Riahi-Madvaar, Ramin; Taher, Mohammad Ali; Fazelirad, Hamid

2017-11-01

In the present paper, a green method was applied for the synthesis of SrAl2O4 nanostructures with the aid of microwave irradiation and pomegranate juice. SrAl2O4 nanocrystals were obtained when the raw materials were irradiated with 720-900 W for 6-10 min and then calcinated at 550 °C for 5 h. Using pomegranate juice as a dispersion and stabilizing agent, SrAl2O4 nanoparticles have been made with better properties in view of morphology and particle size. Also, the effect of some parameters affecting synthesis process such as microwave power and reaction time on the morphology and particle size of product was studied and optimized. X-ray diffraction and field emission-scanning electron microscopy were used to study and characterize the manufactured SrAl2O4 nanoparticles.

Solid-state reactions during mechanical alloying of ternary Fe-Al-X (X=Ni, Mn, Cu, Ti, Cr, B, Si) systems: A review

NASA Astrophysics Data System (ADS)

Hadef, Fatma

2016-12-01

The last decade has witnessed an intensive research in the field of nanocrystalline materials due to their enhanced properties. A lot of processing techniques were developed in order to synthesis these novel materials, among them mechanical alloying or high-energy ball milling. In fact, mechanical alloying is one of the most common operations in the processing of solids. It can be used to quickly and easily synthesize a variety of technologically useful materials which are very difficult to manufacture by other techniques. One advantage of MA over many other techniques is that is a solid state technique and consequently problems associated with melting and solidification are bypassed. Special attention is being paid to the synthesis of alloys through reactions mainly occurring in solid state in many metallic ternary Fe-Al-X systems, in order to improve mainly Fe-Al structural and mechanical properties. The results show that nanocrystallization is the common result occurring in all systems during MA process. The aim of this work is to illustrate the uniqueness of MA process to induce phase transformation in metallic Fe-Al-X (X=Ni, Mn, Cu, Ti, Cr, B, Si) systems.

Microwave-induced Bismuth Salts-mediated Synthesis of Molecules of Medicinal Interests.

PubMed

Bandyopadhyay, Debasish; Chavez, Ashlee; Banik, Bimal K

2017-01-01

Bismuth salts-mediated reactions have become a powerful tool for the synthesis of diverse medicinally-significant compounds because of their low-toxicity (non-toxic) and Lewis acidic capacity. In fact, LD50 of bismuth nitrate is lower than table salt. On the other hand, microwave-induced chemical synthesis is considered as a major greener route in modern chemistry. A total of 139 publications (including a few authentic web links) have been reviewed mainly to discuss bismuth salts-induced electrophilic aromatic substitution, protection-deprotection chemistry of carbonyl compounds, enamination, oxidation, carbohydrate chemistry, hydrolysis, addition-elimination route, Paal-Knorr reaction, Clauson-kaas synthesis, Michael addition, aza-Michael addition, Hantzsch reaction, Biginelli reaction, Ferrier rearrangement, Pechmann condensation, Diels-Alder and aza-Diels- Alder reactions, as well as effects of microwave irradiation in a wide range of chemical transformations. Bismuth salts-mediated reactions are developed for the synthesis of diverse organic molecules of medicinal significance. Reactions conducted with bismuth salts are environmentally benign, economical, rapid and high yielding. Microwave irradiation has accelerated these reactions significantly. It is believed that bismuth salts released corresponding acids in the media during the reaction. However, a coordination of bismuth salt to the electronegative atom is also observed in the NMR study. Bismuth has much less control (less attractive forces) over anions (for example, halides, nitrate, sulfate and triflates) compared to alkali metals. Therefore, it forms weak bond with electronegative atoms more readily and facilitates the reactions significantly. Many products obtained via bismuth salts-mediated reactions are medicinally active or intermediate for the synthesis of biologically active molecules including antifungal, anti-parasitic, anticancer and antibacterial agents, as well as agents to prevent Leishmaniosis and Chagas' diseases. Bismuth salts are able to (i) generate mineral acids in the reaction media and (ii) coordinate with electronegative atoms to facilitate the reaction. When the reagents and the catalyst (bismuth salt) are subjected to microwave irradiation, microwave passes through the (glass) walls of the reaction vessel and heat only the reactants avoiding local overheating at the wall of the vessel. Accordingly, the possibility of side reaction and subsequent by-product formation are reduced abruptly which in turn increases the yield of the desired product. The extreme rapidity with excellent yield of the product can be rationalized as a synergistic effect of the bismuth salts and microwave irradiation. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

A novel route for the synthesis of nanotubes and fullerene-like nanostructures of molybdenum disulfide

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

Panigrahi, Pravas Kumar, E-mail: pravas.iit@gmail.com; Pathak, Amita, E-mail: ami@chem.iitkgp.ernet.in

Graphical abstract: Nanotubes and fullerene-like nanostructures of MoS{sub 2} were synthesized via a microwave-assisted route in solution phase. Highlights: Black-Right-Pointing-Pointer Microwave-assisted route for synthesis of nanotube and fullerene-like nanostructures of MoS{sub 2}. Black-Right-Pointing-Pointer Morphological analysis of the synthesized products. Black-Right-Pointing-Pointer Solvent plays important role in the modification of morphology of MoS{sub 2}. -- Abstract: The paper described the synthesis of nanotubes and fullerene-like nanostructures of MoS{sub 2} through a technically simple, rapid, and energy-efficient microwave-assisted synthesis technique, which involved the use of elemental sulfur dissolved in a mixture of monoethanolamine and hydrazine hydrate as the sulfide source. The microwave inducedmore » reaction between the molybdate with sulfide ions, in the presence of hydrazine hydrate in the reaction medium, resulted in the formation of gray colored powders of amorphous MoS{sub 2}. The as-obtained powders were calcined at 600 Degree-Sign C for 2 h and characterized by different techniques. HRTEM analysis of the calcined samples indicated the formation of fullerene-like MoS{sub 2} structures when the starting solution mixture was irradiated with microwave for a period of 200 s, while on 600 s of irradiation of the same revealed the formation of folded sheets like MoS{sub 2} nanotubes. BET surface areas of the calcined samples have been measured and a plausible reaction mechanism for the formation of nanotubes and fullerene-like nanostructures of MoS{sub 2} has been proposed.« less

Electronic conductivity studies on oxyhalide glasses containing TMO

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

Vijayatha, D.; Department of Physics, Gurunanak Institute of Technology, Hyderabad -040; Viswanatha, R.

2016-05-06

Microwave-assisted synthesis is cleaner, more economical and much faster than conventional methods. The development of new routes for the synthesis of solid materials is an integral part of material science and technology. The electronic conductivity studies on xPbCl{sub 2} – 60 PbO – (40-x) V{sub 2}O{sub 5} (1 ≥ x ≤ 10) glass system has been carried out over a wide range of composition and temperature (300 K to 423 K). X-ray diffraction study confirms the amorphous nature of the samples. The Scanning electron microscopic studies reveal the formation of cluster like morphology in PbCl{sub 2} containing glasses. The d.c conductivity exhibitsmore » Arrhenius behaviour and increases with V{sub 2}O{sub 5} concentration. Analysis of the results is interpreted in view Austin-Mott’s small polaron model of electron transport. Activation energies calculated using regression analysis exhibit composition dependent trend and the variation is explained in view of the structure of lead-vanadate glass.« less

Synthesis, structure, and catalytic performance in cyclooctene epoxidation of a molybdenum oxide/bipyridine hybrid material: {[MoO3(bipy)][MoO3(H2O)]}n.

PubMed

Abrantes, Marta; Amarante, Tatiana R; Antunes, Margarida M; Gago, Sandra; Paz, Filipe A Almeida; Margiolaki, Irene; Rodrigues, Alírio E; Pillinger, Martyn; Valente, Anabela A; Gonçalves, Isabel S

2010-08-02

The reaction of [MoO(2)Cl(2)(bipy)] (1) (bipy = 2,2'-bipyridine) with water in a Teflon-lined stainless steel autoclave (100 degrees C, 19 h), in an open reflux system with oil bath heating (12 h) or in a microwave synthesis system (120 degrees C, 4 h), gave the molybdenum oxide/bipyridine hybrid material {[MoO(3)(bipy)][MoO(3)(H(2)O)]}(n) (2) as a microcrystalline powder in yields of 72-92%. The crystal structure of 2 determined from synchrotron X-ray powder diffraction data is composed of two distinct neutral one-dimensional polymers: an organic-inorganic polymer, [MoO(3)(bipy)](n), and a purely inorganic chain, [MoO(3)(H(2)O)](n), which are interconnected by O-H...O hydrogen bonding interactions. Compound 2 is a moderately active, stable, and selective catalyst for the epoxidation of cis-cyclooctene at 55 degrees C with tert-butylhydroperoxide (tBuOOH, 5.5 M in decane or 70% aqueous) as the oxidant. Biphasic solid-liquid or triphasic solid-organic-aqueous mixtures are formed, and 1,2-epoxycyclooctane is the only reaction product. When n-hexane is employed as a cosolvent and tBuOOH(decane) is the oxidant, the catalytic reaction is heterogeneous in nature, and the solid catalyst can be recycled and reused without a loss of activity. For comparison, the catalytic performance of the precursor 1 was also investigated. The IR spectra of solids recovered after catalysis indicate that 1 transforms into the organic-inorganic polymer [MoO(3)(bipy)] when the oxidant is tBuOOH(decane) and compound 2 when the oxidant is 70% aqueous tBuOOH.

Possible Demonstration of a Polaronic Bose-Einstein(-Mott) Condensate in UO 2(+x) by Ultrafast THz Spectroscopy and Microwave Dissipation

DOE PAGES

Conradson, Steven D.; Gilbertson, Steven M.; Daifuku, Stephanie L.; ...

2015-10-16

Bose-Einstein condensates (BECs) composed of polarons would be an advance because they would combine coherently charge, spin, and a crystal lattice. Following our earlier report of unique structural and spectroscopic properties, we now identify potentially definitive evidence for polaronic BECs in photo- and chemically doped UO 2(+x) on the basis of exceptional coherence in the ultrafast time dependent terahertz absorption and microwave spectroscopy results that show collective behavior including dissipation patterns whose precedents are condensate vortex and defect disorder and condensate excitations. Furthermore, that some of these signatures of coherence in an atom-based system extend to ambient temperature suggests amore » novel mechanism that could be a synchronized, dynamical, disproportionation excitation, possibly via the solid state analog of a Feshbach resonance that promotes the coherence. Such a mechanism would demonstrate that the use of ultra-low temperatures to establish the BEC energy distribution is a convenience rather than a necessity, with the actual requirement for the particles being in the same state that is not necessarily the ground state attainable by other means. Interestingly, a macroscopic quantum object created by chemical doping that can persist to ambient temperature and resides in a bulk solid would be revolutionary in a number of scientific and technological fields.« less

Possible Demonstration of a Polaronic Bose-Einstein(-Mott) Condensate in UO 2(+x) by Ultrafast THz Spectroscopy and Microwave Dissipation

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

Conradson, Steven D.; Gilbertson, Steven M.; Daifuku, Stephanie L.

Bose-Einstein condensates (BECs) composed of polarons would be an advance because they would combine coherently charge, spin, and a crystal lattice. Following our earlier report of unique structural and spectroscopic properties, we now identify potentially definitive evidence for polaronic BECs in photo- and chemically doped UO 2(+x) on the basis of exceptional coherence in the ultrafast time dependent terahertz absorption and microwave spectroscopy results that show collective behavior including dissipation patterns whose precedents are condensate vortex and defect disorder and condensate excitations. Furthermore, that some of these signatures of coherence in an atom-based system extend to ambient temperature suggests amore » novel mechanism that could be a synchronized, dynamical, disproportionation excitation, possibly via the solid state analog of a Feshbach resonance that promotes the coherence. Such a mechanism would demonstrate that the use of ultra-low temperatures to establish the BEC energy distribution is a convenience rather than a necessity, with the actual requirement for the particles being in the same state that is not necessarily the ground state attainable by other means. Interestingly, a macroscopic quantum object created by chemical doping that can persist to ambient temperature and resides in a bulk solid would be revolutionary in a number of scientific and technological fields.« less

Quantitative analysis of time-resolved microwave conductivity data

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

Reid, Obadiah G.; Moore, David T.; Li, Zhen

Flash-photolysis time-resolved microwave conductivity (fp-TRMC) is a versatile, highly sensitive technique for studying the complex photoconductivity of solution, solid, and gas-phase samples. The purpose of this paper is to provide a standard reference work for experimentalists interested in using microwave conductivity methods to study functional electronic materials, describing how to conduct and calibrate these experiments in order to obtain quantitative results. The main focus of the paper is on calculating the calibration factor, K, which is used to connect the measured change in microwave power absorption to the conductance of the sample. We describe the standard analytical formulae that havemore » been used in the past, and compare them to numerical simulations. This comparison shows that the most widely used analytical analysis of fp-TRMC data systematically under-estimates the transient conductivity by ~60%. We suggest a more accurate semi-empirical way of calibrating these experiments. However, we emphasize that the full numerical calculation is necessary to quantify both transient and steady-state conductance for arbitrary sample properties and geometry.« less

Quantitative analysis of time-resolved microwave conductivity data

DOE PAGES

Reid, Obadiah G.; Moore, David T.; Li, Zhen; ...

2017-11-10

Flash-photolysis time-resolved microwave conductivity (fp-TRMC) is a versatile, highly sensitive technique for studying the complex photoconductivity of solution, solid, and gas-phase samples. The purpose of this paper is to provide a standard reference work for experimentalists interested in using microwave conductivity methods to study functional electronic materials, describing how to conduct and calibrate these experiments in order to obtain quantitative results. The main focus of the paper is on calculating the calibration factor, K, which is used to connect the measured change in microwave power absorption to the conductance of the sample. We describe the standard analytical formulae that havemore » been used in the past, and compare them to numerical simulations. This comparison shows that the most widely used analytical analysis of fp-TRMC data systematically under-estimates the transient conductivity by ~60%. We suggest a more accurate semi-empirical way of calibrating these experiments. However, we emphasize that the full numerical calculation is necessary to quantify both transient and steady-state conductance for arbitrary sample properties and geometry.« less

Significant reduction of saturation magnetization and microwave-reflection loss in barium-natural ferrite via Nd3+ substitution

NASA Astrophysics Data System (ADS)

Widanarto, W.; Ardenti, E.; Ghoshal, S. K.; Kurniawan, C.; Effendi, M.; Cahyanto, W. T.

2018-06-01

To minimize the signal degradation, many electronic devices require efficient microwave absorbers with very low reflection-losses within the X-band. We prepared a series of trivalent neodymium-ion (Nd3+) substituted barium-natural ferrite using a modified solid-state reaction method. The effect of the Nd3+-ion content on the structure, surface morphology, magnetic properties, and microwave reflection loss was studied. The composites were characterized using X-ray diffraction, a vibrating sample magnetometer, scanning electron microscopy, and a vector network analyzer. The XRD patterns of the sample without Nd3+ reveal the presence of BaFe12O19 (hexagonal) and BaFe2O4 (rhombohedral) phases. Furthermore, a new hexagonal crystal phase of Ba6Nd2Fe4O15 appeared after substituting Nd3+. The average size of the prepared barium-natural ferrite particles was estimated to be between 0.4 and 0.8 μm. Both saturation magnetization and microwave reflection losses of these barium-ferrites were significantly reduced by increasing the Nd3+ content.

Obtaining and characterization of La0.8Sr0.2CrO3 perovskite by the combustion method

NASA Astrophysics Data System (ADS)

Morales Rivera, A. M.; Gómez Cuaspud, J. A.; López, E. Vera

2017-01-01

This research is focused on the synthesis and characterization of a perovskite oxide based on La0.8Sr0.2CrO3 system by the combustion method. The material was obtained in order to contribute to analyse the effect of synthesis route in the obtaining of advanced anodic materials for solid oxide fuel cells (SOFC). The obtaining of solid was achieved starting from corresponding nitrate dissolutions, which were polymerized by temperature effect in presence of citric acid. The solid precursor as a foam citrate was characterized by infrared (FTIR) and ultraviolet (UV) spectroscopy, confirming the effectiveness in synthesis process. The solid was calcined in oxygen atmosphere at 800°C and characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive of X-ray spectroscopy (EDX) and solid state impedance spectroscopy (IS). Results confirm the obtaining of an orthorhombic solid with space group Pnma (62) and cell parameters a=5.4590Å, b=7.7310Å and c=5.5050Å. At morphological level the solid showed a heterogeneous distribution with an optimal correspondence with proposed and obtained stoichiometry. The electrical characterization, confirm a semiconductor behaviour with a value of 2.14eV Band-gap according with previous works.

Microwave assisted solid phase extraction for separation preconcentration sulfamethoxazole in wastewater using tyre based activated carbon as solid phase material prior to spectrophotometric determination.

PubMed

Mogolodi Dimpe, K; Mpupa, Anele; Nomngongo, Philiswa N

2018-01-05

This work was chiefly encouraged by the continuous consumption of antibiotics which eventually pose harmful effects on animals and human beings when present in water systems. In this study, the activated carbon (AC) was used as a solid phase material for the removal of sulfamethoxazole (SMX) in wastewater samples. The microwave assisted solid phase extraction (MASPE) as a sample extraction method was employed to better extract SMX in water samples and finally the analysis of SMX was done by the UV-Vis spectrophotometer. The microwave assisted solid phase extraction method was optimized using a two-level fractional factorial design by evaluating parameters such as pH, mass of adsorbent (MA), extraction time (ET), eluent ratio (ER) and microwave power (MP). Under optimized conditions, the limit of detection (LOD) and limit of quantification (LOQ) were 0.5μgL -1 and 1.7μgL -1 , respectively, and intraday and interday precision expressed in terms of relative standard deviation were >6%.The maximum adsorption capacity was 138mgg -1 for SMX and the adsorbent could be reused eight times. Lastly, the MASPE method was applied for the removal of SMX in wastewater samples collected from a domestic wastewater treatment plant (WWTP) and river water. Copyright © 2017 Elsevier B.V. All rights reserved.

Plasma-assisted microwave processing of materials

NASA Technical Reports Server (NTRS)

Barmatz, Martin (Inventor); Jackson, Henry (Inventor); Ylin, Tzu-yuan (Inventor)

1998-01-01

A microwave plasma assisted method and system for heating and joining materials. The invention uses a microwave induced plasma to controllably preheat workpiece materials that are poorly microwave absorbing. The plasma preheats the workpiece to a temperature that improves the materials' ability to absorb microwave energy. The plasma is extinguished and microwave energy is able to volumetrically heat the workpiece. Localized heating of good microwave absorbing materials is done by shielding certain parts of the workpiece and igniting the plasma in the areas not shielded. Microwave induced plasma is also used to induce self-propagating high temperature synthesis (SHS) process for the joining of materials. Preferably, a microwave induced plasma preheats the material and then microwave energy ignites the center of the material, thereby causing a high temperature spherical wave front from the center outward.

Liquid-phase and solid-phase microwave irradiations for reduction of graphite oxide

NASA Astrophysics Data System (ADS)

Zhao, Na; Wen, Chen-Yu; Zhang, David Wei; Wu, Dong-Ping; Zhang, Zhi-Bin; Zhang, Shi-Li

2014-12-01

In this paper, two microwave irradiation methods: (i) liquid-phase microwave irradiation (MWI) reduction of graphite oxide suspension dissolved in de-ionized water and N, N-dimethylformamide, respectively, and (ii) solid-phase MWI reduction of graphite oxide powder have been successfully carried out to reduce graphite oxide. The reduced graphene oxide products are thoroughly characterized by scanning electron microscopy, atomic force microscopy, X-ray photoelectron spectroscopy, Fourier transform infrared spectral analysis, Raman spectroscopy, UV-Vis absorption spectral analysis, and four-point probe conductivity measurements. The results show that both methods can efficiently remove the oxygen-containing functional groups attached to the graphite layers, though the solid-phase MWI reduction method can obtain far more efficiently a higher quality-reduced graphene oxide with fewer defects. The I(D)/I(G) ratio of the solid-phase MWI sample is as low as 0.46, which is only half of that of the liquid-phase MWI samples. The electrical conductivity of the reduced graphene oxide by the solid method reaches 747.9 S/m, which is about 25 times higher than that made by the liquid-phase method.

The Application of Microwave Incineration to Regenerative Life Support

NASA Technical Reports Server (NTRS)

Sun, Sidney C.; Srinivasan, Venkatesh; Covington, Al (Technical Monitor)

1995-01-01

Future human exploration missions will require life support systems that are highly regenerative, requiring minimum resupply, enabling the crews to be largely self-sufficient. Solid wastes generated in space will be processed to recover usable material. Researchers at NASA Ames Research Center are studying a commercially-produced microwave incinerator as a solid waste processor. This paper will describe the results of testing to-date.

TM triple-mode microwave filter

NASA Astrophysics Data System (ADS)

Lai, S.-L.; Lin, W.-G.

1990-12-01

A novel realization of triple-mode six-pole microwave filters that use only TM modes is presented. The application involves TM triple degeneracies in cylindrical cavities using triple-mode elliptic function filter synthesis. Experimental results are reported.

EFFICIENT CHEMICAL SYNTHESIS USING MICROWAVES

EPA Science Inventory

Synthetic organic transformations performed under non-traditional conditions are becoming popular primarily to circumvent the growing environmental concerns. A solvent-free approach that involves microwave (MW) exposure of neat reactants catalyzed by the surfaces of less-expensiv...

New microwave spectrometer/imager has possible applications for pollution monitoring

NASA Technical Reports Server (NTRS)

Tooley, R. D.

1970-01-01

Microwave imager forms thermal-emissivity image of solid portion of planet Venus and provides data on the planet's atmosphere, surface, terminator, and temperature changes. These thermally produced multifrequency microwaves for image production of temperature profiles can be applied to water pollution monitoring, agriculture, and forestry survey.

Multicapillary Flow Reactor: Synthesis of 1,2,5-Thiadiazepane 1,1-Dioxide Library Utilizing One-Pot Elimination and Inter-/Intramolecular Double aza-Michael Addition Via Microwave-Assisted, Continuous-Flow Organic Synthesis (MACOS)

PubMed Central

Ullah, Farman; Zang, Qin; Javed, Salim; Zhou, Aihua; Knudtson, Christopher A.; Bi, Danse; Hanson, Paul R.; Organ, Michael G.

2013-01-01

A microwave-assisted, continuous-flow organic synthesis (MACOS) protocol for the synthesis of functionalized 1,2,5-thiadiazepane 1,1-dioxide library, utilizing a one-pot elimination and inter-/intramolecular double aza-Michael addition strategy is reported. The optimized protocol in MACOS was utilized for scale-out and further extended for library production using a multicapillary flow reactor. A 50-member library of 1,2,5-thiadiazepane 1,1-dioxides was prepared on a 100- to 300-mg scale with overall yields between 50 and 80% and over 90 % purity determined by proton nuclear magnetic resonance (1H-NMR) spectroscopy. PMID:24244871

Synthesis of oxide and spinel nanocrystals for use in solid state lighting

NASA Astrophysics Data System (ADS)

Foley, Megan Elizabeth

In this dissertation, microwave chemistry is employed to synthesize a variety of different crystalline nanoparticles (NPs). This introduction will describe the structures, properties and applications of the NPs studied within the dissertation, with a main focus being on ligand sensitization for the goal of enhanced luminescence. The use of metal acetylacetonate complexes to make Europium (III) doped Ytrrium (Y2O3) NPs is explored, where the acetylacetonate acts both as a source of oxygen for the synthesis of Y2O3, as well as an organic chromophore acting as an "antenna" for the absorption of light and subsequent excitation transfer to the incorporated Europium (III) (Chapter 2). Other host materials are investigated by method of metal acetylacetonate decomposition to synthesize a variety of different nanospinels, having the general formula AB2X4, with sulfide variants made by decomposition of diethyldithiocarbamate, (Chapter 3). The antenna ligand thenoyltrifluoroacetone (tta), which is known to undergo a Dexter energy transfer (DET) mechanism to efficiently sensitize Europium (III) emission, is used to determine the distance of energy transfer in Europium (III) doped nanospinels by passivating the surface of the nanospinel with a tta (Chapter 4). A variety of ligands are explored in order to optimize the sensitization efficiency in relation to the difference in energy between the singlet and triplet levels of the ligands versus the 5D0 and 5D4 energy levels of Europium (III) and Terbium (III) respectively (Chapter 5).

Accessing Stereochemically Rich Sultams via Microwave-Assisted, Continuous Flow Organic Synthesis (MACOS) Scale-out

PubMed Central

Organ, Michael G.; Hanson, Paul R.; Rolfe, Alan; Samarakoon, Thiwanka B.; Ullah, Farman

2011-01-01

The generation of stereochemically-rich benzothiaoxazepine-1,1′-dioxides for enrichment of high-throughput screening collections is reported. Utilizing a microwave-assisted, continuous flow organic synthesis platform (MACOS), scale-out of core benzothiaoxazepine-1,1′-dioxide scaffolds has been achieved on multi-gram scale using an epoxide opening/SNAr cyclization protocol. Diversification of these sultam scaffolds was attained via a microwave-assisted intermolecular SNAr reaction with a variety of amines. Overall, a facile, 2-step protocol generated a collection of benzothiaoxazepine-1,1′-dioxides possessing stereochemical complexity in rapid fashion, where all 8 stereoisomers were accessed from commercially available starting materials. PMID:22116791

Fe-containing nanoparticles used as effective catalysts of lignin reforming to syngas and hydrogen assisted by microwave irradiation

NASA Astrophysics Data System (ADS)

Tsodikov, M. V.; Ellert, O. G.; Nikolaev, S. A.; Arapova, O. V.; Bukhtenko, O. V.; Maksimov, Yu. V.; Kirdyankin, D. I.; Vasil'kov, A. Yu.

2018-03-01

Active iron-containing nanosized components have been formed on the lignin surface. The metal was deposited on the lignin from an ethanol solution of Fe(acac)3 and from a colloid solution of iron metal particles obtained beforehand by metal vapor synthesis. These active components are able to absorb microwave radiation and are suitable for microwave-assisted high-rate dehydrogenation and dry reforming of lignin without addition of a carbon adsorbent, as a supplementary radiation absorbing material, to the feedstock. The dependence of the solid lignin heating dynamics on the concentration of supported iron particles was investigated. The threshold Fe concentration equal to 0.5 wt.%, providing the highest rate of sample heating up to the reforming and plasma generation temperature was identified. The microstructure and magnetic properties of iron-containing nanoparticles supported on lignin were studied before and after the reforming. The Fe3O4 nanoparticles and also core-shell Fe3O4@γ-Fe-C nanostructures are formed during the reforming of lignin samples. The catalytic performance of iron-based nanoparticles toward the lignin conversion is manifested as increasing selectivity to hydrogen and syngas, which reaches 94% at the Fe concentration of 2 wt.%. It was found that with microwave irradiation under argon, hydrogen predominates in the gas. In the CO2 atmosphere, dry reforming takes place to give syngas with the CO/H2 ratio of 0.9. In both cases, the degree of hydrogen recovery from lignin reaches 90-94%. [Figure not available: see fulltext.

Ultra-Fast Microwave Synthesis of ZnO Nanorods on Cellulose Substrates for UV Sensor Applications

PubMed Central

Pimentel, Ana; Samouco, Ana; Araújo, Andreia; Martins, Rodrigo; Fortunato, Elvira

2017-01-01

In the present work, tracing and Whatman papers were used as substrates to grow zinc oxide (ZnO) nanostructures. Cellulose-based substrates are cost-efficient, highly sensitive and environmentally friendly. ZnO nanostructures with hexagonal structure were synthesized by hydrothermal under microwave irradiation using an ultrafast approach, that is, a fixed synthesis time of 10 min. The effect of synthesis temperature on ZnO nanostructures was investigated from 70 to 130 °C. An Ultra Violet (UV)/Ozone treatment directly to the ZnO seed layer prior to microwave assisted synthesis revealed expressive differences regarding formation of the ZnO nanostructures. Structural characterization of the microwave synthesized materials was carried out by scanning electron microscopy (SEM) and X-ray diffraction (XRD). The optical characterization has also been performed. The time resolved photocurrent of the devices in response to the UV turn on/off was investigated and it has been observed that the ZnO nanorod arrays grown on Whatman paper substrate present a responsivity 3 times superior than the ones grown on tracing paper. By using ZnO nanorods, the surface area-to-volume ratio will increase and will improve the sensor sensibility, making these types of materials good candidates for low cost and disposable UV sensors. The sensors were exposed to bending tests, proving their high stability, flexibility and adaptability to different surfaces. PMID:29140304

Sustainable Synthesis of Nanomaterials Using Microwave irradiation

EPA Science Inventory

The presentation summarizes our recent activity in MW-assisted synthesis of nanomaterials under benign conditions. Shape-controlled aqueous synthesis of noble nanostructures via MW-assisted spontaneous reduction of noble metal salts using -D-glucose, sucrose, and maltose will be...

Solid-state synthesis of ordered mesoporous carbon catalysts via a mechanochemical assembly through coordination cross-linking

PubMed Central

Zhang, Pengfei; Wang, Li; Yang, Shize; Schott, Jennifer A.; Liu, Xiaofei; Mahurin, Shannon M.; Huang, Caili; Zhang, Yu; Fulvio, Pasquale F.; Chisholm, Matthew F.; Dai, Sheng

2017-01-01

Ordered mesoporous carbons (OMCs) have demonstrated great potential in catalysis, and as supercapacitors and adsorbents. Since the introduction of the organic–organic self-assembly approach in 2004/2005 until now, the direct synthesis of OMCs is still limited to the wet processing of phenol-formaldehyde polycondensation, which involves soluble toxic precursors, and acid or alkali catalysts, and requires multiple synthesis steps, thus restricting the widespread application of OMCs. Herein, we report a simple, general, scalable and sustainable solid-state synthesis of OMCs and nickel OMCs with uniform and tunable mesopores (∼4–10 nm), large pore volumes (up to 0.96 cm3 g−1) and high-surface areas exceeding 1,000 m2 g−1, based on a mechanochemical assembly between polyphenol-metal complexes and triblock co-polymers. Nickel nanoparticles (∼5.40 nm) confined in the cylindrical nanochannels show great thermal stability at 600 °C. Moreover, the nickel OMCs offer exceptional activity in the hydrogenation of bulky molecules (∼2 nm). PMID:28452357

Crystallisation and crystal forms of carbohydrate derivatives

NASA Astrophysics Data System (ADS)

Lennon, Lorna

This thesis is focused on the synthesis and solid state analysis of carbohydrate derivatives, including many novel compounds. Although the synthetic chemistry surrounding carbohydrates is well established in the literature, the crystal chemistry of carbohydrates is less well studied. Therefore this research aims to improve understanding of the solid state properties of carbohydrate derivatives through gaining more information on their supramolecular bonding. Chapter One focuses on an introduction to the solid state of organic compounds, with a background to crystallisation, including issues that can arise during crystal growth. Chapter Two is based on glucopyranuronate derivatives which are understudied in terms of their solid state forms. This chapter reports on the formation of novel glucuronamides and utilising the functionality of the amide bond for crystallisation. TEMPO oxidation was completed to form glucopyranuronates by oxidation of the primary alcohol groups of glucosides to the carboxylic acid derivatives, to increase functionality for enhanced crystal growth. Chapter Three reports on the synthesis of glucopyranoside derivatives by O-glycosylation reactions and displays crystal structures, including a number of previously unsolved acetate protected and deprotected crystal structures. More complex glycoside derivatives were also researched in an aim to study the resultant supramolecular motifs. Chapter Four contains the synthesis of aryl cellobioside derivatives including the novel crystal structures that were solved for the acetate protected and deprotected compounds. Research was carried out to determine if 1-deoxycellodextrins could act as putative isostructures for cellulose. Our research displays the presence of isostructural references with 1-deoxycellotriose shown to be similar to cellulose III11, 1-deoxycellotetraose correlates with cellulose IV11 and 1-deoxycellopentose shows isostructurality similar to that of cellulose II. Chapter Five contains the full experimental details and spectral characterisation of all novel compounds synthesised in this project and relevant crystallographic information.

TiO2 synthesized by microwave assisted solvothermal method: Experimental and theoretical evaluation

NASA Astrophysics Data System (ADS)

Moura, K. F.; Maul, J.; Albuquerque, A. R.; Casali, G. P.; Longo, E.; Keyson, D.; Souza, A. G.; Sambrano, J. R.; Santos, I. M. G.

2014-02-01

In this study, a microwave assisted solvothermal method was used to synthesize TiO2 with anatase structure. The synthesis was done using Ti (IV) isopropoxide and ethanol without templates or alkalinizing agents. Changes in structural features were observed with increasing time of synthesis and evaluated using periodic quantum chemical calculations. The anatase phase was obtained after only 1 min of reaction besides a small amount of brookite phase. Experimental Raman spectra are in accordance with the theoretical one. Micrometric spheres constituted by nanometric particles were obtained for synthesis from 1 to 30 min, while spheres and sticks were observed after 60 min.

Heteropoly acid-catalyzed microwave-assisted three-component aza-Diels-Alder cyclizations: diastereoselective synthesis of potential drug candidates for Alzheimer's disease.

PubMed

Borkin, Dmitry; Morzhina, Elena; Datta, Silpi; Rudnitskaya, Aleksandra; Sood, Abha; Török, Marianna; Török, Béla

2011-03-07

A highly diastereoselective microwave-assisted three component synthesis of azabicyclo[2.2.2]octan-5-ones by a silicotungstic acid-catalyzed aza-Diels-Alder cyclization is described. The one-pot process involves the formation of the in situ generated Schiff base and its immediate cyclization with cyclohex-2-enone. The short reaction times, good yields and excellent diastereoselectivity make this annulation a practical and environmentally attractive method for the synthesis of the target compounds. Preliminary assays were carried out to determine the activity of the products in AChE as well as in amyloid β fibrillogenesis inhibition.

Microwave techniques for measuring complex permittivity and permeability of materials

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

Guillon, P.

1995-08-01

Different materials are of fundamental importance to the aerospace, microwave, electronics and communications industries, and include for example microwave absorbing materials, antennas lenses and radomes, substrates for MMIC and microwave components and antennaes. Basic measurements for the complex permittivity and permeability of those homogeneous solid materials in the microwave spectral region are described including hardware, instrumentation and analysis. Elevated temperature measurements as well as measurements intercomparisons, with a discussion of the strengths and weaknesses of each techniques are also presented.

Trace detection of tetrahydrocannabinol (THC) with a SERS-based capillary platform prepared by the in situ microwave synthesis of AgNPs.

PubMed

Yüksel, Sezin; Schwenke, Almut M; Soliveri, Guido; Ardizzone, Silvia; Weber, Karina; Cialla-May, Dana; Hoeppener, Stephanie; Schubert, Ulrich S; Popp, Jürgen

2016-10-05

In the present study, an ultra-sensitive and highly reproducible novel SERS-based capillary platform was developed and utilized for the trace detection of tetrahydrocannabinol (THC). The approach combines the advantages of microwave-assisted nanoparticle synthesis, plasmonics and capillary forces. By employing a microwave-assisted preparation method, glass capillaries were reproducibly coated with silver nanoparticles in a batch fabrication process that required a processing time of 3 min without needing to use any pre-surface modifications or add surfactants. The coated capillaries exhibited an excellent SERS activity with a high reproducibility and enabled the detection of low concentrations of target molecules. At the same time, only a small amount of analyte and a short and simple incubation process was required. The developed platform was applied to the spectroscopic characterization of tetrahydrocannabinol (THC) and its identification at concentration levels down to 1 nM. Thus, a highly efficient detection system for practical applications, e.g., in drug monitoring/detection, is introduced, which can be fabricated at low cost by using microwave-assisted batch synthesis techniques. Copyright © 2016 Elsevier B.V. All rights reserved.

Cost-effective single-step carbon nanotube synthesis using microwave oven

NASA Astrophysics Data System (ADS)

Algadri, Natheer A.; Ibrahim, K.; Hassan, Z.; Bououdina, M.

2017-08-01

This paper reports the characterization of carbon nanotubes (CNTs) synthesised using a conventional microwave oven method, offering several advantages including fast, simple, low cost, and solvent free growth process. The procedure involves flattening of graphite/ferrocene mixture catalyst inside the microwave oven under ambient conditions for a very short duration of 5 s, which inhibits the loss factor of graphite and ferrocene. The effect of graphite/ferrocene mixture ratio for the synthesis of CNTs is investigated by transmission electron microscopy (TEM), field emission scanning electron microscopy (FESEM), x-ray diffraction (XRD), Raman spectroscopy and UV-NIR-Vis measurements. The samples produced using the different ratios contain nanotubes with an average diameter in the range 44-79 nm. The highest yield of CNTs is attained with graphite/ferrocene mixture ratio of 70:30. The lowest I D/I G ratio intensity as identified by Raman spectroscopy for 70:30 ratio indicates the improved crystallinity of CNTs. Due to the capillary effect of CNTs, Fe nanoparticles are found to be encapsulated inside the tubes at different positions along the tube length. The obtained results showed that the smaller the diameter of graphite and ferrocene favors the synthesis of graphene oxide upon microwave radiation.

Microwave synthesis of noncentrosymmetric BaTiO3 truncated nanocubes for charge storage applications.

PubMed

Swaminathan, V; Pramana, Stevin S; White, T J; Chen, L; Chukka, Rami; Ramanujan, R V

2010-11-01

Truncated nanocubes of barium titanate (BT) were synthesized using a rapid, facile microwave-assisted hydrothermal route. Stoichiometric composition of pellets of nanocube BT powders was prepared by two-stage microwave process. Characterization by powder XRD, Rietveld refinement, SEM, TEM, and dielectric and polarization measurements was performed. X-ray diffraction revealed a polymorphic transformation from cubic Pm3̅m to tetragonal P4mm after 15 min of microwave irradiation, arising from titanium displacement along the c-axis. Secondary electron images were examined for nanocube BT synthesis and annealed at different timings. Transmission electron microscopy showed a narrow particle size distribution with an average size of 70 ± 9 nm. The remanence and saturation polarization were 15.5 ± 1.6 and 19.3 ± 1.2 μC/cm(2), respectively. A charge storage density of 925 ± 47 nF/cm(2) was obtained; Pt/BT/Pt multilayer ceramic capacitor stack had an average leakage current density of 5.78 ± 0.46 × 10(-8) A/cm(2) at ±2 V. The significance of this study shows an inexpensive and facile processing platform for synthesis of high-k dielectric for charge storage applications.

Putting Cocrystal Stoichiometry to Work: A Reactive Hydrogen-Bonded "Superassembly" Enables Nanoscale Enlargement of a Metal-Organic Rhomboid via a Solid-State Photocycloaddition.

PubMed

Chu, Qianli; Duncan, Andrew J E; Papaefstathiou, Giannis S; Hamilton, Tamara D; Atkinson, Manza B J; Mariappan, S V Santhana; MacGillivray, Leonard R

2018-04-11

Enlargement of a self-assembled metal-organic rhomboid is achieved via the organic solid state. The solid-state synthesis of an elongated organic ligand was achieved by a template directed [2 + 2] photodimerization in a cocrystal. Initial cocrystals obtained of resorcinol template and reactant alkene afforded a 1:2 cocrystal with the alkene in a stacked yet photostable geometry. Cocrystallization performed in the presence of excess template resulted in a 3:2 cocrystal composed of novel discrete 10-component hydrogen-bonded "superassemblies" wherein the alkenes undergo a head-to-head [2 + 2] photodimerization. Isolation and reaction of elongated photoproduct with Cu(II) ions afforded a metal-organic rhomboid of nanoscale dimensions that hosts small molecules in the solid state as guests.

Solid State Research.

DTIC Science & Technology

1996-08-01

Failure of Superconducting Microwave Filters: Investigation by Means of Thermal Imaging G. Hampel* P . Kolodner* P . L. Gammel* P . A. Polakos* E...deObaldia* P . M. Mankiewich* A. Anderson R. Slattery D. Zhang* G. C. Liang* C. F. Shih* Appl. Phys. Lett. 69, 571 (1996) Reflective Linearized...Digest Series, Vol. 6 (Optical Society of America, Washington, D.C., 1996), p . 626 Effects of Low-Temperature-Grown GaAs and AlGaAs on the Current

Perturbation of nuclear spin polarizations in solid state NMR of nitroxide-doped samples by magic-angle spinning without microwaves.

PubMed

Thurber, Kent R; Tycko, Robert

2014-05-14

We report solid state (13)C and (1)H nuclear magnetic resonance (NMR) experiments with magic-angle spinning (MAS) on frozen solutions containing nitroxide-based paramagnetic dopants that indicate significant perturbations of nuclear spin polarizations without microwave irradiation. At temperatures near 25 K, (1)H and cross-polarized (13)C NMR signals from (15)N,(13)C-labeled L-alanine in trinitroxide-doped glycerol/water are reduced by factors as large as six compared to signals from samples without nitroxide doping. Without MAS or at temperatures near 100 K, differences between signals with and without nitroxide doping are much smaller. We attribute most of the reduction of NMR signals under MAS near 25 K to nuclear spin depolarization through the cross-effect dynamic nuclear polarization mechanism, in which three-spin flips drive nuclear polarizations toward equilibrium with spin polarization differences between electron pairs. When T1e is sufficiently long relative to the MAS rotation period, the distribution of electron spin polarization across the nitroxide electron paramagnetic resonance lineshape can be very different from the corresponding distribution in a static sample at thermal equilibrium, leading to the observed effects. We describe three-spin and 3000-spin calculations that qualitatively reproduce the experimental observations.

An absorbing microwave micro-solid-phase extraction device used in non-polar solvent microwave-assisted extraction for the determination of organophosphorus pesticides.

PubMed

Wang, Ziming; Zhao, Xin; Xu, Xu; Wu, Lijie; Su, Rui; Zhao, Yajing; Jiang, Chengfei; Zhang, Hanqi; Ma, Qiang; Lu, Chunmei; Dong, Deming

2013-01-14

A single-step extraction-cleanup method, including microwave-assisted extraction (MAE) and micro-solid-phase extraction (μ-SPE), was developed for the extraction of ten organophosphorus pesticides in vegetable and fruit samples. Without adding any polar solvent, only one kind of non-polar solvent (hexane) was used as extraction solvent in the whole extraction step. Absorbing microwave μ-SPE device, was prepared by packing activated carbon with microporous polypropylene membrane envelope, and used as not only the sorbent in μ-SPE, but also the microwave absorption medium. Some experimental parameters effecting on extraction efficiency was investigated and optimized. 1.0 g of sample, 8 mL of hexane and three absorbing microwave μ-SPE devices were added in the microwave extraction vessel, the extraction was carried out under 400 W irradiation power at 60°C for 10 min. The extracts obtained by MAE-μ-SPE were directly analyzed by GC-MS without any clean-up process. The recoveries were in the range of 93.5-104.6%, and the relative standard deviations were lower than 8.7%. Copyright © 2012 Elsevier B.V. All rights reserved.

Solid state green synthesis and catalytic activity of CuO nanorods in thermal decomposition of potassium periodate

NASA Astrophysics Data System (ADS)

Patel, Vinay Kumar; Bhattacharya, Shantanu

2017-09-01

The present study reports a facile solid state green synthesis process using the leaf extracts of Hibiscus rosa-sinensis to synthesize CuO nanorods with average diameters of 15-20 nm and lengths up to 100 nm. The as-synthesized CuO nanorods were characterized by x-ray diffraction, Fourier transform infrared spectroscopy, transmission electron microscopy and selected area electron diffraction. The formation mechanism of CuO nanorods has been explained by involving the individual role of amide I (amino groups) and carboxylate groups under excess hydroxyl ions released from NaOH. The catalytic activity of CuO nanorods in thermal decomposition of potassium periodate microparticles (µ-KIO4) microparticles was studied by thermo gravimetric analysis measurement. The original size (~100 µm) of commercially procured potassium periodate was reduced to microscale length scale to about one-tenth by PEG200 assisted emulsion process. The CuO nanorods prepared by solid state green route were found to catalyze the thermal decomposition of µ-KIO4 with a reduction of 18 °C in the final thermal decomposition temperature of potassium periodate.

Microwave-Assisted Eco-Friendly Synthesis of Organics and Nanomaterials

EPA Science Inventory

This presentation summarizes our recent activity in MW-assisted synthesis, which involves benign alternatives, such as the use of supported reagents, and greener reaction medium in aqueous or solvent-free conditions.1 The greener synthesis of heterocyclic compounds, coupling reac...

Sustainable Synthesis of Organics and Nanomaterials Using Microwave Irradiation

EPA Science Inventory

MW-assisted synthesis of heterocyclic compounds and nanomaterials under benign conditions is summarized. Shape-controlled aqueous synthesis of noble nanostructures via MW spontaneous reduction of metal salts using -D-glucose, sucrose, and maltose will be presented. A general met...

Greener Synthesis and Chemical transformations Using Sustainable Alternative Methods and Applications of Nano-Catalysts

EPA Science Inventory

The presentation summarizes our sustainable chemical synthesis activity involving benign alternatives, namely greener reaction medium in aqueous or solventfree conditions and using alternative activation via microwave or photocatalytic activation. Eco-friendly synthesis of nanoma...

Low-temperature dynamic nuclear polarization with helium-cooled samples and nitrogen-driven magic-angle spinning.

PubMed

Thurber, Kent; Tycko, Robert

2016-03-01

We describe novel instrumentation for low-temperature solid state nuclear magnetic resonance (NMR) with dynamic nuclear polarization (DNP) and magic-angle spinning (MAS), focusing on aspects of this instrumentation that have not been described in detail in previous publications. We characterize the performance of an extended interaction oscillator (EIO) microwave source, operating near 264 GHz with 1.5 W output power, which we use in conjunction with a quasi-optical microwave polarizing system and a MAS NMR probe that employs liquid helium for sample cooling and nitrogen gas for sample spinning. Enhancement factors for cross-polarized (13)C NMR signals in the 100-200 range are demonstrated with DNP at 25K. The dependences of signal amplitudes on sample temperature, as well as microwave power, polarization, and frequency, are presented. We show that sample temperatures below 30K can be achieved with helium consumption rates below 1.3 l/h. To illustrate potential applications of this instrumentation in structural studies of biochemical systems, we compare results from low-temperature DNP experiments on a calmodulin-binding peptide in its free and bound states. Published by Elsevier Inc.

On-Demand Microwave Generator of Shaped Single Photons

NASA Astrophysics Data System (ADS)

Forn-Díaz, P.; Warren, C. W.; Chang, C. W. S.; Vadiraj, A. M.; Wilson, C. M.

2017-11-01

We demonstrate the full functionality of a circuit that generates single microwave photons on demand, with a wave packet that can be modulated with a near-arbitrary shape. We achieve such a high tunability by coupling a superconducting qubit near the end of a semi-infinite transmission line. A dc superconducting quantum interference device shunts the line to ground and is employed to modify the spatial dependence of the electromagnetic mode structure in the transmission line. This control allows us to couple and decouple the qubit from the line, shaping its emission rate on fast time scales. Our decoupling scheme is applicable to all types of superconducting qubits and other solid-state systems and can be generalized to multiple qubits as well as to resonators.

System-Level Integrated Circuit (SLIC) development for phased array antenna applications

NASA Technical Reports Server (NTRS)

Shalkhauser, K. A.; Raquet, C. A.

1991-01-01

A microwave/millimeter wave system-level integrated circuit (SLIC) being developed for use in phased array antenna applications is described. The program goal is to design, fabricate, test, and deliver an advanced integrated circuit that merges radio frequency (RF) monolithic microwave integrated circuit (MMIC) technologies with digital, photonic, and analog circuitry that provide control, support, and interface functions. As a whole, the SLIC will offer improvements in RF device performance, uniformity, and stability while enabling accurate, rapid, repeatable control of the RF signal. Furthermore, the SLIC program addresses issues relating to insertion of solid state devices into antenna systems, such as the reduction in number of bias, control, and signal lines. Program goals, approach, and status are discussed.

System-level integrated circuit (SLIC) development for phased array antenna applications

NASA Technical Reports Server (NTRS)

Shalkhauser, K. A.; Raquet, C. A.

1991-01-01

A microwave/millimeter wave system-level integrated circuit (SLIC) being developed for use in phased array antenna applications is described. The program goal is to design, fabricate, test, and deliver an advanced integrated circuit that merges radio frequency (RF) monolithic microwave integrated circuit (MMIC) technologies with digital, photonic, and analog circuitry that provide control, support, and interface functions. As a whole, the SLIC will offer improvements in RF device performance, uniformity, and stability while enabling accurate, rapid, repeatable control of the RF signal. Furthermore, the SLIC program addresses issues relating to insertion of solid state devices into antenna systems, such as the reduction in number of bias, control, and signal lines. Program goals, approach, and status are discussed.

Strong coupling of a single electron in silicon to a microwave photon.

PubMed

Mi, X; Cady, J V; Zajac, D M; Deelman, P W; Petta, J R

2017-01-13

Silicon is vital to the computing industry because of the high quality of its native oxide and well-established doping technologies. Isotopic purification has enabled quantum coherence times on the order of seconds, thereby placing silicon at the forefront of efforts to create a solid-state quantum processor. We demonstrate strong coupling of a single electron in a silicon double quantum dot to the photonic field of a microwave cavity, as shown by the observation of vacuum Rabi splitting. Strong coupling of a quantum dot electron to a cavity photon would allow for long-range qubit coupling and the long-range entanglement of electrons in semiconductor quantum dots. Copyright © 2017, American Association for the Advancement of Science.

A quasi-optical and corrugated waveguide microwave transmission system for simultaneous dynamic nuclear polarization NMR on two separate 14.1 T spectrometers

PubMed Central

Dubroca, Thierry; Smith, Adam N.; Pike, Kevin J.; Froud, Stuart; Wylde, Richard; Trociewitz, Bianca; McKay, Johannes; Mentink-Vigier, Frederic; van Tol, Johan; Wi, Sungsool; Brey, William; Long, Joanna R.; Frydman, Lucio; Hill, Stephen

2018-01-01

Nuclear magnetic resonance (NMR) is an intrinsically insensitive technique, with Boltzmann distributions of nuclear spin states on the order of parts per million in conventional magnetic fields. To overcome this limitation, dynamic nuclear polarization (DNP) can be used to gain up to three orders of magnitude in signal enhancement, which can decrease experimental time by up to six orders of magnitude. In DNP experiments, nuclear spin polarization is enhanced by transferring the relatively larger electron polarization to NMR active nuclei via microwave irradiation. Here, we describe the design and performance of a quasi-optical system enabling the use of a single 395 GHz gyrotron microwave source to simultaneously perform DNP experiments on two different 14.1 T (1H 600 MHz) NMR spectrometers: one configured for magic angle spinning (MAS) solid state NMR; the other configured for solution state NMR experiments. In particular, we describe how the high power microwave beam is split, transmitted, and manipulated between the two spectrometers. A 13C enhancement of 128 is achieved via the cross effect for alanine, using the nitroxide biradical AMUPol, under MAS-DNP conditions at 110 K, while a 31P enhancement of 160 is achieved via the Overhauser effect for triphenylphosphine using the monoradical BDPA under solution NMR conditions at room temperature. The latter result is the first demonstration of Overhauser DNP in the solution state at a field of 14.1 T (1H 600 MHz). Moreover these results have been produced with large sample volumes (~100 μL, i.e. 3 mm diameter NMR tubes). PMID:29459343

A quasi-optical and corrugated waveguide microwave transmission system for simultaneous dynamic nuclear polarization NMR on two separate 14.1 T spectrometers

NASA Astrophysics Data System (ADS)

Dubroca, Thierry; Smith, Adam N.; Pike, Kevin J.; Froud, Stuart; Wylde, Richard; Trociewitz, Bianca; McKay, Johannes; Mentink-Vigier, Frederic; van Tol, Johan; Wi, Sungsool; Brey, William; Long, Joanna R.; Frydman, Lucio; Hill, Stephen

2018-04-01

Nuclear magnetic resonance (NMR) is an intrinsically insensitive technique, with Boltzmann distributions of nuclear spin states on the order of parts per million in conventional magnetic fields. To overcome this limitation, dynamic nuclear polarization (DNP) can be used to gain up to three orders of magnitude in signal enhancement, which can decrease experimental time by up to six orders of magnitude. In DNP experiments, nuclear spin polarization is enhanced by transferring the relatively larger electron polarization to NMR active nuclei via microwave irradiation. Here, we describe the design and performance of a quasi-optical system enabling the use of a single 395 GHz gyrotron microwave source to simultaneously perform DNP experiments on two different 14.1 T (1H 600 MHz) NMR spectrometers: one configured for magic angle spinning (MAS) solid state NMR; the other configured for solution state NMR experiments. In particular, we describe how the high power microwave beam is split, transmitted, and manipulated between the two spectrometers. A 13C enhancement of 128 is achieved via the cross effect for alanine, using the nitroxide biradical AMUPol, under MAS-DNP conditions at 110 K, while a 31P enhancement of 160 is achieved via the Overhauser effect for triphenylphosphine using the monoradical BDPA under solution NMR conditions at room temperature. The latter result is the first demonstration of Overhauser DNP in the solution state at a field of 14.1 T (1H 600 MHz). Moreover these results have been produced with large sample volumes (∼100 μL, i.e. 3 mm diameter NMR tubes).

A quasi-optical and corrugated waveguide microwave transmission system for simultaneous dynamic nuclear polarization NMR on two separate 14.1 T spectrometers.

PubMed

Dubroca, Thierry; Smith, Adam N; Pike, Kevin J; Froud, Stuart; Wylde, Richard; Trociewitz, Bianca; McKay, Johannes; Mentink-Vigier, Frederic; van Tol, Johan; Wi, Sungsool; Brey, William; Long, Joanna R; Frydman, Lucio; Hill, Stephen

2018-04-01

Nuclear magnetic resonance (NMR) is an intrinsically insensitive technique, with Boltzmann distributions of nuclear spin states on the order of parts per million in conventional magnetic fields. To overcome this limitation, dynamic nuclear polarization (DNP) can be used to gain up to three orders of magnitude in signal enhancement, which can decrease experimental time by up to six orders of magnitude. In DNP experiments, nuclear spin polarization is enhanced by transferring the relatively larger electron polarization to NMR active nuclei via microwave irradiation. Here, we describe the design and performance of a quasi-optical system enabling the use of a single 395 GHz gyrotron microwave source to simultaneously perform DNP experiments on two different 14.1 T ( 1 H 600 MHz) NMR spectrometers: one configured for magic angle spinning (MAS) solid state NMR; the other configured for solution state NMR experiments. In particular, we describe how the high power microwave beam is split, transmitted, and manipulated between the two spectrometers. A 13 C enhancement of 128 is achieved via the cross effect for alanine, using the nitroxide biradical AMUPol, under MAS-DNP conditions at 110 K, while a 31 P enhancement of 160 is achieved via the Overhauser effect for triphenylphosphine using the monoradical BDPA under solution NMR conditions at room temperature. The latter result is the first demonstration of Overhauser DNP in the solution state at a field of 14.1 T ( 1 H 600 MHz). Moreover these results have been produced with large sample volumes (∼100 µL, i.e. 3 mm diameter NMR tubes). Copyright © 2018 Elsevier Inc. All rights reserved.

Transmission Line for 258 GHz Gyrotron DNP Spectrometry

NASA Astrophysics Data System (ADS)

Bogdashov, Alexandr A.; Belousov, Vladimir I.; Chirkov, Alexey V.; Denisov, Gregory G.; Korchagin, Vyacheslav V.; Kornishin, Sergey Yu.; Tai, Evgeny M.

2011-06-01

We describe the design and test results of the transmission line for liquid-state (LS) and solid-state (SS) DNP spectrometers with the second-harmonic 258.6 GHz gyrotron at the Institute of the Biophysical Chemistry Center of Goethe University (Frankfurt). The 13-meter line includes a mode converter, HE11 waveguides, 4 mitre bends, a variable polarizer-attenuator, directional couplers, a water-flow calorimeter and a mechanical switch. A microwave power of about 15 W was obtained in the pure HE11 mode at the spectrometer inputs.

Effect of Mn and Ti substitution on the reflection loss characteristic of Ba{sub 0.6}Sr{sub 0.4}Fe{sub 11-z}MnTi{sub z}O{sub 19} (z = 0, 1, 2 and 3)

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

Gunanto, Y. E., E-mail: yohanes.gunanto@uph.edu; Cahyadi, L., E-mail: lina.cahyadi@uph.edu; Adi, W. Ari, E-mail: dwisnuaa@batan.go.id

2016-04-19

The synthesis and characterization of composition Ba{sub 0.6}Sr{sub 0.4}Fe{sub 11-z}MnTi{sub z}O{sub 19} (z = 0; 1; 2 and 3) compound by solid state reaction using mechanical milling have been performed. The raw materials were BaCO{sub 3}, SrCO{sub 3}, Fe{sub 2}O{sub 3}, MnCO{sub 3}, and TiO{sub 2}. The mixed powder was compacted and sintered at 1000°C for 5 hours. X-ray diffraction studies indicate expansion of hexagonal unit cell and compression of atomic density with substitution of Mn{sup 2+} and Ti{sup 4+} ions. Effect of substitution upon magnetic properties revealed that total magnetization, remanence, and coercivity changed with substitution due to preferentialmore » site occupancy of substituted Mn{sup 2+} and Ti{sup 4+} ions. Since the coercivity and total magnetization may be controlled by substitution while maintaining resistive properties, this material is useful for microwave absorber.« less

Microwave-assisted chemistry: synthetic applications for rapid assembly of nanomaterials and organics.

PubMed

Gawande, Manoj B; Shelke, Sharad N; Zboril, Radek; Varma, Rajender S

2014-04-15

The magic of microwave (MW) heating technique, termed the Bunsen burner of the 21st century, has emerged as a valuable alternative in the synthesis of organic compounds, polymers, inorganic materials, and nanomaterials. Important innovations in MW-assisted chemistry now enable chemists to prepare catalytic materials or nanomaterials and desired organic molecules, selectively, in almost quantitative yields and with greater precision than using conventional heating. By controlling the specific MW parameters (temperature, pressure, and ramping of temperature) and choice of solvents, researchers can now move into the next generation of advanced nanomaterial design and development. Microwave-assisted chemical reactions are now well-established practices in the laboratory setting although some controversy lingers as to how MW irradiation is able to enhance or influence the outcome of chemical reactions. Much of the discussion has focused on whether the observed effects can, in all instances, be rationalized by purely thermal Arrhenius-based phenomena (thermal microwave effects), that is, the importance of the rapid heating and high bulk reaction temperatures that are achievable using MW dielectric heating in sealed reaction vessels, or whether these observations can be explained by so-called "nonthermal" or "specific microwave" effects. In recent years, innovative and significant advances have occurred in MW hardware development to help delineate MW effects, especially the use of silicon carbide (SiC) reaction vessels and the accurate measurement of temperature using fiber optic (FO) temperature probes. SiC reactors appear to be good alternatives to MW transparent borosilicate glass, because of their high microwave absorptivity, and as such they serve as valuable tools to demystify the claimed magical MW effects. This enables one to evaluate the influence of the electromagnetic field on the specific chemical reactions, under truly identical conventional heating conditions, wherein temperature is measured accurately by fiber optic (FO) probe. This Account describes the current status of MW-assisted synthesis highlighting the introduction of various prototypes of equipment, classes of organic reactions pursued using nanomaterials, and the synthesis of unique and multifunctional nanomaterials; the ensuing nanomaterials possess zero-dimensional to three-dimensional shapes, such as spherical, hexagonal, nanoprisms, star shapes, and nanorods. The synthesis of well-defined nanomaterials and nanocatalysts is an integral part of nanotechnology and catalysis science, because it is imperative to control their size, shape, and compositional engineering for unique deployment in the field of nanocatalysis and organic synthesis. MW-assisted methods have been employed for the convenient and reproducible synthesis of well-defined noble and transition core-shell metallic nanoparticles with tunable shell thicknesses. Some of the distinctive attributes of MW-selective heating in the synthesis and applications of magnetic nanocatalysts in organic synthesis under benign reaction conditions are highlighted. Sustainable nanomaterials and their applications in benign media are an ideal blend for the development of greener methodologies in organic synthesis; MW heating provides superb value to the overall sustainable process development via process intensification including the flow systems.

MICROWAVE-ASSISTED SYNTHESIS OF NOBLE NANOSTRUCTURES

EPA Science Inventory

Microwave-assisted (MW) spontaneous reduction of noble metal salts, silver (Ag), gold (Au), platinum (Pt) and palladium (Pd) is reported using sugar solutions such as -D glucose, sucrose and maltose, etc. to generate nanomaterials. These MW-assisted reactions, conducted in aqueo...

Microwave Technology--Applications in Chemical Synthesis

EPA Science Inventory

Microwave heating, being specific and instantaneous, is unique and has found a place for expeditious chemical syntheses. Specifically, the solvent-free reactions are convenient to perform and have advantages over the conventional heating protocols as summarized in the previous se...

GREENER CHEMICAL SYNTHESIS USING MICROWAVES

EPA Science Inventory

A solvent-free approach that involves microwave (MW) exposure of neat reactants (undiluted) catalyzed by the surfaces of recyclable mineral supports such as alumina, silica, clay, or "doped" surfaces is presented which is applicable to a wide range of cleavage, condensation, cyc...

EXPEDITIOUS SYNTHESIS OF IONIC LIQUIDS USING ULTRASOUND AND MICROWAVE IRRADIATION

EPA Science Inventory

Environmentally friendlier preparations of ionic liquids have been developed that proceed expeditiously under the influence of microwave or ultrasound irradiation conditions using neat reactants, alkylimidazoles and alkyl halides. A number of useful ionic liquids have been prepar...

Alternative energy input: Mechanochemical, microwave and ultrasound-assisted organic synthesis

EPA Science Inventory

Microwave, ultrasound, sunlight and mechanochemical mixing can be used to augment conventional laboratory techniques. By applying these alternative means of activation, a number of chemical transformations have been achieved thereby improving many existing protocols with superi...

Microwave Assisted Synthesis of Py-Im Polyamides

PubMed Central

2012-01-01

Microwave synthesis was utilized to rapidly build Py-Im polyamides in high yields and purity using Boc-protection chemistry on Kaiser oxime resin. A representative polyamide targeting the 5′-WGWWCW-3′ (W = A or T) subset of the consensus Androgen and Glucocorticoid Response Elements was synthesized in 56% yield after 20 linear steps and HPLC purification. It was confirmed by Mosher amide derivatization of the polyamide that a chiral α-amino acid does not racemize after several additional coupling steps. PMID:22578091

Excellent acceleration of the Diels-Alder reaction by microwave irradiation for the synthesis of new fluorine-substituted ligands of NMDA receptor.

PubMed

Sasaki, S; Ishibashi, N; Kuwamura, T; Sano, H; Matoba, M; Nisikawa, T; Maeda, M

1998-11-03

A series of 6,11-ethanobenzo[b]quinolizinium derivatives was synthesized through the Diels-Alder reaction between azoniaanthracne and the corresponding 1,1-disubstituted olefin. After a systematic investigation for achieving rapid synthesis, it was found that the reaction is accelerated in polar media such as H2O and trifluoroethanol. In particular, excellent acceleration was effected by microwave irradiation. The new fluorine-substituted ligands thus obtained exhibited potential affinity toward NMDA receptors.

Using liquid and solid state NMR and photoluminescence to study the synthesis and solubility properties of amine capped silicon nanoparticles.

PubMed

Giuliani, J R; Harley, S J; Carter, R S; Power, P P; Augustine, M P

2007-08-01

Water soluble silicon nanoparticles were prepared by the reaction of bromine terminated silicon nanoparticles with 3-(dimethylamino)propyl lithium and characterized with liquid and solid state nuclear magnetic resonance (NMR) and photoluminescence (PL) spectroscopies. The surface site dependent 29Si chemical shifts and the nuclear spin relaxation rates from an assortment of 1H-29Si heteronuclear solid state NMR experiments for the amine coated reaction product are consistent with both the 1H and 13C liquid state NMR results and routine transmission electron microscopy, ultra-violet/visible, and Fourier transform infrared measurements. PL was used to demonstrate the pH dependent solubility properties of the amine passivated silicon nanoparticles.

In-situ aging microwave heating synthesis of LTA zeolite layer on mesoporous TiO2 coated porous alumina support

NASA Astrophysics Data System (ADS)

Baig, Mirza A.; Patel, Faheemuddin; Alhooshani, Khalid; Muraza, Oki; Wang, Evelyn N.; Laoui, Tahar

2015-12-01

LTA zeolite layer was successfully grown on a superhydrophilic mesoporous titania layer coated onto porous α-alumina substrate. Mesoporous titania layer was formed as an intermediate bridge in the pore size variation between the macroporous α-alumina support and micro-porous LTA zeolite layer. In-situ aging microwave heating synthesis method was utilized to deposit the LTA zeolite layer. Mesoporous titania layer was pre-treated with UV photons and this was observed to have played a major role in improving the surface hydrophilicity of the substrate leading to formation of increased number of Ti-OH groups on the surface. This increase in Ti-OH groups enhanced the interaction between the synthesis gel and the substrate leading to strong attachment of the amorphous gel on the substrate, thus enhancing coverage of the LTA zeolite layer to almost the entire surface of the 1-inch (25.4 mm) diameter membrane. LTA zeolite layer was developed via in-situ aged under microwave irradiation to study the effect of synthesis parameters such as in-situ aging time and synthesis time on the formation of the LTA zeolite layer. Optimized process parameters resulted in the formation of crack-free porous zeolite layer yielding a zeolite-titania-alumina multi-layer membrane with a gradient in porosity.

Covellite CuS nanocrystals: realizing rapid microwave-assisted synthesis in air and unravelling the disappearance of their plasmon resonance after coupling with carbon nanotubes

NASA Astrophysics Data System (ADS)

Kim, Mee Rahn; Hafez, Hassan A.; Chai, Xin; Besteiro, Lucas V.; Tan, Long; Ozaki, Tsuneyuki; Govorov, Alexander O.; Izquierdo, Ricardo; Ma, Dongling

2016-06-01

Semiconductor nanocrystals that show plasmonic resonance represent an emerging class of highly promising plasmonic materials with potential applications in diverse fields, such as sensing and optical and optoelectronic devices. We report a new approach to synthesizing homogeneous covellite CuS nanoplatelets in air and the almost complete disappearance of their plasmonic resonance once coupled with multiwalled carbon nanotubes (MWCNTs). These nanoplatelets were rapidly synthesized by a simple microwave-assisted approach at a relatively low reaction temperature in air, instead of under N2 as reported previously. These less severe synthesis conditions were enabled by appropriately selecting a Cu precursor and preparing a precursor sulfur solution (instead of using solid sulfur) and by using microwave radiation as the heat source. The advantages of utilizing microwave irradiation, including uniform and rapid heating, became clear after comparing the results of the synthesis with those achieved using a conventional oil-bath method under N2. The CuS nanoplatelets prepared in this way showed very strong plasmon resonance at c. 1160 nm as a result of their free charge carriers at the calculated density of nh = 1.5 × 1022 cm-3 based on the Drude model. With the aim of exploring their potential for near-infrared responsive optoelectronic devices, they were hybridized with functionalized MWCNTs. Their strong plasmon resonance almost completely disappeared on hybridization. Detailed investigations excluded the effect of possible structural changes in the CuS nanoplatelets during the hybridization process and a possible effect on the plasmon resonance arising from the chemical bonding of surface ligands. Charge transfer was considered to be the main reason for the almost complete disappearance of the plasmon resonance, which was further confirmed by terahertz (THz) time-domain spectrometry and THz time-resolved spectrometry measurements performed on the CuS-MWCNT nanohybrids. By extracting the rising and relaxation constants through fitting a single-exponential rising function and a bi-exponential relaxation function, in combination with the results of THz differential transmission as a function of the NIR pump fluence, it was found that hole injection changed the electronic properties of the MWCNTs only subtly on a short picosecond time scale, whereas the nature of the band structure of the MWCNTs remained largely unchanged. These findings aid our understanding of recently emerging semiconductor plasmonics and will also help in developing practical applications.Semiconductor nanocrystals that show plasmonic resonance represent an emerging class of highly promising plasmonic materials with potential applications in diverse fields, such as sensing and optical and optoelectronic devices. We report a new approach to synthesizing homogeneous covellite CuS nanoplatelets in air and the almost complete disappearance of their plasmonic resonance once coupled with multiwalled carbon nanotubes (MWCNTs). These nanoplatelets were rapidly synthesized by a simple microwave-assisted approach at a relatively low reaction temperature in air, instead of under N2 as reported previously. These less severe synthesis conditions were enabled by appropriately selecting a Cu precursor and preparing a precursor sulfur solution (instead of using solid sulfur) and by using microwave radiation as the heat source. The advantages of utilizing microwave irradiation, including uniform and rapid heating, became clear after comparing the results of the synthesis with those achieved using a conventional oil-bath method under N2. The CuS nanoplatelets prepared in this way showed very strong plasmon resonance at c. 1160 nm as a result of their free charge carriers at the calculated density of nh = 1.5 × 1022 cm-3 based on the Drude model. With the aim of exploring their potential for near-infrared responsive optoelectronic devices, they were hybridized with functionalized MWCNTs. Their strong plasmon resonance almost completely disappeared on hybridization. Detailed investigations excluded the effect of possible structural changes in the CuS nanoplatelets during the hybridization process and a possible effect on the plasmon resonance arising from the chemical bonding of surface ligands. Charge transfer was considered to be the main reason for the almost complete disappearance of the plasmon resonance, which was further confirmed by terahertz (THz) time-domain spectrometry and THz time-resolved spectrometry measurements performed on the CuS-MWCNT nanohybrids. By extracting the rising and relaxation constants through fitting a single-exponential rising function and a bi-exponential relaxation function, in combination with the results of THz differential transmission as a function of the NIR pump fluence, it was found that hole injection changed the electronic properties of the MWCNTs only subtly on a short picosecond time scale, whereas the nature of the band structure of the MWCNTs remained largely unchanged. These findings aid our understanding of recently emerging semiconductor plasmonics and will also help in developing practical applications. Electronic supplementary information (ESI) available: TEM, XRD, SAED and UV-Vis-NIR absorption spectra of the control reaction results. See DOI: 10.1039/c6nr03426h

Ultra-Rapid Crystallization of L-alanine Using Monomode Microwaves, Indium Tin Oxide and Metal-Assisted and Microwave-Accelerated Evaporative Crystallization.

PubMed

Lansiquot, Carisse; Boone-Kukoyi, Zainab; Shortt, Raquel; Thompson, Nishone; Ajifa, Hillary; Kioko, Bridgit; Constance, Edward Ned; Clement, Travis; Ozturk, Birol; Aslan, Kadir

2017-01-01

The use of indium tin oxide (ITO) and focused monomode microwave heating for the ultra-rapid crystallization of L-alanine (a model amino acid) is reported. Commercially available ITO dots (< 5 mm) attached to blank poly(methyl)methacrylate (PMMA, 5 cm in diameter with 21-well silicon isolators: referred to as the iCrystal plates) were found to withstand prolonged microwave heating during crystallization experiments. Crystallization of L-alanine was performed at room temperature (a control experiment), with the use of two microwave sources: a 2.45 GHz conventional microwave (900 W, power level 1, a control experiment) and 8 GHz (20 W) solid state, monomode microwave source with an applicator tip that focuses the microwave field to a 5-mm cavity. Initial appearance of L-alanine crystals and on iCrystal plates with ITO dots took 47 ± 2.9 min, 12 ± 7.6 min and 1.5 ± 0.5 min at room temperature, using a conventional microwave and focused monomode microwave heating, respectively. Complete evaporation of the solvent using the focused microwaves was achieved in 3.2 ± 0.5 min, which is ~52-fold and ~172-fold faster than that observed at room temperature and using conventional microwave heating, respectively. The size and number of L-alanine crystals was dependent on the type of the 21-well iCrystal plates and the microwave heating method: 33 crystals of 585 ± 137 μm in size at room temperature > 37 crystals of 542 ± 100 μm in size with conventional microwave heating > 331 crystals of 311 ± 190 μm in size with focused monomode microwave. FTIR, optical microscopy and powder X-ray diffraction analysis showed that the chemical composition and crystallinity of the L-alanine crystals did not change when exposed to microwave heating and ITO surfaces. In addition, theoretical simulations for the binding of L-alanine molecules to ITO and other metals showed the predicted nature of hydrogen bonds formed between L-alanine and these surfaces.

Ultra-Rapid Crystallization of L-alanine Using Monomode Microwaves, Indium Tin Oxide and Metal-Assisted and Microwave-Accelerated Evaporative Crystallization

PubMed Central

Lansiquot, Carisse; Boone-Kukoyi, Zainab; Shortt, Raquel; Thompson, Nishone; Ajifa, Hillary; Kioko, Bridgit; Constance, Edward Ned; Clement, Travis; Ozturk, Birol; Aslan, Kadir

2018-01-01

The use of indium tin oxide (ITO) and focused monomode microwave heating for the ultra-rapid crystallization of L-alanine (a model amino acid) is reported. Commercially available ITO dots (< 5 mm) attached to blank poly(methyl)methacrylate (PMMA, 5 cm in diameter with 21-well silicon isolators: referred to as the iCrystal plates) were found to withstand prolonged microwave heating during crystallization experiments. Crystallization of L-alanine was performed at room temperature (a control experiment), with the use of two microwave sources: a 2.45 GHz conventional microwave (900 W, power level 1, a control experiment) and 8 GHz (20 W) solid state, monomode microwave source with an applicator tip that focuses the microwave field to a 5-mm cavity. Initial appearance of L-alanine crystals and on iCrystal plates with ITO dots took 47 ± 2.9 min, 12 ± 7.6 min and 1.5 ± 0.5 min at room temperature, using a conventional microwave and focused monomode microwave heating, respectively. Complete evaporation of the solvent using the focused microwaves was achieved in 3.2 ± 0.5 min, which is ~52-fold and ~172-fold faster than that observed at room temperature and using conventional microwave heating, respectively. The size and number of L-alanine crystals was dependent on the type of the 21-well iCrystal plates and the microwave heating method: 33 crystals of 585 ± 137 μm in size at room temperature > 37 crystals of 542 ± 100 μm in size with conventional microwave heating > 331 crystals of 311 ± 190 μm in size with focused monomode microwave. FTIR, optical microscopy and powder X-ray diffraction analysis showed that the chemical composition and crystallinity of the L-alanine crystals did not change when exposed to microwave heating and ITO surfaces. In addition, theoretical simulations for the binding of L-alanine molecules to ITO and other metals showed the predicted nature of hydrogen bonds formed between L-alanine and these surfaces. PMID:29657884

Alternative synthetic approaches for metal-organic frameworks: transformation from solid matters.

PubMed

Zhan, Guowu; Zeng, Hua Chun

2016-12-20

Developing economic and sustainable synthetic strategies for metal-organic frameworks (MOFs) is imperative for promoting MOF materials into large scale industrial use. Very recently, an alternative strategy for MOF synthesis by using solvent-insoluble "solid matters" as cation reservoirs and/or templates has been developed to accomplish this goal, in which the solid matters often refer to metals, metal oxides, hydroxides, carbonates, and so forth, but excluding the soluble metal salts which have been prevailingly used in MOF synthesis. Although most of the pioneering activities in this field have just started in the past 5 years, remarkable achievements have been made covering the synthesis, functionalization, positioning, and applications. A great number of MOFs in powder form, thin-films, or membranes, have been prepared through such solid-to-MOF transformations. This field is rapidly developing and expanding, and the number of related scientific publications has strikingly increased over the last few years. The aim of this review is to summarise the latest developments, highlight the present state-of-the-art, and also provide an overview for future research directions.

Subcarrier multiplexing with dispersion reduction and direct detection

DOEpatents

Sargis, P.D.; Haigh, R.E.; McCammon, K.G.

1997-01-21

An SCM system is disclosed for simultaneously reducing the concomitant problems of receiver complexity and dispersion penalty and without requiring the use of an expensive, high-bandwidth optical detector. The system provides both a dispersion reduction and a direct detection to the receiver, with microwave mixers and lithium niobate external modulators that produce sidebands that are only separated by a few gigahertz from a principal laser optical carrier. Digital data streams are independently impressed upon these sidebands for transmission over an ordinary single-mode fiber. Independent high-speed data streams are upconverted to microwave frequencies. These subcarriers are then combined with a microwave power combiner and amplified with a microwave amplifier. A solid-state 1550-nm laser carrier is modulated by the microwave subcarriers. An erbium-doped fiber amplifier (EDFA) is used just prior to long-distance transmission over ordinary single-mode fiber. The transmitted optical signal may then traverse multiple EDFAs to compensate for long-haul optical fiber losses prior to detection. At a receiving end, the optical signal is split into multiple paths. The subcarrier channels are optically pre-selected using a narrowband optical filter, such as a fiber Fabry-Perot (FFP) filter. An optical detector converts the selected optical signal into a baseband electrical data stream. 2 figs.

Synthesis and photophysical characterizations of thermal-stable naphthalene benzimidazoles.

PubMed

Erten-Ela, Sule; Ozcelik, Serdar; Eren, Esin

2011-07-01

Microwave-assisted synthesis, photophysical and electrochemical properties of thermal-stable naphthalene benzimidazoles and naphthalimides are studied in this paper. Microwave-assisted synthesis of naphthalene benzimidazoles provide higher yields than the conventional thermal synthesis. Comparative photophysical properties of naphthalene benzimidazoles and naphthalimides are revealed that conjugation of electron-donating group onto naphthalimide moiety increases fluorescence quantum yields. Fluorophore-solvent interactions are also investigated using Lippert-Mataga equation for naphthalimides and naphthalene benzimidazoles. Thermal stabilities of naphthalene benzimidazoles are better than naphthalimides due to increased aromaticity. The experimental E(LUMO) levels of naphthalene benzimidazoles are found to be between 3.15 and 3.28 eV. Therefore, naphthalene benzimidazole derivatives consisting of anchoring groups are promising materials in organic dye sensitized solar cells. © Springer Science+Business Media, LLC 2011

Comparison of microwave-assisted and conventional extraction of mangiferin from mango (Mangifera indica L.) leaves.

PubMed

Zou, Tangbin; Wu, Hongfu; Li, Huawen; Jia, Qing; Song, Gang

2013-10-01

Mangiferin is the main bioactive component in mango leaves, which possesses anti-inflammatory, antioxidative, antidiabetic, immunomodulatory, and antitumor activities. In the present study, a microwave-assisted extraction method was developed for the extraction of mangiferin from mango leaves. Some parameters such as ethanol concentration, liquid-to-solid ratio, microwave power, and extraction time were optimized by single-factor experiments and response surface methodology. The optimal extraction conditions were 45% ethanol, liquid-to-solid ratio of 30:1 (mL/g), and extraction time of 123 s under microwave irradiation of 474 W. Under optimal conditions, the yield of mangiferin was 36.10 ± 0.72 mg/g, significantly higher than that of conventional extraction. The results obtained are beneficial for the full utilization of mango leaves and also indicate that microwave-assisted extraction is a very useful method for extracting mangiferin from plant materials. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Influence of deflocculation on microwave disintegration and anaerobic biodegradability of waste activated sludge.

PubMed

Ebenezer, A Vimala; Kaliappan, S; Adish Kumar, S; Yeom, Ick-Tae; Banu, J Rajesh

2015-06-01

In the present study, the potential benefits of deflocculation on microwave pretreatment of waste activated sludge were investigated. Deflocculation in the absence of cell lysis was achieved through the removal of extra polymeric substances (EPS) by sodium citrate (0.1g sodium citrate/g suspended solids), and DNA was used as a marker for monitoring cell lysis. Subsequent microwave pretreatment yielded a chemical oxygen demand (COD) solubilisation of 31% and 21%, suspended solids (SS) reduction of 37% and 22%, for deflocculated and flocculated sludge, respectively, with energy input of 14,000kJ/kg TS. When microwave pretreated sludge was subjected to anaerobic fermentation, greater accumulation of volatile fatty acid (860mg/L) was noticed in deflocculated sludge, indicating better hydrolysis. Among the samples subjected to BMP (Biochemical methane potential test), deflocculated microwave pretreated sludge showed better amenability towards anaerobic digestion with high methane production potential of 0.615L (gVS)(-1). Copyright © 2015 Elsevier Ltd. All rights reserved.

Vapour-induced solid-state C-H bond activation for the clean synthesis of an organopalladium biothiol sensor.

PubMed

Monas, Andrea; Užarević, Krunoslav; Halasz, Ivan; Kulcsár, Marina Juribašić; Ćurić, Manda

2016-10-27

Room-temperature accelerated aging in the solid state has been applied for atom- and energy-efficient activation of either one or two C-H bonds of azobenzene and methyl orange by palladium(ii) acetate. Organopalladium complexes are prepared in quantitative reactions without potentially harmful side products. Dicyclopalladated methyl orange is water-soluble and is a selective chromogenic biothiol sensor at physiologically-relevant micromolar concentrations in buffered aqueous media.

Ultrarapid Multimode Microwave Synthesis of Nano/Submicron β-SiC

PubMed Central

Johnson, Michael; He, Wenzhi; Li, Guangming; Zhao, Chen; Yu, Luling; Huang, Juwen; Zhu, Haochen

2018-01-01

This paper presents the design, development and realization of a fast and novel process for the synthesis of 3C silicon carbide (β-SiC) nanorods and submicron powder. Using SiO2 (or Si) and activated carbon (AC), this process allows β-SiC to be synthesized with almost 100% purity in timeframes of seconds or minutes using multimode microwave rotary tube reactors under open-air conditions. The synthesis temperature used was 1460 ± 50 °C for Si + AC and 1660 ± 50 °C for SiO2 + AC. The shortest β-SiC synthesis time achieved was about 20 s for Si + AC and 100 s for SiO2 + AC. This novel synthesis method allows for scaled-up flow processes in the rapid industrial-scale production of β-SiC, having advantages of time/energy saving and carbon dioxide emission reduction over comparable modern processes. PMID:29470417

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.

Microwave-assisted Ullmann C-S bond formation: synthesis of the P38alpha MAPK clinical candidate VX-745.

PubMed

Bagley, Mark C; Davis, Terence; Dix, Matthew C; Fusillo, Vincenzo; Pigeaux, Morgane; Rokicki, Michal J; Kipling, David

2009-11-06

Microwave irradiation promotes the rapid and efficient reaction of a thiophenol and aryl or heteroaryl halide using a copper or palladium catalyst and a range of ligands, depending upon substrate. Of particular utility is the use of copper(I) iodide (5 mol %) and trans-cyclohexane-1,2-diol as ligand under basic conditions and microwave irradiation to give the corresponding sulfide in high yield. This method for C-S bond formation is applied in the four-step synthesis of the clinical candidate VX-745 in 38% overall yield. The inhibitory activity of VX-745 against p38alpha MAPK is confirmed in Werner syndrome dermal fibroblasts at 1.0 microM concentration by immunoblot assay.

SOLVENT-FREE ACCELERATED ORGANIC SYNTHESES USING MICROWAVES

EPA Science Inventory

Abstract: A solvent-free approach for organic synthesis is described which involves microwave (MW) exposure of neat reactants (undiluted) either in presence of a catalyst or catalyzed by the surfaces of inexpensive and recyclable mineral supports such as alumina, silica, clay, or...

NON-TRADITIONAL 'GREENER' ALTERNATIVES TO SYNTHETIC ORGANIC TRANSFORMATIONS USING MICROWAVES

EPA Science Inventory

A rapid and environmentally friendlier approach for organic synthesis and transformations is described which involves microwave (MW) exposure of neat reactants (undiluted) often in presence of inorganic oxides as recyclable catalysts such as alumina, silica, clay, or 'doped' surf...

'GREENER' CHEMICAL SYNTHESIS USING MICROWAVE IRRADIATION

EPA Science Inventory

A solvent-free approach that involves microwave (MW) exposure of neat reactants (undiluted) catalyzed by the surfaces of recyclable mineral supports such as alumina, silica, clay, or 'doped' surfaces is presented which is applicable to a wide range of cleavage, condensation, cycl...

Microwave-Assisted Synthesis of Mesoporous Nano-Hydroxyapatite Using Surfactant Templates

EPA Science Inventory

Mesoporous nano-hydroxyapatite (n-HAP) was expeditiously synthesized using the pseudo sol-gel microwave-assisted protocol (30 min) in the presence of two novel templates, namely sodium lauryl ether sulfate (SLES) and linear alkylbenzenesulfonate (LABS). The cooperative self-assem...

Microwave-assisted synthesis of porous carbon-titania and highly crystalline titania nanostructures.

PubMed

Parker, Alison; Marszewski, Michal; Jaroniec, Mietek

2013-03-01

Porous carbon-titania and highly crystalline titania nanostructured materials were obtained through a microwave-assisted one-pot synthesis. Resorcinol and formaldehyde were used as carbon precursors, triblock copolymer Pluronic F127 as a stabilizing agent, and titanium isopropoxide as a titania precursor. This microwave-assisted one-pot synthesis involved formation of carbon spheres according to the recently modified Stöber method followed by hydrolysis and condensation of titania precursor. This method afforded carbon-titania composite materials containing anatase phase with specific surface areas as high as 390 m(2) g(-1). The pure nanostructured titania, obtained after removal of carbon through calcination of the composite material in air, was shown to be the anatase phase with considerably higher degree of crystallinity and the specific surface area as high as 130 m(2) g(-1). The resulting titania, because of its high surface area, well-developed porosity, and high crystallinity, is of great interest for catalysis, water treatment, lithium batteries, and other energy-related applications.

Microwave-assisted synthesis of isosorbide-derived diols for the preparation of thermally stable thermoplastic polyurethane

PubMed Central

Kasmi, Nejib; Roso, Martina; Hammami, Nadia; Majdoub, Mustapha; Boaretti, Carlo; Sgarbossa, Paolo; Vianello, Chiara; Maschio, Giuseppe; Modesti, Michele; Lorenzetti, Alessandra

2017-01-01

Abstract In order to prepare thermally stable isosorbide-derived thermoplastic polyurethane, the synthesis of two new chiral exo–exo configured diols, prepared from isosorbide, and two types of diphenols (bisphenol A and thiodiphenol) was described. The synthesis conditions were optimized under conventional heating and microwave irradiations. To prove their suitability in polymerization, these monomers were successfully polymerized using 4,4′-diphenylmethane diisocyanate (MDI) and hexamethylene diisocyanate (HDI). Both monomers and polymers have been studied by NMR, FT-IR, TGA, DSC; intrinsic viscosity of polymers has also been determined. The results showed the effectiveness of the synthetic strategy proposed; moreover, a dramatic reduction of the reaction time and an important improvement of the monomers yield using microwave irradiation have been demonstrated. The monomers, as well as the polymers, showed excellent thermal stability both in air and nitrogen. It was also shown that the introduction of sulphur in the polyurethane backbone was effective in delaying the onset of degradation as well as the degradation rate. PMID:29491826

Selection of Lipases for the Synthesis of Biodiesel from Jatropha Oil and the Potential of Microwave Irradiation to Enhance the Reaction Rate

PubMed Central

2016-01-01

The present study deals with the enzymatic synthesis of biodiesel by transesterification of Jatropha oil (Jatropha curcas L.) with ethanol in a solvent-free system. Seven commercial lipase preparations immobilized by covalent attachment on epoxy-polysiloxane-polyvinyl alcohol composite (epoxy-SiO2-PVA) were tested as biocatalysts. Among them, immobilized lipases from Pseudomonas fluorescens (lipase AK) and Burkholderia cepacia (lipase PS) were the most active biocatalysts in biodiesel synthesis, reaching ethyl ester yields (FAEE) of 91.1 and 98.3% at 72 h of reaction, respectively. The latter biocatalyst exhibited similar performance compared to Novozym® 435. Purified biodiesel was characterized by different techniques. Transesterification reaction carried out under microwave irradiation exhibited higher yield and productivity than conventional heating. The operational stability of immobilized lipase PS was determined in repeated batch runs under conventional and microwave heating systems, revealing half-life times of 430.4 h and 23.5 h, respectively. PMID:27868060

Design and synthesis of the superionic conductor Na10SnP2S12

PubMed Central

Richards, William D.; Tsujimura, Tomoyuki; Miara, Lincoln J.; Wang, Yan; Kim, Jae Chul; Ong, Shyue Ping; Uechi, Ichiro; Suzuki, Naoki; Ceder, Gerbrand

2016-01-01

Sodium-ion batteries are emerging as candidates for large-scale energy storage due to their low cost and the wide variety of cathode materials available. As battery size and adoption in critical applications increases, safety concerns are resurfacing due to the inherent flammability of organic electrolytes currently in use in both lithium and sodium battery chemistries. Development of solid-state batteries with ionic electrolytes eliminates this concern, while also allowing novel device architectures and potentially improving cycle life. Here we report the computation-assisted discovery and synthesis of a high-performance solid-state electrolyte material: Na10SnP2S12, with room temperature ionic conductivity of 0.4 mS cm−1 rivalling the conductivity of the best sodium sulfide solid electrolytes to date. We also computationally investigate the variants of this compound where tin is substituted by germanium or silicon and find that the latter may achieve even higher conductivity. PMID:26984102

An efficient solid-state synthesis of fluorescent surface carboxylated carbon dots derived from C60 as a label-free probe for iron ions in living cells.

PubMed

Lan, Jing; Liu, Chunfang; Gao, Mingxuan; Huang, Chengzhi

2015-11-01

In order to achieve the simple, easily repeated, and large scale preparation of fluorescent CDs, a new solid-state synthesis (SSS) approach was developed by calcining the mixture of fullerenes (C60) and solid sodium hydroxide. The cage of fullerenes could be opened and the hydroxyl and carboxyl were successfully introduced in the presence of sodium hydroxide under high temperature. The as-prepared surface carboxylated CDs possess many good properties, such as high water solubility, good photostability, salt tolerance, and nontoxicity. Especially, the fluorescence of CDs could be highly quenched by Fe(3+) because of the strong interaction of hydroxyl or carboxyl on the as-obtained CDs with Fe(3+), which realized a sensitive detection of Fe(3+) in the linear range of 0.02-0.6 μmol/L. What is more, we further applied the obtained CDs into the intracellular imaging of Fe(3+). Copyright © 2015 Elsevier B.V. All rights reserved.

Parameters for scale-up of lethal microwave treatment to eradicate cerambycid larvae infesting solid wood packing materials

Treesearch

Mary R. Fleming; John J. Janowiak; Joseph Kearns; Jeffrey E. Shield; Rustum Roy; Dinesh K. Agrawal; Leah S. Bauer; Kelli Hoover

2004-01-01

The use of microwave irradiation to eradicate insects infesting wood used to manufacture packing materials such as pallets and crateswas evaluated. The focus of this preliminary studywas to determinewhich microwave parameters, including chamber-volume to sample-volumeratios,variations ofpower and time, and energydensity (total microwavepower/woodvolume), affect the...

Low-temperature sintered Li2(MnxTi1-x)O3 microwave dielectric ceramics with adjustable τf

NASA Astrophysics Data System (ADS)

Liu, Cheng; Zhang, Huaiwu; Su, Hua; Li, Jie; Liao, Yulong; Jia, Lijun; Li, Yuanxun

2017-12-01

B2O3-Bi2O3-SiO2-ZnO (BBSZ) glass-modified Li2(MnxTi1-x)O3 ceramics were fabricated via a solid-state reaction route. Pure phase and dense crystal morphology were obtained at 900∘C. Suitable amount of Mn4+-ion substitution could adjust the τf value of the Li2(MnxTi1-x)O3 system to near zero. Among all of the Li2(MnxTi1-x)O3 samples, the sample with x = 0.9 (marked as BL9 in this paper) possessed good microwave dielectric properties: 𝜀r = 18, Q × f = 14,056 GHz (9.58 GHz) and τf = (+)2.43 ppm/∘C. It is suggested that the Li2(MnxTi1-x)O3 ceramic with BBSZ glass is a suitable low-temperature co-fired ceramic (LTCC) candidate for microwave applications.

Low-loss Ca{sub 5-x}Sr{sub x}A{sub 2}TiO{sub 12} [A=Nb,Ta] ceramics: Microwave dielectric properties and vibrational spectroscopic analysis

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

Bijumon, Pazhoor Varghese; Sebastian, Mailadil Thomas; Dias, Anderson

2005-05-15

Complex perovskite-type Ca{sub 5-x}Sr{sub x}A{sub 2}TiO{sub 12} [A=Nb,Ta] (0{<=}x{<=}5) ceramics were prepared by conventional solid-state ceramic route. The crystal structure, microwave dielectric properties, and vibrational spectroscopic characteristics of these materials are reported. The structure and microstructure were investigated by x-ray diffraction and scanning electron microscopy techniques. The microwave dielectric properties were measured in the 3-5-GHz frequency range by the resonance method. Structural evolutions from orthorhombic to an averaged pseudocubic phase, with associated changes in dielectric properties, were observed as a function of composition. The structure-property relationships in these ceramics were established using Raman and Fourier transform infrared spectroscopic techniques. Ramanmore » analysis showed characteristic bands of ordered perovskite materials, with variation in both intensity and frequency as a function of composition.« less

Satellite Power Systems /SPS/ - Overview of system studies and critical technology

NASA Technical Reports Server (NTRS)

Manson, S. V.

1980-01-01

Systems studies and critical technology issues for the development and evaluation of Satellite Power Systems (SPS) for the photovoltaic generation of electrical energy and its transmission to earth are reviewed. Initial concept studies completed in 1976 and system definition studies initiated in the same year have indicated the technical feasibility of SPS and identified challenging issues to be addressed as part of the SPS Concept Development and Evaluation Program. Systems considered in the study include photovoltaic and solar thermal power conversion configurations employing klystron or solid state microwave generators or lasers for power transmission, and power transmission options, system constructability and in-orbit and ground operations. Technology investigations are being performed in the areas of microwave power transmission, structure/controls interactions and the behavior of key materials in the space/SPS environment. Favorable results have been obtained in the areas of microwave phase distribution and phase control, dc-RF conversion, antenna radiating element, and no insurmountable problems have been discovered in any of the investigations to date.

Cu3Mo2O9: An Ultralow-Firing Microwave Dielectric Ceramic with Good Temperature Stability and Chemical Compatibility with Aluminum

NASA Astrophysics Data System (ADS)

Wen, Wangxi; Li, Chunchun; Sun, Yihua; Tang, Ying; Fang, Liang

2018-02-01

An ultralow-firing microwave dielectric ceramic Cu3Mo2O9 with orthorhombic structure has been fabricated via a solid-state reaction method. X-ray diffraction analysis, Rietveld refinement, Raman spectroscopy, energy-dispersive spectrometry, and scanning electron microscopy were employed to explore the phase purity, crystal structure, and microstructure. Pure and dense Cu3Mo2O9 ceramics could be obtained in the sintering temperature range from 580°C to 680°C. The sample sintered at 660°C for 4 h exhibited the highest relative density (˜ 97.2%) and best microwave dielectric properties with ɛ r = 7.2, Q × f = 19,300 GHz, and τ f = - 7.8 ppm/°C. Chemical compatibility with aluminum electrodes was also confirmed. All the results suggest that Cu3Mo2O9 ceramic is a promising candidate for use in ultralow-temperature cofired ceramic applications.

Current Status of Study on Hydrogen Production with Space Solar Power Systems (SSPS)

NASA Astrophysics Data System (ADS)

Mori, M.; Kagawa, H.; Nagayama, H.; Saito, Y.

2004-12-01

Japan Aerospace Exploration Agency (JAXA) has been conducting studies on Space Solar Power Systems (SSPS) using microwave and laser beams for years since FY1998 organizing a special committee and working groups. The microwave based SSPS are huge solar power systems that generate GW power by solar cells. The electric power is transmitted via microwave from the SSPS to the ground. In the laser based SSPS, a solar condenser equipped with lenses or mirrors and laser-generator would be put into orbit. A laser beam would be sent to Earth-based hydrogen generating device. We are proposing a roadmap that consists of a stepwise approach to achieve commercial SSPS in 20-30 years. The first step is 50kW class Technology Demonstration Satellite to demonstrate microwave power transmission. The second step is to demonstrate robotic assembly of 10MW class large scale flexible structure in space on ISS co-orbit. The third step is to build a prototype SSPS in GEO. The final step is to build commercial SSPS in GEO. We continue the study of SSPS concepts and architectures, technology flight demonstration and major technology development. System design of tens of kW class Technology Demonstration Satellite and conceptual study of 10MW class demonstration system on ISS co-orbit are also conducted. Several key technologies which are needed to be developed in appropriate R&D roadmap, such as high-voltage solar cell array, fiber type of direct solar pumping solid-state laser, high efficiency magnetron, thermal control technology and control technology of large scale flexible structure etc. are also investigated. In the study of concept design of commercial SSPS mentioned above, we have studied some configurations of both microwave based SSPS and laser based SSPS. In case of microwave based SSPS, the solar energy must be converted to electricity and then converted to a microwave beam. The on-ground rectifying antenna will collect the microwave beam and convert it to electricity to connect to commercial power grids. From the past experiences of the conceptual design of the1GW class SSPS, it is clear that system with the mirrors and modularized unit which integrated solar cells and microwave power transmitters is promising. In this type of SSPS, the solar lights are directed to the energy conversion unit integrated solar cells and microwave power transmitters using mirrors. The key factor in designing systems is feasibility of thermal system. Considering above these factors, some reference models are being considered now. FY2003 reference model is the model for formation flight without the center truss which connect to primary mirrors to energy conversion unit. Using this model as basis, we are carrying out examination from various viewpoints aiming at the cost minimum to build and maintain the systems. In case of laser based SSPS, the laser beam would be directly produced from the solar light using the direct solar pumping solid-state laser device. This laser beams would be collected on ground and used to produce hydrogen from seawater. The receiving / energy conversion station is settled on an ocean, and producing hydrogen can be stored and transported by ships to consumers. In designing laser based SSPS, conversion efficiency of the direct solar pumping solid-state laser and feasibility of thermal system are critical factors. Since magnification of solar concentrator is very high, improvement of thermal control system is important. Feasibility of its ground facilities and production technology of hydrogen using laser beams has been also studied. Both hydrogen generating systems with photo-catalyst device and electrolytic ones have been examined. From the past experiences of this study, high efficient electric power generating technology using the solar cell which suited the wavelength of laser is promising. The life cycle cost model of laser based SSPS was created and evaluated its validity. Sensitivity analysis of laser based SSPS are also continued aiming at hydrogen generating cost of around 20 cent per Nm3 . This paper presents a summary of studies on SSPS that JAXA has examined.

Satellite power systems (SPS) concept definition study. Volume 2, part 1: System engineering

NASA Technical Reports Server (NTRS)

Hanley, G. M.

1980-01-01

Top level trade studies are presented, including comparison of solid state and klystron concepts, higher concentration on the solar cells, composite and aluminum structure, and several variations to the reference concept. Detailed trade studies are presented in each of the subsystem areas (solar array, power distribution, structures, thermal control, attitude control and stationkeeping, microwave transmission, and ground receiving station). A description of the selected point design is also presented.

Electrochemically exfoliated graphene as a novel microwave susceptor: the ultrafast microwave-assisted synthesis of carbon-coated silicon-graphene film as a lithium-ion battery anode.

PubMed

Kim, Jong Min; Ko, Dongjin; Oh, Jiseop; Lee, Jeongyeon; Hwang, Taejin; Jeon, Youngmoo; Hooch Antink, Wytse; Piao, Yuanzhe

2017-10-19

Graphene nanocomposites have attracted much attention in many applications due to their superior properties. However, preparing graphene nanocomposites requires a time-consuming thermal treatment to reduce the graphene or synthesize nanomaterials, in most cases. We present an ultrafast synthesis of a carbon-coated silicon-graphene nanocomposite using a commercial microwave system. Electrochemically exfoliated graphene is used as a novel microwave susceptor to deliver efficient microwave energy conversion. Unlike graphene oxide, it does not require a time-consuming pre-thermal reduction or toxic chemical reduction to absorb microwave radiation efficiently. A carbon-coated silicon nanoparticle-electrochemically exfoliated graphene nanocomposite film was prepared by a few seconds' microwave irradiation. The sp 2 domains of graphene absorb microwave radiation and generate heat to simultaneously reduce the graphene and carbonize the polydopamine carbon precursor. The as-prepared N-doped carbon-coated silicon-graphene film was used as a lithium-ion battery anode. The N-doped carbon coating decreases the contact resistance between silicon nanoparticles and graphene provides a wide range conductive network. Consequently, it exhibited a reversible capacity of 1744 mA h g -1 at a current density of 0.1 A g -1 and 662 mA h g -1 at 1.0 A g -1 after 200 cycles. This method can potentially be a general approach to prepare various graphene nanocomposites in an extremely short time.

Microwave-assisted synthesis of HKUST-1 and functionalized HKUST-1-@H3PW12O40: selective adsorption of heavy metal ions in water analyzed with synchrotron radiation.

PubMed

Zou, Fang; Yu, Runhan; Li, Rongguan; Li, Wei

2013-08-26

A simple, rapid and efficient synthesis of the metal-organic framework (MOF) HKUST-1 [Cu3(1,3,5-benzene-tri-carboxilic-acid)2] by microwave irradiation is described, which afforded a homogeneous and highly selective material. The unusually short time to complete the synthesis by microwave irradiation is mainly attributable to rapid nucleation rather than to crystal growth rate. Using this method, HKUST-1-MW (MW=microwave) could be prepared within 20 min, whereas by hydrothermal synthesis, involving conventional heating, the preparation time is 8 h. Work efficiency was improved by the good performance of the obtained HKUST-1-MW which exhibited good selective adsorption of heavy metal ions, as well as a remarkably high adsorption affinity and adsorption capacity, but no adsorption of Hg(2+) under the same experimental conditions. Of particular importance is the preservation of the structure after metal-ion adsorption, which remained virtually intact, with only a few changes in X-ray diffraction intensity and a moderate decline in surface area. Synthesis of the polyoxometalate-containing HKUST-1-MW@H3PW12O40 afforded a MOF with enhanced stability in water, due to the introduced Keggin-type phosphotungstate, which systematically occluded in the cavities constituting the walls between the mesopores. Different Cu/W ratios were investigated according to the extrusion rate of cooper ions concentration, without significant structural changes after adsorption. The MOFs obtained feature particle sizes between 10-20 μm and their structures were determined using synchrotron-based X-ray diffraction. The results of this study can be considered important for potentially wider future applications of MOFs, especially to attend environmental issues. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

One-step synthesis of solid state luminescent carbon-based silica nanohybrids for imaging of latent fingerprints

NASA Astrophysics Data System (ADS)

Li, Feng; Li, Hongren; Cui, Tianfang

2017-11-01

Fluorescent carbon-based nanomaterials(CNs) with tunable visible emission are biocompatible, environment friendly and most suitable for various biomedical applications. Despite the successes in preparing strongly fluorescent CNs, preserving the luminescence in solid materials is still challenging because of the serious emission quenching of CNs in solid state materials. In this work, fluorescent carbon and silica nanohybrids (SiCNHs) were synthesized via a simple one-step hydrothermal approach by carbonizing sodium citrate and (3-aminopropyl)triethoxysilane(APTES), and hydrolysis of tetraethyl orthosilicate(TEOS). The resultant SiCNs were characterized through X-ray diffraction (XRD), transmission electron microscopy (TEM), FT-IR, X-ray photoelectron spectroscopy (XPS), and photoluminescence (PL) spectroscopy. The SiCNs exhibited strong fluorescence in both aqueous and solid states. The luminescent solid state SiCNs power were successfully used as a fluorescent labeling material for enhanced imaging of latent fingerprints(LFPs) on single background colour and multi-coloured surfaces substrates in forensic science for individual identification.

'GREENER' SOLVENT-FREE CHEMICAL SYNTHESIS USING MICROWAVE IRRADIATION

EPA Science Inventory

Solvent-free approach that involves microwave (MW) irradiation of neat reactants (undiluted) catalyzed by the surfaces of less-expensive and recyclable mineral supports such as alumina, silica, clay, or 'doped' surfaces is presented which is applicable to a wide range of cleavage...

MICROWAVE EFFECTS IN ORGANIC SYNTHESIS: MECHANISTIC AND REACTION MEDIUM CONSIDERATIONS

EPA Science Inventory

The scope of applications of microwave irradiation relates to a wide spectrum of organic syntheses with numerous benefits (reduction in reaction times, improved purity of products and better yields) encompassing advantages of both thermal and (or) specific non-purely thermal effe...

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

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

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

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

Simultaneous Microwave Extraction and Separation of Volatile and Non-Volatile Organic Compounds of Boldo Leaves. From Lab to Industrial Scale

PubMed Central

Petigny, Loïc; Périno, Sandrine; Minuti, Matteo; Visinoni, Francesco; Wajsman, Joël; Chemat, Farid

2014-01-01

Microwave extraction and separation has been used to increase the concentration of the extract compared to the conventional method with the same solid/liquid ratio, reducing extraction time and separate at the same time Volatile Organic Compounds (VOC) from non-Volatile Organic Compounds (NVOC) of boldo leaves. As preliminary study, a response surface method has been used to optimize the extraction of soluble material and the separation of VOC from the plant in laboratory scale. The results from the statistical analysis revealed that the optimized conditions were: microwave power 200 W, extraction time 56 min and solid liquid ratio of 7.5% of plants in water. Lab scale optimized microwave method is compared to conventional distillation, and requires a power/mass ratio of 0.4 W/g of water engaged. This power/mass ratio is kept in order to upscale from lab to pilot plant. PMID:24776762

Microwave-assisted synthesis of iron oxide nanoparticles in biocompatible organic environment

NASA Astrophysics Data System (ADS)

Aivazoglou, E.; Metaxa, E.; Hristoforou, E.

2018-04-01

The development of magnetite and maghemite particles in uniform nanometer size has triggered the interest of the research community due to their many interesting properties leading to a wide range of applications, such as catalysis, nanomedicine-nanobiology and other engineering applications. In this study, a simple, time-saving and low energy-consuming, microwave-assisted synthesis of iron oxide nanoparticles, is presented. The nanoparticles were prepared by microwave-assisted synthesis using polyethylene glycol (PEG) or PEG and β-cyclodextrin (β-CD)/water solutions of chloride salts of iron in the presence of ammonia solution. The prepared nano-powders were characterized using X-Ray Diffraction (XRD), Transition Electron Microscopy (TEM), Fourier-transform Infrared Spectroscopy (FTIR), Raman Spectroscopy, Vibrating Sample Magnetometer (VSM), X-Ray Photoelectron Spectroscopy (XPS) and Thermal analysis (TG/DSC). The produced nanoparticles are crystallized mostly in the magnetite and maghemite lattice exhibiting very similar shape and size, with indications of partial PEG coating. Heating time, microwave power and presence of PEG, are the key factors shaping the size properties of nanoparticles. The average size of particles ranges from 10.3 to 19.2 nm. The nanoparticles exhibit a faceted morphology, with zero contamination levels. The magnetic measurements indicate that the powders are soft magnetic materials with negligible coercivity and remanence, illustrating super-paramagnetic behavior.

High Efficiency Ka-Band Solid State Power Amplifier Waveguide Power Combiner

NASA Technical Reports Server (NTRS)

Wintucky, Edwin G.; Simons, Rainee N.; Chevalier, Christine T.; Freeman, Jon C.

2010-01-01

A novel Ka-band high efficiency asymmetric waveguide four-port combiner for coherent combining of two Monolithic Microwave Integrated Circuit (MMIC) Solid State Power Amplifiers (SSPAs) having unequal outputs has been successfully designed, fabricated and characterized over the NASA deep space frequency band from 31.8 to 32.3 GHz. The measured combiner efficiency is greater than 90 percent, the return loss greater than 18 dB and input port isolation greater than 22 dB. The manufactured combiner was designed for an input power ratio of 2:1 but can be custom designed for any arbitrary power ratio. Applications considered are NASA s space communications systems needing 6 to 10 W of radio frequency (RF) power. This Technical Memorandum (TM) is an expanded version of the article recently published in Institute of Engineering and Technology (IET) Electronics Letters.

Thermal phenomena under microwave field in the organic synthesis processes: Application to the Diels Alder reaction

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

Saillard, R.; Poux, M.; Audhuy-Peaudecerf, M.

1996-12-31

The influence of the microwave heating on chemical reactions were investigated. The kinetic of the Diels Alder reaction were studied under microwave irradiation at a frequency of 2.45 GHz in a single mode cavity and were compared to the kinetic obtained by a conventional heating. Experiments were carried out in a liquid solvent in order to have a better control of the medium temperature measurement. In a second part, the presence of a catalytic solid phase was introduced. Some thermal fluctuations which are due to an heterogeneity of the electric field were detected in the medium. They reduce the precisionmore » of the results and cause problems of experimental reproducibility. A thermoluminescent material allow a good visualization of these phenomena. In addition, the profiles of the electric field intensity were modelled by a 2D finite elements method in the reactor in the presence of a solvent. Despite the small size of the sample and the use of a monomode cavity which both limited the heterogeneities of the medium temperature, the authors showed a great heterogeneity of the electric field intensity and as a result the heterogeneity of the temperature in their sample. In order to avoid these phenomena which induce a lack of reproducibility, a stirring device was developed. The values of the kinetics obtained under the 2 heating modes with the introduction of the stirring device. So, it induces a good control of the medium temperature. All those investigations prompted the authors to the conclusion that there is no difference between microwave heating and a classical heating in the studied reaction.« less

Optimisation of microwave-assisted processing in production of pineapple jam

NASA Astrophysics Data System (ADS)

Ismail, Nur Aisyah Mohd; Abdullah, Norazlin; Muhammad, Norhayati

2017-10-01

Pineapples are available all year round since they are unseasonal fruits. Due to the continuous harvesting of the fruit, the retailers and farmers had to find a solution such as the processing of pineapple into jam, to treat the unsuccessfully sold pineapples. The direct heating of pineapple puree during the production of pineapple jam can cause over degradation of quality of the fresh pineapple. Thus, this study aims to optimise the microwave-assisted processing conditions for producing pineapple jam which could reduce water activity and meets minimum requirement for pH and total soluble solids contents of fruit jam. The power and time of the microwave processing were chosen as the factors, while the water activity, pH and total soluble solids (TSS) content of the pineapple jam were determined as responses to be optimised. The microwave treatment on the pineapple jam was able to give significant effect on the water activity and TSS content of the pineapple jam. The optimum power and time for the microwave processing of pineapple jam is 800 Watt and 8 minutes, respectively. The use of domestic microwave oven for the pineapple jam production results in acceptable pineapple jam same as conventional fruit jam sold in the marketplace.

A new mild base-catalyzed Mannich reaction of hetero-arylamines in water: highly efficient stereoselective synthesis of beta-aminoketones under microwave heating.

PubMed

Hao, Wen-Juan; Jiang, Bo; Tu, Shu-Jiang; Cao, Xu-Dong; Wu, Shan-Shan; Yan, Shu; Zhang, Xiao-Hong; Han, Zheng-Guo; Shi, Feng

2009-04-07

A new mild base-catalyzed Mannich reaction of aromatic aldehydes with 1,2-diphenylethanone and hetero-arylamines including pyridin-2-amine and pyrimidin-2-amine is described. In this reaction, a series of new beta-aminoketones were stereoselectively synthesized in water by controlling the steric hindrance of the substrates under microwave heating. This method has the advantages of a short synthetic route, operational simplicity, increased safety for small-scale high-speed synthesis, and minimal environmental impact.

Low-temperature synthesis of allyl dimethylamine by selective heating under microwave irradiation used for water treatment

NASA Astrophysics Data System (ADS)

Tian, Binghui; Luan, Zhaokun; Li, Mingming

2005-08-01

Low-temperature synthesis of allyl dimethylamine (ADA) by selective heating under microwave irradiation (MI) used for water treatment is investigated. The effect of MI, ultrasound irradiation (UI) and conventional heating on yield of ADA, reaction time and the flocculation efficiency of polydiallyl dimethylammunion chloride (PDADMAC) prepared form ADA were studied. The results show that by selective heating at low temperature, MI not only increases yield of ADA and reduces reaction time, but also greatly enhances the flocculation efficiency of PDADMAC.

Smooth and rapid microwave synthesis of MIL-53(Fe) including superparamagnetic γ-Fe2O3 nanoparticles

NASA Astrophysics Data System (ADS)

Wengert, Simon; Albrecht, Joachim; Ruoss, Stephen; Stahl, Claudia; Schütz, Gisela; Schäfer, Ronald

2017-12-01

MIL-53(Fe) linked to superparamagnetic γ-Fe2O3 nanoparticles was created using time-efficient microwave synthesis. Intermediates as well as the final product have been characterized by Dynamic Light Scattering (DLS), Infrared Spectroscopy (FTIR) and Thermal Gravimetric Analysis (TGA). It is found that this route allows the production of Fe nanoparticles with typical sizes of about 80 nm that are embedded inside the metal-organic structures. Detailed magnetization measurements using SQUID magnetometry revealed a nearly reversible magnetization loop indicating essentially superparamagnetic behavior.

Microwave-Assisted Synthesis of Nanomaterials and Nanocomposites

EPA Science Inventory

The aqueous preparation of nanoparticles using vitamins B1 and B2, and vitamin C which can function both as reducing and capping agents prompted us accomplished the bulk syntheses of Ag and Fe nanorods using polyethylene glycol (PEG) under microwave (MW) irradiation conditions; t...

Organo- and nano-catalyst in greener reaction medium: Microwave-assisted expedient synthesis of fine chemicals

EPA Science Inventory

The use of emerging microwave (MW) -assisted chemistry techniques is dramatically reducing chemical waste and reaction times in several organic syntheses and chemical transformations. A brief account of our experiences in developing MW-assisted organic transformations, which invo...

Glutathione promoted expeditious green synthesis of silver nanoparticles in water using microwaves

EPA Science Inventory

Silver nanoparticles with size range 5-10 nm has been synthesized under microwave irradiation conditions using gluathione, an absolutely benign antioxidant that serves as the reducing as well as capping agent in aqueous medium. This rapid protocol yields the nanoparticles within ...

CHEMISTRY UNDER 'GREENER' CONDITIONS: SOLVENT-FREE SYNTHESIS USING MICROWAVE IRRADIATION

EPA Science Inventory

Solvent-free approach is emphasized that involves microwave (MW) irradiation of neat reactants (undiluted) catalyzed by the surfaces of less-expensive and recyclable mineral supports such as alumina, silica, clay, or 'doped' surfaces which is applicable to a wide range of cleavag...

Microwave assisted synthesis of cyclic carbonates from olefins with sodium bicarbonates as the C1 source.

PubMed

Yang, Xiaoqing; Wu, Jie; Mao, Xianwen; Jamison, Timothy F; Hatton, T Alan

2014-03-25

An effective transformation of alkenes into cyclic carbonates has been achieved using NaHCO3 as the C1 source in acetone-water under microwave heating, with selectivities and yields significantly surpassing those obtained using conventional heating.

DEXTRON TEMPLATED MICROWAVE-ASSISTED SYNTHESIS OF POROUS TITANIUM DIOXIDE

EPA Science Inventory

An alternative route to the preparation and formation of porous titania powders and carbon coated titania using microwave radiation is described. Inexpensive dextrose was chosen as capping agent or template in view of its high water solubility when compared to other sugar templat...

Microwave-Assisted Organic Synthesis Using Benign Reaction Medium and Reagents

EPA Science Inventory

Account of chemical reactions expedited by microwave (MW) exposure of neat reactants for the rapid one-pot assembly of heterocyclic compounds from in situ generated reactive intermediates via enamines or using hypervalent iodine reagents will be described that can be adapted for ...

Microwave-assisted synthesis of cyclodextrin polyurethanes

USDA-ARS?s Scientific Manuscript database

Cyclodextrin (CD) has often been incorporated into polyurethanes in order to facilitate its use in encapsulation or removal of organic species for various applications. In this work a microwave-assisted method has been developed to produce polyurethanes consisting of alpha-, ß-, and gamma-CD and thr...

Response surface methodology applied to the study of the microwave-assisted synthesis of quaternized chitosan.

PubMed

dos Santos, Danilo Martins; Bukzem, Andrea de Lacerda; Campana-Filho, Sérgio Paulo

2016-03-15

A quaternized derivative of chitosan, namely N-(2-hydroxy)-propyl-3-trimethylammonium chitosan chloride (QCh), was synthesized by reacting glycidyltrimethylammonium chloride (GTMAC) and chitosan (Ch) in acid medium under microwave irradiation. Full-factorial 2(3) central composite design and response surface methodology (RSM) were applied to evaluate the effects of molar ratio GTMAC/Ch, reaction time and temperature on the reaction yield, average degree of quaternization (DQ) and intrinsic viscosity ([η]) of QCh. The molar ratio GTMAC/Ch was the most important factor affecting the response variables and RSM results showed that highly substituted QCh (DQ = 71.1%) was produced at high yield (164%) when the reaction was carried out for 30min. at 85°C by using molar ratio GTMAC/Ch 6/1. Results showed that microwave-assisted synthesis is much faster (≤30min.) as compared to conventional reaction procedures (>4h) carried out in similar conditions except for the use of microwave irradiation. Copyright © 2015 Elsevier Ltd. All rights reserved.

Microwave Heating of Crystals with Gold Nanoparticles and Synovial Fluid under Synthetic Skin Patches

PubMed Central

2017-01-01

Gout is a disease with elusive treatment options. Reduction of the size of l-alanine crystals as a model crystal for gouty tophi with the use of a monomode solid-state microwave was examined as a possible therapeutic aid. The effect of microwave heating on l-alanine crystals in the presence of gold nanoparticles (Au NPs) in solution and synovial fluid (SF) in a plastic pouch through a synthetic skin patch was investigated. In this regard, three experimental paradigms were employed: Paradigm 1 includes the effect of variable microwave power (5–10 W) and variable heating time (5–60 s) and Au NPs in water (20 nm size, volume of 10 μL) in a plastic pouch (1 × 2 cm2 in size). Paradigm 2 includes the effect of a variable volume of 20 nm Au NPs in a variable volume of SF up to 100 μL in a plastic pouch at a constant microwave power (10 W) for 30 s. Paradigm 3 includes the effect of constant microwave power (10 W) and microwave heating time (30 s), constant volume of Au NPs (100 μL), and variable size of Au NPs (20–200 nm) placed in a plastic pouch through a synthetic skin patch. In these experiments, an average of 60–100% reduction in the size of an l-alanine crystal (initial size = 450 μm) without damage to the synthetic skin or increasing the temperature of the samples beyond the physiological range was reported. PMID:28983527

Miniature hybrid microwave IC's using a novel thin-film technology

NASA Astrophysics Data System (ADS)

Eda, Kazuo; Miwa, Tetsuji; Taguchi, Yutaka; Uwano, Tomoki

1990-12-01

A novel thin-film technology for miniature hybrid microwave ICs is presented. All passive components, such as resistors and capacitors, are fully integrated on ordinary alumina ceramic substrates using the thin-film technology with very high yield. The numbers of parts and wiring processes were significantly reduced. This technology was applied to the fabrication of Ku-band solid-state power amplifiers. This thin-film technology offers the following advantages: (1) a very high yield fabrication process of thin-film capacitor having excellent electrical characteristics in the gigahertz range (Q = 230 at 12 GHz) and reliability: (2) two kinds of thin-film resistors having different temperature coefficients of resistivity and a lift-off process to integrate them with thin-film capacitors; and (3) a matching method using the thin-film capacitor.

Helicons, magnetoplasma edge, and faraday rotation in solid state plasmas at microwave frequencies.

PubMed

Furdyna, J K

1967-04-01

The effect of magnetic field on propagation of electromagnetic waves through free carrier plasmas in semiconductors is discussed. The Faraday configuration and the parameter ranges omega(c),omega(p) > omega and omega(c) > tau(-1) are specifically considered. Dispersion of helicon waves, propagation near the magnetoplasma edge (omega(p)(2) = omegaomega(c)), and the Faraday rotation are developed in terms of the one-electron Drude theory. Microwave transmission measurements at 35 Gc/s on n-type InSb are presented. Experiments near the magnetoplasma edge yield the value of the static dielectric constant of the InSb lattice K(l) = 19.3 +/- 0.8. Faraday rotation, observed beyond the edge, is found to be extremely large. Some practical possibilities for this effect are considered.

Ceramic Transactions. Volume 21. Proceedings of the Symposium on Microwave Theory and Application in Materials Processing Annual Meeting of the American Ceramic Society (23rd) Held in Cincinnati, Ohio on April 29-May 3 1991

DTIC Science & Technology

1992-04-27

spectrum analysis . 4. CONCLUSIONS * The nonthermal synthesis of crystalline nanoparticles of aluminum nitride, silicon carbide and silicon nitride is...51 R.E. Newnham, S.J. Jang, M. Xu, and F. Jones Theory of Microwave Interactions with Ceramic Mz terials .... 69 V.M. Kenkre An Analysis of the...the Performance of Microwave Process Systems Which Utilize High Q Cavities ............ 667 J.F. Gerling and G. Fournier Microwave Thermogravimetric

Efficient synthesis and biological evaluation of new benzopyran-annulated pyrano[2,3-c]pyrazole derivatives.

PubMed

Labana, Balvantsingh M; Brahmbhatt, Gaurangkumar C; Sutariya, Tushar R; Parmar, Narsidas J; Padrón, José M; Kant, Rajni; Gupta, Vivek K

2017-05-01

A one-pot method has been described to synthesize benzopyran-annulated pyrano[2,3-c]pyrazoles, effectively by combining O-alkenyloxy/alkynyloxy-acetophenones with various pyrazolones in triethylammonium acetate (TEAA) under microwave irradiation. While combination of O-allyloxy- or O-prenyloxy-acetophenones with pyrazolones occurred efficiently, that of O-propargyloxy-acetophenones was found effective in the presence of ZnO catalyst, via a domino Knoevenagel-hetero-Diels-Alder (DKHDA) reaction. Aminobenzopyran frameworks were also synthesized, after nitro-containing products were reduced in tandem with iron(II) in an acidic medium. The in vitro antiproliferative activity of these compounds was measured and discussed against gram-positive, gram-negative and M. tuberculosis bacteria, fungi, and various representative human solid tumor cell lines, in addition to their ferric reducing antioxidant capability.

Microwave-assisted one-pot synthesis of ring-fused aminals under catalyst- and solvent-free conditions

EPA Science Inventory

Heterocyclic compounds hold a special place in drug discovery and variety of techniques such as combinatorial synthesis, parallel synthesis, and automated library production to increase the output of these entities has been developed. Although most of these techniques are rapid a...

Macrocyclic molecular rotors with bridged steroidal frameworks.

PubMed

Czajkowska-Szczykowska, Dorota; Rodríguez-Molina, Braulio; Magaña-Vergara, Nancy E; Santillan, Rosa; Morzycki, Jacek W; Garcia-Garibay, Miguel A

2012-11-16

In this work, we describe the synthesis and solid-state dynamics of isomeric molecular rotors 7E and 7Z, consisting of two androstane steroidal frameworks linked by the D rings by triple bonds at their C17 positions to a 1,4-phenylene rotator. They are also linked by the A rings by an alkenyl diester bridge to restrict the conformational flexibility of the molecules and reduce the number of potential crystalline arrays. The analysis of the resulting molecular structures and packing motifs offered insights of the internal dynamics that were later elucidated by means of line shape analyses of the spectral features obtained through variable-temperature solid-state (13)C NMR; such analysis revealed rotations in the solid state occurring at kilohertz frequency at room temperature.

Flying MOFs: polyamine-containing fluidized MOF/SiO 2 hybrid materials for CO 2 capture from post-combustion flue gas

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

Luz, Ignacio; Soukri, Mustapha; Lail, Marty

Solid-state synthesis ensures a high loading and well dispersed growth of a large collection of metal–organic framework (MOF) nanostructures within a series of commercially available mesoporous silica allowing to render MOFs into fluidized solid sorbents for CO 2 capture from post-combustion flue gas in a fluidized-bed reactor.

Flying MOFs: polyamine-containing fluidized MOF/SiO 2 hybrid materials for CO 2 capture from post-combustion flue gas

DOE PAGES

Luz, Ignacio; Soukri, Mustapha; Lail, Marty

2018-01-01

Solid-state synthesis ensures a high loading and well dispersed growth of a large collection of metal–organic framework (MOF) nanostructures within a series of commercially available mesoporous silica allowing to render MOFs into fluidized solid sorbents for CO 2 capture from post-combustion flue gas in a fluidized-bed reactor.

Gordon Research Conferences, 1991

DTIC Science & Technology

1993-04-01

Chemistry Title of Conference Brewster Academy. Wolfeboro, NH Richard D. Adams, Chairman Suzanne Harris, Vice Chairman July 29. 1991 Date Monday. 8:45...am Materials and the Solid State Richard D. Adams Discussion Leader Robert Haushalter Hydrothermal Synthesis of Microporous 1. Speaker Molybdenum...Rouxel Design and Chemical Reactivity in 3. Speaker Low Dimensional Solids Title of Presentation Monday 7:30 om Catalysis Richard D. Adams Discussion

Nonthermal effects in photostimulated solid state reaction of Mn doped SrTiO3

NASA Astrophysics Data System (ADS)

Daraselia, D.; Japaridze, D.; Jibuti, Z.; Shengelaya, A.; Müller, K. A.

2017-04-01

The effect of a photostimulated solid state reaction was investigated in Mn doped SrTiO3 samples. Light irradiation was performed by either halogen or UV lamps in order to study the effect of the spectral composition, and the results were compared with samples prepared at the same temperatures in a conventional furnace. The obtained samples were studied by X-ray diffraction for structural characterization and by Electron Paramagnetic Resonance, which provides microscopic information about the local environment as well as the valence state of Mn ions. It was found that light irradiation significantly enhances the solid state reaction rate compared to synthesis in the conventional furnace. Moreover, it was observed that UV lamp irradiation is much more effective compared to halogen lamps. This indicates that the absorption of light with energy larger than the materials band gap plays an important role and points towards the nonthermal mechanism of the photostimulated solid state reaction.

Physicochemical characterization of microwave assisted synthesis of silver nanoparticles using Aloe Vera (Aloe barbadensis)

NASA Astrophysics Data System (ADS)

Kuponiyi, Abiola John

Biosynthesis of silver nanoparticles (AgNP) using different biological extracts is gaining recognition for its numerous applications in different disciplines. Although different approaches (physical and chemical) have been used for the synthesis of AgNP, the green chemistry method is most preferable because of its high efficacy, cost effectiveness, and environmental benignity. Aloe Vera (AV) contains chemical compounds (anthraquinones) that are known to possess antibacterial, antivirus and anticancer properties and the extract is a good chemical reduction agent for AgNP. Hence, it was hypothesized that a microwave assisted synthesis will produce highly concentrated, homogeneous, stable and biologically active AgNP. Thus, the main objective of the study was to evaluate the effect of microwave assisted synthesis of AgNP, the effect of pulse laser treatment on size reduction of a microwave synthesized AgNP, and the physicochemical characterization of AgNP synthesized with Aloe Vera water and ethanol extract. The experiment was conducted in two phases. Phase 1 was first conducted to optimize the experimental variables, thus establishing the optimum variables to apply in the second phase. The experiment in Phase 1 was conducted using three-factor factorial experimental design comprised of the following factors: 1) Extraction Solvent, 2) Heating Methods, 3) pH; and their corresponding levels were water and ethanol, conventional and microwave, pH (7, 8, 10 and 12), respectively. All synthesis was conducted at constant temperature of 80°C. Phase II experimental treatments were Laser ablation (0, 5, and 10 min) and Storage time (Week 1, 2 & 3). The Phase I of the results showed that increased AgNP concentrations were significantly (p < 0.05) influenced by synthesis time, hence, (15 min) gave the highest concentration. The solvent type, heating methods and pH had a significant effect (p < 0.05) on the concentration AgNP. Hence, ethanol extract (99.2 ppm), microwave method (77 ppm), and pH 10 (125 ppm) are variables that exhibited the maximum contribution to the formation of AgNP. The phase II ANOVA results indicated that laser treatment has a significant effect (p < 0.01) on the concentration of AgNP during synthesis. The intensity of the absorption peak significantly (p < 0.01) increases with laser exposure time. While 214 ppm was observed at laser exposures time 0 min, 224 and 229 ppm at 5 and 10 min and at the following rates of formation 0.384, 0.408 and 0.4288 min -1 respectively. Particle sizes (hydrodynamic diameter) were approximately 37.84 nm with no laser treatment in contrast (p < 0.01) with laser treated samples at 5 and 10 min at week 1 were 10.1 and 8.72 nm, respectively. However, storability up to the maximum storage period of six weeks of the AgNP solutions does not significantly (p > 0.05) impact the particle size distribution. Hence, the Zeta potential of the particles has values typically ranging between +100 mV to -100 mV, hence indicative of colloidal stability matrix. Furthermore, the Polydispersity indexes of Week 1, 2, & 3 treatments were 0.312, 0.591 and 0.768 respectfully, indicating that the control is monodispersed while treatments week 2 & 3 indicating the laser ablation effect in further reduction of sizes to a different level of aggregation. Microwave synthesis showed significantly (p < 0.05) higher concentration of biological compounds such as aliphatic amines, alkenes (=C-H), alkanes (C-H), alcohol (O-H) and unsaturated esters(C-O).

MICROWAVE IRRADIATION IN BENIGN SYNTHESIS OF HETEROCYCLES, NOBLE NANOMETALS AND NANOCOMPOSITES

EPA Science Inventory

A brief historic account of reactions involving microwave (MW) exposure of neat reactants or catalyzed by mineral support surfaces, such as alumina, silica, clay, or their ‘doped’ versions, for the rapid one-pot assembly of heterocyclic compounds [1] from in situ generated reacti...

CHEMISTRY UNDER NON-TRADITIONAL CONDITIONS: SOLVENT-FREE SYNTHESIS USING MICROWAVE IRRADIATION

EPA Science Inventory

A solvent-free approach that involves microwave (MW) irradiation of neat reactants (undiluted) catalyzed by the surfaces of less-expensive and recyclable mineral supports such as alumina, silica, clay, or "doped" surfaces is presented which is applicable to a wide range of cleava...

Microwave-Assisted Chemistry: Synthetic Applications for Rapid Assembly of Nanomaterials and Organics

EPA Science Inventory

The magic of microwave (MW) heating technique, termed as the Bunsen burner of the 21th Century, has emerged as valuable alternative in synthesis of organics, polymers, inorganics, and nanomaterials. Important innovations in MW-assisted chemistry now enable chemists to prepare cat...

A microwave assisted intramolecular-furan-Diels-Alder approach to 4-substituted indoles.

PubMed

Petronijevic, Filip; Timmons, Cody; Cuzzupe, Anthony; Wipf, Peter

2009-01-07

The key steps of a versatile new protocol for the convergent synthesis of 3,4-disubstituted indoles are the addition of an alpha-lithiated alkylaminofuran to a carbonyl compound, a microwave-accelerated intramolecular Diels-Alder cycloaddition and an in situ double aromatization reaction.

AN EFFICIENT AQUEOUS N-HETEROCYCLIZATION OF ANILINE DERIVATIVES: MICROWAVE-ASSISTED SYNTHESIS OF N-ARYL AZACYCLOALKANES

EPA Science Inventory

N-aryl azacycloalkanes, an important class of building blocks in natural product and pharmaceuticals, are synthesized via an efficient and simple eco-friendly protocol that involves double N-alkylation of aniline derivatives. The reaction is accelerated by exposure to microwaves ...

[Condition optimization experiment of microwave extaction of flavonoids in rhizome of Drynaria fortunei].

PubMed

Yang, Bin; Hu, Fu-chao; Chen, Gong-xi; Jiang, Dao-song

2009-12-01

The experiment extracted flavonoids in rhizome of Drynaria fortunei by microwave extraction, and determined the extraction rate through colorimetry. Through the single factor experiment and orthogonal method, the optimum extraction conditions were as follows: ethanol concentration was 40%, solid-liquid ratio was 1:20 (g/mL), microwave power was 325 W, extraction time was 40 s. Under these conditions, the extraction rate reached 1.73%. In all condtions, microwave power has the most significant effect on extraction rate. Microwave extraction has obvious advantages in comparison with traditional sovent refluxing method.

New Generation Lidar Technology and Applications

NASA Technical Reports Server (NTRS)

Spinhirne, James D.

1999-01-01

Lidar has been a tool for atmospheric research for several decades. Until recently routine operational use of lidar was not known. Problems have involved a lack of appropriate technology rather than a lack of applications. Within the last few years, lidar based on a new generation of solid state lasers and detectors have changed the situation. Operational applications for cloud and aerosol research applications are now well established. In these research applications, the direct height profiling capability of lidar is typically an adjunct to other types of sensing, both passive and active. Compact eye safe lidar with the sensitivity for ground based monitoring of all significant cloud and aerosol structure and the reliability to operate full time for several years is now in routine use. The approach is known as micro pulse lidar (MPL). For MPL the laser pulse repetition rate is in the kilohertz range and the pulse energies are in the micro-Joule range. The low pulse energy permits the systems to be eye safe and reliable with solid state lasers. A number of MPL systems have been deployed since 1992 at atmospheric research sites at a variety of global locations. Accurate monitoring of cloud and aerosol vertical distribution is a critical measurement for atmospheric radiation. An airborne application of lidar cloud and aerosol profiling is retrievals of parameters from combined lidar and passive sensing involving visible, infrared and microwave frequencies. A lidar based on a large pulse, solid state diode pumped ND:YAG laser has been deployed on the NASA ER-2 high altitude research aircraft along with multi-spectral visible/IR and microwave imaging radiometers since 1993. The system has shown high reliability in an extensive series of experimental projects for cloud remote sensing. The retrieval of cirrus radiation parameters is an effective application for combined lidar and passive sensing. An approved NASA mission will soon begin long term lidar observation of atmospheric structure from space. The Geoscience Laser Altimeter System (GLAS) of the Earth Observing System is scheduled for deployment in the 2001 time frame. GLAS is both a cloud and aerosol lidar and a surface altimeter, principally for monitoring of polar ice sheets. The GLAS instrument is based on all solid state lasers operating at 40 Hz and high efficiency, solid state detectors. The design lifetime is three to five years. Data from the GLAS mission is expected to revolutionize some aspects of our understanding of the global distribution of cloud and aerosols for global climate prediction.

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

Sharma, Anupam Deep, E-mail: dr.anupamdeep@yahoo.com; Sinha, M. M.

Perovskite oxides find wide range of applications like oxygen sensors, catalyst support, high frequency capacitors, high temperature superconducting microwave devices, solid state oxide fuel cell (SOFC) etc. LaAlO{sub 3} is one of such type of prominent perovskite oxides and very prominent material for protonic conductions. Therefore knowledge of the thermal properties of LaAlO{sub 3} is most significant. Hence in the present study we have studied phonon density of states and specific heat of LaAlO{sub 3} in cubic structure by applying lattice dynamical theoretical model. The calculated results are interpreted with existing experimental or theoretical results.

Low-temperature synthesis of graphene on nickel foil by microwave plasma chemical vapor deposition.

PubMed

Kim, Y; Song, W; Lee, S Y; Jeon, C; Jung, W; Kim, M; Park, C-Y

2011-06-27

Microwave plasma chemical vapor deposition (MPCVD) was employed to synthesize high quality centimeter scale graphene film at low temperatures. Monolayer graphene was obtained by varying the gas mixing ratio of hydrogen and methane to 80:1. Using advantages of MPCVD, the synthesis temperature was decreased from 750 °C down to 450 °C. Optical microscopy and Raman mapping images exhibited that a large area monolayer graphene was synthesized regardless of the temperatures. Since the overall transparency of 89% and low sheet resistances ranging from 590 to 1855 Ω∕sq of graphene films were achieved at considerably low synthesis temperatures, MPCVD can be adopted in manufacturing future large-area electronic devices based on graphene film.

Low-temperature synthesis of graphene on nickel foil by microwave plasma chemical vapor deposition

NASA Astrophysics Data System (ADS)

Kim, Y.; Song, W.; Lee, S. Y.; Jeon, C.; Jung, W.; Kim, M.; Park, C.-Y.

2011-06-01

Microwave plasma chemical vapor deposition (MPCVD) was employed to synthesize high quality centimeter scale graphene film at low temperatures. Monolayer graphene was obtained by varying the gas mixing ratio of hydrogen and methane to 80:1. Using advantages of MPCVD, the synthesis temperature was decreased from 750 °C down to 450 °C. Optical microscopy and Raman mapping images exhibited that a large area monolayer graphene was synthesized regardless of the temperatures. Since the overall transparency of 89% and low sheet resistances ranging from 590 to 1855 Ω/sq of graphene films were achieved at considerably low synthesis temperatures, MPCVD can be adopted in manufacturing future large-area electronic devices based on graphene film.

Spectroscopic study and enhanced thermostability of combustion-derived BaMgAl10O17:Eu2+ blue phosphors for solid-state lighting

NASA Astrophysics Data System (ADS)

Pradal, Nathalie; Potdevin, Audrey; Chadeyron, Geneviève; Bonville, Pierre; Caillier, Bruno; Mahiou, Rachid

2017-02-01

Blue-emitting BaMgAl10O17:Eu2+ (BAM:Eu), suitable for applications in a next generation of Hg-free lamps based on UV LEDs, was prepared by a microwave induced solution combustion synthesis, using urea as combustion fuel and nitrates as oxidizers. Purity control of the as-synthesized blue phosphor was undertaken by a washing step followed by a reduction one. Structural and morphological properties of the outcoming phosphors have been considered. Synthesis process allows producing a well-crystallized and nanostructured BAM phase within only few minutes. The influence of reduction treatment on the relative amounts of Eu2+/Eu3+ in our samples has been investigated through an original study by magnetization and Mössbauer spectroscopy. Furthermore, a complete optical study has been carried out and allowed us to determine the europium localization in the three possible sites in BAM matrix. The percentage of Eu2+ increased twofold after the reduction treatment, entailing an increase in the luminescence efficiency upon UV excitation. Finally, temperature-dependent luminescence of combustion-derived powders has been studied till 170 °C and compared to that of commercial BAM:Eu. MISCS-derived phosphors present a higher thermal stability than commercial one: whereas the emission efficiency of this last was reduced by 64%, the one of combustion-derived BAM:Eu experienced an only 12% decline. Furthermore, while commercial BAM suffered from a severe blue-shift with increasing temperature, our phosphors keep its color quality with a good stability of the photometric parameters.

Computational fluid dynamics and frequency-dependent finite-difference time-domain method coupling for the interaction between microwaves and plasma in rocket plumes

NASA Astrophysics Data System (ADS)

Kinefuchi, K.; Funaki, I.; Shimada, T.; Abe, T.

2012-10-01

Under certain conditions during rocket flights, ionized exhaust plumes from solid rocket motors may interfere with radio frequency transmissions. To understand the relevant physical processes involved in this phenomenon and establish a prediction process for in-flight attenuation levels, we attempted to measure microwave attenuation caused by rocket exhaust plumes in a sea-level static firing test for a full-scale solid propellant rocket motor. The microwave attenuation level was calculated by a coupling simulation of the inviscid-frozen-flow computational fluid dynamics of an exhaust plume and detailed analysis of microwave transmissions by applying a frequency-dependent finite-difference time-domain method with the Drude dispersion model. The calculated microwave attenuation level agreed well with the experimental results, except in the case of interference downstream the Mach disk in the exhaust plume. It was concluded that the coupling estimation method based on the physics of the frozen plasma flow with Drude dispersion would be suitable for actual flight conditions, although the mixing and afterburning in the plume should be considered depending on the flow condition.

Observations of Ball-Lightning-Like Plasmoids Ejected from Silicon by Localized Microwaves.

PubMed

Meir, Yehuda; Jerby, Eli; Barkay, Zahava; Ashkenazi, Dana; Mitchell, James Brian; Narayanan, Theyencheri; Eliaz, Noam; LeGarrec, Jean-Luc; Sztucki, Michael; Meshcheryakov, Oleg

2013-09-11

This paper presents experimental characterization of plasmoids (fireballs) obtained by directing localized microwave power (<1 kW at 2.45 GHz) onto a silicon-based substrate in a microwave cavity. The plasmoid emerges up from the hotspot created in the solid substrate into the air within the microwave cavity. The experimental diagnostics employed for the fireball characterization in this study include measurements of microwave scattering, optical spectroscopy, small-angle X-ray scattering (SAXS), scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDS). Various characteristics of these plasmoids as dusty plasma are drawn by a theoretical analysis of the experimental observations. Aggregations of dust particles within the plasmoid are detected at nanometer and micrometer scales by both in - situ SAXS and ex-situ SEM measurements. The resemblance of these plasmoids to the natural ball-lightning (BL) phenomenon is discussed with regard to silicon nano-particle clustering and formation of slowly-oxidized silicon micro-spheres within the BL. Potential applications and practical derivatives of this study (e.g., direct conversion of solids to powders, material identification by breakdown spectroscopy (MIBS), thermite ignition, and combustion) are discussed.

Universal dynamics and deterministic switching of dissipative Kerr solitons in optical microresonators

NASA Astrophysics Data System (ADS)

Guo, H.; Karpov, M.; Lucas, E.; Kordts, A.; Pfeiffer, M. H. P.; Brasch, V.; Lihachev, G.; Lobanov, V. E.; Gorodetsky, M. L.; Kippenberg, T. J.

2017-01-01

Temporal dissipative Kerr solitons in optical microresonators enable the generation of ultrashort pulses and low-noise frequency combs at microwave repetition rates. They have been demonstrated in a growing number of microresonator platforms, enabling chip-scale frequency combs, optical synthesis of low-noise microwaves and multichannel coherent communications. In all these applications, accessing and maintaining a single-soliton state is a key requirement--one that remains an outstanding challenge. Here, we study the dynamics of multiple-soliton states and report the discovery of a simple mechanism that deterministically switches the soliton state by reducing the number of solitons one by one. We demonstrate this control in Si3N4 and MgF2 resonators and, moreover, we observe a secondary peak to emerge in the response of the system to a pump modulation, an effect uniquely associated with the soliton regime. Exploiting this feature, we map the multi-stability diagram of a microresonator experimentally. Our measurements show the physical mechanism of the soliton switching and provide insight into soliton dynamics in microresonators. The technique provides a method to sequentially reduce, monitor and stabilize an arbitrary state with solitons, in particular allowing for feedback stabilization of single-soliton states, which is necessary for practical applications.

Research Investigation Directed Toward Extending the Useful Range of the Electromagnetic Spectrum. [atomic spectra and electronic structure of alkali metals

NASA Technical Reports Server (NTRS)

Hartmann, S. R.; Happer, W.

1974-01-01

The report discusses completed and proposed research in atomic and molecular physics conducted at the Columbia Radiation Laboratory from July 1972 to June 1973. Central topics described include the atomic spectra and electronic structure of alkali metals and helium, molecular microwave spectroscopy, the resonance physics of photon echoes in some solid state systems (including Raman echoes, superradiance, and two photon absorption), and liquid helium superfluidity.

Methane Synthesis from Automotive Paint Sludge via Microwave Assisted Pyrolysis

NASA Astrophysics Data System (ADS)

Rosli, N. L.; Rahman, N. Abd; Kadri, A.

2018-05-01

Methane gas, which has one atom of carbon and four atoms of hydrogen, is a valuable energy resource, which can be used in the energy sector. The purpose of this research work is to identify methane synthesis from Automotive Paint Sludge (APS) using microwave assisted pyrolysis. APS is known as a hazardous waste since it contains various chemicals that categorized as heavy metals and toxic substances. A modified conventional kitchen microwave was used to pyrolise the APS. The microwave was set with the power level of 600 W and 50 minutes radiation time. Through the experiment, pyrogas was collected into tedlar bag and was analysed using Gas Chromatography with Flame Ionization Detector (GC-FID). Results from the GC-FID were shown that the retention time of 3.3583, 3.2733, and 3.2267 min are proved to be methane gas. The results obtained are resembled with the results from the literature. This indicates methane gas was presented in the pyrogas of pyrolysis of APS and there is a possibility of producing methane gas. The research study suggests that it is possible to synthesize methane gas from the APS via microwave assisted pyrolysis, and in the meantime reduce the volume of APS in the landfill.

rGO-ZnO nanocomposites for high electrocatalytic effect on water oxidation obtained by microwave-hydrothermal method

NASA Astrophysics Data System (ADS)

Romeiro, Fernanda C.; Rodrigues, Mônica A.; Silva, Luiz A. J.; Catto, Ariadne C.; da Silva, Luis F.; Longo, Elson; Nossol, Edson; Lima, Renata C.

2017-11-01

Reduced graphene oxide-zinc oxide (rGO-ZnO) nanocomposites were successfully synthesized using a facile microwave-hydrothermal method under mild conditions, and their electrocatalytic properties towards O2 evolution were investigated. The microwave radiation played an important role in obtainment of well dispersed ZnO nanoparticles directly on reduced graphene oxide sheets without any additional reducing reagents or passivation agent. X-ray diffraction (XRD), Raman and infrared spectroscopies indicated the reduction of GO as well as the successful synthesis of rGO-ZnO nanocomposites. The chemical states of the samples were shown by XPS analyses. Due to the synergic effect, the resulting nanocomposites exhibited high electronic interaction between ZnO and rGO sheets, which improved the electrocatalytic oxidation of water with low onset potential of 0.48 V (vs. Ag/AgCl) in neutral pH and long-term stability, with high current density during electrolysis. The overpotential for water oxidation decreased in alkaline pH, suggesting useful insight on the catalytic mechanism for O2 evolution.

Deterministic transfer of an unknown qutrit state assisted by the low-Q microwave resonators

NASA Astrophysics Data System (ADS)

Liu, Tong; Zhang, Yang; Yu, Chang-Shui; Zhang, Wei-Ning

2017-05-01

Qutrits (i.e., three-level quantum systems) can be used to achieve many quantum information and communication tasks due to their large Hilbert spaces. In this work, we propose a scheme to transfer an unknown quantum state between two flux qutrits coupled to two superconducting coplanar waveguide resonators. The quantum state transfer can be deterministically achieved without measurements. Because resonator photons are virtually excited during the operation time, the decoherences caused by the resonator decay and the unwanted inter-resonator crosstalk are greatly suppressed. Moreover, our approach can be adapted to other solid-state qutrits coupled to circuit resonators. Numerical simulations show that the high-fidelity transfer of quantum state between the two qutrits is feasible with current circuit QED technology.

Enhancement of water removing and the quality of fried purple-fleshed sweet potato in the vacuum frying by combined power ultrasound and microwave technology.

PubMed

Su, Ya; Zhang, Min; Bhandari, Bhesh; Zhang, Weiming

2018-06-01

The combination of ultrasound and microwave in vacuum frying system was investigated to achieve higher drying efficiency and quality attributes of fried products. Purple-fleshed potato were used as test specimen and different power levels of microwave (0 W, 600 W, 800 W) and ultrasound (0 W, 300 W, 600 W) during vacuum frying. Drying kinetics, dielectric properties, moisture state variation and quality attributes of fried samples were measured in a vacuum frying (VF), and an innovatively designed ultrasound and microwave assisted vacuum frying (USMVF) equipment. The USMVF process markedly increased the moisture evaporation rate and effective moisture diffusivity compared to VF process. The oil uptake was reduced by about 16-34%, the water activity and the shrinkage was lowered, the texture (crispness) and the color of fried samples were greatly improved. The higher ultrasound and microwave power level in USMVF made a greater improvement. The total anthocyanin levels and retention of fried purple-fleshed potato chips was the highest (123.52 mg/100 g solids and 79.51% retention, respectively) among all treatments in US600M800VF process. The SEM analysis revealed a more porous and disruption microstructure in USMVF sample. Copyright © 2018 Elsevier B.V. All rights reserved.

Study on preparation and microwave absorption property of the core-nanoshell composite materials doped with La.

PubMed

Wei, Liqiu; Che, Ruxin; Jiang, Yijun; Yu, Bing

2013-12-01

Microwave absorbing material plays a great role in electromagnetic pollution controlling, electromagnetic interference shielding and stealth technology, etc. The core-nanoshell composite materials doped with La were prepared by a solid-state reaction method, which is applied to the electromagnetic wave absorption. The core is magnetic fly-ash hollow cenosphere, and the shell is the nanosized ferrite doped with La. The thermal decomposition process of the sample was investigated by thermogravimetry and differential thermal analysis. The morphology and components of the composite materials were investigated by the X-ray diffraction analysis, the microstructure was observed by scanning electron microscope and transmission electron microscope. The results of vibrating sample magnetometer analysis indicated that the exchange-coupling interaction happens between ferrite of magnetic fly-ash hollow cenosphere and nanosized ferrite coating, which caused outstanding magnetic properties. The microwave absorbing property of the sample was measured by reflectivity far field radar cross section of radar microwave absorbing material with vector network analyzer. The results indicated that the exchange-coupling interaction enhanced magnetic loss of composite materials. Therefore, in the frequency of 5 GHz, the reflection coefficient can achieve -24 dB. It is better than single material and is consistent with requirements of the microwave absorbing material at the low-frequency absorption. Copyright © 2013 The Research Centre for Eco-Environmental Sciences, Chinese Academy of Sciences. Published by Elsevier B.V. All rights reserved.

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.

Elucidation of the surface characteristics and electrochemistry of high-performance LiNiO 2

DOE PAGES

Xu, Jing; Lin, Feng; Nordlund, Dennis; ...

2016-02-25

Phase pure LiNiO 2 was prepared using a solid-state method and the optimal synthesis conditions led to a remarkably high capacity of 200 mA h g $-$1 with excellent retention. The combination of bulk and surface characterization elucidated an essential role of the excess Li in phase formation during synthesis and the subsequent electrochemical performance.

Rapid, Microwave-Assisted Synthesis of Cubic, Three-Dimensional, Highly Porous MOF-205 for Room Temperature CO2 Fixation via Cyclic Carbonate Synthesis.

PubMed

Babu, Robin; Roshan, Roshith; Kathalikkattil, Amal Cherian; Kim, Dong Woo; Park, Dae-Won

2016-12-14

A dual-porous, three-dimensional, metal-organic framework [Zn 4 O(2,6-NDC)(BTB) 4/3 ] (MOF-205, BET = 4200 m 2 /g) has been synthesized using microwave power as an alternative energy source for the first time, and its catalytic activity has been exploited for CO 2 -epoxide coupling reactions to produce five-membered cyclic carbonates under solvent-free conditions. Microwave synthesis was performed at different time intervals to reveal the formation of the crystals. Significant conversion of various epoxides was obtained at room temperature, with excellent selectivity toward the desired five-membered cyclic carbonates. The importance of the dual porosity and the synergistic effect of quaternary ammonium salts on efficiently catalyzed CO 2 conversion were investigated using various experimental and physicochemical characterization techniques, and the results were compared with those of the solvothermally synthesized MOF-205 sample. On the basis of literature and experimental inferences, a rationalized mechanism mediated by the zinc center of MOF-205 for the CO 2 -epoxide cycloaddition reaction has been proposed.

Microwave assisted synthesis and characterization of magnesium substituted calcium phosphate bioceramics.

PubMed

Khan, Nida Iqbal; Ijaz, Kashif; Zahid, Muniza; Khan, Abdul S; Abdul Kadir, Mohammed Rafiq; Hussain, Rafaqat; Anis-Ur-Rehman; Darr, Jawwad A; Ihtesham-Ur-Rehman; Chaudhry, Aqif A

2015-11-01

Hydroxyapatite is used extensively in hard tissue repair due to its biocompatibility and similarity to biological apatite, the mineral component of bone. It differs subtly in composition from biological apatite which contains other ions such as magnesium, zinc, carbonate and silicon (believed to play biological roles). Traditional methods of hydroxyapatite synthesis are time consuming and require strict reaction parameter control. This paper outlines synthesis of magnesium substituted hydroxyapatite using simple microwave irradiation of precipitated suspensions. Microwave irradiation resulted in a drastic decrease in ageing times of amorphous apatitic phases. Time taken to synthesize hydroxyapatite (which remained stable upon heat treatment at 900°C for 1h) reduced twelve folds (to 2h) as compared to traditionally required times. The effects of increasing magnesium concentration in the precursors on particle size, surface area, phase-purity, agglomeration and thermal stability, were observed using scanning electron microscopy, BET surface area analysis, X-ray diffraction and photo acoustic Fourier transform infra-red spectroscopy. Porous agglomerates were obtained after a brief heat-treatment (1h) at 900°C. Copyright © 2015 Elsevier B.V. All rights reserved.

MICROWAVE IRRADIATION IN BENIGN SYNTHESIS OF ORGANIC MOLECULES, NOBLE NANOMETALS AND NANOCOMPOSITES

EPA Science Inventory

A brief historic account of reactions involving microwave (MW) exposure of neat reactants or catalyzed by mineral support surfaces, such as alumina, silica, clay, or their ‘doped’ versions, for the rapid one-pot assembly of heterocyclic compounds [1] from in situ generated reacti...

A microwave assisted intramolecular-furan-Diels–Alder approach to 4-substituted indoles†

PubMed Central

Petronijevic, Filip; Timmons, Cody; Cuzzupe, Anthony; Wipf, Peter

2009-01-01

The key steps of a versatile new protocol for the convergent synthesis of 3,4-disubstituted indoles are the addition of an α-lithiated alkylaminofuran to a carbonyl compound, a microwave-accelerated intramolecular Diels–Alder cycloaddition and an in situ double aromatization reaction. PMID:19082013

GREENER ORGANIC SYNTHESES UNDER NON-TRADITIONAL CONDITIONS USING MICROWAVE AND ULTRASOUND IRRADIATION AND MECHANOCHEMICAL MIXING

EPA Science Inventory

Solvent-free mechanochemical methods that involve the use of hypervalent iodine reagents at room temperature are described for the synthesis of heterocyclic entities and conversion of ketones into -keto sulfones in high yields. A solvent-free approach that involves microwave (MW...

Mixing with microwaves: solvent-free and catalyst-free synthesis of pyrazoles and diazepines

EPA Science Inventory

A simple and facile condensation of hydrazines/hydrazides and diamines with 1,3-diketones/β-ketoester leads to the preparation of pyrazoles and diazepines in high yields. This eco-friendly protocol is accelerated by microwave heating and efficiently carried out without any r...

Microwave plasma generation of arsine from hydrogen and solid arsenic

NASA Astrophysics Data System (ADS)

Omstead, Thomas R.; Annapragada, Ananth V.; Jensen, Klavs F.

1990-12-01

The generation of arsine from the reactions of hydrogen and elemental arsenic in a microwave plasma reactor is described. The arsenic is evaporated from a solid source upstream and carried into the microwave plasma region by a mixture of hydrogen and argon. Stable reaction products, arsine and diarsine are observed by molecular beam sampled mass spectroscopy along with partially hydrogenated species (e.g., AsH and AsH2). The effect of composition and flow rate of the argon/hydrogen carrier gas mixture on the amount of arsine generated is investigated. The arsine production reaches a maximum for an argon-to-hydrogen ratio of unity indicating that metastable argon species act as energy transfer intermediates in the overall reaction. The generation of arsine and diarsine from easily handled solid arsenic by this technique makes it attractive as a possible arsenic source for the growth of compound semiconductors by low-pressure metalorganic chemical vapor deposition.

Solvothermal synthesis of selenium nano and microspheres deposited on silicon surface by microwave-assisted method

NASA Astrophysics Data System (ADS)

Ahmad, Muthanna

2016-10-01

This work describes a new application of the solvothermal method, based on the microwave heating, for the synthesis of nano and microparticles of selenium. The reaction of selenium with hydrofluoric acid on the silicon surface is induced by microwave irradiation under high pressure and temperature of 60 bar and 160 °C, respectively. This method allows the deposition of spherical-like particles on the in situ etched silicon surface. The size of deposited selenium spheres scales from tens of nanometers up to tens of micrometers. The morphology and composition of the deposited selenium were analyzed by various analytical techniques. The formation dynamic of spherical structure is explained on the base of reduction of selenium species by hydrogen inside gas bubbles which are generated on the silicon surface by the etching process.

Conventional and microwave assisted synthesis of pyrazolone Mannich bases possessing anti-inflammatory, analgesic, ulcerogenic effect and antimicrobial properties.

PubMed

Sivakumar, Kullampalayam Krishnasamy; Rajasekaran, Aiyalu; Senthilkumar, Palaniappan; Wattamwar, Prasad P

2014-07-01

In the present study, an efficient synthesis of some Mannich base of 5-methyl-2-[(2-oxo-2H-chromen-3-yl)carbonyl]-2,4-dihydro-3H-pyrazol-3-one (4a-j) have been described by using conventional and non-conventional (microwave) techniques. Microwave assisted reactions showed that require shorter reaction time and good yield. The newly synthesized compounds were screened for their anti-inflammatory, analgesic activity, antioxidant, and antibacterial effects were compared with standard drug. Among the compounds studied, compound (4f) showing nearly equipotent anti-inflammatory and analgesic activity than the standard drug (indomethacin), along with minimum ulcerogenic index. Compounds (4b and 4i) showing 1.06 times more active than ciprofloxacin against tested Gram-negative bacteria. Copyright © 2014 Elsevier Ltd. All rights reserved.

Microwave Synthesis of BCNO/SiO2 Nanocomposite Material

NASA Astrophysics Data System (ADS)

Faryuni, I. D.; Ramdhani, F.; Sampurno, J.; Nuryadin, B. W.; Noor, F. A.; Iskandar, F.

2017-07-01

In the present work, we report the preparation of BCNO/SiO2 phosphor synthesized using a microwave-assisted method. This method allows a lower temperature and a shorter reaction time than simple heating (furnace). The phosphors were prepared from precursors containing, boric acid, urea, citric acid and SiO2 nanoparticles. To These precursors, silica nanoparticles were added at various concentrations from 0 to 5 %wt. The emission wavelength produced by the phosphor was varied by varying the fraction mass of the silica that were added to the precursors. The results showed that higher photoluminescence (PL) intensity was produced by the BCNO/SiO2 with 3 %wt silica addition. The novelty of this research is using microwave heating for BCNO/SiO2 synthesis, which is usually conducted using a simple heating method.

Synthesis of high-oxidation Y-Ba-Cu-O phases in superoxygenated thin films

NASA Astrophysics Data System (ADS)

Zhang, H.; Gauquelin, N.; McMahon, C.; Hawthorn, D. G.; Botton, G. A.; Wei, J. Y. T.

2018-03-01

It is known that solid-state reaction in high-pressure oxygen can stabilize high-oxidation phases of Y-Ba-Cu-O superconductors in powder form. We extend this superoxygenation concept of synthesis to thin films which, due to their large surface-to-volume ratio, are more reactive thermodynamically. Epitaxial thin films of YBa2Cu3O7 -δ grown by pulsed laser deposition are annealed at up to 700 atm O2 and 900 ∘C , in conjunction with Cu enrichment by solid-state diffusion. The films show the clear formation of Y2Ba4Cu7O15 -δ and Y2Ba4Cu8O16 as well as regions of YBa2Cu5O9 -δ and YBa2Cu6O10 -δ phases, according to scanning transmission electron microscopy, x-ray diffraction, and x-ray absorption spectroscopy. Similarly annealed YBa2Cu3O7 -δ powders show no phase conversion. Our results demonstrate a route of synthesis towards discovering more complex phases of cuprates and other superconducting oxides.

Synthesis mechanism and preparation of LaMgAl11O19 powder for plasma spraying

NASA Astrophysics Data System (ADS)

He, Mingtao; Meng, Huimin; Wang, Yuchao; Ren, Pengwei

2018-06-01

Lanthanide magnesium hexaaluminate (LaMgAl11O19) powders were successfully synthesized by the solid-state reaction method. The objective of this study was to investigate the synthesis mechanism of LaMgAl11O19 and prepare LaMgAl11O19 powders suitable for plasma spraying. The results show that LaAlO3 reacts with MgAl2O4 and Al2O3 to form LaMgAl11O19 at approximately 1300 °C. Single-phase LaMgAl11O19 powders were prepared successfully by solid-state reaction at a synthesis temperature of 1600 °C for 6 h. Unlike the particles in the synthesized powders, those of the centrifugally spray-dried powders have a spherical shape with uniform granularity and good flowability, density, and particle size distribution, making them suitable for plasma spraying. The synthesized powders and centrifugally spray-dried powders remained as a single phase after heat treatment at 1300 °C for 100 h, indicating that LaMgAl11O19 has excellent high-temperature stability.

Ion conduction in crystalline superionic solids and its applications

NASA Astrophysics Data System (ADS)

Chandra, Angesh

2014-06-01

Superionic solids an area of multidisciplinary research activity, incorporates to study the physical, chemical and technological aspects of rapid ion movements within the bulk of the special class of ionic materials. It is an emerging area of materials science, as these solids show tremendous technological scopes to develop wide variety of solid state electrochemical devices such as batteries, fuel cells, supercapacitors, sensors, electrochromic displays (ECDs), memories, etc. These devices have wide range of applicabilities viz. power sources for IC microchips to transport vehicles, novel sensors for controlling atmospheric pollution, new kind of memories for computers, smart windows/display panels, etc. The field grew with a rapid pace since then, especially with regards to designing new materials as well as to explore their device potentialities. Amongst the known superionic solids, fast Ag+ ion conducting crystalline solid electrolytes are attracted special attention due to their relatively higher room temperature conductivity as well as ease of materials handling/synthesis. Ion conduction in these electrolytes is very much interesting part of today. In the present review article, the ion conducting phenomenon and some device applications of crystalline/polycrystalline superionic solid electrolytes have been reviewed in brief. Synthesis and characterization tools have also been discussed in the present review article.

Synthesis and characterization of pyrite (FeS{sub 2}) using microwave irradiation

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

Kim, Eun Jung, E-mail: ekim229@uwo.ca; Batchelor, Bill

2009-07-01

A procedure using microwave irradiation was studied to develop a fast and reliable method for synthesizing pyrite. Pyrite was successfully synthesized within a few minutes via reaction of ferric iron and hydrogen sulfide under the influence of irradiation by a conventional microwave oven. The SEM-EDX study revealed that the nucleation and growth of pyrite occurred on the surface of elemental sulfur, where polysulfides are available. Compared to conventional heating, using microwave energy results in rapid (<1 min) formation of smaller particulates of pyrite. Higher levels of microwave power can form pyrite even faster, but faster reaction can lead to themore » formation of pyrite with defects.« less

A novel class of halogen-free, super-conductive lithium argyrodites: Synthesis and characterization

NASA Astrophysics Data System (ADS)

Schneider, Holger; Du, Hui; Kelley, Tracy; Leitner, Klaus; ter Maat, Johan; Scordilis-Kelley, Chariclea; Sanchez-Carrera, Roel; Kovalev, Igor; Mudalige, Anoma; Kulisch, Jörn; Safont-Sempere, Marina M.; Hartmann, Pascal; Weiβ, Thomas; Schneider, Ling; Hinrichsen, Bernd

2017-10-01

Solid electrolytes are the core components for many next generation lithium battery concepts such as all-solid-state batteries (ASSB) or batteries based on metallic lithium anodes protected by a ceramic or composite passivation layer. Therefore, the search for new solid state Li-ion conductors with superior properties and improved electrochemical stabilities remains of high interest. In this work, the synthesis of a new class of silicon-containing, sulfide-based lithium-ion conductors is reported. Very good conductivities of up to ∼2.0-3.0·10-3 S/cm could be achieved for compositions such as Li22SiP2S18, among the highest for silicon sulfide containing materials. Based on the recorded powder XRD diffraction patterns and simulations it could be confirmed that they constitute novel members of the argyrodite family of sulfide lithium-ion conductors. The cubic high-temperature modification of such argyrodites with high lithium-ion conductivity can therefore be stabilized by implementation of silicon into the lattice, while additional doping with halogen atoms is not necessary.

Modulation of surface structure and catalytic properties of cerium oxide nanoparticles by thermal and microwave synthesis techniques

NASA Astrophysics Data System (ADS)

He, Jian; Zhou, Lan; Liu, Jie; Yang, Lu; Zou, Ling; Xiang, Junyu; Dong, Shiwu; Yang, Xiaochao

2017-04-01

Cerium oxide nanoparticles (CNPs) have been intensively explored for biomedical applications in recent few years due to the versatile enzyme mimetic activities of the nanoparticles. However, the control of CNPs quality through the optimization of synthesis conditions remains largely unexplored as most of the previous studies only focus on utilizing the catalytic activities of the nanoparticles. In the present study, CNPs with size about 5 nm were synthesized by thermal decomposition method using traditional convective heating and recently developed microwave irradiation as heating source. The quality of CNPs synthesized by the two heating manner was evaluated. The CNPs synthesized by convective heating were slightly smaller than that synthesized by microwave irradiation heating. The cores of the CNPs synthesized by the two heating manner have similar crystal structure. While the surface subtle structures of the CNPs synthesized by two heating manner were different. The CNPs synthesized by microwave irradiation have more surface reactive hot spot than that synthesized by convective heating as the nanoparticles responded more actively to the redox environment variation. This difference resulted in the higher superoxide dismutase (SOD) mimetic activity of CNPs synthesized by microwave irradiation heating than that of the convective heating. Preliminary experiments indicated that the CNPs synthesized by microwave irradiation heating could better protect cells from oxidative stress due to the higher SOD mimetic activity of the nanoparticles.

Rapid, facile microwave-assisted synthesis of xanthan gum grafted polyaniline for chemical sensor.

PubMed

Pandey, Sadanand; Ramontja, James

2016-08-01

Grafting method, through microwave radiation procedure is extremely productive in terms of time consumption, cost effectiveness and environmental friendliness. In this study, conductive and thermally stable composite (mwXG-g-PANi) was synthesized by grafting of aniline (ANi) on to xanthan gum (XG) using catalytic weight of initiator, ammonium peroxydisulfate in the process of microwave irradiation in an aqueous medium. The synthesis of mwXG-g-PANi were confirm by FTIR, XRD, TGA, and SEM. The influence of altering the microwave power, exposure time of microwave, concentration of monomer and the amount of initiator of graft polymerization were studied over the grafting parameters, for example, grafting percentage (%G) and grafting efficiency (%E). The maximum %G and %E achieved was 172 and 74.13 respectively. The outcome demonstrates that the microwave irradiation strategy can increase the reaction rate by 72 times over the conventional method. Electrical conductivity of XG and mwXG-g-PANi composite film was performed. The fabricated grafted sample film were then examined for the chemical sensor. The mwXG-g-PANi, effectively integrated and handled, are NH3 sensitive and exhibit a rapid sensing in presence of NH3 vapor. Chemiresistive NH3 sensors with superior room temperature sensing performance were produced with sensor response of 905 at 1ppb and 90% recovery within few second. Copyright © 2016 Elsevier B.V. All rights reserved.

Greener Syntheses and Chemical Transformations Using SustainableAlternative Methods and Nano-Catalysts

EPA Science Inventory

The presentation summarizes our sustainable chemical synthesis activity involving benign alternatives, namely greener reaction medium in aqueous or solventfree conditions and using alternative activation via microwave or photocatalytic activation. Eco-friendly synthesis of nanoma...

Optical vector network analysis of ultranarrow transitions in 166Er3+ : 7LiYF4 crystal.

PubMed

Kukharchyk, N; Sholokhov, D; Morozov, O; Korableva, S L; Cole, J H; Kalachev, A A; Bushev, P A

2018-02-15

We present optical vector network analysis (OVNA) of an isotopically purified Er166 3+ :LiYF 4 7 crystal. The OVNA method is based on generation and detection of a modulated optical sideband by using a radio-frequency vector network analyzer. This technique is widely used in the field of microwave photonics for the characterization of optical responses of optical devices such as filters and high-Q resonators. However, dense solid-state atomic ensembles induce a large phase shift on one of the optical sidebands that results in the appearance of extra features on the measured transmission response. We present a simple theoretical model that accurately describes the observed spectra and helps to reconstruct the absorption profile of a solid-state atomic ensemble as well as corresponding change of the refractive index in the vicinity of atomic resonances.

Ka-Band Wide-Bandgap Solid-State Power Amplifier: Hardware Validation

NASA Technical Reports Server (NTRS)

Epp, L.; Khan, P.; Silva, A.

2005-01-01

Motivated by recent advances in wide-bandgap (WBG) gallium nitride (GaN) semiconductor technology, there is considerable interest in developing efficient solid-state power amplifiers (SSPAs) as an alternative to the traveling-wave tube amplifier (TWTA) for space applications. This article documents proof-of-concept hardware used to validate power-combining technologies that may enable a 120-W, 40 percent power-added efficiency (PAE) SSPA. Results in previous articles [1-3] indicate that architectures based on at least three power combiner designs are likely to enable the target SSPA. Previous architecture performance analyses and estimates indicate that the proposed architectures can power combine 16 to 32 individual monolithic microwave integrated circuits (MMICs) with >80 percent combining efficiency. This combining efficiency would correspond to MMIC requirements of 5- to 10-W output power and >48 percent PAE. In order to validate the performance estimates of the three proposed architectures, measurements of proof-of-concept hardware are reported here.

Sub-100 attosecond timing jitter from low-noise passively mode-locked solid-state laser at telecom wavelength.

PubMed

Portuondo-Campa, E; Paschotta, R; Lecomte, S

2013-08-01

We report on the ultralow timing jitter of the 100 MHz pulse trains generated by two identical passively mode-locked diode-pumped solid-state lasers (DPSSLs) emitting at 1556 nm. Ultralow timing jitter of 83 as (integrated from 10 kHz to 50 MHz) for one laser has been measured with a balanced optical cross-correlator as timing discriminator. Extremely low intensity noise has been measured as well. Several measurement techniques have been used and show similar jitter results. Different possible noise sources have been theoretically investigated and compared to the measured jitter power spectral density. It is found that although the measured integrated jitter is quite low, it is still significantly above the quantum limit in the considered frequency span. Therefore, there is a substantial potential for technical improvements that could make passively mode-locked DPSSL outperform fiber lasers as source of microwaves with low phase noise.

Advances in Molecular Rotational Spectroscopy for Applied Science

NASA Astrophysics Data System (ADS)

Harris, Brent; Fields, Shelby S.; Pulliam, Robin; Muckle, Matt; Neill, Justin L.

2017-06-01

Advances in chemical sensitivity and robust, solid-state designs for microwave/millimeter-wave instrumentation compel the expansion of molecular rotational spectroscopy as research tool into applied science. It is familiar to consider molecular rotational spectroscopy for air analysis. Those techniques for molecular rotational spectroscopy are included in our presentation of a more broad application space for materials analysis using Fourier Transform Molecular Rotational Resonance (FT-MRR) spectrometers. There are potentially transformative advantages for direct gas analysis of complex mixtures, determination of unknown evolved gases with parts per trillion detection limits in solid materials, and unambiguous chiral determination. The introduction of FT-MRR as an alternative detection principle for analytical chemistry has created a ripe research space for the development of new analytical methods and sampling equipment to fully enable FT-MRR. We present the current state of purpose-built FT-MRR instrumentation and the latest application measurements that make use of new sampling methods.

A novel synthesis of (E)-3-methylthio-3-substituted arylamino-2-cyanoacrylates under microwave irradiation.

PubMed

Ouyang, Guiping; Song, Baoan; Zhang, Huiping; Yang, Song; Jin, Linhong; Li, Qianzhu; Hu, Deyu

2005-10-31

A facile synthesis of 3-methylthio-3-arylamino-2-cyanoacrylates from 3,3-dimethylthioacrylate and aromatic amines or amino pyridines has been achieved in moderate to high yields (64.0% ~ 93.5%) in 30 minutes at 50 degrees C under microwave irradiation. This method is very simple and the reaction conditions are mild, environmentally friendly and more importantly, quick. In the 3-(4,5-dimethylthiazol- 2-yl)-2,5-diphenyltetrazolium bromide (MTT) test, some of the title compounds were found to possess good antiproliferation activity towards PC3 cells.