Solvothermal fabrication of activated semi-coke supported TiO2-rGO nanocomposite photocatalysts and application for NO removal under visible light

NASA Astrophysics Data System (ADS)

Yang, Weiwei; Li, Chunhu; Wang, Liang; Sun, ShengNan; Yan, Xin

2015-10-01

The photocatalysts of activated semi-coke supported TiO2-rGO nanocomposite (TiO2-rGO/ASC) with different contents of reduced graphene oxide were fabricated by one-step solvothermal method for NO removal under visible light irradiation. It was confirmed that 8% content of reduced graphene oxide presented the best NO photooxidation performance under visible light irradiation at 70 °C with 350-400 mg/m3 NO,5% O2 and 5% relative humidity. The reasons for improved activity were discussed, alloyed with the mechanism of producing CO. Detailed structural information of TiO2-rGO/ASC photocatalysts was characterized by scanning electron microscope (SEM), energy dispersive X-ray Spectroscopy (EDX), X-ray diffraction analysis (XRD), UV-Vis diffuse reflectance spectra (UV-Vis DRS) and photoluminescence (PL), which indicated that the introduction of rGO was responsible for well dispersion, smaller crystalline size, red shift of absorption band and suppressing quick photo-induced charges recombination of TiO2-rGO/ASC photocatalysts. Optimization of operational parameters with 70 °C, 8% O2 and 8% relative humidity were also obtained. Deactivation of TiO2-rGO/ASC photocatalysts for NO removal was investigated by Fourier-transform infrared (FTIR) analysis. Regeneration experiments showed that thermal vapor regeneration would be optimal method owing to excellent regenerative capacity and inexpensive procedure.

Low-temperature solvothermal approach to the synthesis of La4Ni3O8 by topotactic oxygen deintercalation.

PubMed

Blakely, Colin K; Bruno, Shaun R; Poltavets, Viktor V

2011-07-18

A chimie douce solvothermal reduction method is proposed for topotactic oxygen deintercalation of complex metal oxides. Four different reduction techniques were employed to qualitatively identify the relative reduction activity of each including reduction with H(2) and NaH, solution-based reduction using metal hydrides at ambient pressure, and reduction under solvothermal conditions. The reduction of the Ruddlesden-Popper nickelate La(4)Ni(3)O(10) was used as a test case to prove the validity of the method. The completely reduced phase La(4)Ni(3)O(8) was produced via the solvothermal technique at 150 °C--a lower temperature than by other more conventional solid state oxygen deintercalation methods.

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.

Well-crystallized mesoporous TiO2 shells for enhanced photocatalytic activity: prepared by carbon coating and silica-protected calcination.

PubMed

Zhang, Zewu; Zhou, Yuming; Zhang, Yiwei; Zhou, Shijian; Shi, Junjun; Kong, Jie; Zhang, Sicheng

2013-04-14

Mesoporous anatase-phase TiO2 hollow shells were successfully fabricated by the solvothermal and calcination process. This method involves preparation of SiO2@TiO2 core-shell colloidal templates, sequential deposition of carbon and then silica layers through solvothermal and sol-gel processes, crystallization of TiO2 by calcination and finally removal of the inner and outer silica to produce hollow anatase TiO2 shells. The prepared samples were characterized by transmission electron microscopy, X-ray diffraction, N2 adsorption-desorption isotherms and UV-vis absorption spectroscopy. The results show that a uniform carbon layer is coated on the core-shell particles through the solvothermal process. The combustion of carbon offers the space for the TiO2 to further grow into large crystal grains, and the outer silica layer serves as a barrier against the excessive growth of anatase TiO2 nanocrystals. Furthermore, the initial crystallization of TiO2 generated in the carbon coating step and the heat generated by the combustion of the carbon layer allow the crystallization of TiO2 at a relatively low temperature without changing the uniform structure. When used as photocatalysts for the oxidation decomposition of Rhodamine B in aqueous solution under UV irradiation, the hollow TiO2 shells showed enhanced catalytic activity. Moreover, the TiO2 hollow shells prepared with optimal crystallinity by this method showed a higher performance than commercial P25 TiO2.

Solvothermal method as a green chemistry solution for micro-encapsulation of phase change materials for high temperature thermal energy storage

NASA Astrophysics Data System (ADS)

Tudor, Albert Ioan; Motoc, Adrian Mihail; Ciobota, Cristina Florentina; Ciobota, Dan. Nastase; Piticescu, Radu Robert; Romero-Sanchez, Maria Dolores

2018-05-01

Thermal energy storage systems using phase change materials (PCMs) as latent heat storage are one of the main challenges at European level in improving the performances and efficiency of concentrated solar power energy generation due to their high energy density. PCM with high working temperatures in the temperature range 300-500 °C are required for these purposes. However their use is still limited due to the problems raised by the corrosion of the majority of high temperature PCMs and lower thermal transfer properties. Micro-encapsulation was proposed as one method to overcome these problems. Different micro-encapsulation methods proposed in the literature are presented and discussed. An original process for the micro-encapsulation of potassium nitrate as PCM in inorganic zinc oxide shells based on a solvothermal method followed by spray drying to produce microcapsules with controlled phase composition and distribution is proposed and their transformation temperatures and enthalpies measured by differential scanning calorimetry are presented.

Structural, optical and magnetic studies of CuFe2O4, MgFe2O4 and ZnFe2O4 nanoparticles prepared by hydrothermal/solvothermal method

NASA Astrophysics Data System (ADS)

Kurian, Jessyamma; Mathew, M. Jacob

2018-04-01

In this paper we report the structural, optical and magnetic studies of three spinel ferrites namely CuFe2O4, MgFe2O4 and ZnFe2O4 prepared in an autoclave under the same physical conditions but with two different liquid medium and different surfactant. We use water as the medium and trisodium citrate as the surfactant for one method (Hydrothermal method) and ethylene glycol as the medium and poly ethylene glycol as the surfactant for the second method (solvothermal method). The phase identification and structural characterization are done using XRD and morphological studies are carried out by TEM. Cubical and porous spherical morphologies are obtained for hydrothermal and solvothermal process respectively without any impurity phase. The optical studies are carried out using FTIR and UV-Vis reflectance spectra. In order to elucidate the nonlinear optical behaviour of the prepared nanomaterial, open aperture z-scan technique is used. From the fitted z-scan curves nonlinear absorption coefficient and the saturation intensity are determined. The magnetic characterization of the samples is performed at room temperature using vibrating sample magnetometer measurements. The M-H curves obtained are fitted using theoretical equation and the different components of magnetization are determined. Nanoparticles with high saturation magnetization are obtained for MgFe2O4 and ZnFe2O4 prepared under solvothermal reaction. The magnetic hyperfine parameters and the cation distribution of the prepared materials are determined using room temperature Mössbauer spectroscopy. The fitted spectra reveal the difference in the magnetic hyperfine parameters owing to the change in size and morphology.

Ultrasonication of Bismuth Telluride Nanocrystals Fabricated by Solvothermal Method

NASA Technical Reports Server (NTRS)

Chu, Sang-Hyon; Choi, Sang H.; Kim, Jae-Woo; King, Glen C.; Elliott, James R.

2006-01-01

The objective of this study is to evaluate the effect of ultrasonication on bismuth telluride nanocrystals prepared by solvothermal method. In this study, a low dimensional nanocrystal of bismuth telluride (Bi2Te3) was synthesized by a solvothermal process in an autoclave at 180 C and 200 psi. During the solvothermal reaction, organic surfactants effectively prevented unwanted aggregation of nanocrystals in a selected solvent while controlling the shape of the nanocrystal. The atomic ratio of bismuth and tellurium was determined by energy dispersive spectroscopy (EDS). The cavitational energy created by the ultrasonic probe was varied by the ultrasonication process time, while power amplitude remained constant. The nanocrystal size and its size distribution were measured by field emission scanning electron microscopy (FESEM) and a dynamic light scattering system. When the ultrasonication time increased, the average size of bismuth telluride nanocrystal gradually increased due to the direct collision of nanocrystals. The polydispersity of the nanocrystals showed a minimum when the ultrasonication was applied for 5 min. Keywords: bismuth telluride, nanocrystal, low-dimensional, ultrasonication, solvothermal

One-pot solvothermal synthesis of ordered intermetallic Pt2In3 as stable and efficient electrocatalyst towards direct alcohol fuel cell application

NASA Astrophysics Data System (ADS)

Jana, Rajkumar; Peter, Sebastian C.

2016-10-01

Ordered intermetallic Pt2In3 nanoparticles have been synthesized by superhydride reduction of K2PtCl4 and InCl3.xH2O precursors using facile, one-pot solvothermal method. We report surfactant free solvothermal synthesis of a novel ordered Pt2In3 intermetallic nanoparticles for the first time. The structure and morphology of the catalyst has been confirmed by powder X-ray diffraction, transmission electron microscopy, field emission scanning electron microscopy, energy-dispersive spectrometry and X-ray photoelectron spectroscopy. The electrocatalytic properties of the catalysts have been investigated by cyclic voltammetry and chronoamperometry. The as prepared Pt2In3 catalyst exhibit far superior electrocatalytic activity and stability towards alcohol oxidation over commercial Pt/C. The specific activity of as synthesized catalyst was found to be 3.2 and 2.3 times higher than commercial Pt/C for methanol and ethanol oxidation, respectively. This improved activity and durability of the Pt2In3 nanoparticles can make the catalyst an ideal catalyst candidate for direct alcohol fuel cell.

The effect of precursor on the optical properties of carbon quantum dots synthesized by hydrothermal/solvothermal method

NASA Astrophysics Data System (ADS)

Mozdbar, Afsaneh; Nouralishahi, Amideddin; Fatemi, Shohreh; Mirakhori, Ghazaleh

2018-01-01

In the recent decade, Carbon Quantum Dots (CQDs) have attracted lots of attention due to their excellent properties such as tunable photoluminescence, high chemical stability, low toxicity, and biocompatibility. Among all synthesis methods, the hydrothermal/solvothermal rout has been considered as one of the most common and simplest method. The type of precursors can affect the size of CQDs and determine their surface functional groups, the essential properties that deeply influence the optical specifications. In this work, the effect of different precursors on the final properties of carbon quantum dots is investigated. The carbon quantum dots were synthesized by hydrothermal/solvothermal rout using citric acid, thiourea, ethylamine and monoethanolamine as precursors in almost the same conditions of time and temperature. Resultant CQDs were characterized by using FTIR, UV-Visible Spectroscopy and Photoluminescence (PL) analysis. The results of UV-Vis spectroscopy showed that quantum dots synthesized from monoethanolamine have wider absorption band rather than the CQDs from other precursors and the absorption edge shifted from about 270 nm for ethylamine to about 470 nm in monoethanolamine. Furthermore, the results demonstrate that using citric acid and monoethanolamine as precursor improved production efficiency and emission quantum yield of the carbon dots.

Facile preparation of porous carbon from coffee bean waste using low temperature solvothermal method

NASA Astrophysics Data System (ADS)

Baroroh, L. A. Al; Fitria, D.; Amal, M. I.; Wismogroho, A. S.; Widayatno, W. B.

2018-03-01

In this study, porous carbon made from coffee bean waste (CBW) was carbonized at 500 °C, 600 °C, and 700 °C to find effective temperature. It is verified from the IR spectrum that carbonization process at certain temperature can effectively break cellulose bonding and make aromatics functional group while preserving its carbon structure. The TG-DTA curve shows four stages of decomposition process and confirms most effective carbonization temperature. Activation process of as-carbonized CBW was carried out using solvothermal method in KOH and NH4OH steam environment at 200 °C with variation of 30%, 40%, and 50% solvothermal volume. Scanning electron micrographs reveals significant increase of porosity on the carbon surface and differences of structural pores between the variations. The results show the possible potential of utilizing low temperature-solvothermal method for nanoporous carbon material.

MOF-derived hierarchical double-shelled NiO/ZnO hollow spheres for high-performance supercapacitors.

PubMed

Li, Guo-Chang; Liu, Peng-Fei; Liu, Rui; Liu, Minmin; Tao, Kai; Zhu, Shuai-Ru; Wu, Meng-Ke; Yi, Fei-Yan; Han, Lei

2016-09-14

Nanorods-composed yolk-shell bimetallic-organic frameworks microspheres are successfully synthesized by a one-step solvothermal method in the absence of any template or surfactant. Furthermore, hierarchical double-shelled NiO/ZnO hollow spheres are obtained by calcination of the bimetallic organic frameworks in air. The NiO/ZnO hollow spheres, as supercapacitor electrodes, exhibit high capacitance of 497 F g(-1) at the current density of 1.3 A g(-1) and present a superior cycling stability. The superior electrochemical performance is believed to come from the unique double-shelled NiO/ZnO hollow structures, which offer free space to accommodate the volume change during the ion insertion and desertion processes, as well as provide rich electroactive sites for the electrochemical reactions.

Optimization on electrochemical synthesis of HKUST-1 as candidate catalytic material for Green diesel production

NASA Astrophysics Data System (ADS)

Lestari, W. W.; Nugraha, R. E.; Winarni, I. D.; Adreane, M.; Rahmawati, F.

2016-04-01

In the effort to support the discovery of new renewable energy sources in Indonesia, biofuel is one of promising options. The conversion of vegetable oil into ready-biofuel, especially green diesel, needs several steps, one of which is a hydrogenation or hydro-deoxygenation reaction. In this case, the catalyst plays a very important role regarding to its activity and selectivity, and Metal-Organic Frameworks (MOFs) becoming a new generation of heterogeneous catalyst in this area. In this research, a preliminary study to optimize electrochemical synthesis of the catalytic material based on MOFs, namely HKUST-1 [Cu3(BTC)2], has been conducted. Some electrochemical reaction parameters were tested, for example by modifying the electrochemical synthetic conditions, i.e. by performing variation of voltages (12, 13, 14, and 15 Volt), temperatures (RT, 40, 60, and 80 °C) and solvents (ethanol, water, methanol and dimethyl-formamide (DMF)). Material characterization was carried out by XRD, SEM, FTIR, DTA/TG and SAA. The results showed that the optimum synthetic conditions of HKUST-1 are performed at room temperature in a solvent combination of water: ethanol (1: 1) and a voltage of 15 Volt for 2 hours. The XRD-analysis revealed that the resulted peaks are identical to the simulated powder pattern generated from single crystal data and comparable to the peaks of solvothermal method. However, the porosity of the resulting material through electrochemical method is still in the range of micro-pore according to IUPAC and 50% smaller than the porosity resulted from solvothermal synthesis. The corresponding compounds are thermally stable until 300 °C according to TG/DTA.

One-Pot Solvothermal Synthesis of Bi4V2O11 as A New Solar Water Oxidation Photocatalyst

PubMed Central

Jiang, Zaiyong; Liu, Yuanyuan; Li, Mengmeng; Jing, Tao; Huang, Baibiao; Zhang, Xiaoyang; Qin, Xiaoyan; Dai, Ying

2016-01-01

Bi4V2O11 was prepared via a one-pot solvothermal method and characterized via XRD, Raman, XPS, Electrochemical impedance spectroscopy. The as-prepared Bi4V2O11 sample displays excellent photocatalytic activity towards oxygen evolution under light irradiation. The hierarchical structure is in favour of the spatial separation of photogenerated electrons and holes. Furthermore, the internal polar field also plays a role in improving the charge separation. Both of the two results are responsible for excellent activity of O2 evolution. The resulting hierarchical Bi4V2O11 sample should be very promising photocatalyst for the application of photocatalytic O2 evolution in the future. PMID:26947126

Fabrication of selectively functionalized-graphene reinforced copper phthalocyanine nanocomposites with low dielectric loss and high dielectric constant

NASA Astrophysics Data System (ADS)

Wang, Zicheng; Wei, Renbo; Liu, Xiaobo

2017-01-01

A novel kind of selectively functionalized-graphene reinforced copper phthalocyanine (RGO-O-CuPc) nanocomposites was successfully fabricated through a facile and effective three-step method, involving preferential surficial modification and reduction of graphene oxide (GO) sheets, and followed by incorporating with CuPc via in situ polymerization. The results of SEM, AFM, XPS, FTIR, XRD and UV-vis confirmed that GO was effectively surficial functionalized by a ring-open covalent reaction between amino in 3-aminophenoxyphthalonitrile (3-APN) and epoxy groups on the GO sheets, and partly reduced back to graphene under solvothermal conditions. And the RGO-O-CuPc was successfully fabricated by self-assembling of CuPc molecule on graphene sheets via in situ polymerization. As a consequence, the selective surface functionalization and solvothermal reduction of GO facilitated the improvement in the dielectric constant and AC conductivity, and the decrease in the dielectric loss of the graphene/CuPc nanocomposites.

Sea-urchin-like Fe3O4@C@Ag particles: an efficient SERS substrate for detection of organic pollutants

NASA Astrophysics Data System (ADS)

Ye, Yingjie; Chen, Jin; Ding, Qianqian; Lin, Dongyue; Dong, Ronglu; Yang, Liangbao; Liu, Jinhuai

2013-06-01

Ag-coated sea-urchin-like Fe3O4@C core-shell particles can be synthesized by a facile one-step solvothermal method, followed by deposition of high-density Ag nanoparticles onto the carbon surface through an in situ growth process, respectively. The as-synthesized Ag-coated Fe3O4@C particles can be used as a surface-enhanced Raman scattering (SERS) substrate holding reproducible properties under an external magnetic force. The magnetic function of the particles allows concentrating the composite particles into small spatial regions, which can be exploited to decrease the amount of material per analysis while improving its SERS detection limit. In contrast to the traditional SERS substrates, the present Fe3O4@C@Ag particles hold the advantages of enrichment of organic pollutants for improving SERS detection limit and recycled utilization.Ag-coated sea-urchin-like Fe3O4@C core-shell particles can be synthesized by a facile one-step solvothermal method, followed by deposition of high-density Ag nanoparticles onto the carbon surface through an in situ growth process, respectively. The as-synthesized Ag-coated Fe3O4@C particles can be used as a surface-enhanced Raman scattering (SERS) substrate holding reproducible properties under an external magnetic force. The magnetic function of the particles allows concentrating the composite particles into small spatial regions, which can be exploited to decrease the amount of material per analysis while improving its SERS detection limit. In contrast to the traditional SERS substrates, the present Fe3O4@C@Ag particles hold the advantages of enrichment of organic pollutants for improving SERS detection limit and recycled utilization. Electronic supplementary information (ESI) available: Additional XRD patterns and SEM images of Fe3O4@C particles, SERS spectra of 4-ATP and 4-MPY using Fe3O4@C@Ag particles as the active substrates, magnetic behaviour of Fe3O4@C and Fe3O4@C@Ag particles. See DOI: 10.1039/c3nr01273e

Cobalt-based metal organic framework with superior lithium anodic performance

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

Hu, Xiaoshi; Hu, Huiping; Li, Chao

The reversible charging of a Co-1,4-benzenedicarboxylate MOF (Co-BDC MOF) prepared via an one-pot solvothermal method was studied for use as the anode in a Li-ion cell. It was found that this MOF anode provides high reversible capacities (1090 and 611 mA h g{sup −1} at current densities of 0.2 and 1 A g{sup −1}, respectively), and an impressive rate performance. Such an outstanding Li-ion storage property has not been reported previously for the LIB anodes within the MOFs category. Ex-situ X-ray photoelectron spectroscopy (XPS) and infrared spectroscopy (IR) studies of this material at different state of charge suggest that cobaltmore » stays at Co{sup 2+} state during discharge/charge process, so that in this case Li{sup +} may be inserted into the organic moiety without the direct participation of cobalt ions. - Graphical abstract: Co-1,4-benzenedicarboxylate MOF, synthesized through a straightforward solvothermal method, shows outstanding lithium storage performance. - Highlights: • Co-1,4-benzenedicarboxylate MOF is synthesized by a one-pot solvothermal method. • Reversible capacity of 1090 mA h g{sup −1} is achieved at a current density of 200 mA g{sup −1}. • Reversible capacity of 611 mA h g{sup −1} is achieved at a current density of 1 A g{sup −1}. • Li-ions may be inserted into the organic moieties.« less

One-pot engineering TiO2/graphene interface for enhanced adsorption and photocatalytic degradation of multiple organics.

PubMed

Song, Jianhua; Ling, Yun; Xie, Yu; Liu, Lianjun; Zhu, Huihua

2018-06-13

It is challenging to design a multifunctional structure or composite for simultaneously adsorb and photocatalytic degrade organic pollutants in water. Towards this goal, this work innovatively engineered interfacial sites between TiO2 particles and reduced graphene oxide (RGO) sheets by employing in situ one-pot one-step solvothermal method. The interface was associated with the content of RGO, solvothermal time and solvent ratio of n-pentanol to n-hexane. It was found that when at a moderate amount of RGO (25%), TiO2 nanoparticles were well dispersed on the surface of RGO or wrapped by RGO, thus leading to a fully contact and strong interaction to form Ti - O - C interfacial structure. But when at a low content of RGO (6%), TiO2 aggregates were mixture of nanosheets, nanoparticles and nanorods. 25%RGO/TiO2 also had 175% higher surface area (146m2/g), 95% larger volume (0.339 cm3/g) and smaller band gap than 6%RGO/TiO2. More importantly, 25%RGO/TiO2 demonstrated higher adsorption efficiency (25%) and 4 times faster degradation rate than TiO2 (0%). It also exhibited good capability to eliminate multiple organics and stable long-term cycle performance (up to 93% retention after 30 cycles). Its superiority was attributed to the large surface area and unique interface between TiO2 and RGO, which not only provided more active sites to capture pollutants but also enhanced charge transfer (3 µA/cm2, 5 times higher than TiO2). This work offered a promising way to purify water through engineering new materials structure and integrating adsorption and photodegradation technologies. © 2018 IOP Publishing Ltd.

Influence of reaction time on the structural, optical and electrical performance of copper antimony sulfide nanoparticles using solvothermal method

NASA Astrophysics Data System (ADS)

John, Bincy; Genifer Silvena, G.; Leo Rajesh, A.

2018-05-01

The less toxic and cost effective ternary Cu-Sb-S nanoparticles and thin films were synthesized and deposited using solvothermal and drop casting method. The reactions were carried out at different timings as 12-48 h, in steps of 12 h using ethylene glycol as solvent and polyvinylpyrrolidone (PVP) as surfactant. Systematic analysis revealed that due to the influence of different reaction time, significant and unique changes were occurring on the crystal structure, optical and electrical properties of the material. The synthesized nanopowders and deposited films were characterized by means of X-ray diffraction, Raman analysis, field emission scanning electron microscope with energy dispersive spectrometer, UV-Vis-NIR diffuse reflectance spectroscopy and hall measurement. XRD results showed that as the time increases crystallinity improves and phase transformation from chalcostibite to tetrahedrite occurs. The Optical performance revealed that the bandgap of nanoparticles were in the range of 1.21-1.49 eV. Hall measurements showed that the deposited Cu12Sb4S13 and CuSbS2 films exhibited p-type conductivity with carrier concentration ranging from 1016-1019 cm-3, indicating a promising p-type absorber material for photovoltaic applications.

Solvothermal synthesis of Bi2O3/BiVO4 heterojunction with enhanced visible-light photocatalytic performances

NASA Astrophysics Data System (ADS)

Ying, Wu; Jing, Wang; Yunfang, Huang; Yuelin, Wei; Zhixian, Sun; Xuanqing, Zheng; Chengkun, Zhang; Ningling, Zhou; Leqing, Fan; Jihuai, Wu

2016-08-01

Novel, three-dimensional, flower-like Bi2O3/BiVO4 heterojunction photocatalysts have been prepared by the combination of homogeneous precipitation and two-step solvothermal method followed by thermal solution of NaOH etching process. The as-obtained samples were fully characterized by X-ray diffraction, scanning electron microscopy, energy dispersive X-ray analysis, Brunauer-Emmett-Teller surface area, and UV—vis diffuse-reflectance spectroscopy in detail. The crystallinity, microstructure, specific surface area, optical property and photocatalytic activity of samples greatly changed depending on solvothermal reaction time. The photocatalytic activities of samples were evaluated on the degradation of methyl orange (MO) under visible-light irradiation. The Bi2O3/BiVO4 exhibited much higher photocatalytic activities than pure BiVO4 and conventional TiO2 (P25). The result revealed that the three-dimensional heterojunction played a critical role in the separation of the electron and hole pairs and enhancement of the interfacial charge transfer efficiency, which was responsible for the enhanced photocatalytic activity. Project supported by the National Natural Science Foundation of China (Nos. 61306077, 21301060), the Fundamental Research Funds for the Central Universities (Nos. JB-ZR1109, JB-ZR1212), the National Science Foundation of Quanzhou City (No. 2014Z108), the Promotion Program for Young and Middle-aged Teachers in Science and Technology Research of Huaqiao University (No. ZQN-PY207), Discipline Innovation Team Project of Huaqiao University (No. 201320), and the Instrumental Analysis Center Huaqiao University.

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

Observation of magnetic anomalies in one-step solvothermally synthesized nickel-cobalt ferrite nanoparticles.

PubMed

Datt, Gopal; Sen Bishwas, Mousumi; Manivel Raja, M; Abhyankar, A C

2016-03-07

Magnetic anomalies corresponding to the Verwey transition and reorientation of anisotropic vacancies are observed at 151 K and 306 K, respectively, in NiCoFe2O4 nanoparticles (NPs) synthesized by a modified-solvothermal method followed by annealing. Cationic disorder and spherical shape induced non-stoichiometry suppress the Verwey transition in the as-synthesized NPs. On the other hand, reorientation of anisotropic vacancies is quite robust. XRD and electron microscopy investigations confirm a single phase spinel structure and the surface morphology of the as-synthesized NPs changes from spherical to octahedral upon annealing. Rietveld analysis reveals that the Ni(2+) ions migrate from tetrahedral (A) to octahedral (B) sites upon annealing. The Mössbauer results show canted spins in both the NPs and the strength of superexchange is stronger in Co-O-Fe than Ni-O-Fe. Magnetic force images show that the as-synthesised NPs are single-domain whereas the annealed NPs are multi-domain octahedral particles. The FMR study reveals that both the NPs have a broad FMR line-width; and resonance properties are consistent with the random anisotropy model. The broad inhomogeneous FMR line-width, observation of the Verwey transition, tuning of the magnetic domain structure as well as the magnetic properties suggest that the NiCoFe2O4 ferrite NPs may be promising for future generation spintronics, magneto-electronics, and ultra-high-density recording media as well as for radar absorbing applications.

Ionic liquid-assisted solvothermal synthesis of hollow Mn2O3 anode and LiMn2O4 cathode materials for Li-ion batteries

NASA Astrophysics Data System (ADS)

He, Xin; Wang, Jun; Jia, Haiping; Kloepsch, Richard; Liu, Haidong; Beltrop, Kolja; Li, Jie

2015-10-01

Mn-based Mn2O3 anode and LiMn2O4 cathode materials are prepared by a solvothermal method combined with post annealing process. Environmentally friendly ionic liquid 1-Butyl-3-methylimidazolium tetrafluoroborate as both structure-directing agent and fluorine source is used to prepare hollow polyhedron MnF2 precursor. Both target materials Mn2O3 anode and LiMn2O4 cathode have the morphology of the MnF2 precursor. The Mn2O3 anode using carboxymethyl cellulose as binder could deliver slight better electrochemical performance than the one using poly (vinyldifluoride) as binder. The former has an initial charge capacity of 800 mAh g-1 at a current density of 101.8 mA g-1, and exhibits no obvious capacity decay for 150 cycles at 101.8 mA g-1. The LiMn2O4 cathode material prepared with molten salt assistant could display much better electrochemical performance than the one prepared without molten salt assistance. In particular, it has an initial discharge capacity of 117.5 mAh g-1 at a current density of 0.5C and good rate capability. In the field of lithium ion batteries, both the Mn2O3 anode and LiMn2O4 cathode materials could exhibit enhanced electrochemical performance due to the well formed morphology based on the ionic liquid-assisted solvothermal method.

Controllable synthesis of hierarchical nickel cobalt sulfide with enhanced electrochemical activity

NASA Astrophysics Data System (ADS)

Tie, Jinjin; Han, Jiaxi; Diao, Guiqiang; Liu, Jiwen; Xie, Zhuopeng; Cheng, Gao; Sun, Ming; Yu, Lin

2018-03-01

The composition of nickel cobalt sulfide has great influence on its electrochemical performance. Herein, the nickel cobalt sulfide with different composition and mixed phase were synthesized by one-step solvothermal method through changing the molar ratio of Ni to Co in the reaction system. The electrochemical measurements showed that the nickel cobalt sulfide with a theoretical molar ratio of Ni/Co to be 1.5:1.5 (NCS-2) demonstrates the superior pseudocapacitive performance with a high specific capacitance (6.47 F cm-2 at 10 mA cm-2) and a favorable Coulombic efficiency (∼99%). Whereas, when applied as the catalyst for hydrogen evolution reaction in 1 M KOH aqueous electrolyte, the nickel cobalt sulfide with a theoretical molar ratio of Ni/Co is 1:2 (NCS-1) displays better catalytic activity, and it requires a relatively lower overpotential of 282 mV to deliver the current density of 10 mA cm-2.

A strategy of combining SILAR with solvothermal process for In2S3 sensitized quantum dot-sensitized solar cells

NASA Astrophysics Data System (ADS)

Yang, Peizhi; Tang, Qunwei; Ji, Chenming; Wang, Haobo

2015-12-01

Pursuit of an efficient strategy for quantum dot-sensitized photoanode has been a persistent objective for enhancing photovoltaic performances of quantum dot-sensitized solar cell (QDSC). We present here the fabrication of the indium sulfide (In2S3) quantum dot-sensitized titanium dioxide (TiO2) photoanode by combining successive ionic layer adsorption and reaction (SILAR) with solvothermal processes. The resultant QDSC consists of an In2S3 sensitized TiO2 photoanode, a liquid polysulfide electrolyte, and a Co0.85Se counter electrode. The optimized QDSC with photoanode prepared with the help of a SILAR method at 20 deposition cycles and solvothermal method yields a maximum power conversion efficiency of 1.39%.

Solvothermal and electrochemical synthetic method of HKUST-1 and its methane storage capacity

NASA Astrophysics Data System (ADS)

Wahyu Lestari, Witri; Adreane, Marisa; Purnawan, Candra; Fansuri, Hamzah; Widiastuti, Nurul; Budi Rahardjo, Sentot

2016-02-01

A comparison synthetic strategy of Metal-Organic Frameworks, namely, Hongkong University of Techhnology-1 {HKUST-1[Cu3(BTC)]2} (BTC = 1,3,5-benzene-tri-carboxylate) through solvothermal and electrochemical method in ethanol:water (1:1) has been conducted. The obtained material was analyzed using powder X-ray diffraction, Scanning Electron Microscopy (SEM), Fourier Transform Infrared Spectroscopy (FTIR), Thermo-Gravimetric Analysis (TGA) and Surface Area Analysis (SAA). While the voltage in the electrochemical method are varied, ranging from 12 to 15 Volt. The results show that at 15 V the texture of the material has the best degree of crystallinity and comparable with solvothermal product. This indicated from XRD data and supported by the SEM image to view the morphology. The thermal stability of the synthesized compounds is up to 320 °C. The shape of the nitrogen sorption isotherm of the compound corresponds to type I of the IUPAC adsorption isotherm classification for microporous materials with BET surface area of 629.2 and 324.3 m2/g (for solvothermal and electrochemical product respectively) and promising for gas storage application. Herein, the methane storage capacities of these compounds are also tested.

Carbon-encapsulated cobalt nanoparticles: synthesis, properties, and magnetic particle hyperthermia efficiency

NASA Astrophysics Data System (ADS)

Kotoulas, A.; Dendrinou-Samara, C.; Sarafidis, C.; Kehagias, Th.; Arvanitidis, J.; Vourlias, G.; Angelakeris, M.; Kalogirou, Orestis

2017-12-01

A facile and low-cost method for structuring carbon-encapsulated cobalt nanoparticles (Co@C) is presented. Three samples were solvothermally prepared in one step at 220 °C and one in two steps at 200 °C. Three different polyols such as propylene glycol, triethylene glycol, and tetraethylene glycol were used as carbon sources, solvents, and reducing agents. The samples were characterized by X-ray powder diffraction (XRD), transmission electron microscopy (TEM), and Raman spectroscopy. Concerning the crystal structure of the particles, a mixture of hcp/ fcc Co phases was obtained in three of the samples, independently of the polyol used. The coexistence of cubic and hexagonal phases was revealed both from XRD and high-resolution TEM (HRTEM). The formation of the cubic fcc structure, despite the relatively low reaction temperature, is attributed to the role of the interface between carbon coating and metallic core. The presence of carbon coating was demonstrated by Raman spectrometry, exhibiting the characteristic D and G graphitic bands, and by HRTEM observations. All samples showed ferromagnetic behavior with saturation magnetization up to 158 emu/g and coercivity up to 206 Oe. From the magnetic particle hyperthermia measurements recorded at a frequency of 765 kHz, a maximum SLP value of 241 W/g was obtained.

A facile solvothermal synthesis of octahedral Fe 3O 4 nanoparticles

DOE PAGES

DuChene, Joseph S.; Qiu, Jingjing; Graham, Jeremy O.; ...

2015-01-26

Anisotropic Fe 3O 4 octahedrons are obtained via a simple solvothermal synthesis with appropriate sizes for various technological applications. Here, a complete suite of materials characterization methods confirms the magnetite phase for these structures, which exhibit substantial saturation magnetization and intriguing morphologies for a wide range of applications.

Growth-dissolution-regrowth transitions of Fe3O4 nanoparticles as building blocks for 3D magnetic nanoparticle clusters under hydrothermal conditions.

PubMed

Lin, Mouhong; Huang, Haoliang; Liu, Zuotao; Liu, Yingju; Ge, Junbin; Fang, Yueping

2013-12-10

Magnetic nanoparticle clusters (MNCs) are a class of secondary structural materials that comprise chemically defined nanoparticles assembled into clusters of defined size. Herein, MNCs are fabricated through a one-pot solvothermal reaction featuring self-limiting assembly of building blocks and the controlled reorganization process. Such growth-dissolution-regrowth fabrication mechanism overcomes some limitations of conventional solvothermal fabrication methods with regard to restricted available feature size and structural complexity, which can be extended to other oxides (as long as one can be chelated by EDTA-2Na). Based on this method, the nanoparticle size of MNCs is tuned between 6.8 and 31.2 nm at a fixed cluster diameter of 120 nm, wherein the critical size for superparamagnetic-ferromagnetic transition is estimated from 13.5 to 15.7 nm. Control over the nature and secondary structure of MNCs gives an excellent model system to understand the nanoparticle size-dependent magnetic properties of MNCs. MNCs have potential applications in many different areas, while this work evaluates their cytotoxicity and Pb(2+) adsorption capacity as initial application study.

Shape-controlled solvothermal synthesis of bismuth subcarbonate nanomaterials

NASA Astrophysics Data System (ADS)

Cheng, Gang; Yang, Hanmin; Rong, Kaifeng; Lu, Zhong; Yu, Xianglin; Chen, Rong

2010-08-01

Much effort has been devoted to the synthesis of novel nanostructured materials because of their unique properties and potential applications. Bismuth subcarbonate ((BiO) 2CO 3) is one of commonly used antibacterial agents against Helicobacter pylori ( H. pylori). Different (BiO) 2CO 3 nanostructures such as cube-like nanoparticles, nanobars and nanoplates, were fabricated from bismuth nitrate via a simple solvothermal method. The nanostructures were characterized by powder X-ray diffraction (XRD), scanning electron microscope (SEM), transmission electron microscopy (TEM) and high-resolution transmission electron microscopy (HRTEM). It was found that the solvents and precursors have an influence on the morphologies of (BiO) 2CO 3 nanostructures. The possible formation mechanism of different (BiO) 2CO 3 nanostructures fabricated under different conditions was also discussed.

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

Synthesis and characterization of ester and amide derivatives of titanium(IV) carboxymethylphosphonate

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

Melánová, Klára, E-mail: klara.melanova@upce.cz; Beneš, Ludvík; Trchová, Miroslava

2013-06-15

A set of layered ester and amide derivatives of titanium(IV) carboxymethylphosphonate was prepared by solvothermal treatment of amorphous titanium(IV) carboxymethylphosphonate with corresponding 1-alkanols, 1,ω-alkanediols, 1-aminoalkanes, 1,ω-diaminoalkanes and 1,ω-amino alcohols and characterized by powder X-ray diffraction, IR spectroscopy and thermogravimetric analysis. Whereas alkyl chains with one functional group form bilayers tilted to the layers, 1,ω-diaminoalkanes and most of 1,ω-alkanediols form bridges connecting the adjacent layers. In the case of amino alcohols, the alkyl chains form bilayer and either hydroxyl or amino group is used for bonding. This simple method for the synthesis of ester and amide derivatives does not require preparationmore » of acid chloride derivative as a precursor or pre-intercalation with alkylamines and can be used also for the preparation of ester and amide derivatives of titanium carboxyethylphosphonate and zirconium carboxymethylphosphonate. - Graphical abstract: Ester and amide derivatives of layered titanium carboxymethylphosphonate were prepared by solvothermal treatment of amorphous solid with alkanol or alkylamine. - Highlights: • Ester and amide derivatives of titanium carboxymethylphosphonate. • Solvothermal treatment of amorphous solid with alkanol or alkylamine. • Ester and amide formation confirmed by IR spectroscopy.« less

Solvothermal Synthesis of Magnetic Spinel Ferrites

PubMed Central

Rafienia, Mohammad; Bigham, Ashkan; Hassanzadeh-Tabrizi, Seyed Ali

2018-01-01

At present, solvothermal fabrication method has widely been applied in the synthesis of spinel ferrite nanoparticles (SFNs), which is mainly because of its great advantages such as precise control over size, shape distribution, and high crystallinity that do not require postannealing treatment. Among various SFNs, Fe3O4 nanoparticles have attracted tremendous attention because of their favorable physical and structural properties which are advantageous, especially in biomedical applications, among which the vast application of these materials as targeted drug delivery systems, hyperthermia, and imaging agents in cancer therapy can be mentioned. The main focus of this study is to present an introduction to solvothermal method and key synthesis parameters of SFNs through this synthesis route. Moreover, most recent progress on the potential applications of Fe3O4 nanoparticles as the most important compound among the spinel ferrites family members is discussed. PMID:29928636

Enhanced supercapacitive behaviour of Fe3O4/fMWCNT nanoassemblies synthesized by PEG-600 assisted solvothermal method

NASA Astrophysics Data System (ADS)

Aparna, M. L.; Sathyanarayanan, P.; Sahu, Niroj Kumar

2018-04-01

We report a simple PEG-600 assisted solvothermal method for the synthesis iron ferrite with functionalized multi-walled carbon nanotube (Fe3O4/fMWCNT) composite nanoassemblies. The results show that the composite deliver excellent electrochemical activity because of the synergistic effect of each component. The fMWCNT act as a conductive network with high surface area promoting fast movement of electrons which enhances the charge storing nature and stability of Fe3O4 nanoassemblies.

Hierarchical honeycomb-like Co3O4 pores coating on CoMoO4 nanosheets as bifunctional efficient electrocatalysts for overall water splitting

NASA Astrophysics Data System (ADS)

Pei, Zhihao; Xu, Li; Xu, Wei

2018-03-01

Efficient electrocatalytic water splitting is one of the most effective ways to solve the global energy crisis. In this paper, we report on a novel self-assembled hierarchical structure of Co3O4/CoMoO4 grown in situ on a bare nickel foam. The unique, three-dimensional honeycomb-like Co3O4 pores were constructed from one-dimensional nanowires and coated on two-dimensional CoMoO4 nanosheets structures grown on nickel foam. The synthesis involved a step-wise solvothermal method followed by an annealing treatment. Benefiting from the synergistic effect of the hierarchical nanostructures, the materials had more reaction active sites and a smaller electron transfer impedance, and they exhibited excellent electrocatalytic performances for the HER and OER of 143 and 244 mV, respectively, at 10 mA cm-2 in an alkaline solution. Furthermore, the materials remained stable during the long electrolysis period, over 10 h, presenting promising application prospects in the field of electrocatalytic water splitting.

Preparation and thermoelectric properties of sulfur doped Ag2Te nanoparticles via solvothermal methods.

PubMed

Zhou, Wenwen; Zhao, Weiyun; Lu, Ziyang; Zhu, Jixin; Fan, Shufen; Ma, Jan; Hng, Huey Hoon; Yan, Qingyu

2012-07-07

In this work, n-type Ag(2)Te nanoparticles are prepared by a solvothermal approach with uniform and controllable sizes, e.g. 5-15 nm. The usage of dodecanethiol during the synthesis effectively introduces sulfur doping into the sample, which optimizes the charge carrier concentration of the nanoparticles to >1 × 10(20) cm(-3). This allows us to achieve the desired electrical resistivities of <5 × 10(-6)Ω m. It is demonstrated that Ag(2)Te particles prepared by this solvothermal process can exhibit high ZT values, e.g. 15 nm Ag(2)Te nanoparticles with effective sulphur doping show a maximum ZT value of ~0.62 at 550 K.

Evaluation of SiO{sub 2}@CoFe{sub 2}O{sub 4} nano-hollow spheres through THz pulses

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

Rakshit, Rupali, E-mail: rupali12@bose.res.in; Pal, Monalisa; Chaudhuri, Arka

2016-05-06

We have synthesized cobalt ferrite (CFO) nanoparticles (NPs) of diameter 100 nm and nano-hollow spheres (NHSs) of diameter 100, 160, 250, and 350 nm by a facile one step template free solvothermal technique and carried out SiO{sub 2} coating on their surface following Stöber method. The phase and morphology of the nanostructures were confirmed by X-ray diffraction and transmission electron microscope. The magnetic measurements were carried out by vibrating sample magnetometer in order to study the influence of SiO{sub 2} coating on the magnetic properties of bare CFO nanostructures. Furthermore, we have applied THz time domain spectroscopy to investigate the THz absorptionmore » property of these nanostructures in the frequency range 1.0–2.5 THz. Detailed morphology and size dependent THz absorption study unfolds that the absorption property of these nanostructures sensitively carries the unique signature of its dielectric property.« less

One-Step Synthesis of Titanium Oxyhydroxy-Fluoride Rods and Research on the Electrochemical Performance for Lithium-ion Batteries and Sodium-ion Batteries.

PubMed

Li, Biao; Gao, Zhan; Wang, Dake; Hao, Qiaoyan; Wang, Yan; Wang, Yongkun; Tang, Kaibin

2015-12-01

Titanium oxyhydroxy-fluoride, TiO0.9(OH)0.9F1.2 · 0.59H2O rods with a hexagonal tungsten bronze (HTB) structure, was synthesized via a facile one-step solvothermal method. The structure, morphology, and component of the products were characterized by X-ray powder diffraction (XRD), thermogravimetry (TG), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-resolution TEM (HRTEM), inductively coupled plasma optical emission spectroscopy (ICP-OES), ion chromatograph, energy-dispersive X-ray (EDX) analyses, and so on. Different rod morphologies which ranged from nanoscale to submicron scale were simply obtained by adjusting reaction conditions. With one-dimension channels for Li/Na intercalation/de-intercalation, the electrochemical performance of titanium oxyhydroxy-fluoride for both lithium-ion batteries (LIBs) and sodium-ion batteries (SIBs) was also studied. Electrochemical tests revealed that, for LIBs, titanium oxyhydroxy-fluoride exhibited a stabilized reversible capacity of 200 mAh g(-1) at 25 mA g(-1) up to 120 cycles in the electrode potential range of 3.0-1.2 V and 140 mAh g(-1) at 250 mA g(-1) up to 500 cycles, especially; for SIBs, a high capacity of 100 mAh g(-1) was maintained at 25 mA g(-1) after 115 cycles in the potential range of 2.9-0.5 V.

Enhanced photocatalytic hydrogen evolution activity of CuInS{sub 2} loaded TiO{sub 2} under solar light irradiation

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

Li, Changjiang; Xi, Zhenhao; Fang, Wenzhang

2015-03-15

In this paper, p–n type CuInS{sub 2}/TiO{sub 2} particles were prepared in ethylenediamine by the solvothermal method. The microstructural properties of the synthesized p–n type catalysts were characterized by X-ray diffraction (XRD) in order to confirm the existence of crystalline CuInS{sub 2} on the surface of TiO{sub 2}, which was also confirmed by X-ray photoelectron spectroscopy (XPS). Transmission electron microscopy (TEM) images provided the detailed morphological properties about the CuInS{sub 2}/TiO{sub 2} heterostructure. UV–vis diffuse reflectance spectroscopy (UV–vis DRS) was used to investigate the optical properties of the CuInS{sub 2}/TiO{sub 2} particles. The DRS results indicated that both the p–nmore » type structure and CuInS{sub 2} acting as a sensitizer can enhance significantly the absorption of UV and visible light. The photocatalytic activities of the CuInS{sub 2}/TiO{sub 2} particles were evaluated by hydrogen evolution reactions using Xe-lamp irradiation as a simulated solar light source. The greatly enhanced photocatalytic activity of hydrogen evolution under simulated solar light is about ~7 fold higher than that of pure commercial TiO{sub 2} (Degussa P25). - Graphical abstract: The heterojunction structure of CuInS{sub 2}/TiO{sub 2} promoted the efficiency of photoinduced charge carrier transfer and highly inherited the recombination of activated electrons and holes. - Highlight: • CuInS{sub 2}/TiO{sub 2} was prepared by a one-step solvothermal method. • 2.5% CuInS{sub 2}/TiO{sub 2} has the highest activity and keeps the activity stable. • Heterojunction structure of sample promoted the separation of electrons and holes.« less

Morphology and band structure regulation of graphitic carbon nitride microspheres by solvothermal temperature to boost photocatalytic activity

NASA Astrophysics Data System (ADS)

Wang, Shuaijun; Yan, Qingyun; Dong, Pei; Zhao, Chaocheng; Wang, Yongqiang; Liu, Fang; Li, Lin

2018-06-01

Graphitic carbon nitride (g-C3N4) microspheres (CNMS) were fabricated via a solvothermal method by using supramolecular complexes of dicyandiamide and cyanuric chloride as precursors. The effect of solvothermal temperature on the morphology, band structure, and activity was systematically investigated. Structural characterization results indicate that the samples prepared at 180 °C (CNMS-180) and 200 °C (CNMS-200) possess spherical morphology, while irregular bulk particles were obtained at 160 °C (CN-160). In addition, the band gap increased as the solvothermal temperature decreased from 200 to 160 °C. In comparison with CN-160 and CNMS-200, the valence band of CNMS-180 was more positive and thus gives higher photo-oxidation capability. Accordingly, CNMS-180 exhibits higher photocatalytic degradation efficiency on Rhodamine B, stronger photocurrent response, and lower charge transfer resistance. Additionally, CNMS-180 exhibits excellent stability after four runs. This work might provide a guidance for the regulation of morphology and band structure of g-C3N4-based materials prepared at low temperatures.

Microwave-assisted solvothermal synthesis of novel hierarchical BiOI/rGO composites for efficient photocatalytic degardation of organic pollutants

NASA Astrophysics Data System (ADS)

Niu, Jinfen; Dai, Peixuan; Zhang, Qian; Yao, Binghua; Yu, Xiaojiao

2018-02-01

In the present paper, a novel composite of BiOI/rGO with excellent visible-light photocatalytic activity was successfully fabricated via very different simple, fast and mild rapid microwave hydrothermal method. The BiOI/rGO -1(BG-1) was donated as a simple chemical mechanical and the BiOI/rGO -2(BG-2) was donated as one-step rapid microwave hydrothermal method. The BG-1 were composed of the BiOI microspheres with a diameter of about 1 μm and mixed heterogeneously with graphene. While, the BG-2 were consist of the BiOI nanoplates with the thickness of approximately 20 nm dispersed heterogeneously on the surface of rGO. The degradation of 40 mg/L methylene blue (MB) and 20 mg/L levofloxacin (LEV) under visible light irradiation can reach about 11 and 3 times than that of P25, respectively. Furthermore, the reactive species of hole was determined to dominant the photodegradation process. The intensive photocatlytic could ascribe to more effective electron transportation and separations, this conclusion was different with other studies. A possible photocatalytic mechanism of BG-2 was also proposed.

Enhanced photocatalytic CO₂-reduction activity of electrospun mesoporous TiO₂ nanofibers by solvothermal treatment.

PubMed

Fu, Junwei; Cao, Shaowen; Yu, Jiaguo; Low, Jingxiang; Lei, Yongpeng

2014-06-28

Photocatalytic reduction of CO2 into renewable hydrocarbon fuels using semiconductor photocatalysts is considered as a potential solution to the energy deficiency and greenhouse effect. In this work, mesoporous TiO2 nanofibers with high specific surface areas and abundant surface hydroxyl groups are prepared using an electrospinning strategy combined with a subsequent calcination process, followed by a solvothermal treatment. The solvothermally treated mesoporous TiO2 nanofibers exhibit excellent photocatalytic performance on CO2 reduction into hydrocarbon fuels. The significantly improved photocatalytic activity can be attributed to the enhanced CO2 adsorption capacity and the improved charge separation after solvothermal treatment. The highest activity is achieved for the sample with a 2-h solvothermal treatment, showing 6- and 25-fold higher CH4 production rate than those of TiO2 nanofibers without solvothermal treatment and P25, respectively. This work may also provide a prototype for studying the effect of solvothermal treatment on the structure and photocatalytic activity of semiconductor photocatalysts.

High performance humidity sensor and photodetector based on SnSe nanorods

NASA Astrophysics Data System (ADS)

Pawbake, Amit S.; Jadkar, Sandesh R.; Late, Dattatray J.

2016-10-01

Tin selenide (SnSe) nanorods were synthesized using a one-step solvothermal route and their humidity sensing and photodetection performance at room temperature were investigated. The results depict that SnSe nanorod-based humidity and photosensors have good long-term stability, are highly sensitive and have fast response and recovery times. In the case of the humidity sensor it was observed that the resistance of the films decreased with increasing relative humidity (RH). The humidity sensing behaviors were investigated in the range 11-97% RH at room temperature. A response time of ˜68 s and recovery time of ˜149 s were observed for the humidity sensor. The photosensing behavior showed typical response /recovery times of ˜3 s with highly reproducible behavior.

Facile synthesis of bird's nest-like TiO2 microstructure with exposed (001) facets for photocatalytic degradation of methylene blue

NASA Astrophysics Data System (ADS)

Zhang, Guozhong; Zhang, Shuqu; Wang, Longlu; Liu, Ran; Zeng, Yunxiong; Xia, Xinnian; Liu, Yutang; Luo, Shenglian

2017-01-01

The scrupulous design of hierarchical structure and highly active crystal facets exposure is essential for the creation of photocatalytic system. However, it is still a big challenge for scrupulous design of TiO2 architectures. In this paper, bird's nest-like anatase TiO2 microstructure with exposed highly active (001) surface has been successfully synthesized by a facile one-step solvothermal method. Methylene blue (MB) is chosen as a model pollutant to evaluate photocatalytic activity of as-obtained TiO2 samples. The results show that the photocatalytic activity of the bird's nest-like sample is more excellent than P25 in the degradation of MB due to high specific surface area and highly active (001) crystal facets exposure when tested under simulated solar light. Besides, it can be readily separated from the photocatalytic system by sedimentation after photocatalytic reaction, which is a significant advantage against conventional powder photocatalyst. The bird's nest-like microspheres with novel structure may have potential application in photocatalysis and other fields.

Copper Benzenetricarboxylate Metal-Organic Framework Nucleation Mechanisms on Metal Oxide Powders and Thin Films formed by Atomic Layer Deposition.

PubMed

Lemaire, Paul C; Zhao, Junjie; Williams, Philip S; Walls, Howard J; Shepherd, Sarah D; Losego, Mark D; Peterson, Gregory W; Parsons, Gregory N

2016-04-13

Chemically functional microporous metal-organic framework (MOF) crystals are attractive for filtration and gas storage applications, and recent results show that they can be immobilized on high surface area substrates, such as fiber mats. However, fundamental knowledge is still lacking regarding initial key reaction steps in thin film MOF nucleation and growth. We find that thin inorganic nucleation layers formed by atomic layer deposition (ALD) can promote solvothermal growth of copper benzenetricarboxylate MOF (Cu-BTC) on various substrate surfaces. The nature of the ALD material affects the MOF nucleation time, crystal size and morphology, and the resulting MOF surface area per unit mass. To understand MOF nucleation mechanisms, we investigate detailed Cu-BTC MOF nucleation behavior on metal oxide powders and Al2O3, ZnO, and TiO2 layers formed by ALD on polypropylene substrates. Studying both combined and sequential MOF reactant exposure conditions, we find that during solvothermal synthesis ALD metal oxides can react with the MOF metal precursor to form double hydroxy salts that can further convert to Cu-BTC MOF. The acidic organic linker can also etch or react with the surface to form MOF from an oxide metal source, which can also function as a nucleation agent for Cu-BTC in the mixed solvothermal solution. We discuss the implications of these results for better controlled thin film MOF nucleation and growth.

Synthesis of sub-micro-flakes CrSe2 on glass and (110) Si substrates by solvothermal method

NASA Astrophysics Data System (ADS)

Tang, Qingkai; Liu, Changyou; Zhang, Binbin; Jie, Wanqi

2018-06-01

Layered structure MX2 (M = transition metal, X = S, Se and Te) chalcogenides have rich physic properties and potential applications. While it is still a challenge to prepare the chalcogenides by solvothermal method. In this work, we reported a new solution method to prepare CrSe2 sub-micro-flakes on different substrates. The surface morphologies, structures and compositions of the precursor CrSe2(en)1/2 and CrSe2 were investigated by SEM, XRD, thermogravimetric, IR and Raman spectra. The CrSe2 flakes with the sizes of 5-15 μm were obtained on both glass and (110) Si crystalline substrates. The formation mechanism of CrSe2 sub-micro-flakes is suggested.

One-dimensional ZnO nanostructures.

PubMed

Jayadevan, K P; Tseng, T Y

2012-06-01

The wide-gap semiconductor ZnO with nanostructures such as nanoparticle, nanorod, nanowire, nanobelt, nanotube has high potential for a variety of applications. This article reviews the fundamentals of one-dimensional ZnO nanostructures, including processing, structure, property, application and their processing-microstructure-property correlation. Various fabrication methods of the ZnO nanostructures including vapor-liquid-solid process, vapor-solid growth, solution growth, solvothermal growth, template-assisted growth and self-assembly are introduced. The characterization and properties of the ZnO nanostructures are described. The possible applications of these nanostructures are also discussed.

Single-step solvothermal synthesis of mesoporous Ag-TiO2-reduced graphene oxide ternary composites with enhanced photocatalytic activity.

PubMed

Sher Shah, Md Selim Arif; Zhang, Kan; Park, A Reum; Kim, Kwang Su; Park, Nam-Gyu; Park, Jong Hyeok; Yoo, Pil J

2013-06-07

With growing interest in the photocatalytic performance of TiO2-graphene composite systems, the ternary phase of TiO2, graphene, and Ag is expected to exhibit improved photocatalytic characteristics because of the improved recombination rate of photogenerated charge carriers and potential contribution of the generation of localized surface plasmon resonance at Ag sites on a surface of the TiO2-graphene binary matrix. In this work, Ag-TiO2-reduced graphene oxide ternary nanocomposites were successfully synthesized by a simple solvothermal process. In a single-step synthetic procedure, the reduction of AgNO3 and graphene oxide and the hydrolysis of titanium tetraisopropoxide were spontaneously performed in a mixed solvent system of ethylene glycol, N,N-dimethylformamide and a stoichiometric amount of water without resorting to the use of typical reducing agents. The nanocomposites were characterized by X-ray diffraction, X-ray photoelectron spectroscopy, along with different microscopic and spectroscopic techniques, enabling us to confirm the successful reduction of AgNO3 and graphite oxide to metallic Ag and reduced graphene oxide, respectively. Due to the highly facilitated electron transport of well distributed Ag nanoparticles, the synthesized ternary nanocomposite showed enhanced photocatalytic activity for degradation of rhodamine B dye under visible light irradiation.

Synthesis of the complex fluoride LiBaF 3 and optical spectroscopy properties of LiBaF 3: M( M=Eu,Ce) through a solvothermal process

NASA Astrophysics Data System (ADS)

Hua, Ruinian; Lei, Bingfu; Xie, Demin; Shi, Chunshan

2003-11-01

The complex fluoride LiBaF 3 and LiBaF 3: M( M=Eu, Ce) is solvothermally synthesized at 180°C and characterized by means of X-ray powder diffraction, scanning electron microscopy, thermogravimetric analysis and infrared spectroscopy. In the solvothermal process, the solvents, molar ratios of initial mixtures and reaction temperature play important roles in the formation of products. The excitation and emission spectra of the LiBaF 3: M( M=Eu,Ce) have been measured by fluorescence spectrophotometer. In the LiBaF 3:Eu emission spectra, there is one sharp line emission located at 360 nm arising from f→ f transition of Eu 2+ in the host lattice, and typical doublet 5 d-4 f emission of Ce 3+ in LiBaF 3 powder is shown.

Free-standing and porous hierarchical nanoarchitectures constructed with cobalt cobaltite nanowalls for supercapacitors with high specific capacitances

NASA Astrophysics Data System (ADS)

Xiao, Yuanhua; Zhang, Aiqin; Liu, Shaojun; Zhao, Jihong; Fang, Shaoming; Jia, Dianzeng; Li, Feng

2012-12-01

Free-standing and porous hierarchical nanoarchitectures constructed with cobalt cobaltite (Co3O4) nanowalls have been successfully synthesized in large scale by calcining three dimensional (3D) hierarchical nanostructures consisting of single crystalline cobalt carbonate hydroxide hydrate - Co(CO3)0.5(OH)·0.11H2O nanowalls prepared with a solvothermal method. The step-by-step decomposition of the precursor can generate porous Co3O4 nanowalls with BET surface area of 88.34 m2 g-1. The as-prepared Co3O4 nanoarchitectures show superior specific capacitance to the most Co3O4 supercapacitor electrode materials to date. After continuously cycled for 1000 times of charge-discharge at 4 A g-1, the supercapacitors can retain ca 92.3% of their original specific capacitances. The excellent performances of the devices can be attributed to the porous and hierarchical 3D nanostructure of the materials.

Solvothermal synthesis of hierarchical TiO2 nanostructures with tunable morphology and enhanced photocatalytic activity

NASA Astrophysics Data System (ADS)

Fan, Zhenghua; Meng, Fanming; Zhang, Miao; Wu, Zhenyu; Sun, Zhaoqi; Li, Aixia

2016-01-01

This paper presents controllable growth and photocatalytic activity of TiO2 hierarchical nanostructures by solvothermal method at different temperatures. It is revealed by scanning electron microscopy (SEM) and transmission electron microscopy (TEM) that the morphology of TiO2 can be effectively controlled as rose-like, chrysanthemum-like and sea-urchin-like only changing solvothermal temperature. BET surface area analysis confirms the presence of a mesoporous network in all the nanostructures, and shows high surface area at relatively high temperature. The photocatalytic activities of the photocatalysts are evaluated by the photodegradation of RhB under UV light irradiation. The TiO2 samples exhibit high activity on the photodegradation of RhB, which is higher than that of the commercial P25. The enhancement in photocatalytic performance can be attributed to the synergetic effect of the surface area, crystallinity, band gap and crystalline size.

Citric acid induced W18O49 electrochromic films with enhanced optical modulation

NASA Astrophysics Data System (ADS)

Xie, Junliang; Song, Bin; Zhao, Gaoling; Han, Gaorong

2018-06-01

Electrochromic materials exhibit promising applications in energy-saving fields for their ability to control heat from outdoors. Nanostructured W18O49 has drawn attention for its one-dimensional structure to transfer charge efficiently as a remarkable electrochromic material. W18O49 bi-layer films were fabricated through a facile one-step solvothermal process with citric acid as a chelating agent. The addition of citric acid improved the deposition on the substance, and a nanostructured film with a denser layer at the bottom and a tussock-like upper layer was obtained. The bi-layer film exhibited an enhanced optical modulation of 68.7%, a coloration efficiency of 82.1 cm2/C with stability over 400 cycles, and fast response times (1.4 s and 2.3 s for bleaching and coloring), with expectation to be applied in the electrochromic field.

Solvothermal synthesis of Au@Fe3O4 nanoparticles for antibacterial applications

NASA Astrophysics Data System (ADS)

Kelgenbaeva, Zhazgul; Abdullaeva, Zhypargul; Murzubraimov, Bektemir

2018-04-01

We present Au@Fe3O4 nanoparticles obtained from Fe nanoparticles and HAuCl4 using a simple solvothermal method. Trisodium citrate (C6H5Na3O7*2H2O) served as a reducing agent for Au. X-ray diffraction analysis, electronic microscopes and energy-dispersive X-ray spectroscopy revealed cubic structure, elemental composition (Au, Fe and O) and spherical shape of nanoparticles. Antibacterial activity of the sample was tested against E. coli bacteria and obtained results were discussed.

Non-platinum metal-organic framework based electro-catalyst for promoting oxygen reduction reaction

NASA Astrophysics Data System (ADS)

Das, Dipanwita; Raut, Vrushali; Kireeti, Kota V. M. K.; Jha, Neetu

2018-04-01

We developed two non-precious Metal Organic Framework (MOF) based electrocatalysts, MOF-5 and MOF-i using solvothermal and refluxing methods. The MOFs prepared has been characterized by powder X-ray diffractometer (XRD), Fourier Transform Infra-Red Spectroscopy (FTIR) and Scanning Electron Microscopy (SEM) for structural and morphological insights. SEM images reveal cubic shape for solvothermally synthesized MOF-5, whereas refluxing method leads to platelet morphology of MOF-i. The synthesized MOFs has been investigated for Oxygen Reduction Reaction (ORR) studies using Cyclic Voltammetry (CV) and Linear Sweep Voltammetry (LSV), with MOF modified Glassy Carbon (GC) as working electrode. The electrochemical data suggests higher activity of MOF-5 towards ORR compared to MOF-i.

Investigation of luminescent properties of LaF3:Nd3+ nanoparticles

NASA Astrophysics Data System (ADS)

Wyrwas, Marek; Miluski, Piotr; Zmojda, Jacek; Kochanowicz, Marcin; Jelen, Piotr; Sitarz, Maciej; Dorosz, Dominik

2015-09-01

Lanthanum fluoride nanoparticles doped with Nd3+ ions obtained via solvothermal method have been presented. Doped nanoparticles were prepared in two-step method. Firstly rare-earth chlorides were synthesized from oxides and then they were used to prepare LaF3 particles. The luminescence spectra shows typical for crystalline materials Stark splitting at 880 nm corresponding 4F3/2 to 4I9/2 level transition and 1060 nm matching 4F3/2 to 4I11/2 level transition. The highest luminescence intensity was achieved for sample doped with 0.75% wt. of Nd3+, and the longest decay time for sample doped with 0.5% wt. which reached 328 μs. The XRD pattern analysis confirmed that obtained material consists of crystalline LaF3, the grain size was estimated from Sherrer's formula and equaled about 25nm.

Mesoporous TiO2 Yolk-Shell Microspheres for Dye-sensitized Solar Cells with a High Efficiency Exceeding 11%

PubMed Central

Li, Zhao-Qian; Chen, Wang-Chao; Guo, Fu-Ling; Mo, Li-E; Hu, Lin-Hua; Dai, Song-Yuan

2015-01-01

Yolk-shell TiO2 microspheres were synthesized via a one-pot template-free solvothermal method building on the aldol condensation reaction of acetylacetone. This unique structure shows superior light scattering ability resulting in power conversion efficiency as high as 11%. This work provided a new synthesis system for TiO2 microspheres from solid to hollow and a novel material platform for high performance solar cells. PMID:26384004

One-pot solvothermal synthesis of dual-phase titanate/titania Nanoparticles and their adsorption and photocatalytic Performances

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

Cheng, Yu Hua; Gong, Dangguo; Tang, Yuxin

2014-06-01

Dual phase titanate/titania nanoparticles undergo phase transformation gradually with the increase of solvothermal synthesis temperature from 100 °C to 200 °C, and eventually are fully transformed into anatase TiO{sub 2}. The crystal structure change results in the changes of optical absorption, sensitizer/dopant formation and surface area of the materials which finally affect the overall dye removal ability. Reactions under dark and light have been conducted to distinguish the contributions of surface adsorption from photocatalytic degradation. The sample synthesized at 160 °C (S160) shows the best performances for both adsorption under dark and photocatalytic degradation of methylene blue (MB) under visiblemore » light irradiation. The adsorption mechanism for S160 is determined as monolayer adsorption based on the adsorption isotherm test under dark condition, and an impressive adsorption capacity of 162.19 mg/g is achieved. For the photocatalytic application, this sample at 0.1 g/L loading is also able to degrade 20 ppm MB within 6 hours under the visible light (>420 nm) condition. - Graphical abstract: The effect of solvothermal synthesis temperature on the formation and dye removal performance of dual phase titanate/titania nanoparticles was unveiled and optimized. - Highlights: • Low temperature one-pot solvothermal synthesis of dual-phase photocatalysts. • Correlation of the synthesis temperature is made with the phase composition. • Adsorption isotherm, kinetics, photocatalytic degradation were studied. • Synthesis at 160 °C yields the best material for adsorption of MB in dark. • The same sample also shows the best visible light degradation of MB.« less

Preparation of alumina-hercynite nano-spinel via one-step thermal conversion of Fe-doped metal-organic framework MIL-53(Al)

NASA Astrophysics Data System (ADS)

Chen, Shuyi; Lu, Huigong; Wu, Yi-nan; Gu, Yifan; Li, Fengting; Morlay, Catherine

2016-09-01

Alumina-hercynite nano-spinel powders were prepared via one-step pyrolysis of iron-acetylacetone-doped Al-based metal-organic framework (MOF), i.e., MIL-53(Al). Organic ferric source, iron acetylacetone, was incorporated in situ into the framework of MIL-53(Al) during the solvothermal synthesis process. Under high-temperature pyrolysis, alumina derived from the MIL-53(Al) matrix and ferric oxides originated from the decomposition of organic ferric precursor in the framework were thermally converted into hercynite (FeAl2O4). The prepared samples were characterized using transmission electron microscopy, X-ray diffraction, N2 sorption, thermogravimetry, Raman spectroscopy and X-ray photoelectron spectroscopy. The final products were identified to be composed of alumina, hercynite and trace amounts of carbon depending on pyrolysis temperature. The experimental results showed that hercynite phase can be obtained and stabilized at low temperatures between 900 and 1100 °C under inert atmosphere. The final products were composed of nano-sized particles with an average size below 100 nm of individual crystal and specific surface areas of 18-49 m2 g-1.

Low-temperature solvothermal synthesis of EuS hollow microspheres

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

Peng, Yong; Wang, Hong; Li, Peng

2014-09-15

Graphical abstract: Synthesis of EuS hollow microspheres at low-temperature via solvothermal method for the first time. - Highlights: • We adopt an improved method to synthesise the (Phen)Eu(Et{sub 2}CNS{sub 2}){sub 3} in deionized water. • We have successfully synthesised the EuS hollow microsphere at 230 °C in acetonitrile. • The price of acetonitrile is more inexpensive, so the price of preparation was reduced. - Abstract: EuS crystals are synthesized by low-temperature solvothermal decomposition of the single source precursor complex (Phen)Eu(Et{sub 2}CNS{sub 2}){sub 3} in acetonitrile. X-ray powder diffraction, scanning electron microscopy, granulocyte diameter statistical analysis, surface energy-dispersive X-ray spectroscopy analysis,more » and UV–vis absorption spectroscopy are used to characterize the structure and properties of the obtained EuS crystals. The results show that the formed EuS crystals are uniform hollow microspheres with a typical cubic phase structure of rock salt and the average particle size of 2.01 μm. The mechanisms for the thermal decomposition of the precursor complex and the formation of the EuS hollow microspheres are postulated based on the experimental observations and previous reports.« less

Solvothermal synthesis and surface chemistry to control the size and morphology of nanoquartz

DOE PAGES

Sochalski-Kolbus, Lindsay M.; Wang, Hsiu-Wen; Rondinone, Adam Justin; ...

2015-09-29

In this paper, we report a solvothermal synthesis method that allows the crystallization of quartz to occur at a relatively low temperature of 300°C in the form of isolated nanosized euhedral crystals. Transmission electron microscopy (TEM) and small area electron diffraction (SAED) were used to confirm the phases present and their particle sizes, morphologies, and crystallinity of the products. In conclusion, the results show that it is possible to control the size and morphology of the nanoquartz from rough nanospheres to nanorods using fluoride, which templates the nanocrystals and moderates growth.

Solvothermal syntheses, and characterization of [Ln(en){sub 4}(SbSe{sub 4})] (Ln=Ce, Pr) and [Ln(en){sub 4}]SbSe{sub 4}.0.5en (Ln=Eu, Gd, Er, Tm, Yb): The effect of lanthanide contraction on the crystal structures of lanthanide selenidoantimonates(V)

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

Jia Dingxian; Zhu Aimei; Jin Qinyan

Two types of lanthanide selenidoantimonates [Ln(en){sub 4}(SbSe{sub 4})] (Ln=Ce(1a), Pr(1b)) and [Ln(en){sub 4}]SbSe{sub 4}.0.5en (Ln=Eu(2a), Gd(2b), Er(2c), Tm(2d), Yb(2e); en=ethylenediamine) were solvothermally synthesized by reactions of LnCl{sub 3}, Sb and Se with the stoichiometric ratio in en solvent at 140 deg. C. The four-en coordinated lanthanide complex cation [Ln(en){sub 4}]{sup 3+} formed in situ balances the charge of SbSe{sub 4}{sup 3-} anion. In compounds 1a and 1b, the SbSe{sub 4}{sup 3-} anion act as a monodentate ligand to coordinate complex [Ln(en){sub 4}]{sup 3+} and the neutral compound [Ln(en){sub 4}(SbSe{sub 4})] is formed. The Ln{sup 3+} ion has a nine-coordinated environmentmore » involving eight N atoms and one Se atom forming a distorted monocapped square antiprism. In 2a-2e the lanthanide(III) ion exists as isolated complex [Ln(en){sub 4}]{sup 3+}, in which the Ln{sup 3+} ion is in a bicapped trigonal prism geometry. A systematic investigation of the crystal structures reveals that two types of structural features of these lanthanide selenidoantimonates are related with lanthanides contraction across the lanthanide series. TG curves show that compounds 1a-1b and 2a-2e remove their organic components in one and two steps, respectively. - Graphical abstract: Two types of lanthanide selenidoantimonates [Ln(en){sub 4}(SbSe{sub 4})] (Ln=Ce, Pr) and [Ln(en){sub 4}]SbSe{sub 4}.0.5en (Ln=Eu, Gd, Er, Tm, Yb; en=ethylenediamine) have been synthesized under the mild solvothermal conditions, and a systematic investigation of the crystal structures reveals that two types of structural features of these lanthanide selenidoantimonates are related with lanthanides contraction across the lanthanide series.« less

α-Fe2O3 nanosheet-assembled hierarchical hollow mesoporous microspheres: Microwave-assisted solvothermal synthesis and application in photocatalysis.

PubMed

Sun, Tuan-Wei; Zhu, Ying-Jie; Qi, Chao; Ding, Guan-Jun; Chen, Feng; Wu, Jin

2016-02-01

α-Fe2O3 nanosheet-assembled hierarchical hollow mesoporous microspheres (HHMSs) were prepared by thermal transformation of nanosheet-assembled hierarchical hollow mesoporous microspheres of a precursor. The precursor was rapidly synthesized using FeCl3·6H2O as the iron source, ethanolamine (EA) as the alkali source, and ethylene glycol (EG) as the solvent by the microwave-assisted solvothermal method. The samples were characterized by X-ray powder diffraction (XRD), thermogravimetric (TG) analysis, Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM) and nitrogen adsorption-desorption isotherm. The effects of the microwave solvothermal temperature and EA amount on the morphology of the precursor were investigated. The as-prepared α-Fe2O3 HHMSs exhibit a good photocatalytic activity for the degradation of salicylic acid, and are promising for the application in wastewater treatment. Copyright © 2015 Elsevier Inc. All rights reserved.

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.

A facile one-pot solvothermal method for synthesis of magnetically recoverable Pd-Fe3O4 hybrid nanocatalysts for the Mizoroki-Heck reaction

NASA Astrophysics Data System (ADS)

Zhen, Fangchen; Ran, Maofei; Chu, Wei; Jiang, Chengfa; Sun, Wenjing

2018-03-01

Pd-Fe3O4 hybrid nanostructures were prepared using a simple one-pot hydrothermal method. The prepared materials were characterized by Fourier transform-infrared spectroscopy, X-ray diffraction, X-ray photoelectron spectroscopy, scanning electron microscopy, transmission electron microscopy, inductively coupled plasma, N2 adsorption-desorption, and vibrating sample magnetometry. This self-assembled nanosystem acted as an efficient magnetically recyclable noble metal-based multi-functional nanocatalyst. It showed excellent catalytic activity and stability for the Heck reaction of iodobenzene and styrene under mild conditions. The methods used to prepare the Pd-Fe3O4 catalysts were simple and low-cost, which will be useful for the large-scale development and application of a magnetically recoverable Pd catalyst.

Polyvinylpyrrolidone (PVP)-assisted solvothermal synthesis of flower-like SrCO{sub 3}:Tb{sup 3+} phosphors

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

Xue, Yannan; Ren, Xiaolei; Zhai, Xuefeng

Graphical abstract: A simple solvothermal method for the synthesis of flower-like SrCO{sub 3}:Tb{sup 3+} phosphors with the assistance of polyvinylpyrrolidone (PVP, K30). Highlights: Black-Right-Pointing-Pointer Well-crystallized flower-like SrCO{sub 3}:Tb{sup 3+} phosphors could be easily prepared by a simple solvothermal method with the assistance of polyvinylpyrrolidone (PVP). Black-Right-Pointing-Pointer The amount of PVP and the reaction time have a strong effect on controlling the morphology and optical properties of SrCO{sub 3}:Tb{sup 3+} particles. Black-Right-Pointing-Pointer The main synthesizing process and the growth mechanism for the formation of final samples were proposed. -- Abstract: Well-crystallized flower-like SrCO{sub 3}:Tb{sup 3+} phosphors have been synthesized by anmore » inexpensive and friendly solvothermal process using polyvinylpyrrolidone (PVP, K30) as an additive without further annealing treatment. X-ray diffraction (XRD), Fourier transform-infrared spectroscopy (FT-IR), and field emission scanning electron microscopy (FESEM) as well as photoluminescence spectroscopy (PL) were used to characterize the resulting samples. The amount of PVP and the reaction time have strong effect on the morphology of the SrCO{sub 3}:Tb{sup 3+} particles. The results of XRD confirm the formation of a well-crystallized SrCO{sub 3} phase with an orthorhombic structure. The possible formation mechanism for flower-like SrCO{sub 3}:Tb{sup 3+} phosphor is proposed. The SrCO{sub 3}:Tb{sup 3+} phosphors show the characteristic {sup 5}D{sub 4}-{sup 7}F{sub J} (J = 6, 5, 4, 3) emission lines with green emission {sup 5}D{sub 4}-{sup 7}F{sub 5} (544 nm) as the most prominent group under ultraviolet excitation.« less

Enhanced adsorptive removal of p-nitrophenol from water by aluminum metal-organic framework/reduced graphene oxide composite

NASA Astrophysics Data System (ADS)

Wu, Zhibin; Yuan, Xingzhong; Zhong, Hua; Wang, Hou; Zeng, Guangming; Chen, Xiaohong; Wang, Hui; Zhang, Lei; Shao, Jianguang

2016-05-01

In this study, the composite of aluminum metal-organic framework MIL-68(Al) and reduced graphene oxide (MA/RG) was synthesized via a one-step solvothermal method, and their performances for p-nitrophenol (PNP) adsorption from aqueous solution were systematically investigated. The introduction of reduced graphene oxide (RG) into MIL-68(Al) (MA) significantly changes the morphologies of the MA and increases the surface area. The MA/RG-15% prepared at RG-to-MA mass ratio of 15% shows a PNP uptake rate 64% and 123% higher than MIL-68(Al) and reduced graphene oxide (RG), respectively. The hydrogen bond and π - π dispersion were considered to be the major driving force for the spontaneous and endothermic adsorption process for PNP removal. The adsorption kinetics, which was controlled by film-diffusion and intra-particle diffusion, was greatly influenced by solution pH, ionic strength, temperature and initial PNP concentration. The adsorption kinetics and isotherms can be well delineated using pseudo-second-order and Langmuir equations, respectively. The presence of phenol or isomeric nitrophenols in the solution had minimal influence on PNP adsorption by reusable MA/RG composite.

Calcium phosphate-phosphorylated adenosine hybrid microspheres for anti-osteosarcoma drug delivery and osteogenic differentiation.

PubMed

Zhou, Zi-Fei; Sun, Tuan-Wei; Chen, Feng; Zuo, Dong-Qing; Wang, Hong-Sheng; Hua, Ying-Qi; Cai, Zheng-Dong; Tan, Jun

2017-03-01

Biocompatibility, biodegradability and bioactivity are significantly important in practical applications of various biomaterials for bone tissue engineering. Herein, we develop a functional inorganic-organic hybrid system of calcium phosphate-phosphorylated adenosine (CPPA). Both calcium phosphate and phosphorylated adenosine molecules in CPPA are fundamental components in mammalians and play important roles in biological metabolism. In this work, we report our three leading research qualities: (1) CPPA hybrid microspheres with hollow and porous structure are synthesized by a facile one-step microwave-assisted solvothermal method; (2) CPPA hybrid microspheres show high doxorubicin loading capacity and pH-responsive drug release properties, and demonstrate positive therapeutic effects on six osteosarcoma cell lines in vitro and a mouse model of 143B osteosarcoma subcutaneous tumor in vivo; (3) CPPA hybrid microspheres are favorable to promote osteogenic differentiation of human bone mesenchymal stem cells (hBMSCs) by activating the AMPK pathway, with satisfactory evidences from cellular alkaline phosphatase staining, alizarin red staining, real time PCR and western analysis. The as-prepared CPPA hybrid microspheres are promising in anti-osteosarcoma and bone regeneration, which simultaneously display excellent properties on drug delivery and osteogenic differentiation of hBMSCs. Copyright © 2016 Elsevier Ltd. All rights reserved.

High efficient photocatalytic selective oxidation of benzyl alcohol to benzaldehyde by solvothermal-synthesized ZnIn{sub 2}S{sub 4} microspheres under visible light irradiation

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

Chen, Zhixin, E-mail: czx@fzu.edu.cn; Instrumental Measurement and Analysis Center, Fuzhou University, Fuzhou 350002; Xu, Jingjing

Hexagonal ZnIn{sub 2}S{sub 4} samples have been synthesized by a solvothermal method. Their properties have been determined by X-ray diffraction, ultraviolet–visible-light diffuse reflectance spectra, field emission scanning electron microscopy, nitrogen adsorption–desorption and X-ray photoelectron spectra. These results demonstrate that ethanol solvent has significant influence on the morphology, optical and electronic nature for such marigold-like ZnIn{sub 2}S{sub 4} microspheres. The visible light photocatalytic activities of the ZnIn{sub 2}S{sub 4} have been evaluated by selective oxidation of benzyl alcohol to benzaldehyde using molecular oxygen as oxidant. The results show that 100% conversion along with >99% selectivity are reached over ZnIn{sub 2}S{sub 4}more » prepared in ethanol solvent under visible light irradiation (λ>420 nm) of 2 h, but only 58% conversion and 57% yield are reached over ZnIn{sub 2}S{sub 4} prepared in aqueous solvent. A possible mechanism of the high photocatalytic activity for selective oxidation of benzyl alcohol over ZnIn{sub 2}S{sub 4} is proposed and discussed. - Graphical abstract: Marigold-like ZnIn{sub 2}S{sub 4} microspheres were synthesized by a solvothermal method. The high visible photocatalytic activities of ZnIn{sub 2}S{sub 4} were evaluated by selective oxidation of benzyl alcohol to benzaldehyde under mild conditions. Display Omitted - Highlights: • Marigold-like ZnIn{sub 2}S{sub 4} microspheres were synthesized by a solvothermal method. • The solvents have a remarkably influence on the morphology and properties of samples. • It is the first time to apply ZnIn{sub 2}S{sub 4} for selective oxidation of benzyl alcohol. • ZnIn{sub 2}S{sub 4} shows high photocatalytic activity for selective oxidation of benzyl alcohol.« less

Solvothermal crystallization of nanocrystals of metal oxides

NASA Astrophysics Data System (ADS)

Furukawa, S.; Amino, H.; Iwamoto, S.; Inoue, M.

2008-07-01

Solvothermal crystallization of the hydroxide gels obtained by hydrolysis of alkoxides (Zr, Ta, Nb, ln, Sn, Ti and Al) was examined. Nanocrystals having high surface areas (SBET > 170 m2 g-1) were obtained except for the product derived from indium isopropoxide. The effect of water in organic solvent upon the crystallinity of the product was investigated. The increase in the activity of water by using high concentration of alkoxide or intentional addition of water to the solvothermal medium led to crystal growth of the products. In contrast, decrease in activity of water by adding ethylene glycol before solvothermal treatment caused a decrease in crystallinity of the product.

Synthesis, characterization and adsorption properties of magnetite/reduced graphene oxide nanocomposites.

PubMed

Qi, Tingting; Huang, Chenchen; Yan, Shan; Li, Xiu-Juan; Pan, Si-Yi

2015-11-01

Three kinds of magnetite/reduced graphene oxide (MRGO) nanocomposites were prepared by solvothermal, hydrothermal and co-precipitation methods. The as-prepared nanocomposites were characterized and compared by Fourier transform infrared spectroscopy, scanning electron microscopy, transmission electron microscopy, X-ray diffraction and zeta potential. The results showed that MRGO made by different methods differed in surface functional groups, crystal structure, particle sizes, surface morphology and surface charge. Due to their unlike features, these nanocomposites displayed dissimilar performances when they were used to adsorb drugs, dyes and metal ions. The MRGO prepared by the co-precipitation method showed special adsorption ability to negative ions, but those synthesized by the solvothermal method obtained the best extraction ability and reusability to the others and showed a good prospective in magnetic solid-phase extraction. Therefore, it is highly recommended to use the right preparation method before application in order to attain the best extraction performance. Copyright © 2015 Elsevier B.V. All rights reserved.

A facile solvothermal method to produce graphene-ZnS composites for superior photoelectric applications

NASA Astrophysics Data System (ADS)

Lei, Yun; Chen, Feifei; Li, Rong; Xu, Jun

2014-07-01

In this experiment, flake graphite (<30 μm) was prepared as raw materials. Graphite oxide is prepared with Hummers method by low temperature, middle temperature and high temperature, and further treated with super-sonic oscillation to get graphene oxide. Graphene-zinc sulfide composites were synthesized through a simple solvothermal method using thiourea or sodium sulfide as sulfur source in the ethylene glycol or ethylenediamine, respectively. The products were characterized by X-ray and SEM, and analyzed by the transient photocurrent response and electrochemical impedance spectra. The results indicate that the properties of graphene-zinc sulfide composites prepared with thiourea in ethylene glycol are superior to those of blank-ZnS and composites prepared with sodium sulfide and ethylenediamine, which is attributed to electron capture and transfer ability of graphene resulting in a more efficient separation of the photoexcited charge carriers from ZnS-graphene composites.

Highly sensitive detection of explosive triacetone triperoxide by an In2O3 sensor.

PubMed

Zhang, Wen-Hui; Zhang, Wei-De; Chen, Lu-Ya

2010-08-06

Triacetone triperoxide (TATP) is one of the most sensitive known explosives and can be easily synthesized using the commonly available chemicals acetone and hydrogen peroxide, but is difficult to be detected. In this study, In(2)O(3) nanoparticles were synthesized by a glucose-assisted solvothermal method at 120 degrees C for 18 h. The gas sensor based on In(2)O(3) nanoparticles exhibits a high response, fast response and recovery, a wide detecting range of 0.50-500 mg, good stability and excellent stability to TATP.

Method to synthesize metal chalcogenide monolayer nanomaterials

DOEpatents

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

2016-12-13

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

Self-Sacrificial Salt Templating: Simple Auxiliary Control over the Nanoporous Structure of Porous Carbon Monoliths Prepared through the Solvothermal Route

PubMed Central

Feng, Junzong; Jiang, Yonggang; Liu, Ping; Zhang, Qiuhua; Wei, Ronghui; Chen, Xiang; Feng, Jian

2018-01-01

The conventional sol-gel method for preparing porous carbons is tedious and high-cost to prepare porous carbons and the control over the nanoporous architecture by solvents and carbonization is restricted. A simple and novel self-sacrificial salt templating method was first presented to adjust the microporous structure of porous carbon monoliths synthesized via the solvothermal method. Apart from good monolithic appearance, the solvothermal route allowed for ambient drying because it made sure that the polymerization reaction was completed quickly and thoroughly. The intact and crack-free porous carbon monoliths were investigated by scanning electron microscopy (SEM), thermogravimetric differential scanning calorimetry (TG-DSC), Fourier transform infrared (FT-IR), energy dispersive spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD) and nitrogen sorption measurements. It was proven that the self-sacrificial salts NH4SCN had been removed during pyrolyzing and so, porous carbon monoliths could be directly obtained after carbonization without the need of washing removal of salts. Most importantly, the microporous specific surface area of the resultant porous carbon monoliths was dramatically increased up to 770 m2/g and the Brunauer–Emmett–Teller (BET) specific surface area was up to 1131 m2/g. That was because the salts NH4SCN as self-sacrificial templating helped to form more around 0.6 nm, 0.72 nm and 1.1 nm micropores. The self-sacrificial salt templating is also a suitable and feasible method for controlling the nanoporous structure of other porous materials. PMID:29671818

In situ grown hierarchical 50%BiOCl/BiOI hollow flowerlike microspheres on reduced graphene oxide nanosheets for enhanced visible-light photocatalytic degradation of rhodamine B

NASA Astrophysics Data System (ADS)

Su, Xiangde; Yang, Jinjin; Yu, Xiang; Zhu, Yi; Zhang, Yuanming

2018-03-01

50%BiOCl/BiOI/reduced graphene oxide (50%BiOCl/BiOI/rGO) composite photocatalyst was synthesized successfully by a facile one-step solvothermal route in this work. Reduction of graphene oxide (GO) took place in the process of solvothermal reaction and a new Bi-C bond between rGO and 50%BiOCl/BiOI was formed. The introduction of rGO affected the morphology of 50%BiOCl/BiOI, resulting in the transformation of 50%BiOCl/BiOI from solid microspheres to hollow microspheres. Both the introduction of rGO and formation of 50%BiOCl/BiOI hollow microspheres can facilitate the light absorption. The strong interaction between 50%BiOCl/BiOI and rGO and the electrical conductivity of rGO greatly improved the effective separation of photogenerated carriers. Hence, GOB-5 demonstrated the highest photocatalytic activity which was over twice of the pristine 50%BiOCl/BiOI in the presence of visible light. Mechanism study revealed that 50%BiOCl/BiOI generated electrons and holes in the presence of visible light, and holes together with rad O2- generated from reduction of O2 by electrons degraded the pollutant directly. Overall, this work provides an excellent reference to the synthesis of chemically bonded BiOX/BiOY (X, Y = Cl, Br, I)/rGO nanocomposite and helps to promote their applications in environmental protection and photoelectric conversion.

Low-Cost and Scaled-Up Production of Fluorine-Free, Substrate-Independent, Large-Area Superhydrophobic Coatings Based on Hydroxyapatite Nanowire Bundles.

PubMed

Chen, Fei-Fei; Yang, Zi-Yue; Zhu, Ying-Jie; Xiong, Zhi-Chao; Dong, Li-Ying; Lu, Bing-Qiang; Wu, Jin; Yang, Ri-Long

2018-01-09

To date, the scaled-up production and large-area applications of superhydrophobic coatings are limited because of complicated procedures, environmentally harmful fluorinated compounds, restrictive substrates, expensive equipment, and raw materials usually involved in the fabrication process. Herein, the facile, low-cost, and green production of superhydrophobic coatings based on hydroxyapatite nanowire bundles (HNBs) is reported. Hydrophobic HNBs are synthesised by using a one-step solvothermal method with oleic acid as the structure-directing and hydrophobic agent. During the reaction process, highly hydrophobic C-H groups of oleic acid molecules can be attached in situ to the surface of HNBs through the chelate interaction between Ca 2+ ions and carboxylic groups. This facile synthetic method allows the scaled-up production of HNBs up to about 8 L, which is the largest production scale of superhydrophobic paint based on HNBs ever reported. In addition, the design of the 100 L reaction system is also shown. The HNBs can be coated on any substrate with an arbitrary shape by the spray-coating technique. The self-cleaning ability in air and oil, high-temperature stability, and excellent mechanical durability of the as-prepared superhydrophobic coatings are demonstrated. More importantly, the HNBs are coated on large-sized practical objects to form large-area superhydrophobic coatings. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Solar Light Responsive Photocatalytic Activity of Reduced Graphene Oxide-Zinc Selenide Nanocomposite

NASA Astrophysics Data System (ADS)

Chakraborty, Koushik; Ibrahim, Sk; Das, Poulomi; Ghosh, Surajit; Pal, Tanusri

2017-10-01

Solution processable reduced graphene oxide-zinc selenide (RGO-ZnSe) nanocomposite has been successfully synthesized by an easy one-pot single-step solvothermal reaction. The RGO-ZnSe composite was characterized structurally and morphologically by the study of XRD analysis, SEM and TEM imaging. Reduction in graphene oxide was confirmed by FTIR spectroscopy analysis. Photocatalytic efficiency of RGO-ZnSe composite was investigated toward the degradation of Rhodamine B under solar light irradiation. Our study indicates that the RGO-ZnSe composite is catalytically more active compared to the controlled-ZnSe under the solar light illumination. Here, RGO plays an important role for photoinduced charge separation and subsequently hinders the electron-hole recombination probability that consequently enhances photocatalytic degradation efficiency. We expect that this type of RGO-based optoelectronics materials opens up a new avenue in the field of photocatalytic degradation of different organic water pollutants.

Solvothermal synthesis of nanocrystalline TiO 2 in toluene with surfactant

NASA Astrophysics Data System (ADS)

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

2003-10-01

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

Synthesis and characterization of a narrow size distribution of zinc oxide nanoparticles.

PubMed

Zak, A Khorsand; Razali, R; Majid, W H Abd; Darroudi, Majid

2011-01-01

Zinc oxide nanoparticles (ZnO-NPs) were synthesized via a solvothermal method in triethanolamine (TEA) media. TEA was utilized as a polymer agent to terminate the growth of ZnO-NPs. The ZnO-NPs were characterized by a number of techniques, including X-ray diffraction analysis, transition electron microscopy, and field emission electron microscopy. The ZnO-NPs prepared by the solvothermal process at 150°C for 18 hours exhibited a hexagonal (wurtzite) structure, with a crystalline size of 33 ± 2 nm, and particle size of 48 ± 7 nm. The results confirm that TEA is a suitable polymer agent to prepare homogenous ZnO-NPs.

Hierarchical TiO{sub 2} submicron-sized spheres for enhanced power conversion efficiency in dye-sensitized solar cells

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

Wang, Hao; State Key Laboratory of Solid Lubrication, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou 730000; Guo, Zhiguang, E-mail: zguo@licp.cas.cn

Hierarchical TiO{sub 2} submicron-sized sphere scattering layer, with relatively large surface area and effective light scattering, shows enhanced power conversion efficiency in dye-sensitized solar cells. - Highlights: • Hierarchical TiO{sub 2} submicron-sized spheres (TiO{sub 2} HSSs) with diameters of 400–600 nm were synthesized. • The HSSs composed of nanoparticles of ∼14 nm have a relatively large surface area of ∼35 m{sup 2}/g. • DSC exhibited the highest cell efficiency (6.23%) compared with ones with pure P25 (5.50%) or HSS (2.00%) photoanodes. - Abstract: Hierarchical TiO{sub 2} submicron-sized spheres (TiO{sub 2} HSSs) with diameters of 400–600 nm were synthesized by amore » facile one-step solvothermal method in ethanol solvent. The HSSs composed of nanoparticles of ∼14 nm have a relatively large surface area of ∼35 m{sup 2}/g. When applied as the scattering overlayer in dye-sensitized solar cells (DSCs), such TiO{sub 2} HSSs effectively improved light harvesting and led to the increase of photocurrent in DSCs. Furthermore, bilayer-structured photoanode also provided fast electron transportation and long electron lifetime as confirmed by electrochemical impedance spectra. As a result, DSC based on P25 nanoparticle underlayer and HSS-2 overlayer exhibited the highest cell efficiency (6.23%) compared with ones with pure P25 (5.50%) or HSS-2 (2.00%) photoanodes.« less

Enhanced photocatalytic performance of Er-doped Bi{sub 24}O{sub 31}Br{sub 10}: Facile synthesis and photocatalytic mechanism

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

Liu, Zhang Sheng, E-mail: lzsliu2008@hotmail.com; Liu, Zhi Lin; Liu, Jin Long

2016-04-15

Highlights: • Er-doped Bi{sub 24}O{sub 31}Br{sub 10} have been prepared via a one-pot solvothermal method. • Er doping drastically improves the photocatalytic activity of Bi{sub 24}O{sub 31}Br{sub 10}. • The enhanced activity is attributed to effective electron trapping and up-conversion process resulting from Er{sup 3+}. • Holes and super-oxide radicals are main active species. - Abstract: Erbium (Er) doped Bi{sub 24}O{sub 31}Br{sub 10} samples were successfully prepared by using a solvothermal method. The samples were characterized by XRD, XPS, SEM, TEM, BET, DRS, PL and EIS. The photocatalytic activity was evaluated by the degradation of rhodamine B (RhB) and methylmore » orange (MO) under visible light irradiation. The result shows that Er dopant induces a significant improvement in the photocatalytic activity. 1.0% Er–Bi{sub 24}O{sub 31}Br{sub 10} sample exhibits the best photocatalytic performance. The enhanced photocatalytic activity is attributed to the effective trapping of photogenerated electron by Er{sup 3+} ion and the up-conversion process resulting from Er dopant. In addition, it is found that holes and super-oxide radicals play main role in the photocatalytic degradation of RhB and MO.« less

Removal of brominated flame retardant from electrical and electronic waste plastic by solvothermal technique.

PubMed

Zhang, Cong-Cong; Zhang, Fu-Shen

2012-06-30

Brominated flame retardants (BFRs) in electrical and electronic (E&E) waste plastic are toxic, bioaccumulative and recalcitrant. In the present study, tetrabromobisphenol A (TBBPA) contained in this type of plastic was tentatively subjected to solvothermal treatment so as to obtain bromine-free plastic. Methanol, ethanol and isopropanol were examined as solvents for solvothermal treatment and it was found that methanol was the optimal solvent for TBBPA removal. The optimum temperature, time and liquid to solid ratio for solvothermal treatment to remove TBBPA were 90°C, 2h and 15:1, respectively. After the treatment with various alcohol solvents, it was found that TBBPA was finally transferred into the solvents and bromine in the extract was debrominated catalyzed by metallic copper. Bisphenol A and cuprous bromide were the main products after debromination. The morphology and FTIR properties of the plastic were generally unchanged after the solvothermal treatment indicating that the structure of the plastic maintained after the process. This work provides a clean and applicable process for BFRs-containing plastic disposal. Copyright © 2012 Elsevier B.V. All rights reserved.

Three-dimensional sulphur/nitrogen co-doped reduced graphene oxide as high-performance supercapacitor binder-free electrodes

NASA Astrophysics Data System (ADS)

Huo, Jinghao; Zheng, Peng; Wang, Xiaofei; Guo, Shouwu

2018-06-01

Sulphur/nitrogen co-doped reduced graphene oxide (SNG) aerogels were prepared by a simple solvothermal method with l-cysteine-assisted in ethylene glycol. The morphology and composition tests showed that the S/N heteroatoms were evenly distributed on SNG microsheets, and these microsheets were further composed of SNG aerogels with three-dimensional (3D) porous structure. The cyclic voltammetry and galvanostatic charge/discharge tests illustrated the SNG bind-free electrode possessed electric double-layer capacitance and pseudocapacitance, and had a capacitance of 254 F g-1 at a current density of 1 A g-1. After the 5000 cycles tests, the capacitance retained 83.54% at a current density of 2 A g-1. Meanwhile, the electrochemical impedance spectroscopy data shown the electrode materials had excellent capacity and good conductivity. Hence, the SNG aerogel prepared by l-cysteine-assisted solvothermal method is a great material for high-performance supercapacitors.

[100]-Oriented LiFePO4 Nanoflakes toward High Rate Li-Ion Battery Cathode.

PubMed

Li, Zhaojin; Peng, Zhenzhen; Zhang, Hui; Hu, Tao; Hu, Minmin; Zhu, Kongjun; Wang, Xiaohui

2016-01-13

[100] is believed to be a tough diffusion direction for Li(+) in LiFePO4, leading to the belief that the rate performance of [100]-oriented LiFePO4 is poor. Here we report the fabrication of 12 nm-thick [100]-oriented LiFePO4 nanoflakes by a simple one-pot solvothermal method. The nanoflakes exhibit unexpectedly excellent electrochemical performance, in stark contrast to what was previously believed. Such an exceptional result is attributed to a decreased thermodynamic transformation barrier height (Δμb) associated with increased active population.

Synthesis and visible light photocatalytic property of polyhedron-shaped AgNbO3.

PubMed

Li, Guoqiang; Yan, Shicheng; Wang, Zhiqiang; Wang, Xiangyan; Li, Zhaosheng; Ye, Jinhua; Zou, Zhigang

2009-10-28

Polyhedron-shaped AgNbO3 photocatalysts were synthesized by solvothermal and liquid-solid methods. Their photocatalytic properties were evaluated from the photocatalytic O2 evolution under visible light irradiation. The polyhedron-shaped AgNbO3 was induced to grow by shaped silver particles followed by the free-growth model. The photocatalytic results indicate that the polyhedron-shaped morphology is favourable for the photocatalytic O2 evolution under visible light irradiation in comparison with the spherical one. Furthermore, the Cu doping on the surface would enhance the visible light photocatalytic activity significantly.

Enhanced Photodegradation of Paper-making Wastewater by Two-dimensional Heterojunction of Titania Plates with Exposed {001} Facets-Graphene Composite

NASA Astrophysics Data System (ADS)

Liu, Yiming; Wang, Chunxiao; Shen, Tingting; Liu, Qing; Sun, Jing; Wang, Xikui

2017-05-01

As a typical industrial wastewater, paper-making wastewater contains a number of toxic compounds which is harmful to the environment. In this report, TiO2 plates/graphene composite based 2D-2D heterojunctions were synthesized via one-step solvothermal method. The structure and morphology of the as-prepared composite were characterized by Transmission electron microscope (TEM), X-ray diffraction (XRD), and Raman spectra. The results indicated that sheet-like anatase TiO2 with exposed {001} facets was anchored on the graphene nanosheet. In the degradation of papermaking wastewater under UV irradiation, the as synthesized TiO2 plates/graphene composite exhibited higher photocatalytic performance than the commercial Degussa P25. The effects of the amount of catalyst, H2O2 dosage, pH and the time of light irradiation on the photocatalytic efficiency were also discussed. At the optimum condition of 1.0 g ·L-1 RGO/TiO2 with the dosage of 0.3% H2O2 at pH=3, the removal rate of CODCr and chroma could reach 86% and 100%, respectively in 8 h. This work could provide new insights into the wastewater treatment with a well-defined nanocomposite.

Influence of Fe3O4/Fe-phthalocyanine decorated graphene oxide on the microwave absorbing performance

NASA Astrophysics Data System (ADS)

Li, Jingwei; Wei, Junji; Pu, Zejun; Xu, Mingzhen; Jia, Kun; Liu, Xiaobo

2016-02-01

Novel graphene oxide@Fe3O4/iron phthalocyanine (GO@Fe3O4/FePc) hybrid materials were prepared through a facile one-step solvothermal method with graphene oxide (GO) sheets as template in ethylene glycol. The morphology and structure of the hybrid materials were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared spectrophotometer (FTIR) and X-ray diffraction (XRD), respectively. The results indicated that the monodispersed Fe3O4/FePc hybrid microspheres were uniformly self-assembled along the surface of GO sheets through electrostatic attraction and the morphology can be tuned by controlling the amount of 4,4‧-bis(3,4-dicyanophenoxy)biphenyl (BPH). As the BPH content increases, magnetization measurement of the GO@Fe3O4/FePc hybrid materials showed that the coercivity increased, while saturation magnetizations decreased. Electromagnetic properties of the hybrid materials were measured in the range of 0.5-18.0 GHz. The microwave absorbing performance enhanced with the increase of BPH content and a maximum reflection loss of -27.92 dB was obtained at 10.8 GHz when the matching thickness was 2.5 mm. Therefore, the novel electromagnetic hybrid materials can be considered as potential materials in the microwave absorbing field.

Solvothermal synthesis and high optical performance of three-dimensional sea-urchin-like TiO{sub 2}

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

Zhou, Yi, E-mail: zhouyihn@163.com; Wang, Yutang; Li, Mengyao

Graphical abstract: I–V characteristics of different TiO{sub 2} microspheres based DSSCs (a) 3D sphere-like, (b) 3D flower-like, (c) 3D sea-urchin-like. - Highlights: • 3D sea-urchin-like TiO{sub 2} was synthesized by solvothermal method. • The effects of preparation parameters on the microstructure of the microspheres were investigated. • The photoelectric properties of 3D sea-urchin-like TiO{sub 2} were studied upon DSSCs. • The PCE of the 3D sea-urchin-like TiO{sub 2} was higher than that of other morphologies. - Abstract: Three-dimensional (3D) sea-urchin-like TiO{sub 2} microspheres were successfully synthesised by solvothermal method. The effects of preparation parameters including reaction temperature, concentration and massmore » fraction of precursor, and solvent volume on the microstructure of the microspheres were investigated. Results of scanning electron microscopy showed that the preparation parameters played a critical role in the morphology of 3D sea-urchin-like TiO{sub 2}. In addition, when the sea-urchin-like TiO{sub 2} nanostructures were used as the dye-sensitized solar cells (DSSCs) anode, the power-conversion efficiency was higher than that of other morphologies, which was due to the special 3D hierarchical nanostructure, large specific surface area, and enhanced absorption of UV–vis of the TiO{sub 2} nanostructures.« less

Structural and Morphological Tuning of LiCoPO4 Materials Synthesized by Solvo-Thermal Methods for Li-Cell Applications

PubMed Central

Manzi, Jessica; Curcio, Mariangela; Brutti, Sergio

2015-01-01

Olivine-type lithium metal phosphates (LiMPO4) are promising cathode materials for lithium-ion batteries. LiFePO4 (LFP) is commonly used in commercial Li-ion cells but the Fe3+/Fe2+ couple can be usefully substituted with Mn3+/Mn2+, Co3+/Co2+, or Ni3+/Ni2+, in order to obtain higher redox potentials. In this communication we report a systematic analysis of the synthesis condition of LiCoPO4 (LCP) using a solvo-thermal route at low temperature, the latter being a valuable candidate to overcome the theoretical performances of LFP. In fact, LCP shows higher working potential (4.8 V vs. 3.6 V) compared to LFP and similar theoretical capacity (167 mAh·g−1). Our goal is to show the effect of the synthesis condition of the ability of LCP to reversibly cycle lithium in electrochemical cells. LCP samples have been prepared through a solvo-thermal method in aqueous-non aqueous solvent blends. Different Co2+ salts have been used to study the effect of the anion on the crystal growth as well as the effect of solution acidity, temperature and reaction time. Materials properties have been characterized by Fast-Fourier transform infrared spectroscopy, X-ray diffraction and scanning electron microscopies. The correlation between structure/morphology and electrochemical performances has been investigated by galvanostatic charge-discharge cycles. PMID:28347117

Surfactant 1-Hexadecyl-3-methylimidazolium Chloride Can Convert One-Dimensional Viologen Bromoplumbate into Zero-Dimensional.

PubMed

Liu, Guangfeng; Liu, Jie; Nie, Lina; Ban, Rui; Armatas, Gerasimos S; Tao, Xutang; Zhang, Qichun

2017-05-15

A zero-dimensional N,N'-dibutyl-4,4'-dipyridinium bromoplumbate, [BV] 6 [Pb 9 Br 30 ], with unusual discrete [Pb 9 Br 30 ] 12- anionic clusters was prepared via a facile surfactant-mediated solvothermal process. This bromoplumbate exhibits a narrower optical band gap relative to the congeneric one-dimensional viologen bromoplumbates.

A multi-purpose reaction cell for the investigation of reactions under solvothermal conditions

NASA Astrophysics Data System (ADS)

Heidenreich, N.; Rütt, U.; Köppen, M.; Inge, A. Ken; Beier, S.; Dippel, A.-C.; Suren, R.; Stock, N.

2017-10-01

A new versatile and easy-to-use remote-controlled reactor setup aimed at the analysis of chemical reactions under solvothermal conditions has been constructed. The reactor includes a heating system that can precisely control the temperature inside the reaction vessels in a range between ambient temperature and 180 °C. As reaction vessels, two sizes of commercially available borosilicate vessels (Vmax = 5 and 11 ml) can be used. The setup furthermore includes the option of stirring and injecting of up to two liquid additives or one solid during the reaction to initiate very fast reactions, quench reactions, or alter chemical parameters. In addition to a detailed description of the general setup and its functionality, three examples of studies conducted using this setup are presented.

Synthesis and characterization of CdS/BiPO{sub 4} heterojunction photocatalyst

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

Chen, Daimei, E-mail: chendaimei@cugb.edu.cn; Kuang, Zheng; Zhu, Qian

2015-06-15

Highlights: • A CdS/BiPO{sub 4} heterojunction was prepared by the solvothermal method. • The CdS/BiPO{sub 4} composite has the higher photocatalytic activity than the individual ones. • The optimal mass ratio of CdS to BiPO{sub 4} was 0.5. • The heterojunction structure of CdS/BiPO{sub 4} induces an effective electron–hole separation. - Abstract: A series of CdS/BiPO{sub 4} heterojunction photocatalysts with the visible-light response were synthesized by the solvothermal method. The resulting products were characterized by X-ray diffraction, Transmission electron microscopy, X-ray photoelectron spectroscopy, and UV–vis diffuse reflection spectroscopy. CdS nanoparticles with the size at range of 5–7 nm were immobilizedmore » on the surface of BiPO{sub 4} nanorods. The CdS/BiPO{sub 4} composite exhibited much higher photodegradation rate of methylene blue under visible light irradation compared to the pure CdS and BiPO{sub 4}. The optimal mass ratio of CdS to BiPO{sub 4} was 0.5, the photodegradation rate of which is 2.1 times higher than that of CdS. The enhancement of photocatalytic activity is attributed to the heterojunction structure of CdS/BiPO{sub 4} composite which induced the effective electron–hole separation between CdS and BiPO{sub 4}.« less

Solvothermal synthesis, characterization and optical properties of ZnO, ZnO-MgO and ZnO-NiO, mixed oxide nanoparticles

NASA Astrophysics Data System (ADS)

Aslani, Alireza; Arefi, Mohammad Reza; Babapoor, Aziz; Amiri, Asghar; Beyki-Shuraki, Khalil

2011-03-01

ZnO-MgO and ZnO-NiO mixed oxides nanoparticles were produced from a solution containing Zinc acetate, Mg and Ni nitrate by Solvothermal method. The calcination process of the ZnO-MgO and ZnO-NiO composites nanoparticles brought forth polycrystalline two-phase ZnO-MgO and ZnO-NiO nanoparticles of 40-80 nm in diameters. ZnO, MgO and NiO were crystallized into würtzite and rock salt structures, respectively. The optical properties of ZnO-MgO and ZnO-NiO nanoparticles were obtained by solid state UV and solid state florescent. The XRD, SEM and Raman spectroscopies of these nanoparticles were analyzed.

Synthesis and structural properties of Ba(1-x)LaxTiO3 perovskite nanoparticles fabricated by solvothermal synthesis route

NASA Astrophysics Data System (ADS)

Puli, Venkata Sreenivas; Adireddy, Shiva; Elupula, Ravinder; Molugu, Sudheer; Shipman, Josh; Chrisey, Douglas B.

2017-05-01

We report the successful synthesis and structural characterization of barium lanthanum titanate Ba(1-x)LaxTiO3 (x=0.003,0.006,0.010) nanoparticles. The colloidal nanoparticles were prepared with high yield by a solvothermal method at temperatures as low as 150°C for 24h. The as-prepared nanopowders were characterized using X-ray diffraction (XRD), transmission electron microscopy (TEM), and Raman spectroscopy. The XRD studies revealed pseudo-cubic crystalline structure, with no impurity phases at room temperature. However ferroelectric tetragonal modes were clearly observed using Raman spectroscopy measurements. From TEM measurements, uniformly sized BLT nanoparticles were observed. Selected area diffraction TEM images revealed polycrystalline perovskite ring patterns, identified as corresponding to the tetragonal phase.

Antifungal activity of gold nanoparticles prepared by solvothermal method

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

Ahmad, Tokeer, E-mail: tahmad3@jmi.ac.in; Wani, Irshad A.; Lone, Irfan H.

2013-01-15

Graphical abstract: Gold nanoparticles (7 and 15 nm) of very high surface area (329 and 269 m{sup 2}/g) have been successfully synthesized through solvothermal method by using tin chloride and sodium borohydride as reducing agents. As-prepared gold nanoparticles shows very excellent antifungal activity against Candida isolates and activity increases with decrease in the particle size. Display Omitted Highlights: ► Effect of reducing agents on the morphology of gold nanoparticles. ► Highly uniform and monodisperse gold nanoparticles (7 nm). ► Highest surface area of gold nanoparticles (329 m{sup 2/}g). ► Excellent antifungal activity of gold nanoparticles against Candida strains. -- Abstract:more » Gold nanoparticles have been successfully synthesized by solvothermal method using SnCl{sub 2} and NaBH{sub 4} as reducing agents. X-ray diffraction studies show highly crystalline and monophasic nature of the gold nanoparticles with face centred cubic structure. The transmission electron microscopic studies show the formation of nearly spherical gold nanoparticles of average size of 15 nm using SnCl{sub 2}, however, NaBH{sub 4} produced highly uniform, monodispersed and spherical gold nanoparticles of average grain size of 7 nm. A high surface area of 329 m{sup 2}/g for 7 nm and 269 m{sup 2}/g for 15 nm gold nanoparticles was observed. UV–vis studies assert the excitations over the visible region due to transverse and longitudinal surface plasmon modes. The gold nanoparticles exhibit excellent size dependant antifungal activity and greater biocidal action against Candida isolates for 7 nm sized gold nanoparticles restricting the transmembrane H{sup +} efflux of the Candida species than 15 nm sized gold nanoparticles.« less

Tin phosphide-based anodes for sodium-ion batteries: synthesis via solvothermal transformation of Sn metal and phase-dependent Na storage performance

PubMed Central

Shin, Hyun-Seop; Jung, Kyu-Nam; Jo, Yong Nam; Park, Min-Sik; Kim, Hansung; Lee, Jong-Won

2016-01-01

There is a great deal of current interest in the development of rechargeable sodium (Na)-ion batteries (SIBs) for low-cost, large-scale stationary energy storage systems. For the commercial success of this technology, significant progress should be made in developing robust anode (negative electrode) materials with high capacity and long cycle life. Sn-P compounds are considered promising anode materials that have considerable potential to meet the required performance of SIBs, and they have been typically prepared by high-energy mechanical milling. Here, we report Sn-P-based anodes synthesised through solvothermal transformation of Sn metal and their electrochemical Na storage properties. The temperature and time period used for solvothermal treatment play a crucial role in determining the phase, microstructure, and composition of the Sn-P compound and thus its electrochemical performance. The Sn-P compound prepared under an optimised solvothermal condition shows excellent electrochemical performance as an SIB anode, as evidenced by a high reversible capacity of ~560 mAh g−1 at a current density of 100 mA g−1 and cycling stability for 100 cycles. The solvothermal route provides an effective approach to synthesising Sn-P anodes with controlled phases and compositions, thus tailoring their Na storage behaviour. PMID:27189834

Utilization of solvothermally grown InP/ZnS quantum dots as wavelength converters for fabrication of white light-emitting diodes.

PubMed

Jang, Eun-Pyo; Yang, Heesun

2013-09-01

This work reports on a simple solvothermal synthesis of InP/ZnS core/shell quantum dots (QDs) using a much safer and cheaper phosphorus precursor of tris(dimethylamino)phosphine than the most popularly chosen tris(trimethylsilyl)phosphine. The band gap of InP QDs is facilely controlled by varying the solvothermal core growth time (4 vs. 6 h) with a fixed temperature of 150 degrees C, and the successive solvothermal ZnS shelling at 220 degrees C for 6 h results in green- and yellow-emtting InP/ZnS QD with emission quantum yield of 41-42%. The broad size distribution of as-synthesized InP/ZnS QDs, which appears to be inherent in the current solvothermal approach, is improved by a size-selective sorting procedure, and the emission properties of the resulting size-sorted QD fractions are investigated. To produce white emission for general lighting source, a blue light-emitting diode (LED) is combined with non-size-soroted green or yellow QDs as wavelength converters. Furthermore, the QD-LED that includes a blend of green and yellow QDs is fabricated to generate a white lighting source with an enhanced color rendering performance, and its electroluminescent properties are characterized in detail.

Solvothermal synthesis of α-PbO from lead dioxide and its electrochemical performance as a positive electrode material

NASA Astrophysics Data System (ADS)

Gao, Pengran; Liu, Yi; Bu, Xianfu; Hu, Meng; Dai, Yuan; Gao, Xiaorui; Lei, Lixu

2013-11-01

Lead acid batteries have been widely used and have dominated the global secondary battery market. It is very important to recycle the spent batteries efficiently to eliminate possible pollution and to ensure sustainable production. In this paper, we report our investigation on the solvothermal treatment of PbO2, which is one of the model compounds for the positive active mixture, in methanol and the subsequent calcination of its product. The results show that the solvothermal treatment of PbO2 in pure methanol at 140 °C can produce a mixture of PbO and lead oxide carbonate, which can be calcined at a temperature below 500 °C to produce α-PbO. The as-prepared PbO powders are rod-like particles of about 0.5 micrometer in diameter and several micrometers in length, which can achieve a high discharge capacity of 165 mAh g-1 at the discharge current density of 5 mA g-1, and more than 90 mAh g-1 at 200 mA g-1 with excellent cycle stability. This study demonstrates a new way for the reuse of lead dioxide in spent lead acid batteries to produce highly active PbO.

Magnetic and photocatalytic studies on Zn1-xMgxFe2O4 nanocolloids synthesized by solvothermal reflux method.

PubMed

Manohar, A; Krishnamoorthi, C

2017-12-01

Biocompatible magnetic semiconductor Zn 1-x Mg x Fe 2 O 4 (x=0, 0.1, 0.3, 0.5 & 0.7) nanoparticles of around 10nm diameter were synthesized by solvothermal reflux method. The method produces well separated and narrow size distributed nanoparticles. Crystal structure, morphology, particles surface properties, surfactant quantity, colloidal stability, magnetic properties and photocatalytic properties of the synthesized nanoparticles were studied. Different characterizations confirmed that all compounds were single crystals and superparamagnetic at room temperature. Saturation mass magnetization (M s =57.5emu/g) enhances with substituent Mg 2+ concentration due to promotion of mixed spinel (normal and inverse) structure. Photocatalytic activity of all synthesized magnetic semiconductor nanoparticles were studied through methylene blue degradation. The degradation of 98% methylene blue was observed on 60 min irradiation of light. It is observed that photocatalytic activity slightly enhances with substituent Mg 2+ concentration. The synthesized biocompatible magnetic semiconductor nanoparticles can be utilized as photocatalysts and could also be recycled and separated by applying an external magnetic field. Copyright © 2017 Elsevier B.V. All rights reserved.

Solvothermal transformation of a calcium oleate precursor into large-sized highly ordered arrays of ultralong hydroxyapatite microtubes.

PubMed

Lu, Bing-Qiang; Zhu, Ying-Jie; Chen, Feng; Qi, Chao; Zhao, Xin-Yu; Zhao, Jing

2014-06-02

Hydroxyapatite (HAP), a well-known member of the calcium phosphate family, is the major inorganic component of bones and teeth in vertebrates. The highly ordered arrays of HAP structures are of great significance for hard tissue repair and for understanding the formation mechanisms of bones and teeth. However, the synthesis of highly ordered HAP structure arrays remains a great challenge. In this work, inspired by the ordered structure of tooth enamel, we have successfully synthesized three-dimensional bulk materials with large sizes (millimeter scale) that are made of highly ordered arrays of ultralong HAP microtubes (HOAUHMs) by solvothermal transformation of calcium oleate precursor. The core-shell-structured oblate sphere consists of a core that is composed of HAP nanorods and a shell that consists of highly ordered HAP microtube arrays. The prepared HOAUHMs are large: 6.0 mm in diameter and up to 1.4 mm in thickness. With increasing solvothermal reaction time, the HOAUHMs grow larger; the microtubes become more uniform and more ordered. This work provides a new synthetic method for synthesizing highly ordered arrays of uniform HAP ultralong microtubes that are promising for biomedical applications. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Method to synthesize lanthanide fluoride materials from lanthanide fluorinated alkoxides

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

Boyle, Timothy J.

Lanthanide fluorinated alkoxide derivatives can be synthesized from the alcoholysis reaction of the lanthanide bis-trimethylsilyl amide and an excess amount of hexafluoro iso-propanol. Nanoparticles can be formed from the lanthanide fluorinated alkoxide derivatives by a solvothermal or solution precipitation process.

Metal-organic framework materials with ultrahigh surface areas

DOEpatents

Farha, Omar K.; Hupp, Joseph T.; Wilmer, Christopher E.; Eryazici, Ibrahim; Snurr, Randall Q.; Gomez-Gualdron, Diego A.; Borah, Bhaskarjyoti

2015-12-22

A metal organic framework (MOF) material including a Brunauer-Emmett-Teller (BET) surface area greater than 7,010 m.sup.2/g. Also a metal organic framework (MOF) material including hexa-carboxylated linkers including alkyne bond. Also a metal organic framework (MOF) material including three types of cuboctahedron cages fused to provide continuous channels. Also a method of making a metal organic framework (MOF) material including saponifying hexaester precursors having alkyne bonds to form a plurality of hexa-carboxylated linkers including alkyne bonds and performing a solvothermal reaction with the plurality of hexa-carboxylated linkers and one or more metal containing compounds to form the MOF material.

Hollow Rodlike MgF2 with an Ultralow Refractive Index for the Preparation of Multifunctional Antireflective Coatings.

PubMed

Bao, Lei; Ji, Zihan; Wang, Hongning; Chen, Ruoyu

2017-06-27

Antireflective coatings with superhydrophobic, self-cleaning, and wide-spectrum high-transmittance properties and good mechanical strength have important practical value. In this research, hollow nanorod-like MgF 2 sols with different void volumes were prepared by a template-free solvothermal method to further obtain hollow nanorod-like MgF 2 crystals with an ultralow refractive index of 1.14. Besides, a MgF 2 coating with an adjustable refractive index of 1.10-1.35 was also prepared by the template-free solvothermal method. Then through the combination of base/acid two-step-catalyzed TEOS and hydroxyl modification on the surface of nanosilica spheres, the SiO 2 coating with good mechanical strength, a flat surface, and a refractive index of 1.30-1.45 was obtained. Double-layer broadband antireflective coatings with an average transmittance of 99.6% at 400-1400 nm were designed using the relevant optical theory. After the coating thickness was optimized by the dip-coating method, the double-layer antireflective coatings, whose parameters were consistent with those designed by the theory, were obtained. The bottom layer was a SiO 2 coating with a refractive index of 1.34 and a thickness of 155 nm, and the top layer was a hollow rodlike MgF 2 coating with a refractive index of 1.10 and a thickness of 165 nm. The average transmittance of the obtained MgF 2 -SiO 2 antireflective coatings was 99.1% at 400-1400 nm, which was close to the theoretical value. The hydrophobic angle of the coating surface reached 119° at first, and the angle further reached 152° after conducting surface modification by PFOTES. In addition, because the porosity of the coating surface was only 10.7%, the pencil hardness of the coating surface was 5 H and the critical load Lc was 27.05 N. In summary, the obtained antireflective coatings possessed superhydrophobic, self-cleaning, and wide-spectrum high-transmittance properties and good mechanical strength.

Two Ti13-oxo-clusters showing non-compact structures, film electrode preparation and photocurrent properties.

PubMed

Hou, Jin-Le; Luo, Wen; Wu, Yin-Yin; Su, Hu-Chao; Zhang, Guang-Lin; Zhu, Qin-Yu; Dai, Jie

2015-12-14

Two benzene dicarboxylate (BDC) and salicylate (SAL) substituted titanium-oxo-clusters, Ti13O10(o-BDC)4(SAL)4(O(i)Pr)16 (1) and Ti13O10(o-BDC)4(SAL-Cl)4(O(i)Pr)16 (2), are prepared by one step in situ solvothermal synthesis. Single crystal analysis shows that the two Ti13 clusters take a paddle arrangement with an S4 symmetry. The non-compact (non-sphere) structure is stabilized by the coordination of BDC and SAL. Film photoelectrodes are prepared by the wet coating process using the solution of the clusters and the photocurrent response properties of the electrodes are studied. It is found that the photocurrent density and photoresponsiveness of the electrodes are related to the number of coating layers and the annealing temperature. Using ligand coordinated titanium-oxo-clusters as the molecular precursors of TiO2 anatase films is found to be effective due to their high solubility, appropriate stability in solution and hence the easy controllability.

Montmorillonite-supported Ag/TiO(2) nanoparticles: an efficient visible-light bacteria photodegradation material.

PubMed

Wu, Tong-Shun; Wang, Kai-Xue; Li, Guo-Dong; Sun, Shi-Yang; Sun, Jian; Chen, Jie-Sheng

2010-02-01

Montmorillonite (MMT)-supported Ag/TiO(2) composite (Ag/TiO(2)/MMT) has been prepared through a one-step, low-temperature solvothermal technique. Powder X-ray diffraction (XRD) and transmission electron microscopy (TEM) reveal that the Ag particles coated with TiO(2) nanoparticles are well-dispersed on the surface of MMT in the composite. As a support for the Ag/TiO(2) composite, the MMT prevents the loss of the catalyst during recycling test. This Ag/TiO(2)/MMT composite exhibits high photocatalytic activity and good recycling performance in the degradation of E. coli under visible light. The high visible-light photocatalytic activity of the Ag/TiO(2)/MMT composite is ascribed to the increase in surface active centers and the localized surface plasmon effect of the Ag nanoparticles. The Ag/TiO(2)/MMT materials with excellent stability, recyclability, and bactericidal activities are promising photocatalysts for application in decontamination.

A sea cucumber-like BiOBr nanosheet/Zn2GeO4 nanorod heterostructure for enhanced visible light driven photocatalytic activity

NASA Astrophysics Data System (ADS)

Zhang, Zhiping; Ge, Xin; Zhang, Xueyu; Duan, Lianfeng; Li, Xuesong; Yang, Yue; Lü, Wei

2018-01-01

In present work, a two-step hydrothermal/solvothermal method was developed to fabricate sea cucumber-like p-n heterojunctions of p-BiOBr/n-Zn2GeO4. The BiOBr nanosheets were grafted onto the surface of Zn2GeO4 nanorods. BiOBr/Zn2GeO4 nanocomposites exhibit remarkable photocatalytic activity under visible-light irradiation, and photocatalytic activity was studied in the catalytic test of rhodamine B decolorization. The mechanism for improved photocatalytic activity is interpreted in terms of the formation of type II band alignment between BiOBr and Zn2GeO4, which is confirmed by UV-vis diffuse absorption and VB-XPS spectra. BiOBr nanosheet as an admirable electron transport medium provide desirable specific surface area for the nanocomposite and a suitable band gap for heterojunction structure. Furthermore, scavenger experiments confirmed that h+ and {{{{O}}}2}\\cdot - were the main oxygen active species in the decolorization process.

Solvothermal synthesis of gallium-indium-zinc-oxide nanoparticles for electrolyte-gated transistors.

PubMed

Santos, Lídia; Nunes, Daniela; Calmeiro, Tomás; Branquinho, Rita; Salgueiro, Daniela; Barquinha, Pedro; Pereira, Luís; Martins, Rodrigo; Fortunato, Elvira

2015-01-14

Solution-processed field-effect transistors are strategic building blocks when considering low-cost sustainable flexible electronics. Nevertheless, some challenges (e.g., processing temperature, reliability, reproducibility in large areas, and cost effectiveness) are requirements that must be surpassed in order to achieve high-performance transistors. The present work reports electrolyte-gated transistors using as channel layer gallium-indium-zinc-oxide nanoparticles produced by solvothermal synthesis combined with a solid-state electrolyte based on aqueous dispersions of vinyl acetate stabilized with cellulose derivatives, acrylic acid ester in styrene and lithium perchlorate. The devices fabricated using this approach display a ION/IOFF up to 1 × 10(6), threshold voltage (VTh) of 0.3-1.9 V, and mobility up to 1 cm(2)/(V s), as a function of gallium-indium-zinc-oxide ink formulation and two different annealing temperatures. These results validates the usage of electrolyte-gated transistors as a viable and promising alternative for nanoparticle based semiconductor devices as the electrolyte improves the interface and promotes a more efficient step coverage of the channel layer, reducing the operating voltage when compared with conventional dielectrics gating. Moreover, it is shown that by controlling the applied gate potential, the operation mechanism of the electrolyte-gated transistors can be modified from electric double layer to electrochemical doping.

Effects of alcohol solvents on anatase TiO2 nanocrystals prepared by microwave-assisted solvothermal method

NASA Astrophysics Data System (ADS)

Wu, Yu-Chun; Tai, Yu-Chuen

2013-06-01

The effects of solvents on the anatase crystallite size prepared by sol-gel microwave-assisted solvothermal method were investigated in this study. Eight different alcohol solvents classified into two groups, i.e. primary and secondary/ternary alcohols, were used as reaction media and the effects of solvent properties, such as dielectric constant, boiling point, and internal pressure during the solvothermal process, on the crystallite size and shape were analyzed. According to the experimental results, selecting the solvent type allowed not only the alteration of the crystallite size but also the crystallite shape without the need of any additives. The boiling point of solvent was determined as the major factor influencing the crystallite size. Among the solvents with similar boiling points, the solvent with a higher carbon number produced the smaller crystallite size because of steric hindrance effect. In addition, the carboxyl groups dissociated from the alcohol solvent can play a role as a structural capping agent to retard the anatase crystal growth along the [001] direction and led to a rectangular crystallite shape with preferred development in {001} facets. On the other hand, the alcoholysis reaction was found easily occurred between the primary alcohol and isopropoxide that effectively limited the hydrolysis and condensation processes but also suppressed the structural capping effect. Therefore, the anatase crystals prepared in the primary alcohols became exceptionally small and showed spherical shape. Finally, the anatase crystals prepared using isopropanol demonstrated the highest photocatalytic activity due to its evident preferred crystallization in the {001} facets.

Highly efficient decomposition of organic dye by aqueous-solid phase transfer and in situ photocatalysis using hierarchical copper phthalocyanine hollow spheres.

PubMed

Zhang, Mingyi; Shao, Changlu; Guo, Zengcai; Zhang, Zhenyi; Mu, Jingbo; Zhang, Peng; Cao, Tieping; Liu, Yichun

2011-07-01

The hierarchical tetranitro copper phthalocyanine (TNCuPc) hollow spheres were fabricated by a simple solvothermal method. The formation mechanism was proposed based on the evolution of morphology as a function of solvothermal time, which involved the initial formation of nanoparticles followed by their self-aggregation to microspheres and transformation into hierarchical hollow spheres by Ostwald ripening. Furthermore, the hierarchical TNCuPc hollow spheres exhibited high adsorption capacity and excellent simultaneously visible-light-driven photocatalytic performance for Rhodamine B (RB) under visible light. A possible mechanism for the "aqueous-solid phase transfer and in situ photocatalysis" was suggested. Repetitive tests showed that the hierarchical TNCuPc hollow spheres maintained high catalytic activity over several cycles, and it had a better regeneration capability under mild conditions.

Highly flexible sub-1 nm tungsten oxide nanobelts as efficient desulfurization catalysts.

PubMed

He, Jie; Liu, Huiling; Xu, Biao; Wang, Xun

2015-03-01

Ultrathin tungsten oxide nanobelts are successfully synthesized via a facile solvothermal method. Sub-1 nm thickness and hydrophobic surface property endow the nanobelts with flexibility, viscosity, gelation, and good catalytic performance in oxidative desulfurization. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

One-Pot Synthesis of Graphene-Supported Monodisperse Pd Nanoparticles as Catalyst for Formic Acid Electro-oxidation

PubMed Central

Yang, Sudong; Dong, Jing; Yao, Zhaohui; Shen, Chengmin; Shi, Xuezhao; Tian, Yuan; Lin, Shaoxiong; Zhang, Xiaogang

2014-01-01

To synthesize monodisperse palladium nanoparticles dispersed on reduced graphene oxide (RGO) sheets, we have developed an easy and scalable solvothermal reduction method from an organic solution system. The RGO-supported palladium nanoparticles with a diameter of 3.8 nm are synthesized in N-methyl-2-pyrrolidone (NMP) and in the presence of oleylamine and trioctylphosphine, which facilitates simultaneous reduction of graphene oxide and formation of Pd nanocrystals. So-produced Pd/RGO was tested for potential use as electrocatalyst for the electro-oxidation of formic acid. Pd/RGO catalyzes formic acid oxidation very well compared to Pd/Vulcan XC-72 catalyst. This synthesis method is a new way to prepare excellent electrocatalysts, which is of great significance in energy-related catalysis. PMID:24675779

Processable Conducting Polyaniline, Carbon Nanotubes, Graphene and Their Composites

NASA Astrophysics Data System (ADS)

Wang, Kan

Good processability is often required for applications of conducting materials like polyaniline (PANI), carbon nanotubes (CNTs) and graphene. This can be achieved by either physical stabilization or chemical functionalization. Functionalization usually expands the possible applications for the conducting materials depending on the properties of the functional groups. Processable conducting materials can also be combined with other co-dissolving materials to prepare composites with desired chemical and physical properties. Polyanilines (PANI) doped with dodecylbenzenesulfonic acid (DBSA) are soluble in many organic solvents such as chloroform and toluene. Single wall carbon nanotubes (SWCNTs) can be dispersed into PANI/DBSA to form homogeneous solutions. PANI/DBSA functions as a conducting surfactant for SWCNTs. The mixture can be combined with two-parts polyurethanes that co-dissolve in the organic solvent to produce conducting polymer composites. The composite mixtures can be applied onto various substrates by simple spray-on methods to obtain transparent and conducting coatings. Graphene, a single layer of graphite, has drawn intense interest for its unique properties. Processable graphene has been produced in N-methyl-2-pyrrolidone (NMP) by a one-step solvothermal reduction of graphite oxide without the aid of any reducing reagent and/or surfactant. The as-synthesized graphene disperses well in a variety of organic solvents such as dimethylsulfoxide (DMSO), ethanol and tetrahydrogenfuran (THF). The conductivity of solvothermal reduced graphite oxide is comparable to hydrazine reduced graphite oxide. Attempts were made to create intrinsically conducting glue comparable to mussel adhesive protiens using polyaniline and graphene. Mussels can attach to a variety of substrates under water. Catechol residue in 3,4-dihydroxyphenylalanine (L-DOPA) is the key to the wet adhesion. Tyrosine and phosphoserine with primary alkyl amine groups also participate in adhesion. A novel water soluble synthetic mussel adhesive containing both catechol and amine groups are synthesized in a simple approach. A polyallylamine backbone is used to take the place of the polyamide chain. Catechol is appended to the backbone as the key cross-linking group. Compared to polyallyamine, poly[N-(3,4- dihydroxybenzylidene)allylamine] exhibits good adhesion under alkaline water due to moderate cross-linking. When exposed to cross-linkers, this synthetic mussel adhesive can form a hydrogel at a very low concentration. Various methods were tried to attach catechol group onto polyaniline and graphene to make synthetic conductive mussel adhesive. Although the chemistry proved to be successful, the material doesn't show great adhesion to selected substrates probably due the nature of the backbone and difficulties associated with its processability

Designed hybrid nanostructure with catalytic effect: beyond the theoretical capacity of SnO2 anode material for lithium ion batteries

PubMed Central

Wang, Ye; Huang, Zhi Xiang; Shi, Yumeng; Wong, Jen It; Ding, Meng; Yang, Hui Ying

2015-01-01

Transition metal cobalt (Co) nanoparticle was designed as catalyst to promote the conversion reaction of Sn to SnO2 during the delithiation process which is deemed as an irreversible reaction. The designed nanocomposite, named as SnO2/Co3O4/reduced-graphene-oxide (rGO), was synthesized by a simple two-step method composed of hydrothermal (1st step) and solvothermal (2nd step) synthesis processes. Compared to the pristine SnO2/rGO and SnO2/Co3O4 electrodes, SnO2/Co3O4/rGO nanocomposites exhibit significantly enhanced electrochemical performance as the anode material of lithium-ion batteries (LIBs). The SnO2/Co3O4/rGO nanocomposites can deliver high specific capacities of 1038 and 712 mAh g−1 at the current densities of 100 and 1000 mA g−1, respectively. In addition, the SnO2/Co3O4/rGO nanocomposites also exhibit 641 mAh g−1 at a high current density of 1000 mA g−1 after 900 cycles, indicating an ultra-long cycling stability under high current density. Through ex-situ TEM analysis, the excellent electrochemical performance was attributed to the catalytic effect of Co nanoparticles to promote the conversion of Sn to SnO2 and the decomposition of Li2O during the delithiation process. Based on the results, herein we propose a new method in employing the catalyst to increase the capacity of alloying-dealloying type anode material to beyond its theoretical value and enhance the electrochemical performance. PMID:25776280

Facile synthesis of zinc oxide nanoparticles decorated graphene oxide composite via simple solvothermal route and their photocatalytic activity on methylene blue degradation.

PubMed

Atchudan, Raji; Edison, Thomas Nesakumar Jebakumar Immanuel; Perumal, Suguna; Karthikeyan, Dhanapalan; Lee, Yong Rok

2016-09-01

Zinc oxide nanoparticles decorated graphene oxide (ZnO@GO) composite was synthesized by simple solvothermal method where zinc oxide (ZnO) nanoparticles and graphene oxide (GO) were synthesized via simple thermal oxidation and Hummers method, respectively. The obtained materials were thoroughly characterized by various physico-chemical techniques such as X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, field emission scanning electron microscopy (FESEM), high resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS), and Raman spectroscopy. Raman spectrum shows the intensity of D to G value was close to one which confirms the obtained GO and ZnO@GO composite possesses moderate graphitization. TEM images shows the ZnO nanoparticles mean size of 15±5nm were dispersed over the wrinkled graphene layers. The photocatalytic performance of ZnO@GO composite on degradation of methylene blue (MB) is investigated and the results show that the GO plays an important role in the enhancement of photocatalytic performance. The synthesized ZnO@GO composite achieves a maximum degradation efficiency of 98.5% in a neutral solution under UV-light irradiation for 15min as compared with pure ZnO (degradation efficiency is 49% after 60min of irradiation) due to the increased light absorption, the reduced charge recombination with the introduction of GO. Moreover, the resulting ZnO@GO composite possesses excellent degradation efficiency as compared to ZnO nanoparticles alone on MB. Copyright © 2016 Elsevier B.V. All rights reserved.

Hierarchical nanostructures of copper(II) phthalocyanine on electrospun TiO(2) nanofibers: controllable solvothermal-fabrication and enhanced visible photocatalytic properties.

PubMed

Zhang, Mingyi; Shao, Changlu; Guo, Zengcai; Zhang, Zhenyi; Mu, Jingbo; Cao, Tieping; Liu, Yichun

2011-02-01

In the present work, 2,9,16,23-tetranitrophthalocyanine copper(II) (TNCuPc)/TiO(2) hierarchical nanostructures were successfully fabricated by a simple combination method of electrospinning technique and solvothermal processing. Scanning electron microscopy (SEM), energy-dispersive X-ray (EDX) spectroscopy, X-ray diffraction (XRD), UV-vis diffuse reflectance (DR), Fourier transform infrared spectrum (FT-IR), X-ray photoelectron spectroscopy (XPS), and thermal gravimetric and differential thermal analysis (TG-DTA) were used to characterize the as-synthesized TNCuPc/TiO(2) hierarchical nanostructures. The results showed that the secondary TNCuPc nanostructures were not only successfully grown on the primary TiO(2) nanofibers substrates but also uniformly distributed without aggregation. By adjusting the solvothermal fabrication parameters, the TNCuPc nanowires or nanoflowers were facilely fabricated, and also the loading amounts of TNCuPc could be controlled on the TNCuPc/TiO(2) hierarchical nanostructural nanofibers. And, there might exist the interaction between TNCuPc and TiO(2). A possible mechanism for the formation of TNCuPc/TiO(2) hierarchical nanostructures was suggested. The photocatalytic studies revealed that the TNCuPc/TiO(2) hierarchical nanostructures exhibited enhanced photocatalytic efficiency of photodegradation of Rhodamine B (RB) compared with the pure TNCuPc or TiO(2) nanofibers under visible-light irradiation.

[Cu(I)(bpp)]BF4: the first extended coordination network prepared solvothermally in an ionic liquid solvent.

PubMed

Jin, Kun; Huang, Xiaoying; Pan, Long; Li, Jing; Appel, Aaron; Wherland, Scot; Pang, Long

2002-12-07

Use of an ionic liquid [bmim][BF4] (bmim = 1-butyl-3-methylimidazolium) as solvent has resulted in the first extended coordination structure, the two-dimensional network [Cu(bpp)]BF4 [bpp = 1,3-bis(4-pyridyl)propane], produced via a solvothermal route.

Growth, morphological and optical characteristics of ZnSSe nanorods

NASA Astrophysics Data System (ADS)

Chen, Lin-Jer; Dai, Jia-Heng

2017-02-01

Zinc seledide sulfide (ZnSxSe1-x) nanorods with wurtzite structure were synthesized by a low temperature solvothermal pathway. In a typical condition of solvothermal at 180 °C for 8 h, the ZnSxSe1-x was composed of nanorods 10-15 nm in diameter and 50-75 nm length. These results indicate that the nanoscale of ZnSSe nanocrystals may contribute to the solvothermal process and exhibit a tunable photoluminescence (PL) and band gap that depends on the variation of reaction conditions. The work suggests a promising route to single-mode "mirror-less" amplified spontaneous emission (ASE) from inorganic nanomaterials with the Cholesteric liquid crystals (CLC) providing additional potential functionality. The obtained products are characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), selected area electron diffraction (SAED), UV-visible spectroscopy, and X-ray photoelectron spectroscopy (XPS). This approach for solvothermal growth can also be used with primary ZnSSe nanorods to achieve tunable optical properties and can likely be extended to nanomaterials of different shapes and other optical devices.

Facile consecutive solvothermal growth of highly fluorescent InP/ZnS core/shell quantum dots using a safer phosphorus source.

PubMed

Byun, Ho-June; Song, Woo-Seuk; Yang, Heesun

2011-06-10

The work presents a facile, stepwise synthetic approach for the production of highly fluorescent InP/ZnS core/shell quantum dots (QDs) by using a safer phosphorus (P) precursor. First, InP quantum dots (QDs) were solvothermally prepared at 180 °C for 24 h by using a P source of P(N(CH(3))(2))(3). The as-grown InP QDs were consecutively placed in another solvothermal condition for ZnS shell overcoating. In contrast to the almost non-fluorescent InP QDs, due to their highly defective surface states, the ZnS-coated InP QDs were highly fluorescent as a result of effective surface passivation. After the shell growth, the resulting InP/ZnS core/shell QDs were subjected to a size-sorting processing, by which red- to green-emitting QDs with quantum yields (QYs) of 24-60% were produced. Solvothermal shell growth parameters such as the reaction time and Zn/In solution concentration ratio were varied and optimized toward the highest QYs of core/shell QDs.

Facile consecutive solvothermal growth of highly fluorescent InP/ZnS core/shell quantum dots using a safer phosphorus source

NASA Astrophysics Data System (ADS)

Byun, Ho-June; Song, Woo-Seuk; Yang, Heesun

2011-06-01

The work presents a facile, stepwise synthetic approach for the production of highly fluorescent InP/ZnS core/shell quantum dots (QDs) by using a safer phosphorus (P) precursor. First, InP quantum dots (QDs) were solvothermally prepared at 180 °C for 24 h by using a P source of P(N(CH3)2)3. The as-grown InP QDs were consecutively placed in another solvothermal condition for ZnS shell overcoating. In contrast to the almost non-fluorescent InP QDs, due to their highly defective surface states, the ZnS-coated InP QDs were highly fluorescent as a result of effective surface passivation. After the shell growth, the resulting InP/ZnS core/shell QDs were subjected to a size-sorting processing, by which red- to green-emitting QDs with quantum yields (QYs) of 24-60% were produced. Solvothermal shell growth parameters such as the reaction time and Zn/In solution concentration ratio were varied and optimized toward the highest QYs of core/shell QDs.

Single-step solvothermal synthesis of mesoporous Ag-TiO2-reduced graphene oxide ternary composites with enhanced photocatalytic activity

NASA Astrophysics Data System (ADS)

Arif Sher Shah, Md. Selim; Zhang, Kan; Park, A. Reum; Kim, Kwang Su; Park, Nam-Gyu; Park, Jong Hyeok; Yoo, Pil J.

2013-05-01

With growing interest in the photocatalytic performance of TiO2-graphene composite systems, the ternary phase of TiO2, graphene, and Ag is expected to exhibit improved photocatalytic characteristics because of the improved recombination rate of photogenerated charge carriers and potential contribution of the generation of localized surface plasmon resonance at Ag sites on a surface of the TiO2-graphene binary matrix. In this work, Ag-TiO2-reduced graphene oxide ternary nanocomposites were successfully synthesized by a simple solvothermal process. In a single-step synthetic procedure, the reduction of AgNO3 and graphene oxide and the hydrolysis of titanium tetraisopropoxide were spontaneously performed in a mixed solvent system of ethylene glycol, N,N-dimethylformamide and a stoichiometric amount of water without resorting to the use of typical reducing agents. The nanocomposites were characterized by X-ray diffraction, X-ray photoelectron spectroscopy, along with different microscopic and spectroscopic techniques, enabling us to confirm the successful reduction of AgNO3 and graphite oxide to metallic Ag and reduced graphene oxide, respectively. Due to the highly facilitated electron transport of well distributed Ag nanoparticles, the synthesized ternary nanocomposite showed enhanced photocatalytic activity for degradation of rhodamine B dye under visible light irradiation.With growing interest in the photocatalytic performance of TiO2-graphene composite systems, the ternary phase of TiO2, graphene, and Ag is expected to exhibit improved photocatalytic characteristics because of the improved recombination rate of photogenerated charge carriers and potential contribution of the generation of localized surface plasmon resonance at Ag sites on a surface of the TiO2-graphene binary matrix. In this work, Ag-TiO2-reduced graphene oxide ternary nanocomposites were successfully synthesized by a simple solvothermal process. In a single-step synthetic procedure, the reduction of AgNO3 and graphene oxide and the hydrolysis of titanium tetraisopropoxide were spontaneously performed in a mixed solvent system of ethylene glycol, N,N-dimethylformamide and a stoichiometric amount of water without resorting to the use of typical reducing agents. The nanocomposites were characterized by X-ray diffraction, X-ray photoelectron spectroscopy, along with different microscopic and spectroscopic techniques, enabling us to confirm the successful reduction of AgNO3 and graphite oxide to metallic Ag and reduced graphene oxide, respectively. Due to the highly facilitated electron transport of well distributed Ag nanoparticles, the synthesized ternary nanocomposite showed enhanced photocatalytic activity for degradation of rhodamine B dye under visible light irradiation. Electronic supplementary information (ESI) available: XRD of GO, EDX analysis of AgTG composites, tables show the size of graphitic domains and peak area analysis, dye adsorption plot, UV-visible absorption spectra of dye at different times, and plots of ln(Ct/C0) vs. time with the corresponding fitting curves of different samples. See DOI: 10.1039/c3nr00579h

Solvothermal synthesis of nickel-tungsten sulfides for 2-propanol dehydration.

PubMed

Gómez-Gutiérrez, Claudia M; Luque, P A; Guerra-Rivas, G; López-Sánchez, J A; Armenta, M A; Quintana, J M; Olivas, A

2015-01-01

The bimetallic nickel-tungsten catalysts were prepared via solvothermal method. The X-ray Diffractometer (XRD) analysis revealed that the corresponding peaks at 14°, 34°, and 58° were for tungsten disulfide (WS2 ) hexagonal phase. The catalysts displayed different crystalline phase with nickel addition, and as an effect the WS2 surface area decreased from 74.7 to 2.0 m(2) g(--1) . In this sense, high-resolution transmission electron microscopy (HRTEM) showed the layers set in direction (002) with an onion-like morphology, and in the center of the particles there is a large amount of nickel contained with 6-8 layers covering it. The catalytic dehydration of 2-propanol was selective to propene in 100% at 250 °C for the sample with 0.7 of atomic ratio of Ni/Ni + W. © Wiley Periodicals, Inc.

Template-Free Solvothermal Synthesis of Flower-Like BiOBr Microspheres in Ethanol Medium for Photocatalytic Applications

NASA Astrophysics Data System (ADS)

Hong, Shaoming; Ren, Huijun; Fang, Yanfeng; Huang, Yingping; Li, Ruiping

2018-05-01

Three-dimensionally (3D) BiOBr microflowers were prepared by a simple solvothermal method, employing Bi(NO3)3 · 5H2O and NaBr as starting reagents in ethanol. The structural, light absorption and morphological properties of as-prepared BiOBr microspheres were determined by X-ray diffraction (XRD), scanning electron microscopy (SEM), and UV-Vis diffuse reflectance spectroscopy (DRS), etc. The results showed that ethanol acted not only as a solvent but also as a template in 3D BiOBr preparation. The BiOBr microspheres exhibited superior photocatalytic activity compared with 2D BiOBr nanosheets, far exceeding that of TiO2 (Degussa, P25). It was found that both superoxide radical (O2 •-) and holes (h+) played a key role in the degradation of RhB by BiOBr microflowers.

Solvothermal synthesis of N-doped graphene supported PtCo nanodendrites with highly catalytic activity for 4-nitrophenol reduction

NASA Astrophysics Data System (ADS)

Zhang, Xiao-Fang; Zhu, Xiao-Yan; Feng, Jiu-Ju; Wang, Ai-Jun

2018-01-01

A simple solvothermal method was developed to prepare N-doped reduced graphene oxide supported homogeneous PtCo nanodendrites (PtCo NDs/N-rGO), where ethylene glycol (EG) served as the reducing agent and the solvent, and linagliptin as the structure-directing and stabilizing agent for PtCo NDs and dopant for rGO, respectively. Controlled researches showed that the dosage of linagliptin and the ratios of the two metal precursors were important in the current synthesis. The PtCo NDs/N-rGO nanocomposite exhibited higher catalytic activity towards the reduction of 4-nitrophnol (4-NP) in contrast with the referenced Pt1Co3 NCs/N-rGO, Pt3Co1 NCs/N-rGO and commercial Pt/C catalysts. More importantly, the constructed catalyst exhibited the superior stability without sacrificing the catalytic activity, showing great prospect for the reduction of 4-NP in practice.

Solvothermal preparation of phthalocyanine nanorod/rGO composites and their application to visible-light-responsive photocatalysts

NASA Astrophysics Data System (ADS)

Zhang, Shuai; Lu, Yongting; Zhang, Fan; Qu, Jie; Lin, Bencai; Yuan, Ningyi; Fang, Bijun; Ding, Jian-Ning

2016-09-01

Phthalocyanine (Pc) nanorod/reduced graphene oxide (rGO) composites were prepared by a simple solvothermal method, in which Pc nanosheet and graphene oxide (GO) suspensions were mixed in methanol. As characterized by scanning electron microscopy, transmission electron microscopy, and selected area electron diffraction, Pc nanorods with an amorphous structure and an average diameter of 250nm are partially covered by rGO sheets. In the photodegradation experiments, all the composites with different rGO content show enhanced photocatalytic activity for Rhodamine B decomposition under visible-light compared to pure Pc nanorods or rGO sheets. The enhanced photocatalytic activity shall be ascribed to the large surface area offered by rGO and the charge-transfer from Pc to rGO as indicated by the photoluminescence measurement, in which fluorescence intensity of the composites is much weaker than that of Pc nanorods.

Monodisperse NixFe3-xO4 nanospheres: Metal-ion-steered size/composition control mechanism, static magnetic and enhanced microwave absorbing properties

NASA Astrophysics Data System (ADS)

Jiang, Kedan; Liu, Yun; Pan, Yefei; Wang, Ru; Hu, Panbing; He, Rujia; Zhang, Lingli; Tong, Guoxiu

2017-05-01

An easy metal-ion-steered solvothermal method was developed for the one-step synthesis of monodisperse, uniform NixFe3-xO4 polycrystalline nanospheres with tunable sphere diameter (40-400 nm) and composition (0 ≤ x ≤ 0.245) via changing just Ni2+/Fe3+ molar ratio (γ). With g increased from 0:1 to 2:1, sphere diameter gradually decreased and crystal size exhibited an inversed U-shaped change tendency, followed by increased Ni/Fe atom ratio from 0% to 0.0888%. An in situ-reduction, coordination-precipitation transformation mechanism was proposed to interpret the metal-ion-steered growth. Size- and composition-dependent static magnetic and microwave absorbing properties were systematically investigated. Saturation magnetization declines with g in a Boltzmann model due to the changes of crystal size, sphere diameter, and Ni content. The coercivity reaches a maximum at γ = 0.75:1 because of the critical size of Fe3O4 single domain (25 nm). Studies on microwave absorption reveal that 150-400 nm Fe3O4 nanospheres mainly obey the quarter-wavelength cancellation model with the single-band absorption; 40-135 nm NixFe3-xO4 nanospheres (0 ≤ x ≤ 0.245) obey the one and three quarter-wavelength cancellation model with the multi-band absorption. 150 nm Fe3O4 nanospheres exhibit the optimal EM wave-absorbing property with an absorbing band of 8.94 GHz and the maximum RL of -50.11 dB.

Solvothermal synthesis of graphene-Sb{sub 2}S{sub 3} composite and the degradation activity under visible light

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

Tao, Wenguang; Chang, Jiuli; Wu, Dapeng

2013-02-15

Graphical abstract: Display Omitted Highlights: ► Graphene-Sb{sub 2}S{sub 3} composites were synthesized through a facile solvothermal method. ► Hydroxyl radicals are the main species responsible for the photodegradation activity. ► Graphene-Sb{sub 2}S{sub 3} demonstrated dramatically improved visible light degradation activity. -- Abstract: Novel graphene-Sb{sub 2}S{sub 3} (G-Sb{sub 2}S{sub 3}) composites were synthesized via a facile solvothermal method with graphene oxide (GO), SbCl{sub 3} and thiourea as the reactants. GO played an important role in controlling the size and the distribution of the formed Sb{sub 2}S{sub 3} nanoparticles on the graphene sheets with different density. Due to the negative surface charge,more » smaller Sb{sub 2}S{sub 3} particles size and efficient electrons transfer from Sb{sub 2}S{sub 3} to graphene, the composites demonstrated improved photodegradation activity on rhodamine B (RhB). Among these composites, the product G-Sb{sub 2}S{sub 3} 0.1, which was synthesized with the GO concentration of 0.1 mg/mL, exhibited the highest photodegradation activity owing to the considerable density of Sb{sub 2}S{sub 3} nanoparticles onto graphene sheet free of aggregation. Hydroxyl radicals (·OH) derived from conduction band (CB) electrons of Sb{sub 2}S{sub 3} is suggested to be responsible for the photodegradation of RhB. The high visible light degradation activity and the satisfactory cycling stability made the as-prepared G-Sb{sub 2}S{sub 3} 0.1 an applicable photocatalyst.« less

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

Sornadurai, D.; Ravindran, T. R.; Paul, V. Thomas

Synthesis parameters are optimized in order to grow single crystals of multiferroic BiFeO{sub 3}. 2 to 3 mm size pyramid (tetrahedron) shaped single crystals were successfully obtained by solvothermal method. Scanning electron microscopy with EDAX confirmed the phase formation. Raman scattering spectra of bulk BiFeO3 single crystals have been measured which match well with reported spectra.

Defect engineering of UiO-66 for CO2 and H2O uptake - a combined experimental and simulation study.

PubMed

Liang, Weibin; Coghlan, Campbell J; Ragon, Florence; Rubio-Martinez, Marta; D'Alessandro, Deanna M; Babarao, Ravichandar

2016-03-21

Defect concentrations and their compensating groups have been systematically tuned within UiO-66 frameworks by using modified microwave-assisted solvothermal methods. Both of these factors have a pronounced effect on CO2 and H2O adsorption at low and high pressure.

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.

Microstructure and thermoelectric properties of CuInSe2/In2Se3 compound

NASA Astrophysics Data System (ADS)

Wang, Kang; Feng, Jing; Ge, Zhen-Hua; Qin, Peng; Yu, Jie

2018-01-01

CuInSe2 powders were synthesized by solvothermal method, and then the CuInSe2/In2Se3 bulk samples were fabricated by spark plasma sintering (SPS) technique. To investigate the phase composition, the powders were determined by X-ray diffraction (XRD). The microstructures of the powders and bulk samples were observed by scanning electron microscopy (SEM). The transportation of the electronic properties and thermal conductivity were measured at room temperature to 700 K. According to the results, the CuInSe2 powders appeared in flower-like patterns which ranged from 3 μm to 6 μm. CuInSe2 powders were synthesized at 180∘C with a chalcopyrite structure. The Seebeck coefficient increased significantly in composite thermoelectric materials up to 200μVṡK-1 at 623 K. The thermal conductivity of the sample significantly decreases from the room temperature to 700 K. The CuInSe2 bulk composite by solvothermal method achieves the highest ZT value of 0.187 at 700 K.

Effect of precursor concentration on the electrical properties of LiFePO{sub 4} prepared by solvothermal method

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

Rabbani, Ahmad Yasin; Fakhri, Hafizh A.; Arifin, Muhammad

2016-02-08

Lithium iron phosphate (LiFePO{sub 4}) is frequently used for Li-ion battery cathode. LiFePO{sub 4} has the high specific capacity at 170 mAhg{sup −1}, stable voltage at 3.45 V, stable structure, cheap, and low toxicity. The objective of this research is investigating the effect of precursor concentration on the electrical properties of LiFePO{sub 4} prepared by solvothermal method. LiOH, FeSO{sub 4}, H{sub 3}PO{sub 4}, and citric acid were used as the precursors. The LiOH concentration was varied from 0.3 M to 1.8 M. The Fourier Transform Infrared Spectroscopy (FTIR) measurement identified the Fe-O, O-P-O, and P-O bonds which corresponding to LiFePO{sub 4}.more » The result of 4-point probe measurement shows that, among the prepared samples, the sample from the precursor concentration of 1.8 M has the highest electrical conductivity.« less

Copper nanocoils synthesized through solvothermal method

PubMed Central

Liu, Yanjuan; Liu, Xiaowei; Zhan, Yongjie; Fan, Haiming; Lu, Yang

2015-01-01

Recently helical nanostructures such as nanosprings and nanocoils have drawn great interests in nanotechnology, due to their unique morphologies and physical properties, and they may be potential building blocks in sorts of electromechanical, magnetic, photoelectronic and plasmonic devices at micro/nanoscales. In this report, multi-turns copper nanocoils were synthesized through a modified solvothermal method, in which the mixture of water and N-methyl-2-pyrrolidone (NMP) were selected as reaction medium and copolymer poly(1-vinylpyrrolidone-co-vinyl acetate) (PVP/VA 64E) as reductant. In the liquid solution, nanosprings could be formed from relaxed nanocoils and demonstrated high elasticity. These nanocoils and nanosprings are of single crystalline structure, with the characteristics wire diameters ranging from tens to a few hundreds of nanometers and the ring/coil diameters mostly ~10–35 microns. Their growth and deformation mechanisms were then investigated and discussed along with that of previously reported single-turn copper nanorings. This work could be of importance for researchers working on synthesis and applications of novel 1-D helical nanomaterials and their functional devices. PMID:26607386

[Comparison between one-step and two-step space closing methods of sliding mechanics using three-dimensional finite element].

PubMed

Han, Yaohui; Mou, Lan; Xu, Gengchi; Yang, Yiqiang; Ge, Zhenlin

2015-03-01

To construct a three-dimensional finite element model comparing between one-step and two-step methods in torque control of anterior teeth during space closure. Dicom image data including maxilla and upper teeth were obtained though cone-beam CT. A three-dimensional model was set up and the maxilla, upper teeth and periodontium were separated using Mimics software. The models were instantiated using Pro/Engineer software, and Abaqus finite element analysis software was used to simulate the sliding mechanics by loading 1.47 Nforce on traction hooks with different heights (2, 4, 6, 8, 10, 12 and 14 mm, respectively) in order to compare the initial displacement between six maxillary anterior teeth (one-step method) and four maxillary anterior teeth (two-step method). When moving anterior teeth bodily, initial displacements of central incisors in two-step method and in one-step method were 29.26 × 10⁻⁶ mm and 15.75 × 10⁻⁶ mm, respectively. The initial displacements of lateral incisors in two-step method and in one-step method were 46.76 × 10(-6) mm and 23.18 × 10(-6) mm, respectively. Under the same amount of light force, the initial displacement of anterior teeth in two-step method was doubled compared with that in one-step method. The root and crown of the canine couldn't obtain the same amount of displacement in one-step method. Two-step method could produce more initial displacement than one-step method. Therefore, two-step method was easier to achieve torque control of the anterior teeth during space closure.

Synthesis and characterization of metastable, 20 nm-sized Pna2{sub 1}-LiCoPO{sub 4} nanospheres

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

Ludwig, Jennifer; Nordlund, Dennis; Doeff, Marca M.

The majority of research activities on LiCoPO{sub 4} are focused on the phospho-olivine (space group Pnma), which is a promising high-voltage cathode material for Li-ion batteries. In contrast, comparably little is known about its metastable Pna2{sub 1} modification. Herein, we present a comprehensive study on the structure–property relationships of 15–20 nm Pna2{sub 1}-LiCoPO{sub 4} nanospheres prepared by a simple microwave-assisted solvothermal process. Unlike previous reports, the results indicate that the compound is non-stoichiometric and shows cation-mixing with Co ions on the Li sites, which provides an explanation for the poor electrochemical performance. Co L{sub 2,3}-edge X-ray absorption spectroscopic data confirmmore » the local tetrahedral symmetry of Co{sup 2+}. Comprehensive studies on the thermal stability using thermogravimetric analysis, differential scanning calorimetry, and in situ powder X-ray diffraction show an exothermic phase transition to olivine Pnma-LiCoPO{sub 4} at 527 °C. The influence of the atmosphere and the particle size on the thermal stability is also investigated. - Graphical abstract: Blue nano-sized Pna2{sub 1}-LiCoPO{sub 4,} featuring tetrahedrally-coordinated Co{sup 2+}, was synthesized in a rapid one-step microwave-assisted solvothermal process. The phase relation between this metastable and the stable polymorph was analyzed and electrochemical properties are discussed. - Highlights: • Preparation of uniform 15–20 nm nanospheres of metastable Pna2{sub 1}-LiCoPO{sub 4} polymorph. • Structure redetermination shows cation-mixing (Co blocking Li sites). • In situ investigation of phase transformation to olivine Pnma-LiCoPO{sub 4} at 527 °C. • Pna2{sub 1}-LiCoPO{sub 4} reemerges as a stable high-temperature phase above 800 °C. • X-ray absorption spectroscopy confirms local tetrahedral symmetry (T{sub d} Co{sup 2+}).« less

Particle size-controllable microwave-assisted solvothermal synthesis of the high-voltage cathode material LiCoPO4 using water/ethylene glycol solvent blends

NASA Astrophysics Data System (ADS)

Ludwig, Jennifer; Haering, Dominik; Doeff, Marca M.; Nilges, Tom

2017-03-01

Particle size-tuned platelets of the high-voltage cathode material LiCoPO4 for Li-ion batteries have been synthesized by a simple one-step microwave-assisted solvothermal process using an array of water/ethylene glycol (EG) solvent mixtures. Particle size control was achieved by altering the concentration of the EG co-solvent in the mixture between 0 and 100 vol%, with amounts of 0-80 vol% EG producing single phase, olivine-type LiCoPO4. The particle sizes of the olivine materials were significantly reduced from about 1.2 μm × 1.2 μm × 500 nm (0 vol% EG) to 200 nm × 100 nm × 50 nm (80 vol% EG) with increasing EG content, while specific surface areas increased from 2 to 13 m2 g-1. The particle size reduction could mainly be attributed to the modified viscosities of the solvent blends. Owing to the soft template effect of EG, the crystals exhibited the smallest dimensions along the [010] direction of the Li diffusion pathways in the olivine crystal structure, resulting in enhanced lithium diffusion properties. The relationship between the synthesis, crystal properties and electrochemical performance was further elucidated, indicating that the electrochemical performances of the as-prepared materials mainly depend on the solvent composition and the respective particle size range. LiCoPO4 products obtained from reaction media with low and high EG contents exhibited good electrochemical performances (initial discharge capacities of 87-124 mAh g-1 at 0.1 C), whereas materials made from medium EG concentrations (40-60 vol% EG) showed the highest capacities and gravimetric energy densities (up to 137 mAh g-1 and 658 Wh kg-1 at 0.1 C), excellent rate capabilities, and cycle life.

Porous Metal Carboxylate Boron Imidazolate Frameworks (MC-BIFs)

PubMed Central

Zheng, Shoutian; Wu, Tao; Zhang, Jian; Chow, Mina; Nieto, Ruben A.

2011-01-01

Integrated Material for Efficient CO2 Storage A new family of porous materials with tunable gas sorption properties have been made by integrating metal carboxylates and boron imidazolates under hydro- or solvothermal conditions. One hydrothermally synthesized phase exhibits a very high volumetric CO2 storage capacity at 81 L/L (273K, 1atm). PMID:20583020

Solvothermal syntheses, crystal structures, and properties of lanthanide(III) thioarsenates [Ln(dien){sub 2}(μ-1κ,2κ{sup 2}-AsS{sub 4})]{sub n} (Ln==Sm, Eu, Gd) and [Ln(dien){sub 2}(1κ{sup 2}-AsS{sub 4})] (Ln==Tb, Dy, Ho)

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

Wang, Fang; Tang, Chunying; Chen, Ruihong

2013-10-15

Solvothermal reactions of Ln{sub 2}O{sub 3}, As and S in diethylenetriamine (dien) at 170 °C for 6 days afforded two structural types of lanthanide thioarsenates with the general formulae [Ln(dien){sub 2}(μ-1κ,2κ{sup 2}-AsS{sub 4})]{sub n} [Ln=Sm(1), Eu(2), Gd(3)] and [Ln(dien){sub 2}(1κ{sup 2}-AsS{sub 4})] [Ln=Tb(4), Dy(5), Ho(6)]. The Ln{sub 2}O{sub 3} oxides were converted to [Ln(dien){sub 2}]{sup 3+} complex units in the solvothermal reactions. The As atom binds four S atoms, forming a tetrahedral AsS{sub 4} unit. In 1−3, the AsS{sub 4} units interconnect the [Ln(dien){sub 2}]{sup 3+} cations via Ln−S bonds as tridentate μ-1κ,2κ{sup 2}-AsS{sub 4} bridging ligands, resulting in themore » neutral coordination polymers [Ln(dien){sub 2}(μ-1κ,2κ{sup 2}-AsS{sub 4})]{sub n} (Ln1). In 4−6, the AsS{sub 4} units coordinate with the Ln{sup 3+} ion of [Ln(dien){sub 2}]{sup 3+} as 1κ{sup 2}-AsS{sub 4} chelating ligands to form neutral coordination compounds [Ln(dien){sub 2}(1κ{sup 2}-AsS{sub 4})] (Ln2). The Ln{sup 3+} ions are in nine- and eight-coordinated environments in Ln1 and Ln2, respectively. The formation of Ln1 and Ln2 is related with ionic size of the Ln{sup 3+} ions. Optical absorption spectra showed that 1−6 have potential use as semiconductors with the band gaps in the range 2.18−3.21 eV. - Graphical abstract: Two types of Ln-thioarsenates [Ln(dien){sub 2}(μ-1κ,2κ{sup 2}-AsS{sub 4})]{sub n} and [Ln(dien){sub 2}(1κ{sup 2}-AsS{sub 4})] were prepared by solvothermal methods and the soft Lewis basic AsS{sub 4}{sup 3–} ligand to Ln(III) centers with polyamine co-ligand was obtained. Display Omitted - Highlights: • Lanthanide thioarsenates were prepared by solvothermal methods. • The soft Lewis basic AsS{sub 4} ligand coordinate Ln{sup 3+} ions with coexistence polyamine ligands. • Two structural types of Ln-thioarsenates with structural turnover at Tb were obtained along Ln series. • The Ln-thioarsenates are potential semiconductors with optical band gaps in the range 2.18−3.21 eV.« less

Microwave-Assisted Solvothermal Synthesis of VO2 Hollow Spheres and Their Conversion into V2O5 Hollow Spheres with Improved Lithium Storage Capability.

PubMed

Pan, Jing; Zhong, Li; Li, Ming; Luo, Yuanyuan; Li, Guanghai

2016-01-22

Monodispersed hierarchically structured V2O5 hollow spheres were successfully obtained from orthorhombic VO2 hollow spheres, which are in turn synthesized by a simple template-free microwave-assisted solvothermal method. The structural evolution of VO2 hollow spheres has been studied and explained by a chemically induced self-transformation process. The reaction time and water content in the reaction solution have a great influence on the morphology and phase structure of the resulting products in the solvothermal reaction. The diameter of the VO2 hollow spheres can be regulated simply by changing vanadium ion content in the reaction solution. The VO2 hollow spheres can be transformed into V2O5 hollow spheres with nearly no morphological change by annealing in air. The nanorods composed of V2O5 hollow spheres have an average length of about 70 nm and width of about 19 nm. When used as a cathode material for lithium-ion batteries, the V2O5 hollow spheres display a diameter-dependent electrochemical performance, and the 440 nm hollow spheres show the highest specific discharge capacity of 377.5 mAhg(-1) at a current density of 50 mAg(-1) , and are better than the corresponding solid spheres and nanorod assemblies. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Elemental Anisotropic Growth and Atomic-Scale Structure of Shape-Controlled Octahedral Pt-Ni-Co Alloy Nanocatalysts.

PubMed

Arán-Ais, Rosa M; Dionigi, Fabio; Merzdorf, Thomas; Gocyla, Martin; Heggen, Marc; Dunin-Borkowski, Rafal E; Gliech, Manuel; Solla-Gullón, José; Herrero, Enrique; Feliu, Juan M; Strasser, Peter

2015-11-11

Multimetallic shape-controlled nanoparticles offer great opportunities to tune the activity, selectivity, and stability of electrocatalytic surface reactions. However, in many cases, our synthetic control over particle size, composition, and shape is limited requiring trial and error. Deeper atomic-scale insight in the particle formation process would enable more rational syntheses. Here we exemplify this using a family of trimetallic PtNiCo nanooctahedra obtained via a low-temperature, surfactant-free solvothermal synthesis. We analyze the competition between Ni and Co precursors under coreduction "one-step" conditions when the Ni reduction rates prevailed. To tune the Co reduction rate and final content, we develop a "two-step" route and track the evolution of the composition and morphology of the particles at the atomic scale. To achieve this, scanning transmission electron microscopy and energy dispersive X-ray elemental mapping techniques are used. We provide evidence of a heterogeneous element distribution caused by element-specific anisotropic growth and create octahedral nanoparticles with tailored atomic composition like Pt1.5M, PtM, and PtM1.5 (M = Ni + Co). These trimetallic electrocatalysts have been tested toward the oxygen reduction reaction (ORR), showing a greatly enhanced mass activity related to commercial Pt/C and less activity loss than binary PtNi and PtCo after 4000 potential cycles.

Reduced graphene oxide-CdS nanocomposite with enhanced photocatalytic 4-Nitrophenol degradation

NASA Astrophysics Data System (ADS)

Chakraborty, Koushik; Ibrahim, Sk; Das, Poulomi; Ghosh, Surajit; Pal, Tanusri

2017-05-01

We report the photocatalytic activity of reduced graphene oxide cadmium sulfide (RGO-CdS) composite towards the degradation of 4-Nitrophenol (4-NP) under simulated solar light illumination. The solution processable RGO-CdS composite was synthesized by one pot single step low cost solvothermal process, where the reduction of graphene oxide (GO), synthesis and attachment of CdS onto RGO sheets were done simultaneously. The structural and morphological characterization of the RGO-CdS composite and the reduction of GO was confirmed by X-ray diffractometry, TEM imaging and Fourier transform infrared spectroscopy respectively. The photocatalytic efficiency of RGO-CdS composite is 2.6 times higher in compare to controlled CdS. In RGO-CdS composite the photo induced electrons transfer from CdS nanorod to RGO sheets, which reduces the recombination probability of photo generated electron-hole in the CdS. These well separated photoinduced charges enhanced the photocatalytic activity of the RGO-CdS composite. Our study establishes the RGO-CdS composite as a potential photocatalyst for the degradation of organic water pollutant.

An ultrasensitive electrochemiluminescent sensor based on a pencil graphite electrode modified with CdS nanorods for detection of chlorogenic acid in honeysuckle.

PubMed

Zheng, Ruijuan; Zhong, Jianhai; Zhao, Chenhao; Lang, Xiaoling; Hu, Zhibiao; Luo, Jiangshui

2017-08-01

In this paper, a novel and ultrasensitive electrochemiluminescent sensor employing a solvothermal-synthesized CdS nanorod-modified pencil graphite electrode (CdS/PGE) for the determination of chlorogenic acid (CA) is fabricated. In the first step, the PGE surface is modified using CdS nanorods. In the next step, the developed electrode is used to detect CA using a electrochemiluminescent (ECL) technique, in which potassium persulfate (K 2 S 2 O 8 ) served as a co-reactant. The possible ECL mechanism is investigated, and the influences of pH and cyclic voltammetric scanning rate on the signal response are studied. The ECL intensity decreases quantitatively in relation to the concentration of the target molecule. Under optimized conditions, the linear correlation between the quenched ECL intensity and the logarithm of CA concentration is observed in the range from 2 × 10 -9 to 8 × 10 -7  mol L -1 with a limit of detection of 1 × 10 -9  mol L -1 . This proposed method is applied to the analysis of CA in honeysuckle flower, giving recoveries of 99-107%. The experimental results demonstrate that this ECL sensor shows good stability and reproducibility. Copyright © 2016 John Wiley & Sons, Ltd.

TiO2 Hollow Spheres: One-Pot Synthesis and Enhanced Photocatalysis

NASA Astrophysics Data System (ADS)

Jia, Changchao; Cao, Yongqiang; Yang, Ping

2013-04-01

Hollow TiO2 microspheres were successfully fabricated by metal salts with low solubility in ethanol acting as intelligent templates using a simple one-pot solvothermal method. Hollow spheres with large diameter were obtained using CuSO4ṡ5H2O as templates while small ones were obtained using Sr(NO3)2 as templates. It is found that titanium precursor plays an important role for the morphology of samples. Solid TiO2 microspheres were prepared by using titanium tetrabutoxide (TBT). In contrast, bowl-like hollow microspheres were obtained by using titanium tetrachloride (TiCl4). Furthermore, the amount of H2O can stimulate the hydrolysis rate of TiCl4 to form solid spheres. Compared with solid microspheres, hollow TiO2 microspheres depending on their interior cavity structure exhibited enhanced photocatalysis efficiency for the UV-light photodegradation of methyl orange. Quantificationally, the apparent photocatalytic degradation pseudo-first-rate constant of the hollow microspheres is 1.25 times of that of the solid ones.

Mn(II)-coordinated Fluorescent Carbon Dots: Preparation and Discrimination of Organic Solvents

NASA Astrophysics Data System (ADS)

Wang, Yuru; Wang, Tianren; Chen, Xi; Xu, Yang; Li, Huanrong

2018-04-01

Herein, we prepared a Mn(II)-coordinated carbon dots (CDs) with fluorescence and MRI (magnetic resonance imaging) bimodal properties by a one-pot solvothermal method and separated via silica column chromatography. The quantum yield of the CDs increased greatly from 2.27% to 6.75% with increase of Mn(II) doping, meanwhile the CDs exhibited a higher MR activity (7.28 mM-1s-1) than that of commercial Gd-DTPA (4.63 mM-1s-1). In addition, white light emitting CDs were obtained by mixing the different types of CDs. Notably, these CDs exhibited different fluorescence emissions in different organic solvents and could be used to discriminate organic solvents based on the polarity and protonation of the solvents.

Facile solvothermal synthesis of highly active and robust Pd1.87Cu0.11Sn electrocatalyst towards direct ethanol fuel cell applications

NASA Astrophysics Data System (ADS)

Jana, Rajkumar; Dhiman, Shikha; Peter, Sebastian C.

2016-08-01

Ordered intermetallic Pd1.87Cu0.11Sn ternary electrocatalyst has been synthesized by sodium borohydride reduction of precursor salts Pd(acac)2, CuCl2.2H2O and SnCl2 using one-pot solvothermal synthesis method at 220 °C with a reaction time of 24 h. To the best of our knowledge, here for the first time we report surfactant free synthesis of a novel ordered intermetallic ternary Pd1.87Cu0.11Sn nanoparticles. The ordered structure of the catalyst has been confirmed by powder x-ray diffraction, transmission electron microscopy (TEM). Composition and morphology of the nanoparticles have been confirmed through field emission scanning electron microscopy, energy-dispersive spectrometry and TEM. The electrocatalytic activity and stability of the ternary electrocatalyst towards ethanol oxidation in alkaline medium was investigated by cyclic voltammetry and chronoamperometry techniques. The catalyst is proved to be highly efficient and stable upto 500th cycle and even better than commercially available Pd/C (20 wt%) electrocatalysts. The specific and mass activity of the as synthesized ternary catalyst are found to be ∼4.76 and ∼2.9 times better than that of commercial Pd/C. The enhanced activity and stability of the ordered ternary Pd1.87Cu0.11Sn catalyst can make it as a promising candidate for the alkaline direct ethanol fuel cell application.

A Co16 cluster and a 1-D Mn chain complex supported by benzohydroxamic acid.

PubMed

Cao, Yanyuan; Chen, Yanmei; Li, Lei; Gao, Dandan; Liu, Wei; Hu, Hailiang; Li, Wu; Li, Yahong

2013-08-14

The syntheses, crystal structures and magnetic properties are described for a {Co16} cluster [Co(II)16O(OH)2(bha)12(PhCO2)4(Phen)2(MeOH)4]·2MeOH (1) and a 1-D Mn(II) chain complex [Mn(Hbha)2]n·(2MeOH)n (2) (H2bha = benzohydroxamic acid; Phen = 1,10-phenanthroline). The 1 : 1 : 0.5 reaction of Co(O2CMe)2·4H2O, H2bha and 1,10-phenanthroline in MeOH at 100 °C under autogenous pressure gave cluster 1. Complex 2 was obtained from the 1 : 1 reaction mixture of Mn(O2CMe)2·2H2O and H2bha in MeOH under solvothermal conditions. The {Co16} cluster can be thought as a face-centered cube with two wings. The H2bha ligands show hydroximic form in 1 and exhibit hydroxamic mode in 2. The hydroximate ligands in 1 display three distinct binding modes, one of which is novel. Variable-temperature solid-state dc magnetic susceptibility studies have been performed in the 2.0-300 K range for complexes 1 and 2. Antiferromagnetic M(II)···M(II) exchange interactions were found for both 1 and 2. This work also demonstrates that solvothermal method is a potential synthetic approach for the design and growth of high nuclearity clusters or chain complexes of the H2bha ligand.

Polyethylene imine-grafted ACF@BiOI0.5Cl0.5 as a recyclable photocatalyst for high-efficient dye removal by adsorption-combined degradation

NASA Astrophysics Data System (ADS)

Li, Hongyan; Li, Najun; Chen, Dongyun; Xu, Qingfeng; Lu, Jianmei

2017-05-01

A recyclable photocatalyst with adsorption property was prepared for high-efficient complete removal of anionic dyes from water by synergetic adsorption and photocatalytic degradation. Firstly, binary bismuth oxyhalide composed as BiOI0.5Cl0.5 was immobilized on activated carbon fibers (ACF) to get a recyclable photocatalyst (ACF@BiOI0.5Cl0.5) via one-step solvothermal method. Then it was modified with branched polyethylene imine (PEI) whose abundant amino groups can adsorb contaminants from water by electrostatic interaction. SEM images showed that the nanosheets-based flower-like photocatalytic microspheres uniformly distributed on the ACF surface after grafting of small amount of PEI. But from TGA results we can deduce that the percentage of PEI grafted onto ACF@BiOI0.5Cl0.5 is about 18 wt%. During the synergistic process, the grafted PEI and immobilized BiOI0.5Cl0.5 are worked as the adsorbent and the photocatalyst, respectively. In addition, ACF, as flexible, conductive and corrosion-resistant supports, are beneficial to the photocatalytic degradation process. So the obtained composite PEI-g-ACF@BiOI0.5Cl0.5 has a high removal efficiency of contaminants under visible light irradiation with the synergistic effect of adsorption and photocatalytic degradation. And after facial separation without centrifuge, it can be reused without regeneration because of the real-time complete degradation of the adsorbed contaminants on the surface of the composite photocatalyst.

Synthesis of hierarchical ZnV2O6 nanosheets with enhanced activity and stability for visible light driven CO2 reduction to solar fuels

NASA Astrophysics Data System (ADS)

Bafaqeer, Abdullah; Tahir, Muhammad; Amin, Nor Aishah Saidina

2018-03-01

Hierarchical nanostructures have lately garnered enormous attention because of their remarkable performances in energy storage and catalysis applications. In this study, novel hierarchical ZnV2O6 nanosheets, formulated by one-step solvothermal method, for enhanced photocatalytic CO2 reduction with H2O to solar fuels has been investigated. The structure and properties of the catalysts were characterized by XRD, FESEM, TEM, BET, UV-vis, Raman and PL spectroscopy. The hierarchical ZnV2O6 nanosheets show excellent performance towards photoreduction of CO2 with H2O to CH3OH, CH3COOH and HCOOH under visible light. The main product yield, CH3OH of 3253.84 μmol g-cat-1 was obtained over ZnV2O6, 3.4 times the amount of CH3OH produced over the ZnO/V2O5 composite (945.28 μmol g-cat-1). In addition, CH3OH selectivity of 39.96% achieved over ZnO/V2O5, increased to 48.78% in ZnV2O6 nanosheets. This significant improvement in photo-activity over ZnV2O6 structure was due to hierarchical structure with enhanced charge separation by V2O5. The obtained ZnV2O6 hierarchical nanosheets exhibited excellent photocatalytic stability for selective CH3OH production.

Porous Nanocomposite Comprising Ultralong Hydroxyapatite Nanowires Decorated with Zinc-Containing Nanoparticles and Chitosan: Synthesis and Application in Bone Defect Repair.

PubMed

Sun, Tuan-Wei; Yu, Wei-Lin; Zhu, Ying-Jie; Chen, Feng; Zhang, Yong-Gang; Jiang, Ying-Ying; He, Yao-Hua

2018-06-21

Hydroxyapatite nanowires exhibit a great potential in biomedical applications owing to their high specific surface area, high flexibility, excellent mechanical properties, and similarity to mineralized collagen fibrils of natural bone. In this work, zinc-containing nanoparticle-decorated ultralong hydroxyapatite nanowires (Zn-UHANWs) with a hierarchical nanostructure have been synthesized by a one-step solvothermal method. The highly flexible Zn-UHANWs exhibit a hierarchical rough surface and enhanced specific surface area as compared with ultralong hydroxyapatite nanowires (UHANWs). To evaluate the potential application of Zn-UHANWs in bone regeneration, the biomimetic Zn-UHANWs/chitosan (CS) (Zn-UHANWs/CS) composite porous scaffold with 80 wt % Zn-UHANWs was prepared by incorporating Zn-UHANWs into the chitosan matrix by the freeze-drying process. The as-prepared Zn-UHANWs/CS composite porous scaffold exhibits enhanced mechanical properties, highly porous structure, and excellent water retention capacity. In addition, the Zn-UHANWs/CS porous scaffold has a good biodegradability with the sustainable release of Zn, Ca, and P elements in aqueous solution. More importantly, the Zn-UHANWs/CS porous scaffold can promote the osteogenic differentiation of rat bone marrow derived mesenchymal stem cells and facilitate in vivo bone regeneration as compared with the pure CS porous scaffold or UHANWs/CS porous scaffold. Thus, both the Zn-UHANWs and Zn-UHANWs/CS porous scaffold developed in this work are promising for application in bone defect repair. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

In situ synthesis of water-soluble magnetic graphitic carbon nitride photocatalyst and its synergistic catalytic performance.

PubMed

Zhang, Shouwei; Li, Jiaxing; Zeng, Meiyi; Zhao, Guixia; Xu, Jinzhang; Hu, Wenping; Wang, Xiangke

2013-12-11

Water-soluble magnetic-functionalized graphitic carbon nitride (g-C3N4) composites were synthesized successfully by in situ decorating spinel ZnFe2O4 nanoparticles on g-C3N4 sheets (CN-ZnFe) through a one-step solvothermal method. The magnetic properties of CN-ZnFe can be effectively controlled via tuning the coverage density and the size of ZnFe2O4 nanoparticles. The results indicate that the CN-ZnFe exhibits excellent photocatalytic efficiency for methyl orange (MO) and fast separation from aqueous solution by magnet. Interestingly, the catalytic performance of the CN-ZnFe is strongly dependent on the loading of ZnFe2O4. The optimum activity of 160CN-ZnFe photocatalyst is almost 6.4 and 5.6 times higher than those of individual g-C3N4 and ZnFe2O4 toward MO degradation, respectively. By carefully investigating the influence factors, a possible mechanism is proposed and it is believed that the synergistic effect of g-C3N4 and ZnFe2O4, the smaller particle size, and the high solubility in water contribute to the effective electron-hole pairs separation and excellent photocatalytic efficiency. This work could provide new insights that g-C3N4 sheets function as good support to develop highly efficient g-C3N4-based magnetic photocatalysts in environmental pollution cleanup.

One-pot solvothermal synthesis of graphene wrapped rice-like ferrous carbonate nanoparticles as anode materials for high energy lithium-ion batteries

NASA Astrophysics Data System (ADS)

Zhang, Fan; Zhang, Ruihan; Feng, Jinkui; Ci, Lijie; Xiong, Shenglin; Yang, Jian; Qian, Yitai; Li, Lifei

2014-11-01

Well dispersed rice-like FeCO3 nanoparticles were produced and combined with reduced graphene oxide (RGO) via a one-pot solvothermal route. SEM characterization shows that rice-like FeCO3 nanoparticles are homogeneously anchored on the surface of the graphene nanosheets; the addition of RGO is helpful to form a uniform morphology and reduce the particle size of FeCO3 to nano-grade. As anode materials for lithium-ion batteries, the FeCO3/RGO nanocomposites exhibit significantly improved lithium storage properties with a large reversible capacity of 1345 mA h g-1 for the first cycle and a capacity retention of 1224 mA h g-1 after 50 cycles with a good rate capability compared with pure FeCO3 particles. The superior electrochemical performance of the FeCO3/RGO nanocomposite electrode compared to the pure FeCO3 electrode can be attributed to the well dispersed RGO which enhances the electronic conductivity and accommodates the volume change during the conversion reactions. Our study shows that the FeCO3/RGO nanocomposite could be a suitable candidate for high capacity lithium-ion batteries.

Deep eutectic-solvothermal synthesis of nanostructured ceria

PubMed Central

Hammond, Oliver S.; Edler, Karen J.; Bowron, Daniel T.; Torrente-Murciano, Laura

2017-01-01

Ceria is a technologically important material with applications in catalysis, emissions control and solid-oxide fuel cells. Nanostructured ceria becomes profoundly more active due to its enhanced surface area to volume ratio, reactive surface oxygen vacancy concentration and superior oxygen storage capacity. Here we report the synthesis of nanostructured ceria using the green Deep Eutectic Solvent reline, which allows morphology and porosity control in one of the less energy-intensive routes reported to date. Using wide Q-range liquid-phase neutron diffraction, we elucidate the mechanism of reaction at a molecular scale at considerably milder conditions than the conventional hydrothermal synthetic routes. The reline solvent plays the role of a latent supramolecular catalyst where the increase in reaction rate from solvent-driven pre-organization of the reactants is most significant. This fundamental understanding of deep eutectic-solvothermal methodology will enable future developments in low-temperature synthesis of nanostructured ceria, facilitating its large-scale manufacturing using green, economic, non-toxic solvents. PMID:28120829

Synthesis of belt-like BiOBr hierarchical nanostructure with high photocatalytic performance

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

Li, Haiping; Liu, Jingyi; Hu, Tingxia

2016-05-15

Highlights: • BiOBr hierarchical nanobelts (NBs) were solvothermally prepared. • NBs show higher specific surface area and photoabsorption than BiOBr nanosheets. • NBs exhibit higher photoactivity than the nanosheets. - Abstract: One-dimensional (1D) bismuth oxyhalide (BiOX) hierarchical nanostructures are always difficult to prepare. Herein, we report, for the first time, a simple synthesis of BiOBr nanobelts (NBs) via a facile solvothermal route, using bismuth subsalicylate as the template and bismuth source. The BiOBr nanobelts are composed of irregular single crystal nanoparticles with highly exposed (0 1 0) facets. Compared with the BiOBr nanosheets (NSs) with dominant exposed (0 0 1)more » facets, they exhibit higher photocatalytic activity toward degradation of Rhodamine B and Methylene Blue under visible light irradiation. The higher photocatalytic performance of BiOBr NBs arises from their larger specific surface area and higher photoabsorption capability. This study provides a simple route for synthesis of belt-like Bi-based hierarchical nanostructures.« less

One-Pot Synthesis of Reduced Graphene Oxide/Anatase Titanium Dioxide Composites for Photocatalytic Degradation of Methylene Blue.

PubMed

Lee, Hyo In; Park, Soo-Jin

2018-09-01

In this work, highly ordered TiO2-reduced graphene oxide sheets (TGS) were successfully fabricated via a one-pot solvothermal method with different amounts of graphene oxide (0.01, 0.03, 0.05, and 0.07 g). This was achieved by reacting graphene oxide (GO) layers with titanium isopropoxide as the TiO2 precursor. The TGS exhibited superior efficiency compared to pristine TiO2 and the best results were recorded for the TGS-0.05 sample. The presence of the reduced graphene oxide (rGO) component was determined to be an important factor governing the separation of the photogenerated electron-hole pair via interfacial charge transfer. The significantly increased activity of the TGS under simulated solar light in the degradation of methylene blue (MB) indicates that these materials are promising photocatalysts for efficient water purification.

One-Pot Synthesis of Co-Based Coordination Polymer Nanowire for Li-Ion Batteries with Great Capacity and Stable Cycling Stability

NASA Astrophysics Data System (ADS)

Wang, Peng; Lou, Xiaobing; Li, Chao; Hu, Xiaoshi; Yang, Qi; Hu, Bingwen

2018-06-01

Nanowire coordination polymer cobalt-terephthalonitrile (Co-BDCN) was successfully synthesized using a simple solvothermal method and applied as anode material for lithium-ion batteries (LIBs). A reversible capacity of 1132 mAh g-1 was retained after 100 cycles at a rate of 100 mA g-1, which should be one of the best LIBs performances among metal organic frameworks and coordination polymers-based anode materials at such a rate. On the basis of the comprehensive structural and morphology characterizations including fourier transform infrared spectroscopy, 1H NMR, 13C NMR, and scanning electron microscopy, we demonstrated that the great electrochemical performance of the as-synthesized Co-BDCN coordination polymer can be attributed to the synergistic effect of metal centers and organic ligands, as well as the stability of the nanowire morphology during cycling.[Figure not available: see fulltext.

Enhanced electrochemical capacitance of polyimidazole coated covellite CuS dispersed CNT composite materials for application in supercapacitors.

PubMed

Ravi, Seenu; Gopi, Chandu V V M; Kim, Hee Je

2016-08-02

Great attention has been paid to the design and synthesis of distinct core/shell heterostructures for high-performance supercapacitors. We have prepared unique heterostructures consisting of polyimidazole-coated copper sulphide over a carbon nanotube network (CuS@CNT) on nickel foam, which was accomplished through a facile and cost-effective solvothermal method combined with a dip coating process. Hexagonal covellite CuS nanoparticles were dispersed on CNTs using a solvothermal method where dimethylformamide and distilled water were used as solvents. The synthesized CuS and CuS@CNT supercapacitor electrode materials were thoroughly characterized. The polymer supported electrode (PIM/CuS@CNT) shows a high areal capacitance of 1.51 F cm(-2) at a current density of 1.2 A g(-1), which is higher than the CuS@CNT electrode and many other previously reported CuS electrode materials. After 1000 cycles at a high current density of 1.2 A g(-1), the retention rate is 92%, indicating good long-term cycling stability. These results indicate that the PIM/CuS@CNT electrode is promising for high-performance supercapacitor applications.

Synthesis of nanocrystalline TiO 2 in toluene by a solvothermal route

NASA Astrophysics Data System (ADS)

Kim, Chung-Sik; Moon, Byung Kee; Park, Jong-Ho; Tae Chung, Su; Son, Se-Mo

2003-07-01

A solvothermal synthetic method to TiO 2 nanoparticles has been investigated in toluene solutions with titanium isopropoxide (TIP) as precursor. Weight ratios of precursor to solvent prepared in the mixture are 5/100, 10/100, 20/100, 30/100 and 40/100. At the weight ratio of 10/100, 20/100 and 30/100, TiO 2 nanocrystalline particles were obtained after synthesis at 250°C for 3 h in an autoclave. X-ray diffraction and tranmission electron microscopy shows that the product has uniform anatase structure with average particle size below 20 nm. As the composition of TIP in the solution increases, the particle size of TiO 2 powder tends to increase. At 5/100 and 40/100, however, pale yellow colloidal solution is obtained after synthesis and crystalline phase of TiO 2 is not produced. The specific surface area of the TiO 2 nanocrystalline powder was also investigated using BET surface area analyzer.

Solvothermal synthesis and structure of 3D frameworks of Nd(III) and Y(III) with thiophene-2,5-dicarboxylate and N,N‧-diethylformamide

NASA Astrophysics Data System (ADS)

Sharma, Swati; Yawer, Mohd; Kariem, Mukaddus; Sheikh, Haq Nawaz

2016-08-01

Two new 3D MOFs [Nd2(TDA)3(DEF)2(H2O)]n (1) and [Y4(TDA)6(DEF)4]n (2) [Thiophene-2,5-dicarboxylic acid (H2TDA) and N,N‧-diethylformamide (DEF)] were synthesized by solvothermal method. They were characterized by elemental analyses, infrared spectroscopy and single crystal X-ray diffraction studies. The two MOFs (1) and (2) belong to the monoclinic system with space group P21/n and C 2 respectively. Structural characterizations by single-crystal X-ray crystallography reveal that 1 and 2 adopt three-dimensional frameworks constructed by cross-linking of rod shaped infinite chain secondary building unit (SBU) by thiophene-2,5-dicarboxylates as linker. These frameworks feature rhomboidal channels, inside which coordinated DEF/H2O solvent molecules are located. DEF plays pivotal role in reaction and design of MOFs. Thermogravimetric analysis shows that both MOFs are thermally robust.

Water molecule-enhanced CO{sub 2} insertion in lanthanide coordination polymers

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

Luo Liushan; Huang Xiaoyuan; Wang Ning

2009-08-15

Two new lanthanide coordination polymers H{sub 2}N(CH{sub 3}){sub 2}.[Eu{sup III}{sub 2}(L{sub 1}){sub 3}(L{sub 2})] (1, L{sub 1}=isophthalic acid dianion, L{sub 2}=formic acid anion) and [La{sup III}(2,5-PDC)(L{sub 2})](2, 2,5-PDC=2,5-pyridinedicarboxylate dianion) were synthesized under solvothermal conditions. It is of interest that the formic ligand (L{sub 2}) is not contained in the stating materials, but arises from the water molecule-enhanced CO{sub 2} insertion during the solvothermal process. Both of the two compounds exhibit complicated three dimensional sandwich-like frameworks. - Graphical abstract: Two new lanthanide coordination polymers involving water molecule-enhanced CO{sub 2} insertion resulting in the formation of formic anion and dimethylammonium cation weremore » synthesized under solvothermal conditions.« less

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

Tian, Yue; College of Life Science, Dalian Nationalities University, Dalian, Liaoning 116600; Chen, Baojiu, E-mail: chenmbj@sohu.com

Tb{sup 3+}, Eu{sup 3+} codoped YF{sub 3} nano- and micro-crystals with the morphologies of ellipsoid-like nanoplate, spindle, sandwich-structural rhombus and nanoaggregate were synthesized through a solvothermal method. The morphologies of the prepared products can be tailored by controlling the volume ratio of ethylene glycol (EG) to H{sub 2}O, solvent type or the reaction time. A possible formation mechanism of the sandwich-structural rhombus like YF{sub 3} phosphor was proposed. The emitting colors of YF{sub 3}:Tb{sup 3+},Eu{sup 3+} phosphors can be easily tuned from yellowish green, yellow to orange by increasing Eu{sup 3+} concentration. The energy transfer from Tb{sup 3+} to Eu{supmore » 3+} in YF{sub 3} phosphors was studied. It was found that the interaction type between Tb{sup 3+} and Eu{sup 3+} is electric dipole-dipole interaction. - Graphical abstract: Sandwich-structural rhombus like YF{sub 3}:Tb{sup 3+}, Eu{sup 3+} phosphors were synthesized through a solvothermal process. The formation mechanism of the sandwich-structural rhombus like YF{sub 3}:Tb{sup 3+}, Eu{sup 3+} phosphors was studied. Highlights: Black-Right-Pointing-Pointer YF{sub 3} nano- and micro-crystals were synthesized through solvothermal route. Black-Right-Pointing-Pointer A formation mechanism of the sandwich-structural rhombus like YF{sub 3} was proposed. Black-Right-Pointing-Pointer The emitting colors of YF{sub 3}:Tb{sup 3+},Eu{sup 3+} phosphors can be tuned. Black-Right-Pointing-Pointer Energy transfer from Tb{sup 3+} to Eu{sup 3+} is confirmed as electric dipole-dipole interaction.« less

A nanoporous 3D zinc(II) metal–organic framework for selective absorption of benzaldehyde and formaldehyde

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

Moradpour, Tahereh; Abbasi, Alireza, E-mail: aabbassi@khayam.ut.ac.ir; Van Hecke, Kristof

A new 3D nanoporous metal–organic framework (MOF), [[Zn{sub 4}O(C{sub 24}H{sub 15}N{sub 6}O{sub 6}){sub 2}(H{sub 2}O){sub 2}]·6H{sub 2}O·DMF]{sub n} (1) based on 4,4′,4″-s-triazine-1,3,5-triyltri-p-aminobenzoate (TATAB) ligand was solvothermally synthesized and characterized by single–crystal X-ray diffraction, Powder X-ray diffraction (PXRD), infrared spectroscopy (IR) and Brunauer–Emmett–Teller (BET) analyses. X-ray single crystal diffraction analysis reveals that 1 exhibits a 3D network with new kvh1 topology. Semi-empirical (AM1) calculations were carried out to obtain stable conformers for TATAB ligand. In addition, the absorption of two typical aldehydes (benzaldehyde and formaldehyde) in the presence of 1 was investigated and the effect of the aldehyde concentration, exposure timemore » and temperature was studied. It was found that compound 1 has a potential for the absorption of aldehydes under mild conditions. - Graphical abstract: Absorption of two typical aldehydes (formaldehyde and benzaldehyde) by solvothermally synthesized of a 3D nano-porous MOF based on TATAB tricarboxylate ligand and Zn (NO{sub 3}){sub 2}·6H{sub 2}O. - Highlights: • We present a 3D Zn(II)-MOF with TATAB linker by solvothermal method. • The framework possesses a new kvh1 topology. • The framework displays formaldehyde and benzaldehyde absorption property. • Conformational analysis was performed to determine the stable linker geometry.« less

Simple solvothermal synthesis of hydrophobic magnetic monodispersed Fe{sub 3}O{sub 4} nanoparticles

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

Liu, Jing; Wang, Lu; Wang, Jing, E-mail: Jingwang@home.ipe.ac.cn

Graphical abstract: A facile method to produce monodispersed magnetite nanoparticles is based on the solvothermal reaction of iron acetylacetonate (Fe(acac)3) decomposition. The sizes ranged from 7 to 12 nm, which could be controlled by adjusting the volume ratio of oleylamine to n-hexane. Display Omitted Highlights: ► The solvethermal reaction of Fe(acac){sub 3} decomposition was carried out at mild temperature in the presence of oleylamine and n-hexane. ► The size of nanocrystals is controlled by adjusting the volume ratio of oleylamine to n-hexane. ► The low-boiling-point solvent n-hexane offered autogenous pressure parameter after gasified in the reaction temperature. ► The asmore » prepared hydrophobic monodisperse Fe{sub 3}O{sub 4} NPs can be used to prepare the magnetic micelles for future biomedical applications. -- Abstract: A new solvothermal method is proposed for the preparation of Fe{sub 3}O{sub 4} nanoparticles (NPs) from iron acetylacetonate in the presence of oleylamine and n-hexane. The products are characterized by X-ray powder diffraction, infrared (IR) spectroscopy, transmission electron microscopy, thermogravimetry/differential thermogravimetry (TG/DTG) analysis, and vibrating sample magnetometery. The new procedure yields superparamagnetic monodispersed Fe{sub 3}O{sub 4} particles with sizes ranging from 7 nm to 12 nm. The nanocrystal sizes are controlled by adjusting the volume ratio of oleylamine to n-hexane. IR and TG/DTG analyses indicate that the oleylamine molecules, as stabilizers, are adsorbed on the surface of Fe{sub 3}O{sub 4} NPs as bilayer adsorption models. The surface adsorption quantities of oleylamine on 7.5 and 10.4 nm-diameter Fe{sub 3}O{sub 4} NPs are 18% and 11%, respectively. The hydrophobic surface of the obtained nanocrystals is passivated by adsorbed organic solvent molecules. These molecules provide stability against agglomeration, enable solubility in nonpolar solvents, and allow the formation of magnetic polymer micelles.« less

A new method for the preparation of a Fe{sub 3}O{sub 4}/graphene hybrid material and its applications in electromagnetic wave absorption

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

Wu, Tsung-Yung; Lu, Kai-Tai; Peng, Cheng-Hsiung

2015-10-15

Graphical abstract: A microwave-assisted solvothermal process was used to prepare Fe{sub 3}O{sub 4} nanoparticles/graphene hybrids, which could be applied as an electromagnetic (EM) radiation absorbent. The absorber, composed of 20 wt% Fe{sub 3}O{sub 4}/graphene–epoxy, exhibited a dual-frequency reflection characteristic covering the C and Ku bands with maximum reflection losses of less than −20 dB at thicknesses of 4 and 5 mm. - Highlights: • Fe{sub 3}O{sub 4}/graphene composites were prepared by a microwave-assisted solvothermal route. • Uniform loading of Fe{sub 3}O{sub 4} nanoparticles on graphene was obtained. • The products as-synthesized show great promise as a microwave absorption material. •more » Synergistic effects of Fe{sub 3}O{sub 4} and graphene caused improved absorption efficiency. • The Fe{sub 3}O{sub 4}/graphene product possessed a dual-frequency reflection characteristic. - Abstract: A rapid, simple, and inexpensive process combining a microwave-assisted technique and a solvothermal method has been developed using graphene sheets and FeCl{sub 3}·6H{sub 2}O as the reactant to prepare graphene/Fe{sub 3}O{sub 4} nanoparticle hybrids, which can be applied as an electromagnetic radiation absorbent. The experimental factors (i.e., composition ratio, microwave power, and irradiation time) on the products’ characteristics were examined. Under optimal conditions, the morphological analysis revealed that the graphene sheet was homogeneously covered with Fe{sub 3}O{sub 4} nanoparticles (∼50 nm). The electromagnetic parameters of the composites made from 20 wt% Fe{sub 3}O{sub 4}/graphene–epoxy were measured by a vector network analyzer. It was found that the 4- and 5 mm-thick composites could attain a reflection loss below −20 dB in the dual-ranges of 4–8 and 12–18 GHz.« less

Fabrication of nickel-foam-supported layered zinc-cobalt hydroxide nanoflakes for high electrochemical performance in supercapacitors.

PubMed

Yuan, Peng; Zhang, Ning; Zhang, Dan; Liu, Tao; Chen, Limiao; Liu, Xiaohe; Ma, Renzhi; Qiu, Guanzhou

2014-10-04

Nickel foam supported Zn-Co hydroxide nanoflakes were fabricated by a facile solvothermal method. Benefited from the unique structure of Zn-Co hydroxide nanoflakes on a nickel foam substrate, the as prepared materials exhibited an excellent specific capacitance of 901 F g(-1) at 5 A g(-1) and remarkable cycling stability as electrode materials in supercapacitors.

CeO₂ Enhanced Ethanol Sensing Performance in a CdS Gas Sensor.

PubMed

Li, Meishan; Ren, Wei; Wu, Rong; Zhang, Min

2017-07-05

CdS nanowires (NWs) were fabricated through a facile low-temperature solvothermal method, following which CeO₂ nanoparticles were modified on the NWs. The ethanol sensing characteristics of pure CdS and decorated ones with different CeO₂ content were studied. It was found that the sensing performance of CdS was significantly improved after CeO₂ decoration. In particular, the 5 at% CeO₂/CdS composite exhibited a much higher response to 100 ppm ethanol (about 52), which was 2.6 times larger than that of pure CdS. A fast response and recovery time (less than 12 s and 3 s, respectively) were obtained as well as an excellent selectivity. These results make the CeO₂-decorated CdS NWs good candidates for ethanol sensing applications.

Ag/MnO₂ Nanorod as Electrode Material for High-Performance Electrochemical Supercapacitors.

PubMed

Guo, Zengcai; Guan, Yuming; Dai, Chengxiang; Mu, Jingbo; Che, Hongwei; Wang, Guangshuo; Zhang, Xiaoliang; Zhang, Zhixiao; Zhang, Xiliang

2018-07-01

A one-dimensional hierarchical Ag nanoparticle (AgNP)/MnO2 nanorod (MND) nanocomposite was synthesized by combining a simple solvothermal method and a facile reduction approach in situ. Owing to its high electrical conductivity, the resulting AgNP/MND nanocomposite displayed a high specific capacitance of 314 F g-1 at a current density of 2 A g-1, which was much higher than that of pure MNDs (178 F g-1). Resistances of the electrolyte (Rs) and charge transportation (Rct) of the nanocomposite were much lower than that of pure MNDs. Moreover, the nanocomposite exhibited outstanding long-term cycling ability (9% loss of initial capacity after 1000 cycles). These results indicated that the nanocomposite could serve as a promising and useful electrode material for future energy-storage applications.

Solvothermal growth of a ruthenium metal-organic framework featuring HKUST-1 structure type as thin films on oxide surfaces.

PubMed

Kozachuk, Olesia; Yusenko, Kirill; Noei, Heshmat; Wang, Yuemin; Walleck, Stephan; Glaser, Thorsten; Fischer, Roland A

2011-08-14

Phase-pure crystalline thin films of a mixed-valence Ru(2)(II,III) metal-organic framework with 1,3,5-benzenetricarboxylate (btc) as a linker were solvothermally grown on amorphous alumina and silica surfaces. Based on the Rietveld refinement, the structure of Ru-MOF was assigned to be analogous to [Cu(3)(btc)(2)] (HKUST-1). This journal is © The Royal Society of Chemistry 2011

Preparation of weak-light-driven TiO2-based catalysts via adsorbed-layer nanoreactor synthesis and enhancement of their photo-degradation performance in seawater

NASA Astrophysics Data System (ADS)

Wang, Ting; Xu, Zhi-yong; Zhu, Yi-chen; Wu, Li-guang; Yuan, Hao-xuan; Li, Chang-chun; Liu, Ya-yu; Cai, Jing

2017-11-01

Graphene oxide (GO) was first employed as a support in preparing TiO2 nanoparticles by adsorbed-layer nanoreactor synthesis (ALNS). Both TiO2 crystallization and GO reduction simultaneously occurred during solvothermal treatment with alcohol as a solvent. By transmission electron microscopy, high resolution transmission electron microscopy, X-ray diffraction, X-ray photoelectron spectroscopy, Fourier transform infrared spectroscopy, and photoluminescence spectroscopy, the results showed that TiO2 nanoparticles with less than 10 nm of size distributed very homogeneously on the GO surface. Tight interaction between TiO2 particles and GO surface could effectively inhibit the aggregation of TiO2 particles, during solvothermal treatment for anatase TiO2 formation. Alcohol could also reduce oxygenated functional groups on GO surface after solvothermal treatment. TiO2 particles with small size and the decrease in oxygenated functional groups on the GO surface both caused high separation efficiency of photo-generated charge carriers, thus resulting in high photo-degradation performance of catalysts. Strong phenol adsorption on photocatalyst was key to enhancing photo-degradation efficiency for phenol in seawater. Moreover, the change in catalyst structure was minimal at different temperatures of solvothermal treatment. But, the degradation rate and efficiency for phenol in seawater were obviously enhanced because of the sensitive structure-activity relationship of catalysts under weak-light irradiation.

Validation of a One-Step Method for Extracting Fatty Acids from Salmon, Chicken and Beef Samples.

PubMed

Zhang, Zhichao; Richardson, Christine E; Hennebelle, Marie; Taha, Ameer Y

2017-10-01

Fatty acid extraction methods are time-consuming and expensive because they involve multiple steps and copious amounts of extraction solvents. In an effort to streamline the fatty acid extraction process, this study compared the standard Folch lipid extraction method to a one-step method involving a column that selectively elutes the lipid phase. The methods were tested on raw beef, salmon, and chicken. Compared to the standard Folch method, the one-step extraction process generally yielded statistically insignificant differences in chicken and salmon fatty acid concentrations, percent composition and weight percent. Initial testing showed that beef stearic, oleic and total fatty acid concentrations were significantly lower by 9-11% with the one-step method as compared to the Folch method, but retesting on a different batch of samples showed a significant 4-8% increase in several omega-3 and omega-6 fatty acid concentrations with the one-step method relative to the Folch. Overall, the findings reflect the utility of a one-step extraction method for routine and rapid monitoring of fatty acids in chicken and salmon. Inconsistencies in beef concentrations, although minor (within 11%), may be due to matrix effects. A one-step fatty acid extraction method has broad applications for rapidly and routinely monitoring fatty acids in the food supply and formulating controlled dietary interventions. © 2017 Institute of Food Technologists®.

Small-sized PdCu nanocapsules on 3D graphene for high-performance ethanol oxidation

NASA Astrophysics Data System (ADS)

HuThese Authors Contributed Equally To This Work., Chuangang; Zhai, Xiangquan; Zhao, Yang; Bian, Ke; Zhang, Jing; Qu, Liangti; Zhang, Huimin; Luo, Hongxia

2014-02-01

A one-pot solvothermal process has been developed for direct preparation of PdCu nanocapsules (with a size of ca. 10 nm) on three-dimensional (3D) graphene. Due to the 3D pore-rich network of graphene and the unique hollow structure of PdCu nanocapsules with a wall thickness of ca. 3 nm, the newly-prepared PdCu/3D graphene hybrids activated electrochemically have great electrocatalytic activity towards ethanol oxidation in alkaline media, much better than single-phase Pd and commercial E-TEK 20% Pt/C catalysts promising for application in direct ethanol fuel cells.A one-pot solvothermal process has been developed for direct preparation of PdCu nanocapsules (with a size of ca. 10 nm) on three-dimensional (3D) graphene. Due to the 3D pore-rich network of graphene and the unique hollow structure of PdCu nanocapsules with a wall thickness of ca. 3 nm, the newly-prepared PdCu/3D graphene hybrids activated electrochemically have great electrocatalytic activity towards ethanol oxidation in alkaline media, much better than single-phase Pd and commercial E-TEK 20% Pt/C catalysts promising for application in direct ethanol fuel cells. Electronic supplementary information (ESI) available. See DOI: 10.1039/c3nr05722d

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

Facile synthesis of ultrafine cobalt oxide nanoparticles for high-performance supercapacitors.

PubMed

Liu, Fangyan; Su, Hai; Jin, Long; Zhang, Haitao; Chu, Xiang; Yang, Weiqing

2017-11-01

The ultrafine Co 3 O 4 nanoparticles are successfully prepared by a novel solvothermal-precipitation approach which exploits the supernatant liquid of Co 3 O 4 nanoflake micropheres synthesized by solvothermal method before. Interestingly, the water is only employed to obtain the ultrafine nanoparticles in supernatant liquid which was usually thrown away before. The microstructure measurement results of the as-grown samples present the homogeneous disperse ultrafine Co 3 O 4 nanoparticles with the size of around 5-10nm. The corresponding synthesis mechanism of the ultrafine Co 3 O 4 nanoparticles is proposed. More importantly, these ultrafine Co 3 O 4 nanoparticles obtained at 250°C show the highest specific capacitance of 523.0Fg -1 at 0.5Ag -1 , 2.6 times that of Co 3 O 4 nanoflake micropheres due to the quantum size effect. Meanwhile, the sample annealed under 350°C possesses the best cycling stability with capacitance retention of 104.9% after 1500 cycles. These results unambiguously demonstrate that this work not only provides a novel, facile, and eco-friendly approach to prepare high-performance Co 3 O 4 nanoparticles electrode materials for supercapacitors but also develops a widely used method for the preparation of other materials on a large scale. Copyright © 2017 Elsevier Inc. All rights reserved.

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

Sun, Shibin; College of Electromechanical Engineering, Qingdao University of Science and Technology, Qingdao 266061; Chang, Xueting, E-mail: xuetingchang@yahoo.cn

Cobalt-doped tungsten oxide mesocrystals with different morphologies have been successfully generated using a solvothermal method with tungsten hexachloride and cobalt chloride salts as precursors. The resulting mesocrystals were characterized by X-ray diffraction, field emission scanning electron microscopy, transmission electron microscopy, Brunauer-Emmet-Teller analysis of nitrogen sorptometer, and UV-vis diffuse reflectance spectroscopy. The photocatalytic properties of the cobalt-doped tungsten oxide mesocrystals were evaluated on the basis of their ability to degrade methyl orange in an aqueous solution under simulated sunlight irradiation. Results showed that the cobalt doping had obvious effect on the morphologies of the final products, and lenticular and blocky cobalt-dopedmore » tungsten oxide mesocrystals could be obtained with 1.0 wt.% and 2.0 wt.% cobalt doping, respectively. The cobalt-doped tungsten oxides exhibited superior photocatalytic activities to that of the undoped tungsten oxide. - Graphical abstract: Schematic illustrations of the growth of the bundled nanowires, lenticular mesocrystals, and blocky mesocrystals. Highlights: Black-Right-Pointing-Pointer Co-doped W{sub 18}O{sub 49} mesocrystals were synthesized using a solvothermal method. Black-Right-Pointing-Pointer The Co doping has obvious effect on the morphology of the final mesocrystals. Black-Right-Pointing-Pointer The Co-doped W{sub 18}O{sub 49} exhibited superior photocatalytic activity to the undoped W{sub 18}O{sub 49}.« less

Nonstoichiometric Zn Ferrite and ZnFe2O4/Fe2O3 Composite Spheres: Preparation, Magnetic Properties, and Chromium Removal

NASA Astrophysics Data System (ADS)

Hang, Chun-Liang; Yang, Li-Xia; Sun, Chang-Mei; Liang, Ying

2018-03-01

Monodisperse and porous nonstoichiometric Zn ferrite can be prepared by a solvothermal method. Such non-Zn ferrite was used to be the precursor for synthesis of ZnFe2O4/Fe2O3 composite via calcination at 600°C for 3 h in air. X-ray powder diffractometer (XRD) and Energy Dispersive Spectrometer (EDS) proved the nonstoichiometry of Zn ferrite synthesized by solvothermal method and the formation of ZnFe2O4/Fe2O3 composite via calcination. TEM image showed that non-Zn ferrite spheres with wormlike nanopore structure were made of primary nanocrystals. BET surface area of non-Zn ferrite was much higher than that of ZnFe2O4/Fe2O3 composite. Saturation magnetization of non-Zn ferrites was significantly higher than that of ZnFe2O4/Fe2O3 composites. Calcination of non-Zn ferrite resulted in the formation of large amount of non-magnetic Fe2O3,which caused a low magnetization of composite. Because of higher BET surface area and higher saturation magnetization, non-Zn ferrite presented better Cr6+ adsorption property than ZnFe2O4/Fe2O3 composites.

Synthesis of gadolinium carbonate-conjugated-poly(ethylene)glycol (Gd{sub 2}(CO{sub 3}){sub 3}@PEG) particles via a modified solvothermal method

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

Nasution, Erika L. Y.; Ahab, Atika; Nuryadin, Bebeh W.

2016-02-08

PEGylated gadolinium carbonate ((Gd{sub 2}(CO{sub 3}){sub 3})@PEG) powder was successfully synthesized by a modified solvothermal method. The synthesized products were characterized by means of X-ray diffraction (XRD), Fourier Transform Infrared spectroscopy (FTIR), Scanning Electron Microscopy (SEM), and Energy Dispersive X-ray Spectroscopy (EDS). A systematic change in the chemical surface composition, crystallinity and size properties of the Gd{sub 2}(CO{sub 3}){sub 3}@PEG particles was observed by increasing the reaction time at 5 hours, 7 hours, and 8 hours. The corresponding XRD patterns showed that the Gd{sub 2}(CO{sub 3}){sub 3} particles had hexagonal symmetry (JCPDS No. 37-0559) with a crystallite size of 3.5,more » 2.9, and 4.6 nm. FTIR spectra showed that the Gd{sub 2}(CO{sub 3}){sub 3})@PEG particles were formed with the PEG as carbonyl and hydroxyl group attached to the surface. SEM analysis showed that the Gd{sub 2}(CO{sub 3}){sub 3})@PEG particles had a flake-like morphology of homogeneous sized particles and agglomerates. EDS analysis confirmed the presence of constituent Gd{sub 2}(CO{sub 3}){sub 3} elements.« less

Preparation of flower-like CuS by solvothermal method for photocatalytic, UV protection and EMI shielding applications

NASA Astrophysics Data System (ADS)

Hu, Xiao-Sai; Shen, Yong; Xu, Li-Hui; Wang, Li-Ming; Lu, Li-sha; Zhang, Ya-ting

2016-11-01

The flower-like CuS hierarchical structures were synthesized by solvothermal method. The as-prepared products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infrared(FTIR) spectroscopy, UV-vis optical absorption spectroscopy and thermogravimetric analysis (TGA). The results demonstrated that the as-prepared flower-like CuS with the diameter of 1-5 um was pure hexagonal phase CuS and had well-defined flower-like structures. (1) The as-prepared CuS was proved to possess high photocatalytic performance with band gap of 1.45 eV. The degradation rate of Methylene blue (MB) was up to, 98.26%, 100% after 30 min under UV and visible irradiation. (2)The UPF of cotton fabric treated with CuS reached up to 174 compared with the original untreated fabric with the UPF 20.62. (3) The electromagnetic interference shielding effectiveness (EMI SE) of CuS coating was up to 27-31 dB when the content of CuS increased to 28.6%wt in the frequency of 300 KHz-3 GHz. Furthermore, the influence of reaction conditions on the morphology of the as-prepared CuS was investigated systematically and the possible formation mechanism of the CuS hierarchical structure was also proposed.

Biocompatible PEGylated MoS2 nanosheets: controllable bottom-up synthesis and highly efficient photothermal regression of tumor.

PubMed

Wang, Shige; Li, Kai; Chen, Yu; Chen, Hangrong; Ma, Ming; Feng, Jingwei; Zhao, Qinghua; Shi, Jianlin

2015-01-01

Two-dimensional transition metal dichalcogenides, particularly MoS2 nanosheets, have been deemed as a novel category of NIR photothermal transducing agent. Herein, an efficient and versatile one-pot solvothermal synthesis based on "bottom-up" strategy has been, for the first time, proposed for the controlled synthesis of PEGylated MoS2 nanosheets by using a novel "integrated" precursor containing both Mo and S elements. This facile but unique PEG-mediated solvothermal procedure endowed MoS2 nanosheets with controlled size, increased crystallinity and excellent colloidal stability. The photothermal performance of nanosheets was optimized via modulating the particulate size and surface PEGylation. PEGylated MoS2 nanosheets with desired photothermal conversion performance and excellent colloidal and photothermal stability were further utilized for highly efficient photothermal therapy of cancer in a tumor-bearing mouse xenograft. Without showing observable in vitro and in vivo hemolysis, coagulation and toxicity, the optimized MoS2-PEG nanosheets showed promising in vitro and in vivo anti-cancer efficacy. Copyright © 2014 Elsevier Ltd. All rights reserved.

Reduced Graphene Oxide-Cadmium Zinc Sulfide Nanocomposite with Controlled Band Gap for Large-Area Thin-Film Optoelectronic Device Application

NASA Astrophysics Data System (ADS)

Ibrahim, Sk; Chakraborty, Koushik; Pal, Tanusri; Ghosh, Surajit

2017-12-01

Herein, we report the one pot single step solvothermal synthesis of reduced grapheme oxide-cadmium zinc sulfide (RGO-Cd0.5Zn0.5S) composite. The reduction in graphene oxide (GO), synthesis of Cd0.5Zn0.5S (mentioned as CdZnS in the text) nanorod and decoration of CdZnS nanorods onto RGO sheet were done simultaneously. The structural, morphological and optical properties were studied thoroughly by different techniques, such as XRD, TEM, UV-Vis and PL. The PL intensity of CdZnS nanorods quenches significantly after the attachment of RGO, which confirms photoinduced charge transformation from CdZnS nanorods to RGO sheet through the interface of RGO-CdZnS. An excellent photocurrent generation in RGO-CdZnS thin-film device has been observed under simulated solar light irradiation. The photocurrent as well as photosensitivity increases linearly with the solar light intensity for all the composites. Our study establishes that the synergistic effect of RGO and CdZnS in the composite is capable of getting promising applications in the field of optoelectronic devising.

Erbium and nitrogen co-doped SrTiO{sub 3} with highly visible light photocatalytic activity and stability by solvothermal synthesis

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

Xu, Jing; Wei, Yuelin, E-mail: ylwei@hqu.edu.cn; Huang, Yunfang

Highlights: • Er/N co-doped SrTiO{sub 3} was prepared by a solvothermal process at low temperature. • The co-doping induces the band gap narrowing and prominent absorbance in visible light region. • The samples show excellent catalytic activity and stability under visible light irradiation. - Abstract: Erbium–nitrogen co-doped SrTiO{sub 3} photocatalysts have been synthesized by a facile solvothermal method. The resulting samples were analyzed by FE-SEM, XRD, BET-surface area and UV–vis. The UV–vis absorption spectra of these powders indicated that erbium–nitrogen co-doped SrTiO{sub 3} possessed stronger absorption bands in the visible light region in comparison with that of pure SrTiO{sub 3}.more » The occurrence of the erbium–nitrogen co-doped cubic SrTiO{sub 3} induced the higher photocatalytic activities for the degradation of methyl orange (MO) under irradiation by ultraviolet light and visible light, respectively, being superior to that of pure SrTiO{sub 3} and commercial TiO{sub 2} (P-25) powders. In addition, the Er–N co-doped SrTiO{sub 3} (initial molar ratios of Sr/Er/N = 1:0.015:0.1, designated as S5) sample showed the best photocatalytic activity with the degradation rate as high as 98% after 30 min under the visible light irradiation. After five cycles, the photocatalytic activity of the S5 catalyst showed no significant decrease, which indicated that the photocatalysts were stable under visible light irradiation.« less

In-situ synthesis of monodisperse micro-nanospherical LiFePO4/carbon cathode composites for lithium-ion batteries

NASA Astrophysics Data System (ADS)

Gong, Hao; Xue, Hairong; Wang, Tao; He, Jianping

2016-06-01

The LiFePO4 is recognized as the promising cathode material, due to its high specific capacity, excellent, structural stability and environmental benignity. However, it is blamed for the low tap density and poor rate performance when served as the cathode materials for a long time. Here, the microspheric LiFePO4/C composites are successfully synthesized through a one-step in-situ solvothermal method combined with carbothermic reduction. These LiFePO4/C microspheres are assembled by LiFePO4 nanoparticles (∼100 nm) and uniformly coated by the carbon, which show a narrow diameter distribution of 4 μm. As a cathode material for lithium ion batteries, the LiFePO4/C composites can deliver an initiate charge capacity of 155 mAh g-1 and retain 90% of initial capacity after 200 cycles at 0.1 C. When cycled at high current densities up to 20 C, it shows a discharge capacity of ∼60 mAh g-1, exhibiting superior rate performance. The significantly improved electrochemical performance of LiFePO4/C composites material can be attributed to its special micro-nano hierarchical structure. Microspheric LiFePO4/C composites exhibit a high tap density about 1.3 g cm-3. What's more, the well-coated carbon insures the high electrical conductivity and the nano-sized LiFePO4/C particles shorten lithium ion transport, thus exhibiting the high specific capacity, high cycling stability and good rate performance.

Enhanced photocatalytic performance and degradation pathway of Rhodamine B over hierarchical double-shelled zinc nickel oxide hollow sphere heterojunction

NASA Astrophysics Data System (ADS)

Zhang, Ying; Zhou, Jiabin; Cai, Weiquan; Zhou, Jun; Li, Zhen

2018-02-01

In this study, hierarchical double-shelled NiO/ZnO hollow spheres heterojunction were prepared by calcination of the metallic organic frameworks (MOFs) as a sacrificial template in air via a one-step solvothermal method. Additionally, the photocatalytic activity of the as-prepared samples for the degradation of Rhodamine B (RhB) under UV-vis light irradiation were also investigated. NiO/ZnO microsphere comprised a core and a shell with unique hierarchically porous structure. The photocatalytic results showed that NiO/ZnO hollow spheres exhibited excellent catalytic activity for RhB degradation, causing complete decomposition of RhB (200 mL of 10 g/L) under UV-vis light irradiation within 3 h. Furthermore, the degradation pathway was proposed on the basis of the intermediates during the photodegradation process using liquid chromatography analysis coupled with mass spectroscopy (LC-MS). The improvement in photocatalytic performance could be attributed to the p-n heterojunction in the NiO/ZnO hollow spheres with hierarchically porous structure and the strong double-shell binding interaction, which enhances adsorption of the dye molecules on the catalyst surface and facilitates the electron/hole transfer within the framework. The degradation mechanism of pollutant is ascribed to the hydroxyl radicals (rad OH), which is the main oxidative species for the photocatalytic degradation of RhB. This work provides a facile and effective approach for the fabrication of porous metal oxides heterojunction with high photocatalytic activity and thus can be potentially used in the environmental purification.

Ti2Nb10O29-x mesoporous microspheres as promising anode materials for high-performance lithium-ion batteries

NASA Astrophysics Data System (ADS)

Deng, Shengjue; Luo, Zhibin; Liu, Yating; Lou, Xiaoming; Lin, Chunfu; Yang, Chao; Zhao, Hua; Zheng, Peng; Sun, Zhongliang; Li, Jianbao; Wang, Ning; Wu, Hui

2017-09-01

Ti2Nb10O29 has recently been reported as a promising anode material for lithium-ion batteries. However, its poor electronic conductivity and insufficient Li+-ion diffusion coefficient significantly limit its rate capability. To tackle this issue, a strategy combining nanosizing and crystal-structure modification is employed. Ti2Nb10O29-x mesoporous microspheres with a sphere-size range of 0.5-4 μm are prepared by a one-step solvothermal method followed by thermal treatment in N2. These Ti2Nb10O29-x mesoporous microspheres exhibit primary nanoparticles, a large specific surface area (22.9 m2 g-1) and suitable pore sizes, leading to easy electron/Li+-ion transport and good interfacial reactivity. Ti2Nb10O29-x shows a defective shear ReO3 crystal structure with O2- vacancies and an increased unit cell volume, resulting in its increased Li+-ion diffusion coefficient. Besides Ti4+ and Nb5+ ions, Ti2Nb10O29-x comprises Nb4+ ions with unpaired 4d electrons, which significantly increase its electronic conductivity. As a result of these improvements, the Ti2Nb10O29-x mesoporous microspheres reveal superior electrochemical performances in term of large reversible specific capacity (309 mAh g-1 at 0.1 C), outstanding rate capability (235 mAh g-1 at 40 C) and durable cyclic stability (capacity retention of 92.1% over 100 cycles at 10 C).

Effects of rare earth doping on multi-core iron oxide nanoparticles properties

NASA Astrophysics Data System (ADS)

Petran, Anca; Radu, Teodora; Borodi, Gheorghe; Nan, Alexandrina; Suciu, Maria; Turcu, Rodica

2018-01-01

New multi-core iron oxide magnetic nanoparticles doped with rare earth metals (Gd, Eu) were obtained by a one step synthesis procedure using a solvothermal method for potential biomedical applications. The obtained clusters were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), energy-dispersive X-ray microanalysis (EDX), X-ray photoelectron spectroscopy (XPS) and magnetization measurements. They possess high colloidal stability, a saturation magnetization of up to 52 emu/g, and nearly spherical shape. The presence of rare earth ions in the obtained samples was confirmed by EDX and XPS. XRD analysis proved the homogeneous distribution of the trivalent rare earth ions in the inverse-spinel structure of magnetite and the increase of crystal strain upon doping the samples. XPS study reveals the valence state and the cation distribution on the octahedral and tetrahedral sites of the analysed samples. The observed shift of the XPS valence band spectra maximum in the direction of higher binding energies after rare earth doping, as well as theoretical valence band calculations prove the presence of Gd and Eu ions in octahedral sites. The blood protein adsorption ability of the obtained samples surface, the most important factor of the interaction between biomaterials and body fluids, was assessed by interaction with bovine serum albumin (BSA). The rare earth doped clusters surface show higher afinity for binding BSA. In vitro cytotoxicity test results for the studied samples showed no cytotoxicity in low and medium doses, establishing a potential perspective for rare earth doped MNC to facilitate multiple therapies in a single formulation for cancer theranostics.

Synthesis of framework isomer MOFs containing zinc and 4-tetrazolyl benzenecarboxylic acid via a structure directing solvothermal approach

DOE PAGES

Ordonez, Carlos; Kinnibrugh, Tiffany L.; Xu, Hongwu; ...

2015-04-02

The solvothermal synthesis of framework isomers was carried out using the hybrid carboxylate and tetrazolate functional ligand, 4-tetrazolyl benzenecarboxylic acid (H₂TBC, TBC = 4-tetrazolyl benzenecarboxylate) and zinc. H₂TBC was also synthesized with the solvothermal approach, and is referred herein as structure 1. Using single-crystal X-ray diffraction, we found that the tetrazolate groups of TBC show an unusual “opposite-on” coordination mode with zinc. Three previously characterized metal-organic frameworks (MOFs) were obtained by systematically changing the solvents of the H₂TBC-Zn reaction, (1) ZnTBC, 2, which has a non-porous structure; (2) Zn₂(TBC)₂(H2O), 3, which has an amphiphilic pore structure and (3) Zn₂(TBC)₂{guest}, 4,more » which is porous and has channels containing uncoordinated N heteroatoms. Fluorescence spectra of 4 reveal a strong blue emission mainly from the TBC ligands.« less

Swift tuning from spherical molybdenum microspheres to hierarchical molybdenum disulfide nanostructures by switching from solvothermal to hydrothermal synthesis route

NASA Astrophysics Data System (ADS)

Qureshi, Nilam; Arbuj, Sudhir; Shinde, Manish; Rane, Sunit; Kulkarni, Milind; Amalnerkar, Dinesh; Lee, Haiwon

2017-09-01

Herein, we report the synthesis of metallic molybdenum microspheres and hierarchical MoS2 nanostructures by facile template-free solvothermal and hydrothermal approach, respectively. The morphological transition of the Mo microspheres to hierarchical MoS2 nanoflower architectures is observed to be accomplished with change in solvent from ethylenediamine to water. The resultant marigold flower-like MoS2 nanostructures are few layers thick with poor crystallinity while spherical ball-like molybdenum microspheres exhibit better crystalline nature. This is the first report pertaining to the synthesis of Mo microspheres and MoS2 nanoflowers without using any surfactant, template or substrate in hydro/solvothermal regime. It is opined that such nanoarchitectures of MoS2 are useful candidates for energy related applications such as hydrogen evolution reaction, Li ion battery and pseudocapacitors. Inquisitively, metallic Mo can potentially act as catalyst as well as fairly economical Surface Enhanced Raman Spectroscopy (SERS) substrate in biosensor applications.

Solvothermal indium fluoride chemistry: Syntheses and crystal structures of K{sub 5}In{sub 3}F{sub 14}, beta-(NH{sub 4}){sub 3}InF{sub 6} and [NH{sub 4}]{sub 3}[C{sub 6}H{sub 21}N{sub 4}]{sub 2}[In{sub 4}F{sub 21}

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

Jayasundera, Anil C.A.; Goff, Richard J.; Li Yang

2010-02-15

The solvothermal syntheses and crystal structures of three indium fluorides are presented. K{sub 5}In{sub 3}F{sub 14} (1) and beta-(NH{sub 4}){sub 3}InF{sub 6} (2) are variants on known inorganic structure types chiolite and cryolite, respectively, with the latter exhibiting a complex and apparently novel structural distortion. [NH{sub 4}]{sub 3}[C{sub 6}H{sub 21}N{sub 4}]{sub 2}[In{sub 4}F{sub 21}] (3) represents a new hybrid composition displaying a unique trimeric metal fluoride building unit. - Graphical abstract: Solvothermal synthesis has been used to prepare three indium fluorides, including a novel hybrid material containing a unique [In{sub 3}F{sub 15}] trimer templated by tren.

Solvo-thermal in situ transesterification of wet spent coffee grounds for the production of biodiesel.

PubMed

Park, Jeongseok; Kim, Bora; Son, Jeesung; Lee, Jae W

2018-02-01

This work addresses non-catalytic biodiesel production from spent coffee ground (SCG) by integrating solvo-thermal effect of 1,2-dichloroethane (DCE) with in situ transesterification over 160 °C. The SCG water content has a positive effect on the DCE hydrolysis up to 60 wt% due to the bimolecular substitution mechanism. The hydrolysis gives an acidic environment favorable for cellulose decomposition, SCG particle size reduction and lipid conversion. The optimal fatty acid ethyl ester yield was 11.8 wt% based on the mass of dried SCG with 3.36 ml ethanol and 3.16 ml DCE at 196.8 °C through the response surface methodology. Using the solvo-thermal effect, direct utilization of wet SCG as a biodiesel feedstock provides not only economic feasibility without using drying process and additional acid catalyst but also environmental advantage of recycling the municipal waste. Copyright © 2017 Elsevier Ltd. All rights reserved.

High efficient photocatalytic selective oxidation of benzyl alcohol to benzaldehyde by solvothermal-synthesized ZnIn2S4 microspheres under visible light irradiation

NASA Astrophysics Data System (ADS)

Chen, Zhixin; Xu, Jingjing; Ren, Zhuyun; He, Yunhui; Xiao, Guangcan

2013-09-01

Hexagonal ZnIn2S4 samples have been synthesized by a solvothermal method. Their properties have been determined by X-ray diffraction, ultraviolet-visible-light diffuse reflectance spectra, field emission scanning electron microscopy, nitrogen adsorption-desorption and X-ray photoelectron spectra. These results demonstrate that ethanol solvent has significant influence on the morphology, optical and electronic nature for such marigold-like ZnIn2S4 microspheres. The visible light photocatalytic activities of the ZnIn2S4 have been evaluated by selective oxidation of benzyl alcohol to benzaldehyde using molecular oxygen as oxidant. The results show that 100% conversion along with >99% selectivity are reached over ZnIn2S4 prepared in ethanol solvent under visible light irradiation (λ>420 nm) of 2 h, but only 58% conversion and 57% yield are reached over ZnIn2S4 prepared in aqueous solvent. A possible mechanism of the high photocatalytic activity for selective oxidation of benzyl alcohol over ZnIn2S4 is proposed and discussed.

Solvothermal Synthesis of Hierarchical TiO2 Microstructures with High Crystallinity and Superior Light Scattering for High-Performance Dye-Sensitized Solar Cells.

PubMed

Li, Zhao-Qian; Mo, Li-E; Chen, Wang-Chao; Shi, Xiao-Qiang; Wang, Ning; Hu, Lin-Hua; Hayat, Tasawar; Alsaedi, Ahmed; Dai, Song-Yuan

2017-09-20

In this article, hierarchical TiO 2 microstructures (HM-TiO 2 ) were synthesized by a simple solvothermal method adopting tetra-n-butyl titanate as the titanium source in a mixed solvent composed of N,N-dimethylformamide and acetic acid. Due to the high crystallinity and superior light-scattering ability, the resultant HM-TiO 2 are advantageous as photoanodes for dye-sensitized solar cells. When assembled to the entire photovoltaic device with C101 dye as a sensitizer, the pure HM-TiO 2 -based solar cells showed an ultrahigh photovoltage up to 0.853 V. Finally, by employing the as-obtained HM-TiO 2 as the scattering layer and optimizing the architecture of dye-sensitized solar cells, both higher photovoltage and incident photon-to-electron conversion efficiency value were harvested with respect to TiO 2 nanoparticles-based dye-sensitized solar cells, resulting in a high power conversion efficiency of 9.79%. This work provides a promising strategy to develop photoanode materials with outstanding photoelectric conversion performance.

Solvothermal synthesis of P25/Bi2WO6 nanocomposite photocatalyst and photocatalytic degradation of ethylene under visible light

NASA Astrophysics Data System (ADS)

Song, Xianliang; Wang, Haidan; Li, Yingying; Ye, Shengying; Dionysiou, Dionysios D.

2018-05-01

P25/Bi2WO6 nanocomposite photocatalysts were synthesized by solvothermal method, and their photocatalytic activities were evaluated for the degradation of ethylene under visible light irradiation. The results show that P25/Bi2WO6 nanocomposites have higher photocatalytic activity than P25 and pure Bi2WO6. When the loading amount of P25 is 35%, the photocatalytic degradation of ethylene under visible light is the highest, which is 4.5 and 2.2 times higher than that of P25 and Bi2WO6, respectively. The improvement of the photocatalytic activity of the nanocomposite is mainly due to the formation of the staggered heterojunctions in the contact interface of P25 and Bi2WO6. This can refine the grain and produce lattice defects in the interface of the composite, which could provide more active sites. Therefore, the separation efficiency of the photogenerated electron-hole pair is improved, and the spectral response range is extended to the visible light region, thereby the absorption and utilization of light energy is improved.

Solvothermal Synthesis of Hierarchical Colloidal Nanocrystal Assemblies of ZnFe₂O₄ and Their Application in Water Treatment.

PubMed

Guo, Peizhi; Lv, Meng; Han, Guangting; Wen, Changna; Wang, Qianbin; Li, Hongliang; Zhao, Xiusong

2016-09-29

Hierarchical colloidal nanocrystal assemblies (CNAs) of ZnFe₂O₄ have been synthesized controllably by a solvothermal method. Hollow ZnFe₂O₄ spheres can be formed with the volume ratios of ethylene glycol to ethanol of 1:4 in the starting systems, while solid ZnFe₂O₄ CNAs are obtained by adjusting the volume proportion of ethylene glycol to ethanol from 1:2 to 2:1. Magnetometric measurement data showed that the ZnFe₂O₄ CNAs obtained with the volume ratios of 1:2 and 1:1 exhibited weak ferromagnetic behavior with high saturation magnetization values of 60.4 and 60.3 emu·g -1 , respectively. However, hollow spheres showed a saturation magnetization value of 52.0 emu·g -1 , but the highest coercivity among all the samples. It was found that hollow spheres displayed the best ability to adsorb Congo red dye among all the CNAs. The formation mechanisms of ZnFe₂O₄ CNAs, as well as the relationship between their structure, crystallite size, and properties were discussed based on the experimental results.

Efficient Perovskite Solar Cells Depending on TiO2 Nanorod Arrays.

PubMed

Li, Xin; Dai, Si-Min; Zhu, Pei; Deng, Lin-Long; Xie, Su-Yuan; Cui, Qian; Chen, Hong; Wang, Ning; Lin, Hong

2016-08-24

Perovskite solar cells (PSCs) with TiO2 materials have attracted much attention due to their high photovoltaic performance. Aligned TiO2 nanorods have long been used for potential application in highly efficient perovskite solar cells, but the previously reported efficiencies of perovskite solar cells based on TiO2 nanorod arrays were underrated. Here we show a solvothermal method based on a modified ketone-HCl system with the addition of organic acids suitable for modulation of the TiO2 nanorod array films to fabricate highly efficient perovskite solar cells. Photovoltaic measurements indicated that efficient nanorod-structured perovskite solar cells can be achieved with the length of the nanorods as long as approximately 200 nm. A record efficiency of 18.22% under the reverse scan direction has been optimized by avoiding direct contact between the TiO2 nanorods and the hole transport materials, eliminating the organic residues on the nanorod surfaces using UV-ozone treatment and tuning the nanorod array morphologies through addition of different organic acids in the solvothermal process.

A novel ethanol gas sensor-ZnS/ cyclohexylamine hybrid nanowires.

PubMed

Xu, Lin; Song, Hongwei; Zhang, Tong; Fan, Huitao; Fan, Libo; Wang, Yu; Dong, Biao; Bai, Xue

2011-03-01

We fabricated a novel ethanol gas sensor based on organic-inorganic ZnS/cyclohexylamine (CHA) nanowires via a solvothermal route. The sensor exhibited significantly better performance with response time of approximately 0.6 s and recovery time of approximately 10 s even under a low ethanol concentration and the high surface area, small nanofiber diameter, and hybrid nature made the ZnS/CHA nanowire gas sensor have high sensitivity to ethanol gas at a lower operating current of 160 mA. Moreover, the gas sensing mechanism was proposed on the basis of the two simultaneous steps to explain the adsorbing process due to the hybrid nature. This work indicates that the ZnS/CHA hybrid can be a novel candidate for the ethanol gas sensor with high performance.

Enhanced adsorptive removal of p-nitrophenol from water by aluminum metal–organic framework/reduced graphene oxide composite

PubMed Central

Wu, Zhibin; Yuan, Xingzhong; Zhong, Hua; Wang, Hou; Zeng, Guangming; Chen, Xiaohong; Wang, Hui; zhang, Lei; Shao, Jianguang

2016-01-01

In this study, the composite of aluminum metal–organic framework MIL-68(Al) and reduced graphene oxide (MA/RG) was synthesized via a one–step solvothermal method, and their performances for p–nitrophenol (PNP) adsorption from aqueous solution were systematically investigated. The introduction of reduced graphene oxide (RG) into MIL-68(Al) (MA) significantly changes the morphologies of the MA and increases the surface area. The MA/RG-15% prepared at RG-to-MA mass ratio of 15% shows a PNP uptake rate 64% and 123% higher than MIL-68(Al) and reduced graphene oxide (RG), respectively. The hydrogen bond and π – π dispersion were considered to be the major driving force for the spontaneous and endothermic adsorption process for PNP removal. The adsorption kinetics, which was controlled by film–diffusion and intra–particle diffusion, was greatly influenced by solution pH, ionic strength, temperature and initial PNP concentration. The adsorption kinetics and isotherms can be well delineated using pseudo–second–order and Langmuir equations, respectively. The presence of phenol or isomeric nitrophenols in the solution had minimal influence on PNP adsorption by reusable MA/RG composite. PMID:27181188

Efficient solvothermal wet in situ transesterification of Nannochloropsis gaditana for biodiesel production.

PubMed

Kim, Bora; Chang, Yong Keun; Lee, Jae W

2017-05-01

In situ transesterification of wet microalgae is a promising, simplified alternative biodiesel production process that replaces multiple operations of cell drying, extraction, and transesterification reaction. This study addresses enhanced biodiesel production from Nannochloropsis gaditana at elevated temperatures. Compared with the previously reported in situ transesterification process of conducting the reaction at a temperature ranging from 95 to 125 °C, the present work employs higher temperatures of at least 150 °C. This relatively harsh condition allows much less acid catalyst with or without co-solvent to be used during this single extraction-conversion process. Without any co-solvent, 0.58% (v/v) of H 2 SO 4 in the reaction medium can achieve 90 wt% of the total lipid conversion to biodiesel at 170 °C when the moisture content of wet algal paste is 80 wt%. Here, the effects of temperature, acid catalyst, and co-solvent on the FAEE yield and specification were scrutinized, and the reaction kinetic was investigated to understand the solvothermal in situ transesterification reaction at the high temperature. Having a biphasic system (water/chloroform) during the reaction also helped to meet biodiesel quality standard EN 14214, as Na + , K + , Ca 2+ , Mg 2+ cations and phosphorus were detected only below 5 ppm. With highlights on the economic feasibility, wet in situ transesterification at the high temperature can contribute to sustainable production of biodiesel from microalgae by reducing the chemical input and relieve the burden of extensive post purification process, therefore a step towards green process.

Engineering of Metal Oxide Nanoparticles for Application in Electrochemical Devices

NASA Astrophysics Data System (ADS)

Santos, Lidia Sofia Leitao

The growing demand for materials and devices with new functionalities led to the increased interest in the field of nanomaterials and nanotechnologies. Nanoparticles, not only present a reduced size as well as high reactivity, which allows the development of electronic and electrochemical devices with exclusive properties, when compared with thin films. This dissertation aims to explore the development of several nanostructured metal oxides by solvothermal synthesis and its application in different electrochemical devices. Within this broad theme, this study has a specific number of objectives: a) research of the influence of the synthesis parameters to the structure and morphology of the nanoparticles; b) improvement of the performance of the electrochromic devices with the application of the nanoparticles as electrode; c) application of the nanoparticles as probes to sensing devices; and d) production of solution-pro-cessed transistors with a nanostructured metal oxide semiconductor. Regarding the results, several conclusions can be exposed. Solvothermal synthesis shows to be a very versatile method to control the growth and morphology of the nanoparticles. The electrochromic device performance is influenced by the different structures and morphologies of WO3 nanoparticles, mainly due to the surface area and conductivity of the materials. The deposition of the electrochromic layer by inkjet printing allows the patterning of the electrodes without wasting material and without any additional steps. Nanostructured WO3 probes were produced by electrodeposition and drop casting and applied as pH sensor and biosensor, respectively. The good performance and sensitivity of the devices is explained by the high number of electrochemical reactions occurring at the surface of the na-noparticles. GIZO nanoparticles were deposited by spin coating and used in electrolyte-gated transistors, which promotes a good interface between the semiconductor and the dielectric. The produced transistors work at low potential and with improved ON-OFF current ratio, up to 6 orders of mag-nitude. To summarize, the low temperatures used in the production of the devices are compatible with flexible substrates and additionally, the low cost of the techniques involved can be adapted for disposable devices.

The effect of adopting the IADPSG screening guidelines on the risk profile and outcomes of the gestational diabetes population.

PubMed

March, Melissa I; Modest, Anna M; Ralston, Steven J; Hacker, Michele R; Gupta, Munish; Brown, Florence M

2016-01-01

To compare characteristics and outcomes of women diagnosed with gestational diabetes mellitus (GDM) by the newer one-step glucose tolerance test and those diagnosed with the traditional two-step method. This was a retrospective cohort study of women with GDM who delivered in 2010-2011. Data are reported as proportion or median (interquartile range) and were compared using a Chi-square, Fisher's exact or Wilcoxon rank sum test based on data type. Of 235 women with GDM, 55.7% were diagnosed using the two-step method and 44.3% with the one-step method. The groups had similar demographics and GDM risk factors. The two-step method group was diagnosed with GDM one week later [27.0 (24.0-29.0) weeks versus 26.0 (24.0-28.0 weeks); p = 0.13]. The groups had similar median weight gain per week before diagnosis. After diagnosis, women in the one-step method group had significantly higher median weight gain per week [0.67 pounds/week (0.31-1.0) versus 0.56 pounds/week (0.15-0.89); p = 0.047]. In the one-step method group more women had suspected macrosomia (11.7% versus 5.3%, p = 0.07) and more neonates had a birth weight >4000 g (13.6% versus 7.5%, p = 0.13); however, these differences were not statistically significant. Other pregnancy and neonatal complications were similar. Women diagnosed with the one-step method gained more weight per week after GDM diagnosis and had a non-statistically significant increased risk for suspected macrosomia. Our data suggest the one-step method identifies women with at least equally high risk as the two-step method.

Cobalt-based metal organic framework with superior lithium anodic performance

NASA Astrophysics Data System (ADS)

Hu, Xiaoshi; Hu, Huiping; Li, Chao; Li, Tian; Lou, Xiaobing; Chen, Qun; Hu, Bingwen

2016-10-01

The reversible charging of a Co-1,4-benzenedicarboxylate MOF (Co-BDC MOF) prepared via an one-pot solvothermal method was studied for use as the anode in a Li-ion cell. It was found that this MOF anode provides high reversible capacities (1090 and 611 mA h g-1 at current densities of 0.2 and 1 A g-1, respectively), and an impressive rate performance. Such an outstanding Li-ion storage property has not been reported previously for the LIB anodes within the MOFs category. Ex-situ X-ray photoelectron spectroscopy (XPS) and infrared spectroscopy (IR) studies of this material at different state of charge suggest that cobalt stays at Co2+ state during discharge/charge process, so that in this case Li+ may be inserted into the organic moiety without the direct participation of cobalt ions.

Vanadium based materials as electrode materials for high performance supercapacitors

NASA Astrophysics Data System (ADS)

Yan, Yan; Li, Bing; Guo, Wei; Pang, Huan; Xue, Huaiguo

2016-10-01

As a kind of supercapacitors, pseudocapacitors have attracted wide attention in recent years. The capacitance of the electrochemical capacitors based on pseudocapacitance arises mainly from redox reactions between electrolytes and active materials. These materials usually have several oxidation states for oxidation and reduction. Many research teams have focused on the development of an alternative material for electrochemical capacitors. Many transition metal oxides have been shown to be suitable as electrode materials of electrochemical capacitors. Among them, vanadium based materials are being developed for this purpose. Vanadium based materials are known as one of the best active materials for high power/energy density electrochemical capacitors due to its outstanding specific capacitance and long cycle life, high conductivity and good electrochemical reversibility. There are different kinds of synthetic methods such as sol-gel hydrothermal/solvothermal method, template method, electrospinning method, atomic layer deposition, and electrodeposition method that have been successfully applied to prepare vanadium based electrode materials. In our review, we give an overall summary and evaluation of the recent progress in the research of vanadium based materials for electrochemical capacitors that include synthesis methods, the electrochemical performances of the electrode materials and the devices.

Large low-field magnetoresistance in Fe3O4/molecule nanoparticles at room temperature

NASA Astrophysics Data System (ADS)

Yue, F. J.; Wang, S.; Lin, L.; Zhang, F. M.; Li, C. H.; Zuo, J. L.; Du, Y. W.; Wu, D.

2011-01-01

Acetic acid molecule-coated Fe3O4 nanoparticles, 450-650 nm in size, have been synthesized using a chemical solvothermal reduction method. Fourier transform infrared spectroscopy measurements confirm one monolayer acetic acid molecules chemically bond to the Fe3O4 nanoparticles. The low-field magnetoresistance (LFMR) of more than -10% at room temperature and -23% at 140 K is achieved with saturation field of less than 2 kOe. In comparison, the resistivity of cold-pressed bare Fe3O4 nanoparticles is six orders of magnitudes smaller than that of Fe3O4/molecule nanoparticles, and the LFMR ratio is one order of magnitude smaller. Our results indicate that the large LFMR in Fe3O4/molecule nanoparticles is associated with spin-polarized electrons tunnelling through molecules instead of direct nanoparticle contacts. These results suggest that magnetic oxide-molecule hybrid materials are an alternative type of materials to develop spin-based devices by a simple low-cost approach.

Highly intensified upconversion luminescence of Ca(2+) -doped Yb/Er:NaGdF(4) nanocrystals prepared by a solvothermal route.

PubMed

Lei, Lei; Chen, Daqin; Xu, Ju; Zhang, Rui; Wang, Yuansheng

2014-03-01

Upon introducing Ca(2+) dopants into the grain lattices by substituting Gd(3+) ions, irregular Yb/Er:NaGdF4 nanocrystals prepared through a simple solvothermal route convert into highly uniform nanorods. Meanwhile, their upconversion luminescence intensifies by about 200 times, probably due to a modification of the crystal structure of NaGdF4 and an improvement in the crystallinity of the nanophase. Copyright © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Solvothermally Synthesized Sb2Te3 Platelets Show Unexpected Optical Contrasts in Mid-Infrared Near-Field Scanning Microscopy.

PubMed

Hauer, Benedikt; Saltzmann, Tobias; Simon, Ulrich; Taubner, Thomas

2015-05-13

We report nanoscale-resolved optical investigations on the local material properties of Sb2Te3 hexagonal platelets grown by solvothermal synthesis. Using mid-infrared near-field microscopy, we find a highly symmetric pattern, which is correlated to a growth spiral and which extends over the entire platelet. As the origin of the optical contrast, we identify domains with different densities of charge carriers. On Sb2Te3 samples grown by other means, we did not find a comparable domain structure.

Solvothermal synthesis of fusiform hexagonal prism SrCO{sub 3} microrods via ethylene glycol solution

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

Shi Liange; Du Fanglin

2007-08-07

Fusiform hexagonal prism SrCO{sub 3} microrods were prepared by a simple solvothermal route at 120 deg. C, and characterized by X-ray powder diffraction (XRD), field-emission scanning electron microscopy (FE-SEM) and Fourier transform infrared (FT-IR) spectroscopy. By controlling the content of ethylene glycol (EG), it was found that ethylene glycol (EG) played an important role in the formation of such SrCO{sub 3} microrods. Finally, effects of other solvents on the products, including 1,2-propanediol and glycerin, were also investigated.

A Lyapunov and Sacker–Sell spectral stability theory for one-step methods

DOE PAGES

Steyer, Andrew J.; Van Vleck, Erik S.

2018-04-13

Approximation theory for Lyapunov and Sacker–Sell spectra based upon QR techniques is used to analyze the stability of a one-step method solving a time-dependent (nonautonomous) linear ordinary differential equation (ODE) initial value problem in terms of the local error. Integral separation is used to characterize the conditioning of stability spectra calculations. The stability of the numerical solution by a one-step method of a nonautonomous linear ODE using real-valued, scalar, nonautonomous linear test equations is justified. This analysis is used to approximate exponential growth/decay rates on finite and infinite time intervals and establish global error bounds for one-step methods approximating uniformly,more » exponentially stable trajectories of nonautonomous and nonlinear ODEs. A time-dependent stiffness indicator and a one-step method that switches between explicit and implicit Runge–Kutta methods based upon time-dependent stiffness are developed based upon the theoretical results.« less

A Lyapunov and Sacker–Sell spectral stability theory for one-step methods

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

Steyer, Andrew J.; Van Vleck, Erik S.

Approximation theory for Lyapunov and Sacker–Sell spectra based upon QR techniques is used to analyze the stability of a one-step method solving a time-dependent (nonautonomous) linear ordinary differential equation (ODE) initial value problem in terms of the local error. Integral separation is used to characterize the conditioning of stability spectra calculations. The stability of the numerical solution by a one-step method of a nonautonomous linear ODE using real-valued, scalar, nonautonomous linear test equations is justified. This analysis is used to approximate exponential growth/decay rates on finite and infinite time intervals and establish global error bounds for one-step methods approximating uniformly,more » exponentially stable trajectories of nonautonomous and nonlinear ODEs. A time-dependent stiffness indicator and a one-step method that switches between explicit and implicit Runge–Kutta methods based upon time-dependent stiffness are developed based upon the theoretical results.« less

The effect of adopting the IADPSG screening guidelines on the risk profile and outcomes of the gestational diabetes population

PubMed Central

March, Melissa I.; Modest, Anna M.; Ralston, Steven J.; Hacker, Michele R.; Gupta, Munish; Brown, Florence M.

2016-01-01

Abstract Objective: To compare characteristics and outcomes of women diagnosed with gestational diabetes mellitus (GDM) by the newer one-step glucose tolerance test and those diagnosed with the traditional two-step method. Research design and methods: This was a retrospective cohort study of women with GDM who delivered in 2010–2011. Data are reported as proportion or median (interquartile range) and were compared using a Chi-square, Fisher's exact or Wilcoxon rank sum test based on data type. Results: Of 235 women with GDM, 55.7% were diagnosed using the two-step method and 44.3% with the one-step method. The groups had similar demographics and GDM risk factors. The two-step method group was diagnosed with GDM one week later [27.0 (24.0–29.0) weeks versus 26.0 (24.0–28.0 weeks); p = 0.13]. The groups had similar median weight gain per week before diagnosis. After diagnosis, women in the one-step method group had significantly higher median weight gain per week [0.67 pounds/week (0.31–1.0) versus 0.56 pounds/week (0.15–0.89); p = 0.047]. In the one-step method group more women had suspected macrosomia (11.7% versus 5.3%, p = 0.07) and more neonates had a birth weight >4000 g (13.6% versus 7.5%, p = 0.13); however, these differences were not statistically significant. Other pregnancy and neonatal complications were similar. Conclusions: Women diagnosed with the one-step method gained more weight per week after GDM diagnosis and had a non-statistically significant increased risk for suspected macrosomia. Our data suggest the one-step method identifies women with at least equally high risk as the two-step method. PMID:25958989

Solvothermal Synthesis of Three-Dimensional Hierarchical CuS Microspheres from a Cu-Based Ionic Liquid Precursor for High-Performance Asymmetric Supercapacitors.

PubMed

Zhang, Jing; Feng, Huijie; Yang, Jiaqin; Qin, Qing; Fan, Hongmin; Wei, Caiying; Zheng, Wenjun

2015-10-07

It is meaningful to exploit copper sulfide materials with desired structure as well as potential application due to their cheapness and low toxicity. A low-temperature and facile solvothermal method for preparing three-dimensional (3D) hierarchical covellite (CuS) microspheres from an ionic liquid precursor [Bmim]2Cu2Cl6 (Bmim = 1-butyl-3-methylimidazolium) is reported. The formation of CuS nanostructures was achieved by decomposition of intermediate complex Cu(Tu)3Cl (thiourea = Tu), which produced CuS microspheres with diameters of 2.5-4 μm assembled by nanosheets with thicknesses of 10-15 nm. The ionic liquid, as an "all-in-one" medium, played a key role for the fabrication and self-assembly of CuS nanosheets. The alkylimidazolium rings ([Bmim](+)) were found to adsorb onto the (001) facets of CuS crystals, which inhibited the crystal growth along the [001] direction, while the alkyl chain had influence on the assembly of CuS nanosheets. The CuS microspheres showed enhanced electrochemical performance and high stability for the application in supercapacitors due to intriguing structural design and large specific surface area. When this well-defined CuS electrode was assembled into an asymmetric supercapacitor (ASC) with an activated carbon (AC) electrode, the CuS//AC-ASC demonstrated good cycle performance (∼88% capacitance after 4000 cycles) and high energy density (15.06 W h kg(-1) at a power density of 392.9 W kg(-1)). This work provides new insights into the use of copper sulfide electrode materials for asymmetric supercapacitors and other electrochemical devices.

Solvent-Controlled Synthesis of Highly Luminescent Carbon Dots with a Wide Color Gamut and Narrowed Emission Peak Widths.

PubMed

Ding, Hui; Wei, Ji-Shi; Zhang, Peng; Zhou, Zi-Yuan; Gao, Qing-Yu; Xiong, Huan-Ming

2018-05-01

Carbon dots (CDs) have tremendous potential applications in bioimaging, biomedicine, and optoelectronics. By far, it is still difficult to produce photoluminescence (PL) tunable CDs with high quantum yield (QY) across the entire visible spectrum and narrow the emission peak widths of CDs close to those of typical quantum dots. In this work, a series of CDs with tunable emission from 443 to 745 nm, quantum yield within 13-54%, and narrowed full width at half maximum (FWHM) from 108 to 55 nm, are obtained by only adjusting the reaction solvents in a one-pot solvothermal route. The distinct optical features of these CDs are based on their differences in the particle size, and the content of graphitic nitrogen and oxygen-containing functional groups, which can be modulated by controlling the dehydration and carbonization processes during solvothermal reactions. Blue, green, yellow, red, and even pure white light emitting films (Commission Internationale de L'Eclairage (CIE)= 0.33, 0.33, QY = 39%) are prepared by dispersing one or three kinds of CDs into polyvinyl alcohol with appropriate ratios. The near-infrared emissive CDs are excellent fluorescent probes for both in vitro and in vivo bioimaging because of their high QY in water, long-term stability, and low cytotoxicity. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Review on the progress in synthesis and application of magnetic carbon nanocomposites.

PubMed

Zhu, Maiyong; Diao, Guowang

2011-07-01

This review focuses on the synthesis and application of nanostructured composites containing magnetic nanostructures and carbon-based materials. Great progress in fabrication of magnetic carbon nanocomposites has been made by developing methods including filling process, template-based synthesis, chemical vapor deposition, hydrothermal/solvothermal method, pyrolysis procedure, sol-gel process, detonation induced reaction, self-assembly method, etc. The applications of magnetic carbon nanocomposites expanded to a wide range of fields such as environmental treatment, microwave absorption, magnetic recording media, electrochemical sensor, catalysis, separation/recognization of biomolecules and drug delivery are discussed. Finally, some future trends and perspectives in this research area are outlined.

Review on the progress in synthesis and application of magnetic carbon nanocomposites

NASA Astrophysics Data System (ADS)

Zhu, Maiyong; Diao, Guowang

2011-07-01

This review focuses on the synthesis and application of nanostructured composites containing magnetic nanostructures and carbon-based materials. Great progress in fabrication of magnetic carbon nanocomposites has been made by developing methods including filling process, template-based synthesis, chemical vapor deposition, hydrothermal/solvothermal method, pyrolysis procedure, sol-gel process, detonation induced reaction, self-assembly method, etc. The applications of magnetic carbon nanocomposites expanded to a wide range of fields such as environmental treatment, microwave absorption, magnetic recording media, electrochemical sensor, catalysis, separation/recognization of biomolecules and drug delivery are discussed. Finally, some future trends and perspectives in this research area are outlined.

Ratiometric near infrared luminescent thermometer based on lanthanide metal-organic frameworks

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

Yue, Dan; Zhang, Jun; Zhao, Dian

2016-09-15

A near infrared luminescent MOFs thermometer (Nd{sub 0.676}Yb{sub 0.324}BTC) was prepared via a simple solvothermal method using Ln{sup 3+} (Ln=Nd, Yb) ions and 1, 3, 5-benznenetricarboxylic acid (H{sub 3}BTC), and characterized by PXRD, TGA, ICP, and photoluminescence (PL) spectrum. These results indicate that the Nd{sub 0.676}Yb{sub 0.324}BTC displays high relative sensitivity and excellent repeatability in the physiological temperature range (288–323 K), and the maximum relative sensitivity is determined to be 1.187% K{sup −1} at 323 K. These NIR luminescent MOFs may have potential applications in physiological temperature sensing. - Graphical abstract: A near infrared luminescent MOFs thermometer (Nd{sub 0.054}Yb{sub 0.946}BTCmore » ) displays high relative sensitivity and excellent repeatability in the physiological temperature range (288–323 K). Display Omitted - Highlights: • A ratiometric near infrared luminescent MOFs thermometer (Nd{sub 0.676}Yb{sub 0.324}BTC) was prepared via a simple solvothermal method. • The maximum relative sensitivity of Nd{sub 0.676}Yb{sub 0.324}BTC is determined to be 1.187% K{sup −1} at 323 K. • Nd{sub 0.676}Yb{sub 0.324}BTC showed excellent repeatability in the physiological temperature range (288–323 K).« less

Mg doped Li2FeSiO4/C nanocomposites synthesized by the solvothermal method for lithium ion batteries.

PubMed

Kumar, Ajay; Jayakumar, O D; Jagannath; Bashiri, Parisa; Nazri, G A; Naik, Vaman M; Naik, Ratna

2017-10-14

A series of porous Li 2 Fe 1-x Mg x SiO 4 /C (x = 0, 0.01, 0.02, 0.04) nanocomposites (LFS/C, 1Mg-LFS/C, 2Mg-LFS and 4Mg-LFS/C) have been synthesized via a solvo-thermal method using the Pluronic P123 polymer as an in situ carbon source. Rietveld refinement of the X-ray diffraction data of Li 2 Fe 1-x Mg x SiO 4 /C composites confirms the formation of the monoclinic P2 1 structure of Li 2 FeSiO 4 . The addition of Mg facilitates the growth of impurity-free Li 2 FeSiO 4 with increased crystallinity and particle size. Despite having the same percentage of carbon content (∼15 wt%) in all the samples, the 1Mg-LFS/C nanocomposite delivered the highest initial discharge capacity of 278 mA h g -1 (∼84% of the theoretical capacity) at the C/30 rate and also exhibited the best rate capability and cycle stability (94% retention after 100 charge-discharge cycles at 1C). This is attributed to its large surface area with a narrow pore size distribution and a lower charge transfer resistance with enhanced Li-ion diffusion coefficient compared to other nanocomposites.

Hierarchical structures of ZnO spherical particles synthesized solvothermally

NASA Astrophysics Data System (ADS)

Saito, Noriko; Haneda, Hajime

2011-12-01

We review the solvothermal synthesis, using a mixture of ethylene glycol (EG) and water as the solvent, of zinc oxide (ZnO) particles having spherical and flower-like shapes and hierarchical nanostructures. The preparation conditions of the ZnO particles and the microscopic characterization of the morphology are summarized. We found the following three effects of the ratio of EG to water on the formation of hierarchical structures: (i) EG restricts the growth of ZnO microcrystals, (ii) EG promotes the self-assembly of small crystallites into spheroidal particles and (iii) the high water content of EG results in hollow spheres.

Anomalous magnetic behavior in nanocomposite materials of reduced graphene oxide-Ni/NiFe{sub 2}O{sub 4}

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

Kollu, Pratap, E-mail: pk419@cam.ac.uk, E-mail: anirmalagrace@vit.ac.in, E-mail: dhirenb@iitb.ac.in; Prathapani, Sateesh; Varaprasadarao, Eswara K.

2014-08-04

Magnetic Reduced Graphene Oxide-Nickel/NiFe{sub 2}O{sub 4} (RGO-Ni/NF) nanocomposite has been synthesized by one pot solvothermal method. Respective phase formations and their purities in the composite are confirmed by High Resolution Transmission Electron Microscope and X Ray Diffraction, respectively. For the RGO-Ni/NF composite material finite-size effects lead to the anomalous magnetic behavior, which is corroborated in temperature and field dependent magnetization curves. Here, we are reporting the behavior of higher magnetization values for Zero Field Cooled condition to that of Field Cooled for the RGO-Ni/NF nanocomposite. Also, the observed negative and positive moments in Hysteresis loops at relatively smaller applied fieldsmore » (100 Oe and 200 Oe) are explained on the basis of surface spin disorder.« less

Enhanced Air Stability in REPb3 (RE = Rare Earths) by Dimensional Reduction Mediated Valence Transition.

PubMed

Subbarao, Udumula; Sarkar, Sumanta; Jana, Rajkumar; Bera, Sourav S; Peter, Sebastian C

2016-06-06

We conceptually selected the compounds REPb3 (RE = Eu, Yb), which are unstable in air, and converted them to the stable materials in ambient conditions by the chemical processes of "nanoparticle formation" and "dimensional reduction". The nanoparticles and the bulk counterparts were synthesized by the solvothermal and high-frequency induction furnace heating methods, respectively. The reduction of the particle size led to the valence transition of the rare earth atom, which was monitored through magnetic susceptibility and X-ray absorption near edge spectroscopy (XANES) measurements. The stability was checked by X-ray diffraction and thermogravimetric analysis over a period of seven months in oxygen and argon atmospheres and confirmed by XANES. The nanoparticles showed outstanding stability toward aerial oxidation over a period of seven months compared to the bulk counterpart, as the latter one is more prone to the oxidation within a few days.

Ultrasonically assisted solvothermal synthesis of novel Ni/Al layered double hydroxide for capturing of Cd(II) from contaminated water

NASA Astrophysics Data System (ADS)

Rahmanian, Omid; Maleki, Mohammad Hassan; Dinari, Mohammad

2017-11-01

A novel adsorbent of nickel aluminum layered double hydroxide (Ni/Al-LDH) was prepared through the precipitation of metal nitrates by ultrasonically assisted solvothermal method. The surface morphology, chemical structure and thermal properties of this compound were examined by X-ray diffraction (XRD), Fourier Transform Infrared (FT-IR), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), and thermogravimetric analysis (TGA) techniques. The XRD, TEM and FE-SEM results established that the synthesized LDH have a well-ordered layer structure with good crystalline nature. Then it was applied to remove excessive Cd(II) ions from water and the effects of contact time, pH and adsorbent dose were examined at initial Cd(II) concentration of 10 mg/L. Results show that the time required to reach equilibrium was fast (40 min) and working pH solution was neutral (pH 7). Langmuir and Freundlich model of adsorption isotherms were explored; the results show that the Freundlich model was better fitted than that Langmuir model. This results predicting a multilayer adsorption of Cd(II) on LDH. The equilibrium kinetic adsorption data were fixed to the pseudo-second order kinetic equation.

Solvothermal modification of BiOCl nanosheets with Bi nanoparticles using ascorbic acid as reductant and the superoxide radicals dominated photocatalytic performance

NASA Astrophysics Data System (ADS)

Cui, Zhankui; Gao, Keke; Ge, Suxiang; Fa, Wenjun

2017-11-01

BiOCl nanosheets were solvothermally modified with Bi nanoparticles (NPs) using ascorbic acid as the reductant. The structures of Bi/BiOCl composites were characterized by XRD, Raman spectroscopy, FTIR spectroscopy and SEM. The light absorption properties were measured by UV-vis-NIR spectroscopy. The photocatalytic performances were evaluated by photodegrading methyl orange (MO) and the photocatalytic mechanism was investigated using trapping experiments and a fluorescent probe method. The results show that Bi NPs are uniformly distributed on the surfaces of BiOCl nanosheets and the modification amount of Bi NPs could be well controlled because of the mild property of ascorbic acid as reducing agent. The photocatalytic activities for the composites are improved obviously and the best photocatalytic performance is obtained when the weight ratio of Bi and BiOCl is1:10 and the photochemical reaction rate is 3.5 times that of pure BiOCl nanosheets and 19.7 times of Bi powders. The enhanced photocatalytic efficiency is ascribed to the favorable formation of dominant \\cdot O2- radicals caused by the increased photoinduced electrons from both Bi NPs and BiOCl nanosheets.

A novel conversion of the groundwater treatment sludge to magnetic particles for the adsorption of methylene blue.

PubMed

Zhu, Suiyi; Fang, Shuai; Huo, Mingxin; Yu, Yang; Chen, Yu; Yang, Xia; Geng, Zhi; Wang, Yi; Bian, Dejun; Huo, Hongliang

2015-07-15

Iron sludge, produced from filtration and backwash of groundwater treatment plant, has long been considered as a waste for landfill. In this study, iron sludge was reused to synthesize Fe3O4 magnetic particles (MPs) by using a novel solvothermal process. Iron sludge contained abundant amounts of silicon, iron, and aluminum and did not exhibit magnetic properties. After treatment for 4h, the amorphous Fe in iron sludge was transformed into magnetite Fe3O4, which could be easily separated from aqueous solution with a magnet. The prepared particles demonstrated the intrinsic properties of soft magnetic materials and could aggregate into a size of 1 μm. MPs treated for 10h exhibited excellent magnetic properties and a saturation magnetization value of 9 emu/g. The obtained particles presented the optimal adsorption of methylene blue under mild conditions, and the maximum adsorption capacity was 99.4 mg/g, which was higher than that of granular active carbon. The simple solvothermal method can be used to prepare Fe3O4 MPs from iron sludge, and the products could be applied to treatment of dyeing wastewater. Copyright © 2015. Published by Elsevier B.V.

Evaluation of a Rapid One-step Real-time PCR Method as a High-throughput Screening for Quantification of Hepatitis B Virus DNA in a Resource-limited Setting.

PubMed

Rashed-Ul Islam, S M; Jahan, Munira; Tabassum, Shahina

2015-01-01

Virological monitoring is the best predictor for the management of chronic hepatitis B virus (HBV) infections. Consequently, it is important to use the most efficient, rapid and cost-effective testing systems for HBV DNA quantification. The present study compared the performance characteristics of a one-step HBV polymerase chain reaction (PCR) vs the two-step HBV PCR method for quantification of HBV DNA from clinical samples. A total of 100 samples consisting of 85 randomly selected samples from patients with chronic hepatitis B (CHB) and 15 samples from apparently healthy individuals were enrolled in this study. Of the 85 CHB clinical samples tested, HBV DNA was detected from 81% samples by one-step PCR method with median HBV DNA viral load (VL) of 7.50 × 10 3 lU/ml. In contrast, 72% samples were detected by the two-step PCR system with median HBV DNA of 3.71 × 10 3 lU/ml. The one-step method showed strong linear correlation with two-step PCR method (r = 0.89; p < 0.0001). Both methods showed good agreement at Bland-Altman plot, with a mean difference of 0.61 log 10 IU/ml and limits of agreement of -1.82 to 3.03 log 10 IU/ml. The intra-assay and interassay coefficients of variation (CV%) of plasma samples (4-7 log 10 IU/ml) for the one-step PCR method ranged between 0.33 to 0.59 and 0.28 to 0.48 respectively, thus demonstrating a high level of concordance between the two methods. Moreover, elimination of the DNA extraction step in the one-step PCR kit allowed time-efficient and significant labor and cost savings for the quantification of HBV DNA in a resource limited setting. Rashed-Ul Islam SM, Jahan M, Tabassum S. Evaluation of a Rapid One-step Real-time PCR Method as a High-throughput Screening for Quantification of Hepatitis B Virus DNA in a Resource-limited Setting. Euroasian J Hepato-Gastroenterol 2015;5(1):11-15.

Evaluation of a Rapid One-step Real-time PCR Method as a High-throughput Screening for Quantification of Hepatitis B Virus DNA in a Resource-limited Setting

PubMed Central

Jahan, Munira; Tabassum, Shahina

2015-01-01

Virological monitoring is the best predictor for the management of chronic hepatitis B virus (HBV) infections. Consequently, it is important to use the most efficient, rapid and cost-effective testing systems for HBV DNA quantification. The present study compared the performance characteristics of a one-step HBV polymerase chain reaction (PCR) vs the two-step HBV PCR method for quantification of HBV DNA from clinical samples. A total of 100 samples consisting of 85 randomly selected samples from patients with chronic hepatitis B (CHB) and 15 samples from apparently healthy individuals were enrolled in this study. Of the 85 CHB clinical samples tested, HBV DNA was detected from 81% samples by one-step PCR method with median HBV DNA viral load (VL) of 7.50 × 103 lU/ml. In contrast, 72% samples were detected by the two-step PCR system with median HBV DNA of 3.71 × 103 lU/ml. The one-step method showed strong linear correlation with two-step PCR method (r = 0.89; p < 0.0001). Both methods showed good agreement at Bland-Altman plot, with a mean difference of 0.61 log10 IU/ml and limits of agreement of -1.82 to 3.03 log10 IU/ml. The intra-assay and interassay coefficients of variation (CV%) of plasma samples (4-7 log10 IU/ml) for the one-step PCR method ranged between 0.33 to 0.59 and 0.28 to 0.48 respectively, thus demonstrating a high level of concordance between the two methods. Moreover, elimination of the DNA extraction step in the one-step PCR kit allowed time-efficient and significant labor and cost savings for the quantification of HBV DNA in a resource limited setting. How to cite this article Rashed-Ul Islam SM, Jahan M, Tabassum S. Evaluation of a Rapid One-step Real-time PCR Method as a High-throughput Screening for Quantification of Hepatitis B Virus DNA in a Resource-limited Setting. Euroasian J Hepato-Gastroenterol 2015;5(1):11-15. PMID:29201678

One step synthesis of Co/Cr-codoped ZnO nanoparticle with superb adsorption properties for various anionic organic pollutants and its regeneration.

PubMed

Li, Zhenjiang; Sun, Yongkai; Xing, Jing; Xing, Yucheng; Meng, Alan

2018-06-15

Adsorption is an effective means to remove organic pollutant. However, it is challenging to prepare the adsorbents with high adsorption capacities and their regeneration. Herein, Co/Cr-codoped ZnO nanoparticles (NPs) with superb adsorption for dyes and antibiotics have been successfully synthesized by a mild solvothermal method. At the optimal Co:Cr:Zn doping moral ratio of 4:6:100, the maximum adsorption capacities of methyl orange (MO) and tetracycline hydrochloride (TC-HCl) on Co/Cr-codoped ZnO NPs is 1057.90 mg g -1 and 874.46 mg g -1 , respectively. The adsorption process of the sample over MO and TC-HCl both agreed well with the pseudo-second-order kinetic model and Langmuir isotherm model. Adsorption thermodynamics proved that the adsorption of MO and TC-HCl on Co/Cr-codoped ZnO NPs was a spontaneous and endothermic process. The mechanism shows that the surface of Co/Cr-codoped ZnO NPs have more positive charges, larger specific surface area and more crystal defects due to Co 3+ and Cr 3+ substitutes Zn 2+ in ZnO lattice, improving their adsorption property. In addition, Co/Cr-codoped ZnO NPs have also excellent adsorption capacity for Direct Red, Congo Red, Evans Blue and Methyl Blue. More importantly, the regeneration of adsorbents was studied to achieve the reuse of materials, and avoid secondary pollution. Co/Cr-codoped ZnO NPs will be a promising choice for wastewater treatment owing to its excellent adsorption capacity and relatively low cost. Copyright © 2018 Elsevier B.V. All rights reserved.

Zinc Oxide—From Synthesis to Application: A Review

PubMed Central

Kołodziejczak-Radzimska, Agnieszka; Jesionowski, Teofil

2014-01-01

Zinc oxide can be called a multifunctional material thanks to its unique physical and chemical properties. The first part of this paper presents the most important methods of preparation of ZnO divided into metallurgical and chemical methods. The mechanochemical process, controlled precipitation, sol-gel method, solvothermal and hydrothermal method, method using emulsion and microemulsion enviroment and other methods of obtaining zinc oxide were classified as chemical methods. In the next part of this review, the modification methods of ZnO were characterized. The modification with organic (carboxylic acid, silanes) and inroganic (metal oxides) compounds, and polymer matrices were mainly described. Finally, we present possible applications in various branches of industry: rubber, pharmaceutical, cosmetics, textile, electronic and electrotechnology, photocatalysis were introduced. This review provides useful information for specialist dealings with zinc oxide. PMID:28788596

A multifunctional chemical sensor based on a three-dimensional lanthanide metal-organic framework

NASA Astrophysics Data System (ADS)

Du, Pei-Yao; Liao, Sheng-Yun; Gu, Wen; Liu, Xin

2016-12-01

A 3D lanthanide MOF with formula [Sm2(abtc)1.5(H2O)3(DMA)]·H2O·DMA (1) has been successfully synthesized via solvothermal method. Luminescence studies reveal that 1 exhibits dual functional detection benzyl alcohol and benzaldehyde among different aromatic molecules. In addition, 1 displays a turn-on luminescence sensing with respect to ethanol among different alcohol molecules, which suggests that 1 is also a promising luminescent probe for high selective sensing of ethanol.

Synthesis of silver nanowires using hydrothermal technique for flexible transparent electrode application

NASA Astrophysics Data System (ADS)

Vijila, C. V. Mary; Rahman, K. K. Arsina; Parvathy, N. S.; Jayaraj, M. K.

2016-05-01

Transparent conducting films are becoming increasingly interesting because of their applications in electronics industry such as their use in solar energy applications. In this work silver nanowires were synthesized using solvothermal method by reducing silver nitrate and adding sodium chloride for assembling silver into nanowires. Absorption spectra of nanowires in the form of a dispersion in deionized water, AFM and SEM images confirm the nanowire formation. Solution of nanowire was coated over PET films to obtain transparent conducting films.

Synthesis of silver nanowires using hydrothermal technique for flexible transparent electrode application

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

Vijila, C. V. Mary; Rahman, K. K. Arsina; Parvathy, N. S.

2016-05-23

Transparent conducting films are becoming increasingly interesting because of their applications in electronics industry such as their use in solar energy applications. In this work silver nanowires were synthesized using solvothermal method by reducing silver nitrate and adding sodium chloride for assembling silver into nanowires. Absorption spectra of nanowires in the form of a dispersion in deionized water, AFM and SEM images confirm the nanowire formation. Solution of nanowire was coated over PET films to obtain transparent conducting films.

Highly effective synthesis of a cobalt(ii) metal-organic coordination polymer by using continuous flow chemistry.

PubMed

Gong, Chunhua; Zhang, Junyong; Zeng, Xianghua; Xie, Jingli

2016-12-20

The coordination polymer [Co 2 L 4 (H 2 O) 2 ]·CH 3 CN·H 2 O (HL = (E)-2-[2-(4-chlorophenyl)vinyl]-8-hydroxyquinoline) has been achieved with 95% yield by using an Asia flow synthesis system (chip reactor). Compared with the conventional batch-type methods such as diffusion, reflux and solvothermal reactions, higher yielding reactions carried out in a flow reactor have demonstrated that this technique is a powerful strategy to obtain coordination compounds.

Graphene oxide and carbon nanodots co-modified BiOBr nanocomposites with enhanced photocatalytic 4-chlorophenol degradation and mechanism insight.

PubMed

Qu, Songying; Xiong, Yuhan; Zhang, Jun

2018-05-15

Non-metallic graphene oxide (GO) and carbon nanodots (CDots) co-doped BiOBr ternary system (GO/CDots/BiOBr) were successfully synthesized via a simple one-step solvothermal process. The compositional characterization, optical and electrical properties of photocatalysts were investigated in detail. The prepared ternary photocatalysts possessed the excellent visible-light driven photocatalytic 4-chlorophenol (4-CP) degradation. Additionally, the 4-CP removal efficiencies decreased in the order of GO/CDots/BiOBr (88.9%) > CDots/BiOBr (62.9%) > GO/BiOBr (60.5%) > pristine BiOBr (46.9%) in 6 h under visible light irradiation. The dissolved organic carbon (DOC) removal and the dechlorination efficiency by the GO/CDots/BiOBr were 58.4% and 78.2%, respectively, much higher than pristine BiOBr. The co-existence of GO and CDots on the BiOBr greatly promoted visible light harvesting and utilizing ability and inhibited the recombination of photogenerated electron/hole pairs. The synergistic effect between GO, CDots and BiOBr was expounded, and the photocatalytic reaction mechanism was proposed in detail via the band structure analysis and free radical trapping experiments. Copyright © 2018 Elsevier Inc. All rights reserved.

Structure–property insights into nanostructured electrodes for Li-ion batteries from local structural and diffusional probes

DOE PAGES

Laveda, Josefa Vidal; Johnston, Beth; Paterson, Gary W.; ...

2017-12-04

Microwave heating presents a faster, lower energy synthetic methodology for the realization of functional materials. Here, we demonstrate for the first time that employing this method also leads to a decrease in the occurrence of defects in olivine structured LiFe 1–xMn xPO 4. For example, the presence of antisite defects in this structure precludes Li + diffusion along the b-axis leading to a significant decrease in reversible capacities. Total scattering measurements, in combination with Li + diffusion studies using muon spin relaxation (μ+SR) spectroscopy, reveal that this synthetic method generates fewer defects in the nanostructures compared to traditional solvothermal routes.more » Our interest in developing these routes to mixed-metal phosphate LiFe 1–xMn xPO 4 olivines is due to the higher Mn 2+/ 3+ redox potential in comparison to the Fe 2+/ 3+ pair. Here, single-phase LiFe 1–xMn xPO 4 (x = 0, 0.25, 0.5, 0.75 and 1) olivines have been prepared following a microwave-assisted approach which allows for up to 4 times faster reaction times compared to traditional solvothermal methods. Interestingly, the resulting particle morphology is dependent on the Mn content. We also examine their electrochemical performance as active electrodes in Li-ion batteries. In conclusion, these results present microwave routes as highly attractive for reproducible, gram-scale syntheses of high quality nanostructured electrodes which display close to theoretical capacity for the full iron phase.« less

Structure–property insights into nanostructured electrodes for Li-ion batteries from local structural and diffusional probes

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

Laveda, Josefa Vidal; Johnston, Beth; Paterson, Gary W.

Microwave heating presents a faster, lower energy synthetic methodology for the realization of functional materials. Here, we demonstrate for the first time that employing this method also leads to a decrease in the occurrence of defects in olivine structured LiFe 1–xMn xPO 4. For example, the presence of antisite defects in this structure precludes Li + diffusion along the b-axis leading to a significant decrease in reversible capacities. Total scattering measurements, in combination with Li + diffusion studies using muon spin relaxation (μ+SR) spectroscopy, reveal that this synthetic method generates fewer defects in the nanostructures compared to traditional solvothermal routes.more » Our interest in developing these routes to mixed-metal phosphate LiFe 1–xMn xPO 4 olivines is due to the higher Mn 2+/ 3+ redox potential in comparison to the Fe 2+/ 3+ pair. Here, single-phase LiFe 1–xMn xPO 4 (x = 0, 0.25, 0.5, 0.75 and 1) olivines have been prepared following a microwave-assisted approach which allows for up to 4 times faster reaction times compared to traditional solvothermal methods. Interestingly, the resulting particle morphology is dependent on the Mn content. We also examine their electrochemical performance as active electrodes in Li-ion batteries. In conclusion, these results present microwave routes as highly attractive for reproducible, gram-scale syntheses of high quality nanostructured electrodes which display close to theoretical capacity for the full iron phase.« less

Unique dielectric features of a ceramic-semiconductor nanocomposite MgNb2O6 + 0.25Zn0.5Cd0.5S

NASA Astrophysics Data System (ADS)

Pukazhselvan, D.; Selvaraj, Nivas Babu; Bdikin, Igor; Saravanan, R. Sakthi Sudar; Jakka, Suresh Kumar; Soares, M. J.; Fagg, Duncan Paul

2017-12-01

The present communication deals with the optical/dielectric characteristics of MgNb2O6 + 0.25Zn0.5Cd0.5S nanocomposite (10-30 nm) mixture. Zn0.5Cd0.5S (size ∼10 nm) was synthesized by microwave assisted solvo-thermal method. Monophase magnesium niobate (MN) nanoparticles (10-20 nm) were synthesized in a single step by mechanochemical treatment of MgO + Nb2O5 under dry N2 atmosphere. The nanocomposite, MgNb2O6 + 0.25Zn0.5Cd0.5S, was prepared by mechanical admixing of MgNb2O6 and Zn0.5Cd0.5S taken in 4:1 molar ratio. The photoluminescence study shows violet, yellow and orange-red emissions by the MgNb2O6 + 0.25Zn0.5Cd0.5S composite. The observed dielectric constant value (ε) for MgNb2O6 + 0.25Zn0.5Cd0.5S is only 4.7, which is ∼5 times smaller than the ε value of MgNb2O6 while a dielectric loss for the composite being closer to zero ensures promising commercial applications.

Solvothermal tuning of photoluminescent graphene quantum dots: from preparation to photoluminescence mechanism

NASA Astrophysics Data System (ADS)

Qi, Bao-Ping; Zhang, Xiaoru; Shang, Bing-Bing; Xiang, Dongshan; Zhang, Shenghui

2018-02-01

Solvothermal synthesis was employed to tune the surface states of graphene quantum dots (GQDs). Two series of GQDs with the particle sizes from 2.6 to 4.5 nm were prepared as follows: (I) GQDs with the same size but different oxygen degrees; (II) GQDs with different core sizes but the similar surface chemistry. Both the large sizes and the high surface oxidation degrees led to the redshift photoluminescence (PL) of GQDs. Electrochemiluminescence (ECL) spectra from two series of GQDs were all in accordance with their PL spectra, respectively, which provided good evidence for the conjugated structures in GQDs responsible for PL. [Figure not available: see fulltext.

Understanding the formation mechanism of graphene frameworks synthesized by solvothermal and rapid pyrolytic processes based on an alcohol-sodium hydroxide system.

PubMed

Cui, Huijuan; Zheng, Jianfeng; Yang, Pengju; Zhu, Yanyan; Wang, Zhijian; Zhu, Zhenping

2015-06-03

The determination of ways to facilitate the 2D-oriented assembly of carbons into graphene instead of other carbon structures while restraining the π-π stacking interaction is a challenge for the controllable bulk synthesis of graphene, which is vital both scientifically and technically. In this study, graphene frameworks (GFs) are synthesized by solvothermal and rapid pyrolytic processes based on an alcohol-sodium hydroxide system. The evolution mechanism of GFs is investigated systematically. Under sodium catalysis, the abundant carbon atoms produced by the fast decomposition of solvothermal intermediate self-assembled to graphene. The existence of abundant ether bonds may be favorable for 3D graphene formation. More importantly, GFs were successfully obtained using acetic acid as the carbon source in the synthetic process, suggesting the reasonability of analyzing the formation mechanism. It is quite possible to determine more favorable routes to synthesize graphene under this cognition. The electrochemical energy storage capacity of GFs was also studied, which revealed a high supercapacitor performance with a specific capacitance of 310.7 F/g at the current density of 0.2 A/g.

A two-step database search method improves sensitivity in peptide sequence matches for metaproteomics and proteogenomics studies.

PubMed

Jagtap, Pratik; Goslinga, Jill; Kooren, Joel A; McGowan, Thomas; Wroblewski, Matthew S; Seymour, Sean L; Griffin, Timothy J

2013-04-01

Large databases (>10(6) sequences) used in metaproteomic and proteogenomic studies present challenges in matching peptide sequences to MS/MS data using database-search programs. Most notably, strict filtering to avoid false-positive matches leads to more false negatives, thus constraining the number of peptide matches. To address this challenge, we developed a two-step method wherein matches derived from a primary search against a large database were used to create a smaller subset database. The second search was performed against a target-decoy version of this subset database merged with a host database. High confidence peptide sequence matches were then used to infer protein identities. Applying our two-step method for both metaproteomic and proteogenomic analysis resulted in twice the number of high confidence peptide sequence matches in each case, as compared to the conventional one-step method. The two-step method captured almost all of the same peptides matched by the one-step method, with a majority of the additional matches being false negatives from the one-step method. Furthermore, the two-step method improved results regardless of the database search program used. Our results show that our two-step method maximizes the peptide matching sensitivity for applications requiring large databases, especially valuable for proteogenomics and metaproteomics studies. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Facile synthesis of upconversion nanoparticles with high purity using lanthanide oleate compounds

NASA Astrophysics Data System (ADS)

Kang, Ning; Ai, Chao-Chao; Zhou, Ya-Ming; Wang, Zuo; Ren, Lei

2018-02-01

A novel strategy for preparing highly pure NaYF4-based upconversion nanoparticles (UCNPs) was developed using lanthanide oleate compounds [Ln(OA)3] as the precursor, denoted as the Ln-OA preparation method. Compared to the conventional solvothermal method for synthesizing UCNPs using lanthanide chloride compounds (LnCl3) as the precursor (denoted as the Ln-Cl method), the Ln-OA strategy exhibited the merits of high purity, reduced purification process and a uniform size in preparing core and core-shell UCNPs excited by a 980 or 808 nm near infrared (NIR) laser. This work sheds new insight on the preparation of UCNPs and promotes their application in biomedical fields.

3D hierarchical porous cobalt monoxide nanoplates with a book-like structure derived from Co(CO3)0.5(OH)·0.11H2O: two-steps oriented attachment and high-performance asymmetric supercapacitors

NASA Astrophysics Data System (ADS)

Xiao, Yuanhua; Zhao, Xiaobing; Jin, Qingxian; Su, Dangcheng; Wang, Xuezhao; Wu, Shide; Zhou, Liming; Fang, Shaoming

2017-10-01

3D Hierarchical porous cobalt monoxide (CoO) nanoplates with a book-like structure derive from Co(CO3)0.5(OH)·0.11H2O by a two-steps oriented attachment mechanism in the solvothermal process. Firstly, nanoplates are formed by oriented attachment of nanorods. Secondly, new nanoplates could be generated on the old nanoplates by a sloped oriented attachment of nanorods with the based nanoplates shape into a 3D hierarchical book-like structure. The CoO nanoplates show superior specific capacitance about 1221.7 F g-1 at 1 A g-1 to most of the Co-based supercapacitor materials up to date. An asymmetric supercapacitor (ASC) based on positive electrode CoO and negative electrode active carbon (AC) exhibits an excellent energy density of 50.1 Wh kg-1 at a power density of 589 W kg-1 and gets a satisfactory cycling stability (86.3% of its initial capacitance retention at 10 A g-1 over 10 000 cycles).

48 CFR 14.503-1 - Step one.

Code of Federal Regulations, 2010 CFR

2010-10-01

... 48 Federal Acquisition Regulations System 1 2010-10-01 2010-10-01 false Step one. 14.503-1 Section... AND CONTRACT TYPES SEALED BIDDING Two-Step Sealed Bidding 14.503-1 Step one. (a) Requests for... use the two step method. (3) The requirements of the technical proposal. (4) The evaluation criteria...

Multifunctionality in coating films including Nb-doped TiO2 and Cs x WO3: near infrared shielding and photocatalytic properties.

PubMed

Asakura, Yusuke; Anada, Yuto; Hamanaka, Ryo; Sato, Tsugio; Katsumata, Ken-Ichi; Wu, Xiaoyong; Yin, Shu

2018-06-01

Various types of coating films were obtained from hydrothermally synthesized Nb-doped TiO 2 (NTO) and Cs x WO 3 (CWO) nanoparticles. The coating films possessed multifunctionality including near infrared (NIR) absorption and photocatalysis abilities. The NTO and CWO nanoparticles were synthesized by a unique solvothermal reaction in which water induced by an esterification reaction between alcohol and carboxylic acid can act as a hydrolyzing agent for metal precursors. NTO was synthesized by the unique solvothermal reaction for the first time. The reaction accompanied by the reduction of Ti 4+ to Ti 3+ led to the formation of nanoparticles with both NIR absorption and photocatalytic properties. The effect of the ethanol-acetic acid ratio on the morphology of the obtained NTO was investigated, and the larger amount of acetic acid led to a larger nanoparticle size, indicating the size controllability. The two types of coating film, including CWO and NTO nanoparticles, were obtained for comparison: (1) coexistent coating film: one side of the quartz glass was coated with a dispersion, including both CWO and NTO nanoparticles, and (2) double-sided coating film: a quartz glass coated with a CWO dispersion on one side and an NTO dispersion on the other side. The double-sided coating led to higher multifunctionality. Furthermore, the optimized condition for the double-sided coating was investigated by using various NTO particles obtained using different ethanol-acetic acid ratios.

Multifunctionality in coating films including Nb-doped TiO2 and Cs x WO3: near infrared shielding and photocatalytic properties

NASA Astrophysics Data System (ADS)

Asakura, Yusuke; Anada, Yuto; Hamanaka, Ryo; Sato, Tsugio; Katsumata, Ken-ichi; Wu, Xiaoyong; Yin, Shu

2018-06-01

Various types of coating films were obtained from hydrothermally synthesized Nb-doped TiO2 (NTO) and Cs x WO3 (CWO) nanoparticles. The coating films possessed multifunctionality including near infrared (NIR) absorption and photocatalysis abilities. The NTO and CWO nanoparticles were synthesized by a unique solvothermal reaction in which water induced by an esterification reaction between alcohol and carboxylic acid can act as a hydrolyzing agent for metal precursors. NTO was synthesized by the unique solvothermal reaction for the first time. The reaction accompanied by the reduction of Ti4+ to Ti3+ led to the formation of nanoparticles with both NIR absorption and photocatalytic properties. The effect of the ethanol–acetic acid ratio on the morphology of the obtained NTO was investigated, and the larger amount of acetic acid led to a larger nanoparticle size, indicating the size controllability. The two types of coating film, including CWO and NTO nanoparticles, were obtained for comparison: (1) coexistent coating film: one side of the quartz glass was coated with a dispersion, including both CWO and NTO nanoparticles, and (2) double-sided coating film: a quartz glass coated with a CWO dispersion on one side and an NTO dispersion on the other side. The double-sided coating led to higher multifunctionality. Furthermore, the optimized condition for the double-sided coating was investigated by using various NTO particles obtained using different ethanol–acetic acid ratios.

Incidence, risk factors, and pregnancy outcomes of gestational diabetes mellitus using one-step versus two-step diagnostic approaches: A population-based cohort study in Isfahan, Iran.

PubMed

Hosseini, Elham; Janghorbani, Mohsen; Aminorroaya, Ashraf

2018-06-01

To study the incidence, risk factors, and pregnancy outcomes associated with gestational diabetes mellitus (GDM) diagnosed with one-step and two-step screening approaches. 1000 pregnant women who were eligible and consented to participate underwent fasting plasma glucose testing at the first prenatal visit (6-14 weeks). The women free from GDM or overt diabetes were screened at 24-28 weeks using the 50-g glucose challenge test (GCT) followed by 100-g, 3-h oral glucose tolerance test (OGTT) (two-step method). Regardless of the GCT result, all women underwent a 75-g, 2-h OGTT within one-week interval (one-step method). GDM incidence using the one-step and two-step methods was 9.3% (95% CI: 7.4-11.2) and 4.2% (95% CI: 2.9-5.5). GDM significantly increased the risk of macrosomia, gestational hypertension, preeclampsia, and cesarean section and older age and family history of diabetes significantly increased the risk of developing GDM in both approaches. In two-step method, higher pre-pregnancy body mass index and lower physical activity during pregnancy along with higher earlier cesarean section also increased significantly the risk of developing GDM. Despite a higher incidence of GDM using the one-step approach, more risk factors for and a stronger effect of GDM on adverse pregnancy outcomes were found when using the two-step approach. Longer follow-up of women with and without GDM may change the results using both approaches. Copyright © 2018 Elsevier B.V. All rights reserved.

A new theory for multistep discretizations of stiff ordinary differential equations: Stability with large step sizes

NASA Technical Reports Server (NTRS)

Majda, G.

1985-01-01

A large set of variable coefficient linear systems of ordinary differential equations which possess two different time scales, a slow one and a fast one is considered. A small parameter epsilon characterizes the stiffness of these systems. A system of o.d.e.s. in this set is approximated by a general class of multistep discretizations which includes both one-leg and linear multistep methods. Sufficient conditions are determined under which each solution of a multistep method is uniformly bounded, with a bound which is independent of the stiffness of the system of o.d.e.s., when the step size resolves the slow time scale, but not the fast one. This property is called stability with large step sizes. The theory presented lets one compare properties of one-leg methods and linear multistep methods when they approximate variable coefficient systems of stiff o.d.e.s. In particular, it is shown that one-leg methods have better stability properties with large step sizes than their linear multistep counter parts. The theory also allows one to relate the concept of D-stability to the usual notions of stability and stability domains and to the propagation of errors for multistep methods which use large step sizes.

Synthesis of Metal-organic Frameworks Based on Zr4+ and Benzene 1,3,5-Tricarboxylate Linker as Heterogeneous Catalyst in the Esterification Reaction of Palmitic Acid

NASA Astrophysics Data System (ADS)

Larasati, I.; Winarni, D.; Putri, F. R.; Hanif, Q. A.; Lestari, W. W.

2017-07-01

The conversion of the biomass into biodiesels via catalytic esterification and trans-esterification became an interesting topic due to the depletion of fossil-based energy. Homogenous catalysts such as HCl, H2SO4 and NaOH commonly used as catalyst, however, the use of this kind of catalyst causes more problems, such as the difficulties on the separation from the product and the pollution effect on the environment. Heterogeneous catalysts, such as Metal-Organic Frameworks (MOFs) give an alternative promising way to substitute these limitations due to their strong catalytic site, porosity, high specific surface area, and easy-separation and reusable properties. Herein, we reported the synthesis of MOFs based on zirconium(IV) and H3BTC linker (H3BTC = benzene-1,3,5-tricarboxylic acid) by solvothermal and reflux method. Solvothermal reaction at 120 °C was found to be the optimum method, that was indicated by most crystalline product compared to the simulated pattern in XRD analysis. The formation of the framework was characterized by FTIR analysis, which showed a significant shift from 1722 cm-1 to 1620 cm-1. The synthesized Zr(IV)-BTC was thermally stable up to 322°C as shown by TG/DTA analysis. This high thermal stability was related to the high oxidation state of Zr(IV), which give a significant covalent character to the Zr-O bond.

Potassium-doped copper oxide nanoparticles synthesized by a solvothermal method as an anode material for high-performance lithium ion secondary battery

NASA Astrophysics Data System (ADS)

Thi, Trang Vu; Rai, Alok Kumar; Gim, Jihyeon; Kim, Jaekook

2014-06-01

A simple and efficient approach was developed to synthesize CuO nanoparticles with improved electrochemical performance. Potassium (K+)-doped CuO nanoparticles were synthesized by a simple and cost-effective solvothermal method followed by annealing at 500 °C for 5 h under air atmosphere. For comparison, an undoped CuO sample was also synthesized under the same conditions. X-ray diffraction analysis demonstrates that the K+ ion doping caused no change in the phase structure, and highly crystalline KxCu1-xO1-δ (x = 0.10) powder without any impurity was obtained. As an anode material for a lithium ion battery, the K+-doped CuO nanoparticle electrode exhibited better capacity retention with a reversible capacity of over 354.6 mA h g-1 for up to 30 cycles at 0.1 C, as well as a high charge capacity of 162.3 mA h g-1 at a high current rate of 3.2 C, in comparison to an undoped CuO electrode (275.9 mA h g-1 at 0.1 C and 68.9 mA h g-1 at 3.2 C). The high rate capability and better cycleability of the doped electrode can be attributed to the influence of the K+ ion nanostructure on the increased electronic conductivity, diffusion efficiency, and kinetic properties of CuO during the lithiation and delithiation process.

Method and apparatus for single-stepping coherence events in a multiprocessor system under software control

DOEpatents

Blumrich, Matthias A.; Salapura, Valentina

2010-11-02

An apparatus and method are disclosed for single-stepping coherence events in a multiprocessor system under software control in order to monitor the behavior of a memory coherence mechanism. Single-stepping coherence events in a multiprocessor system is made possible by adding one or more step registers. By accessing these step registers, one or more coherence requests are processed by the multiprocessor system. The step registers determine if the snoop unit will operate by proceeding in a normal execution mode, or operate in a single-step mode.

Comparison of the Screening Tests for Gestational Diabetes Mellitus between "One-Step" and "Two-Step" Methods among Thai Pregnant Women.

PubMed

Luewan, Suchaya; Bootchaingam, Phenphan; Tongsong, Theera

2018-01-01

To compare the prevalence and pregnancy outcomes of GDM between those screened by the "one-step" (75 gm GTT) and "two-step" (100 gm GTT) methods. A prospective study was conducted on singleton pregnancies at low or average risk of GDM. All were screened between 24 and 28 weeks, using the one-step or two-step method based on patients' preference. The primary outcome was prevalence of GDM, and secondary outcomes included birthweight, gestational age, rates of preterm birth, small/large-for-gestational age, low Apgar scores, cesarean section, and pregnancy-induced hypertension. A total of 648 women were screened: 278 in the one-step group and 370 in the two-step group. The prevalence of GDM was significantly higher in the one-step group; 32.0% versus 10.3%. Baseline characteristics and pregnancy outcomes in both groups were comparable. However, mean birthweight was significantly higher among pregnancies with GDM diagnosed by the two-step approach (3204 ± 555 versus 3009 ± 666 g; p =0.022). Likewise, the rate of large-for-date tended to be higher in the two-step group, but was not significant. The one-step approach is associated with very high prevalence of GDM among Thai population, without clear evidence of better outcomes. Thus, this approach may not be appropriate for screening in a busy antenatal care clinic like our setting or other centers in developing countries.

Low temperature synthesis and characterization of Na–M–(O)–F phases with M=Ti, V

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

Nava-Avendaño, Jessica; Ayllón, José A.; Frontera, Carlos

2015-03-15

Na{sub 5}Ti{sub 3}O{sub 3}F{sub 11} was prepared by the microwave assisted method, and presents a chiolite related structure with cell parameters a=10.5016(5), b=10.4025(5), and c=10.2911(5) Å and Cmca (no. 64) space group. From solvothermal synthesis at 100 °C the cryolite Na{sub 3−δ}VO{sub 1−δ}F{sub 5+δ} was prepared, which crystallizes in the monoclinic system with a=5.5403(2), b=5.6804(2), c=7.9523(2) Å, β=90.032(7)° cell parameters and P2{sub 1}/n (no. 14) space group. Under similar synthesis conditions but with higher HF concentration the chiolite-type phase Na{sub 5−δ}V{sub 3}F{sub 14} was achieved, which exhibits a=10.5482(2), b=10.4887(1) and c=10.3243(1) Å cell parameters and Cmc2{sub 1} (no. 36) spacemore » group. A single crystal also having the chiolite structure was synthesized at 200 °C which exhibits tetragonal symmetry (a=7.380(3) and c=10.381(11) Å and space group P4{sub 2}2{sub 1}2 (no. 94)). Bond valence sum indicates that it contains V{sup 4+} and therefore can be formulated as Na{sub 5}V{sub 3}O{sub 3}F{sub 11}. - Graphical abstract: Na{sub 5}M{sub 3}(O,F){sub 14} with M=Ti and V having chiolite structure and Na{sub 3−δ}VO{sub 1−δ}F{sub 5+δ} cryolite were prepared by means of microwave-assisted and solvothermal synthesis. - Highlights: • Na{sub 5}Ti{sub 3}O{sub 3}F{sub 11} chiolite was prepared by a microwave assisted method and characterized. • Na{sub 3−δ}VO{sub 1−δ}F{sub 5+δ} and Na{sub 5−δ}V{sub 3}F{sub 14} were prepared by solvothermal synthesis. • The compounds were structurally characterized by diffraction techniques. • O/F distribution was estimated by applying Pauling’s second rule.« less

Synergistically Active NiCo2 S4 Nanoparticles Coupled with Holey Defect Graphene Hydrogel for High-Performance Solid-State Supercapacitors.

PubMed

Tiruneh, Sintayehu Nibret; Kang, Bong Kyun; Kwag, Sung Hoon; Lee, YoungHun; Kim, MinSeob; Yoon, Dae Ho

2018-03-02

Nickel cobalt sulfide nanoparticles embedded in holey defect graphene hydrogel (HGH) that exhibit highly porous structures and uniform nickel cobalt sulfide nanoparticle sizes are successfully prepared by a facile solvothermal-hydrothermal method. As an electrode material for supercapacitors, the as-prepared NiCo 2 S 4 @HGH shows ultra-high specific capacitances of 1000 F g -1 and 800 F g -1 at 0.5 and 6 A g -1 , respectively, owing to the outstanding electrical conductivity of HGH and high specific capacitance of NiCo 2 S 4 . After 2100 charge/discharge cycles at a current density of 6 A g -1 , 96.6 % of the specific capacitance was retained, signifying the superb durability of NiCo 2 S 4 @HGH. Moreover, remarkable specific capacitance (312.6 F g -1 ) and capacity retention (87 % after 5000 cycles) at 6 A g -1 were displayed by the symmetric solid-state supercapacitor fabricated by using NiCo 2 S 4 @HGH electrodes. These auspicious supercapacitor performances demonstrate that the as-developed solvothermal-hydrothermal approach can be widely used to prepare graphene-coupled binary metal sulfides for high-performance supercapacitor applications. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Synthesis of highly efficient flame retardant polypropylene nanocomposites with surfactant intercalated layered double hydroxides.

PubMed

Qiu, Lei; Gao, Yanshan; Zhang, Cheng; Yan, Qinghua; O'Hare, Dermot; Wang, Qiang

2018-02-27

The thermal and flame retardant performances of polypropylene (PP) nanocomposites with sodium dodecyl sulfate (DDS) and stearic acid intercalated layered double hydroxides (DDS-LDHs and stearic-LDHs) were investigated in this study. The DDS- and stearic-LDHs were treated using the aqueous miscible organic solvent treatment (AMOST) method to give highly dispersed platelets in PP composites. The incorporation of AMO-DDS- and stearic-LDHs improved the thermal stability and flame retardancy of the PP matrix significantly. The T 0.5 (temperature at 50% weight loss) of PP/AMO-stearic-LDH (20 wt%) nanocomposites dramatically increased by 80 °C compared to that of neat PP. The flame retardant performance was dependent on both surfactants and the loading of LDHs. The AMO-stearic-LDHs showed better flame retardant properties than the AMO-DDS-LDHs, especially when the LDH loading was higher than ca. 7 wt%. In addition, stearic-LDHs with different solvothermal times including 5, 10, 24 and 72 h were studied. It was found that the nanocomposites with LDHs solvothermally treated for 10 h showed the best thermal stability. The PP/stearic-LDH (24 h) nanocomposites with 20 wt% LDH loading possessed a better flame retardant performance, with PHRR reduction reaching 70%.

Solvothermal Synthesis of a Hollow Micro-Sphere LiFePO4/C Composite with a Porous Interior Structure as a Cathode Material for Lithium Ion Batteries

PubMed Central

Liu, Yang; Zhang, Jieyu; Li, Ying; Hu, Yemin; Li, Wenxian; Zhu, Mingyuan; Hu, Pengfei; Chou, Shulei; Wang, Guoxiu

2017-01-01

To overcome the low lithium ion diffusion and slow electron transfer, a hollow micro sphere LiFePO4/C cathode material with a porous interior structure was synthesized via a solvothermal method by using ethylene glycol (EG) as the solvent medium and cetyltrimethylammonium bromide (CTAB) as the surfactant. In this strategy, the EG solvent inhibits the growth of the crystals and the CTAB surfactant boots the self-assembly of the primary nanoparticles to form hollow spheres. The resultant carbon-coat LiFePO4/C hollow micro-spheres have a ~300 nm thick shell/wall consisting of aggregated nanoparticles and a porous interior. When used as materials for lithium-ion batteries, the hollow micro spherical LiFePO4/C composite exhibits superior discharge capacity (163 mAh g−1 at 0.1 C), good high-rate discharge capacity (118 mAh g−1 at 10 C), and fine cycling stability (99.2% after 200 cycles at 0.1 C). The good electrochemical performances are attributed to a high rate of ionic/electronic conduction and the high structural stability arising from the nanosized primary particles and the micro-sized hollow spherical structure. PMID:29099814

Solvothermal synthesis of monodisperse LiFePO4 micro hollow spheres as high performance cathode material for lithium ion batteries.

PubMed

Yang, Shiliu; Hu, Mingjun; Xi, Liujiang; Ma, Ruguang; Dong, Yucheng; Chung, C Y

2013-09-25

A microspherical, hollow LiFePO4 (LFP) cathode material with polycrystal structure was simply synthesized by a solvothermal method using spherical Li3PO4 as the self-sacrificed template and FeCl2·4H2O as the Fe(2+) source. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) show that the LFP micro hollow spheres have a quite uniform size of ~1 μm consisting of aggregated nanoparticles. The influences of solvent and Fe(2+) source on the phase and morphology of the final product were chiefly investigated, and a direct ion exchange reaction between spherical Li3PO4 templates and Fe(2+) ions was firstly proposed on the basis of the X-ray powder diffraction (XRD) transformation of the products. The LFP nanoparticles in the micro hollow spheres could finely coat a uniform carbon layer ~3.5 nm by a glucose solution impregnating-drying-sintering process. The electrochemical measurements show that the carbon coated LFP materials could exhibit high charge-discharge capacities of 158, 144, 125, 101, and even 72 mAh g(-1) at 0.1, 1, 5, 20, and 50 C, respectively. It could also maintain 80% of the initial discharge capacity after cycling for 2000 times at 20 C.

Study of TiO2 anatase nano and microstructures with dominant {001} facets for NO oxidation.

PubMed

Sofianou, Maria-Veronica; Trapalis, Christos; Psycharis, Vassils; Boukos, Nikos; Vaimakis, Tiverios; Yu, Jiaguo; Wang, Wenguang

2012-11-01

TiO(2) anatase nanoplates and hollow microspheres were fabricated by a solvothermal-hydrothermal method using titanium isopropoxide as a titanium precursor and hydrofluoric acid as a capping agent in order to enhance the formation of the {001} crystal facets of the anatase nanocrystals. These different morphological structures of TiO(2) anatase can be achieved by only changing the solvent, keeping the amount of the precursor and of the capping agent identical during the solvothermal-hydrothermal process. After calcination of the samples, the adsorbed fluoride atoms on the {001} crystal facets of the TiO(2) anatase nanocrystals were completely removed from their surface according to XPS analysis. The calcined TiO(2) anatase structures were higher crystallized and the specific surface area of the catalysts increased, enhancing their photocatalytic activity in comparison to the non-calcined TiO(2) anatase structures. All TiO(2) anatase samples with adsorbed as well as non-adsorbed fluoride atoms on their {001} crystal facets, exhibited a higher photonic efficiency than Degussa P25, which was used as a reference. The fluoride free TiO(2) anatase nanoplates exhibited the best photocatalytic activity in oxidizing the NO gas to NO(2) and NO(3) (-).

Solvo-thermal synthesis of a unique alkaline earth-transition Ba-Cd micro-porous coordination framework as hetero-metallic luminescent sensor for Cu2+ and real-time detection of benzaldehyde

NASA Astrophysics Data System (ADS)

Ding, Bin; Ma, Dian Xue; Zhang, Hui Min; Meng, Xin; Qiu, Rong Rong; Ren, Rong; Wu, Jie; Wu, Xiang Xia; Huo, Jian Zhong; Liu, Yuan Yuan; Shi, Xue Fang

2018-06-01

In this work a unique hetero-metallic alkaline earth-transition Ba-Cd luminescent micro-porous metal-organic framework {[BaCd(μ6-tp)1.5(μ2-Cl)(H2O) (DMF)2]·0.75H2O}n (H2tp = terephthalic acid) (1) has been prepared under solvo-thermal conditions. In 1 infinite 1D {Ba-X-Cd} (X = O, Cl) inorganic chains are linked via these full de-pronated tp2- ligands forming a unique 3D I1O2 type micro-porous coordination framework. PXRD patterns of 1 have been determined confirming pure phases of 1. Luminescence investigations suggested that 1 exhibits highly selective and sensitive sensing for trace amounts of benzaldehyde in ethanol, which provides a facile method for real-time detection of benzaldehyde. Meanwhile 1 also exhibits highly selective and sensitive sensing for Cu2+ over other cations with high quenching efficiency Ksv value 1.15 × 104 L·mol-1. As far as we know, 1 represents the first example of alkaline earth-transition hetero-metallic Ba-Cd micro-porous coordination framework as bi-functional luminescent probes for Cu2+ and benzaldehyde.

Solvo-thermal synthesis of a unique alkaline earth-transition Ba-Cd micro-porous coordination framework as hetero-metallic luminescent sensor for Cu2+ and real-time detection of benzaldehyde.

PubMed

Ding, Bin; Ma, Dian Xue; Zhang, Hui Min; Meng, Xin; Qiu, Rong Rong; Ren, Rong; Wu, Jie; Wu, Xiang Xia; Huo, Jian Zhong; Liu, Yuan Yuan; Shi, Xue Fang

2018-06-15

In this work a unique hetero-metallic alkaline earth-transition Ba-Cd luminescent micro-porous metal-organic framework {[BaCd(μ 6 -tp) 1.5 (μ 2 -Cl)(H 2 O) (DMF) 2 ]·0.75H 2 O} n (H 2 tp=terephthalic acid) (1) has been prepared under solvo-thermal conditions. In 1 infinite 1D {Ba-X-Cd} (X=O, Cl) inorganic chains are linked via these full de-pronated tp 2- ligands forming a unique 3D I 1 O 2 type micro-porous coordination framework. PXRD patterns of 1 have been determined confirming pure phases of 1. Luminescence investigations suggested that 1 exhibits highly selective and sensitive sensing for trace amounts of benzaldehyde in ethanol, which provides a facile method for real-time detection of benzaldehyde. Meanwhile 1 also exhibits highly selective and sensitive sensing for Cu 2+ over other cations with high quenching efficiency K sv value 1.15×10 4 L·mol -1 . As far as we know, 1 represents the first example of alkaline earth-transition hetero-metallic Ba-Cd micro-porous coordination framework as bi-functional luminescent probes for Cu 2+ and benzaldehyde. Copyright © 2018 Elsevier B.V. All rights reserved.

High efficient perovskite solar cell material CH3NH3PbI3: Synthesis of films and their characterization

NASA Astrophysics Data System (ADS)

Bera, Amrita Mandal; Wargulski, Dan Ralf; Unold, Thomas

2018-04-01

Hybrid organometal perovskites have been emerged as promising solar cell material and have exhibited solar cell efficiency more than 20%. Thin films of Methylammonium lead iodide CH3NH3PbI3 perovskite materials have been synthesized by two different (one step and two steps) methods and their morphological properties have been studied by scanning electron microscopy and optical microscope imaging. The morphology of the perovskite layer is one of the most important parameters which affect solar cell efficiency. The morphology of the films revealed that two steps method provides better surface coverage than the one step method. However, the grain sizes were smaller in case of two steps method. The films prepared by two steps methods on different substrates revealed that the grain size also depend on the substrate where an increase of the grain size was found from glass substrate to FTO with TiO2 blocking layer to FTO without any change in the surface coverage area. Present study reveals that an improved quality of films can be obtained by two steps method by an optimization of synthesis processes.

Nanostructured N-doped TiO2 marigold flowers for an efficient solar hydrogen production from H2S

NASA Astrophysics Data System (ADS)

Chaudhari, Nilima S.; Warule, Sambhaji S.; Dhanmane, Sushil A.; Kulkarni, Milind V.; Valant, Matjaz; Kale, Bharat B.

2013-09-01

Nitrogen-doped TiO2 nanostructures in the form of marigold flowers have been synthesized for the first time using a facile solvothermal method. The structural analysis has shown that such an N-doped TiO2 system crystallizes in the anatase structure. The optical absorption spectra have clearly shown the shift in the absorption edge towards the visible-light range, which indicates successful nitrogen doping. The nitrogen doping has been further confirmed by photoluminescence and photoemission spectroscopy. Microscopy studies have shown the thin nanosheets (petals) of N-TiO2 with a thickness of ~2-3 nm, assembled in the form of the marigold flower with a high surface area (224 m2 g-1). The N-TiO2 nanostructure with marigold flowers is an efficient photocatalyst for the decomposition of H2S and production of hydrogen under solar light. The maximum hydrogen evolution obtained is higher than other known N-TiO2 systems. It is noteworthy that photohydrogen production using the unique marigold flowers of N-TiO2 from abundant H2S under solar light is hitherto unattempted. The proposed synthesis method can also be utilized to design other hierarchical nanostructured N-doped metal oxides.Nitrogen-doped TiO2 nanostructures in the form of marigold flowers have been synthesized for the first time using a facile solvothermal method. The structural analysis has shown that such an N-doped TiO2 system crystallizes in the anatase structure. The optical absorption spectra have clearly shown the shift in the absorption edge towards the visible-light range, which indicates successful nitrogen doping. The nitrogen doping has been further confirmed by photoluminescence and photoemission spectroscopy. Microscopy studies have shown the thin nanosheets (petals) of N-TiO2 with a thickness of ~2-3 nm, assembled in the form of the marigold flower with a high surface area (224 m2 g-1). The N-TiO2 nanostructure with marigold flowers is an efficient photocatalyst for the decomposition of H2S and production of hydrogen under solar light. The maximum hydrogen evolution obtained is higher than other known N-TiO2 systems. It is noteworthy that photohydrogen production using the unique marigold flowers of N-TiO2 from abundant H2S under solar light is hitherto unattempted. The proposed synthesis method can also be utilized to design other hierarchical nanostructured N-doped metal oxides. Electronic supplementary information (ESI) available: GC-MS graph of the filtrate obtained in solvothermal reaction after 16 h and FESEM images without guanidine carbonate for 16 h. See DOI: 10.1039/c3nr02975a

Touching the theoretical capacity: synthesizing cubic LiTi2(PO4)3/C nanocomposites for high-performance lithium-ion battery.

PubMed

Deng, Wenjun; Wang, Xusheng; Liu, Chunyi; Li, Chang; Xue, Mianqi; Li, Rui; Pan, Feng

2018-04-05

A cubic LiTi2(PO4)3/C composite is successfully prepared via a simple solvothermal method and further glucose-pyrolysis treatment. The as-fabricated LTP/C material delivers an ultra-high reversible capacity of 144 mA h g-1 at 0.2C rate, which is the highest ever reported, and shows considerable performance improvement compared with before. Combining this with the stable cycling performance and high rate capability, such material has a promising future in practical application.

[Effect of two-step sintering method on properties of zirconia ceramic].

PubMed

Huang, Hui; Wei, Bin; Zhang, Fu-Qiang; Sun, Jing; Gao, Lian

2008-04-01

To study the influence of two-step sintering method on the sintering property, mechanical properties and microstructure of zirconia ceramic. The nano-size zirconia powder were compacted and divided into two groups, one group for one-step sintering method, another group for two-step sintering method. All samples sintered at different temperature. The relative density, three-bend strength, HV hardness, fracture toughness and microstructure of sintered block were investigated. Two-step sintering method influenced the sintering property and mechanical properties of zirconia ceramic. The maximal relative density was 98.49% at 900 degrees C/1,450 degrees C sintering temperature. There were significant difference of mechanical properties between one-step sintering and two-step sintering, the three-bend strength and fracture toughness declined, hardness increased at two-step sintering. The three-bend strength, HV hardness and fracture toughness reached to maximum value as 1,059.08 MPa +/- 75.24 MPa, 1,377.00 MPa +/- 16.37 MPa and 5.92 MPa x m1/2 +/- 0.37 MPa x m1/2 at 900 degrees C/1,450 degrees C sintering temperature respectively. Microscopy revealed the relationship between the porosity and shapes of grains was correlated to strength of the zirconia ceramics. Despite of the two-step sintering method influences the properties of zirconia, it also is a promising esthetic all-ceramic dental material.

Solvothermal-induced self-assembly of Fe2O3/GS aerogels for high Li-storage and excellent stability.

PubMed

Wang, Ronghua; Xu, Chaohe; Du, Meng; Sun, Jing; Gao, Lian; Zhang, Peng; Yao, Heliang; Lin, Chucheng

2014-06-12

A novel solvothermal-induced self-assembly approach, using colloid sol as precursor, is developed to construct monolithic 3D metal oxide/GS (graphene sheets) aerogels. During the solvothermal process, graphene oxide (GO) is highly reduced to GS and self-assembles into 3D macroscopic hydrogels, accompanying with in situ transformation of colloid sol to metal oxides. As a proof of concept, Fe2 O3 /GS aerogels are synthesized based on Fe(OH)3 sol, in which GS self-assemble into an interconnected macroporous framework and Fe2 O3 nanocrystals (20-50 nm) uniformly deposit on GS. Benefitting from the integration of macroporous structures, large surface area, high electrical conductivity, and good electrode homogeneity, the hybrid electrode manifests a superior rate capability (930, 660 and 520 mAh g(-1) at 500, 2000 and 4000 mA g(-1), respectively) and excellent prolonged cycling stability at high rates (733 mAh g(-1) during 1000 charge/discharge cycles at 2000 mA g(-1)), demonstrating its great potential for application in high performance lithium ion batteries. The work described here provides a versatile pathway to construct various graphene-based hybrid aerogels. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Solvothermal synthesis of V{sub 4}O{sub 9} flake-like morphology and its photocatalytic application in the degradation of methylene blue

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

Chine, M.K.; Sediri, F., E-mail: faouzi.sediri@ipeit.rnu.tn; Faculté des Sciences de Tunis, Université, Tunis-Elmanar, 2092 Elmanar, Tunis

2012-11-15

Highlights: ► Flake-like nanocrystalline V{sub 4}O{sub 9} was synthesized by a solvothermal route. ► Photocatalytic activity has been evaluated by the degradation of methylene blue under visible light irradiation. ► V{sub 4}O{sub 9} nanoflakes exhibited much higher photocatalytic activity two times higher than the bulk V{sub 2}O{sub 5}. -- Abstract: Flake-like nanocrystalline V{sub 4}O{sub 9} has been successfully synthesized by solvothermal process using V{sub 2}O{sub 5} as vanadium source and phenolphthalein as a reducing agent and a structure-directing template. Techniques X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infrared (FTIR) spectroscopy and ultraviolet–visible (UV–vis) spectroscopy have been used tomore » characterize the structure, the morphology and the composition of the material. The photocatalytic activity of the material has been evaluated by the degradation of methylene blue under visible light irradiation. As a result, after the lapse of 150 min, around 93.54% bleaching was observed, with V{sub 4}O{sub 9} nanoflakes yielding more photodegradation compared to that of bulk V{sub 2}O{sub 5}. This presents a degradation percentage of about 44.67%.« less

One-step leapfrog ADI-FDTD method for simulating electromagnetic wave propagation in general dispersive media.

PubMed

Wang, Xiang-Hua; Yin, Wen-Yan; Chen, Zhi Zhang David

2013-09-09

The one-step leapfrog alternating-direction-implicit finite-difference time-domain (ADI-FDTD) method is reformulated for simulating general electrically dispersive media. It models material dispersive properties with equivalent polarization currents. These currents are then solved with the auxiliary differential equation (ADE) and then incorporated into the one-step leapfrog ADI-FDTD method. The final equations are presented in the form similar to that of the conventional FDTD method but with second-order perturbation. The adapted method is then applied to characterize (a) electromagnetic wave propagation in a rectangular waveguide loaded with a magnetized plasma slab, (b) transmission coefficient of a plane wave normally incident on a monolayer graphene sheet biased by a magnetostatic field, and (c) surface plasmon polaritons (SPPs) propagation along a monolayer graphene sheet biased by an electrostatic field. The numerical results verify the stability, accuracy and computational efficiency of the proposed one-step leapfrog ADI-FDTD algorithm in comparison with analytical results and the results obtained with the other methods.

A hybrid-perturbation-Galerkin technique which combines multiple expansions

NASA Technical Reports Server (NTRS)

Geer, James F.; Andersen, Carl M.

1989-01-01

A two-step hybrid perturbation-Galerkin method for the solution of a variety of differential equations type problems is found to give better results when multiple perturbation expansions are employed. The method assumes that there is parameter in the problem formulation and that a perturbation method can be sued to construct one or more expansions in this perturbation coefficient functions multiplied by computed amplitudes. In step one, regular and/or singular perturbation methods are used to determine the perturbation coefficient functions. The results of step one are in the form of one or more expansions each expressed as a sum of perturbation coefficient functions multiplied by a priori known gauge functions. In step two the classical Bubnov-Galerkin method uses the perturbation coefficient functions computed in step one to determine a set of amplitudes which replace and improve upon the gauge functions. The hybrid method has the potential of overcoming some of the drawbacks of the perturbation and Galerkin methods as applied separately, while combining some of their better features. The proposed method is applied, with two perturbation expansions in each case, to a variety of model ordinary differential equations problems including: a family of linear two-boundary-value problems, a nonlinear two-point boundary-value problem, a quantum mechanical eigenvalue problem and a nonlinear free oscillation problem. The results obtained from the hybrid methods are compared with approximate solutions obtained by other methods, and the applicability of the hybrid method to broader problem areas is discussed.

Mesoporous TiO2 nanosheets anchored on graphene for ultra long life Na-ion batteries.

PubMed

Zhang, Ruifang; Wang, Yuankun; Zhou, Han; Lang, Jinxin; Xu, Jingjing; Xiang, Yang; Ding, Shujiang

2018-06-01

Sodium-ion batteries, which have a similar electrochemical reaction mechanism to lithium-ion batteries, have been considered as one of the most potential lithium-ion battery alternatives due to the rich reserves of sodium. However, it is very hard to find appropriate electrode materials imputing the large radius of sodium-ion. TiO 2 is particularly interesting as anodes for sodium-ion batteries due to their reasonable operation voltage, cost, and nontoxicity. To obtain a better electrochemical property, mesoporous TiO 2 nanosheets (NSs)/reduced graphene oxide (rGO) composites have been synthesized via a scalable hydrothermal-solvothermal method with a subsequent calcination process. Benefitting from unique structure design, TiO 2 NSs@rGO exhibits a superior cycle stability (90 mAh g -1 after 10 000 cycles at a high current rate of 20 C) and satisfactory rate performance (97.3 mAh g -1 at 25 C). To our knowledge, such ultra long cycle life has not previously been reported.

Development of high-sensitive, reproducible colloidal surface-enhanced Raman spectroscopy active substrate using silver nanocubes for potential biosensing applications

NASA Astrophysics Data System (ADS)

Hasna, Kudilatt; Lakshmi, Kiran; Ezhuthachan Jayaraj, Madambi Kunjukuttan; Kumar, Kumaran Rajeev; Matham, Murukeshan Vadakke

2016-04-01

Surface-enhanced Raman spectroscopy (SERS) has emerged as one of the thrust research areas that could find potential applications in bio and chemical sensing. We developed colloidal SERS active substrate with excellent sensitivity and high reproducibility using silver nanocube (AgNC) synthesized via the solvothermal method. Finite-difference time-domain simulation was carried out in detail to visualize dipole generation in the nanocube during localized surface plasmon resonance and to locate the respective hot spots in AgNC responsible for the huge Raman enhancement. The prediction is verified by the SERS analysis of the synthesized nanocubes using Rhodamine 6G molecule. An excellent sensitivity with a detection limit of 10-17 M and a very high enhancement factor of 1.2×108 confirms the "hot spots" in the nanocube. SERS activity is also carried out for crystal violet and for food adulterant Sudan I molecule. Finally, label-free DNA detection is performed to demonstrate the versatility of SERS as a potential biosensor.

Multitopic ligand directed assembly of low-dimensional metal-chalcogenide organic frameworks.

PubMed

Liu, Yi; Ye, Kaiqi; Wang, Yue; Zhang, Qichun; Bu, Xianhui; Feng, Pingyun

2017-01-31

Despite tremendous progress in metal-organic frameworks, only limited success has been achieved with metal-chalcogenide organic frameworks. Metal-chalcogenide organic frameworks are desirable because they offer a promising route towards tunable semiconducting porous frameworks. Here, four novel semiconducting chalcogenide-organic hybrid compounds have been synthesized through a solvothermal method. Multitopic organic molecules, i.e., 1,2-di-(4-pyridyl)ethylene (L 1 ), 1,3,5-tris(4-pyridyl-trans-ethenyl)benzene (L 2 ) and tetrakis(4-pyridyloxymethylene)methane (L 3 ), have been used as linkers to assemble Zn(SAr) 2 or Zn 2 (SAr) 4 units to generate different patterns of spatial organizations. Single-crystal structural analyses indicate that compounds NTU-2, NTU-3 and NTU-4 possess two-dimensional layer structures, while compound NTU-1 adopts a one-dimensional coordination framework (NTU-n, where n is the number related to a specific structure). The diffuse-reflectance spectra demonstrate that these four compounds possess indirect bandgaps and their tunable bandgaps are correlated with their compositions and crystal structures.

Mesoporous TiO2 nanosheets anchored on graphene for ultra long life Na-ion batteries

NASA Astrophysics Data System (ADS)

Zhang, Ruifang; Wang, Yuankun; Zhou, Han; Lang, Jinxin; Xu, Jingjing; Xiang, Yang; Ding, Shujiang

2018-06-01

Sodium-ion batteries, which have a similar electrochemical reaction mechanism to lithium-ion batteries, have been considered as one of the most potential lithium-ion battery alternatives due to the rich reserves of sodium. However, it is very hard to find appropriate electrode materials imputing the large radius of sodium-ion. TiO2 is particularly interesting as anodes for sodium-ion batteries due to their reasonable operation voltage, cost, and nontoxicity. To obtain a better electrochemical property, mesoporous TiO2 nanosheets (NSs)/reduced graphene oxide (rGO) composites have been synthesized via a scalable hydrothermal-solvothermal method with a subsequent calcination process. Benefitting from unique structure design, TiO2 NSs@rGO exhibits a superior cycle stability (90 mAh g‑1 after 10 000 cycles at a high current rate of 20 C) and satisfactory rate performance (97.3 mAh g‑1 at 25 C). To our knowledge, such ultra long cycle life has not previously been reported.

Surfactant-free solvothermal synthesis of Hydroxyapatite nested bundles for the effective photodegradation of cationic dyes

NASA Astrophysics Data System (ADS)

Reeta Mary, I.; Sonia, S.; Navadeepthy, D.; Mangalaraj, D.; Viswanathan, C.; Ponpandian, N.

2018-05-01

In this study, hydroxyapatite nested bundles (HNBs) were successfully constructed from nanosticks as nanoscale building blocks via a facile, solvothermal process without using any surfactant. The fabricated HNBs were structurally analyzed using X-ray diffraction and Fourier transform infrared spectroscopy, which confirmed the purity of the HNBs. The surface characteristics were determined by field emission scanning electron microscopy and Brunauer-Emmett-Teller analysis, and the optical characteristics by ultraviolet (UV)-visible spectroscopy. The synthesized HNBs were tested to determine their activity during the degradation of methylene blue, methylene violet, and rhodamine B via photocatalysis under UV irradiation. The degradation efficiency of HNBs and the rate of degradation can be explained based on the properties of the HNBs and cationic dyes.

Improved open-circuit voltage in polymer/oxide-nanoarray hybrid solar cells by formation of homogeneous metal oxide core/shell structures.

PubMed

Wu, Fan; Cui, Qi; Qiu, Zeliang; Liu, Changwen; Zhang, Hui; Shen, Wei; Wang, Mingtai

2013-04-24

Incorporation of vertically aligned nanorod/nanowire arrays of metal oxide (oxide-NAs) with a polymer can produce efficient hybrid solar cells with an ideal bulk-heterojunction architecture. However, polymer/oxide-NAs solar cells still suffer from a rather low (normally, < 0.4 V) open-circuit voltage (Voc). Here we demonstrate, for the first time, a novel strategy to improve the Voc in polymer/oxide-NAs solar cells by formation of homogeneous core/shell structures and reveal the intrinsic principles involved therein. A feasible hydrothermal-solvothermal combined method is developed for preparing homogeneous core/shell nanoarrays of metal oxides with a single-crystalline nanorod as core and the aggregation layer of corresponding metal oxide quantum dots (QDs) as shell, and the shell thickness (L) is easily controlled by the solvothermal reaction time for growing QDs on the nanorod. The core/shell formation dramatically improves the device Voc up to ca. 0.7-0.8 V depending on L. Based on steady-state and dynamic measurements, as well as modeling by space-charge-limited current method, it is found that the improved Voc originates from the up-shifted conduction band edge in the core by the interfacial dipole field resulting from the decreased mobility difference between photogenerated electrons and holes after the shell growth, which increases the energy difference between the quasi-Fermi levels of photogenerated electrons in the core and holes in the polymer for a higher Voc. Our results indicate that increasing Voc by the core/shell strategy seems not to be dependent on the kinds of metal oxides.

Facile synthesis of morphology-controlled Co3O4 nanostructures through solvothermal method with enhanced catalytic activity for H2O2 electroreduction

NASA Astrophysics Data System (ADS)

Cheng, Kui; Cao, Dianxue; Yang, Fan; Xu, Yang; Sun, Gaohui; Ye, Ke; Yin, Jinling; Wang, Guiling

2014-05-01

Hydrogen peroxide (H2O2) replaced oxygen (O2) as oxidant has been widely investigated due to its faster reduction kinetics, easier storage and handling than gaseous oxygen. The main challenge of using H2O2 as oxidant is the chemical decomposition. In this article, by using different C2H5OH/H2O volume ratio as the solvent, Co3O4 with different morphologies (nanosheet, nanowire, ultrafine nanowire net, nanobelts, and honeycomb-like) direct growth on Ni foam are synthesized via a simple solvothermal method for the first time. Results show that the introduction of ethanol could obviously improve the catalytic performance toward H2O2 electroreduction. The sample prepared in the solution with the C2H5OH/H2O volume ratio of 1:2 shows the best catalytic performance among the five samples and a current density of 0.214 A cm-2 is observed in 3.0 mol L-1 KOH + 0.5 mol L-1 H2O2 at -0.4 V (vs. Ag/AgCl KCl), which is much larger than that on the other metal oxides reported previously, almost comparable with the precious metals. This electrode of Co3O4 directly grown on Ni foam has superior mass transport property, which combining with its low-cost and facile preparation, make it a promising electrode for fuel cell using H2O2 as the oxidant.

Facile and low temperature route to synthesis of CuS nanostructure in mesoporous material by solvothermal method.

PubMed

Sohrabnezhad, Sh; Zanjanchi, M A; Hosseingholizadeh, S; Rahnama, R

2014-04-05

The synthesis of CuS nanomaterial in MCM-41 matrix has been realized by chemical synthesis between MCM-41, copper sulfate pentahydrate and thiourea via a solvothermal method in ethylene glycol and water, separately. X-ray diffraction analysis (XRD), diffuse reflectance spectroscopy (DRS), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and fourier transform infrared (FT-IR) were used to characterize the products. At synthesized CuS/MCM-41 sample in ethylene glycol, X-ray diffraction and diffuse reflectance spectroscopy showed pure covellite phase of copper sulfide with high crystality. But prepared CuS/MCM-41 sample in water shows the covellite, chalcocite and the djurleite phase of copper sulfide nanostructures. The formation of CuS nanostructures was confirmed by FT-IR. Photocatalytic activity of CuS/MCM-41 nanocomposites was studied for degradation of Methylene Blue (MB) under visible light. The CuS/MCM-41 nanocomposite is more effective nanocatalyst than synthesized CuS/MCM-41 sample in water for degradation of methylene blue. Several parameters were examined, catalyst amount (0.1-1gL(-1)), pH (1-13) and initial concentration of MB (0.96-10ppm). The extent of degradation was estimated from the residual concentration by spectrophotometrically. The support size was obtained in the range 60-145nm by TEM. In the same way, the average size of copper sulfide in CuSMCM-41E and CuS/MCM-41W nanostructures were obtained about 10nm and 16nm, respectively. Copyright © 2013 Elsevier B.V. All rights reserved.

Structural variation from heterometallic cluster-based 1D chain to heterometallic tetranuclear cluster: Syntheses, structures and magnetic properties

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

Zhang, Shu-Hua, E-mail: zsh720108@163.com; Zhao, Ru-Xia; Li, He-Ping

Using the solvothermal method, we present the comparative preparation of ([Co{sub 3}Na(dmaep){sub 3}(ehbd)(N{sub 3}){sub 3}]·DMF){sub n} (1) and [Co{sub 2}Na{sub 2}(hmbd){sub 4}(N{sub 3}){sub 2}(DMF){sub 2}] (2), where Hehbd is 3-ethoxy-2-hydroxy-benzaldehyde, Hhmbd is 3-methoxy-2-hydroxy-benzaldehyde, and Hdmaep is 2-dimethylaminomethyl-6-ethoxy-phenol, which was synthesized by an in-situ reaction. Complexes 1 and 2 were characterized by elemental analysis, IR spectroscopy, and X-ray single-crystal diffraction. Complex 1 is a novel heterometallic cluster-based 1-D chain and 2 is a heterometallic tetranuclear cluster. The (Co{sub 3}{sup II}Na) and (Co{sub 2}{sup II}Na{sub 2}) cores display dominant ferromagnetic interaction from the nature of the binding modes through μ{sub 1,1,1}-N{sub 3}{supmore » –} (end-on, EO). - Graphical abstract: Two novel cobalt complexes have been prepared. Compound 1 consists of tetranuclear (Co{sub 3}{sup II}Na) units, which further formed a 1-D chain. Compound 2 is heterometallic tetranuclear cluster. Two complexes display dominant ferromagnetic interaction. - Highlights: • Two new heterometallic complexes have been synthesized by solvothermal method. • The stereospecific blockade of the ligands in the synthesis system seems to be the most important synthetic parameter. • The magnetism studies show that 1 and 2 exhibit ferromagnetic interactions. • Complex 1 shows slowing down of magnetization and not blocking of magnetization.« less

Phenoxo bridged dinuclear Zn(II) Schiff base complex as new precursor for preparation zinc oxide nanoparticles: Synthesis, characterization, crystal structures and photoluminescence studies

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

Saeednia, S., E-mail: sami_saeednia@yahoo.com; Iranmanesh, P.; Ardakani, M. Hatefi

Highlights: • A novel nano-scale Zn(II) complex was synthesized by solvothermal method. • Chemical structure of the nanostructures was characterized as well as bulk complex. • The photoluminescence property of the complex was investigated at room temperature. • The thermogravimetry and differential thermal analysis were carried out. • Thermal decomposition of the nanostructures was prepared zinc oxide nanoparticles. - Abstract: Nanoparticles of a novel Zn(II) Schiff base complex, [Zn(HL)NO{sub 3}]{sub 2} (1), (H{sub 2}L = 2-[(2-hydroxy-propylimino) methyl] phenol), was synthesized by using solvothermal method. Shape, morphology and chemical structure of the synthesized nanoparticles were characterized by scanning electron microscopy (SEM),more » X-ray powder diffraction (XRD), Fourier Transform Infrared Spectoscopy (FT-IR) and UV–vis spectroscopy. Structural determination of compound 1 was determined by single-crystal X-ray diffraction. The results were revealed that the zinc complex is a centrosymmetric dimer in which deprotonated phenolates bridge the two five-coordinate metal atoms and link the two halves of the dimer. The thermal stability of compound 1 was analyzed by thermal gravimetric analysis (TGA) and differential scanning calorimetry (DSC). The effect of the initial substrates concentration and reaction time on size and morphology of compound 1 nanostructure was investigated as well. Furthermore, the luminescent properties of the complex 1 were examined. ZnO nanoparticles with diameter between 15 and 20 nm were simply synthesized by solid-state transformation of compound 1 at 700 °C.« less

Evolution of Reduced Graphene Oxide-SnS2 Hybrid Nanoparticle Electrodes in Li-Ion Batteries.

PubMed

Modarres, Mohammad H; Lim, Jonathan Hua-Wei; George, Chandramohan; De Volder, Michael

2017-06-22

Hybrid nanomaterials where active battery nanoparticles are synthesized directly onto conductive additives such as graphene hold the promise of improving the cyclability and energy density of conversion and alloying type Li-ion battery electrodes. Here we investigate the evolution of hybrid reduced graphene oxide-tin sulfide (rGO-SnS 2 ) electrodes during battery cycling. These hybrid nanoparticles are synthesized by a one-step solvothermal microwave reaction which allows for simultaneous synthesis of the SnS 2 nanocrystals and reduction of GO. Despite the hybrid architecture of these electrodes, electrochemical impedance spectroscopy shows that the impedance doubles in about 25 cycles and subsequently gradually increases, which may be caused by an irreversible surface passivation of rGO by sulfur enriched conversion products. This surface passivation is further confirmed by post-mortem Raman spectroscopy of the electrodes, which no longer detects rGO peaks after 100 cycles. Moreover, galvanostatic intermittent titration analysis during the 1st and 100th cycles shows a drop in Li-ion diffusion coefficient of over an order of magnitude. Despite reports of excellent cycling performance of hybrid nanomaterials, our work indicates that in certain electrode systems, it is still critical to further address passivation and charge transport issues between the active phase and the conductive additive in order to retain high energy density and cycling performance.

Evolution of Reduced Graphene Oxide–SnS2 Hybrid Nanoparticle Electrodes in Li-Ion Batteries

PubMed Central

2017-01-01

Hybrid nanomaterials where active battery nanoparticles are synthesized directly onto conductive additives such as graphene hold the promise of improving the cyclability and energy density of conversion and alloying type Li-ion battery electrodes. Here we investigate the evolution of hybrid reduced graphene oxide–tin sulfide (rGO-SnS2) electrodes during battery cycling. These hybrid nanoparticles are synthesized by a one-step solvothermal microwave reaction which allows for simultaneous synthesis of the SnS2 nanocrystals and reduction of GO. Despite the hybrid architecture of these electrodes, electrochemical impedance spectroscopy shows that the impedance doubles in about 25 cycles and subsequently gradually increases, which may be caused by an irreversible surface passivation of rGO by sulfur enriched conversion products. This surface passivation is further confirmed by post-mortem Raman spectroscopy of the electrodes, which no longer detects rGO peaks after 100 cycles. Moreover, galvanostatic intermittent titration analysis during the 1st and 100th cycles shows a drop in Li-ion diffusion coefficient of over an order of magnitude. Despite reports of excellent cycling performance of hybrid nanomaterials, our work indicates that in certain electrode systems, it is still critical to further address passivation and charge transport issues between the active phase and the conductive additive in order to retain high energy density and cycling performance. PMID:28804530

One-step solvothermal synthesis of magnetic Fe3O4-graphite composite for Fenton-like degradation of levofloxacin.

PubMed

Wang, Long; Zhao, Qi; Hou, Juan; Yan, Jin; Zhang, Fengshuang; Zhao, Jiahui; Ding, Hong; Li, Yi; Ding, Lan

2016-01-01

A novel Fe3O4-graphite composite was prepared, characterized, and investigated as a heterogeneous Fenton-like catalyst for the degradation of levofloxacin (LEV) in an aqueous solution. The results revealed that the Fe3O4-graphite composite exhibited excellent properties for the degradation and mineralization of LEV, achieving a nearly complete degradation of 50 mg L(-1) LEV in 15 min and 48% of total organic carbon removal in 60 min under optimal conditions. A large electronic conjugation structure exists in graphite, which may lead to the fast production of •OH radical species because of the easy reduction of Fe(III) to Fe(II). In addition, we observed that the graphite can degrade LEV in the presence of H2O2. Therefore, the synergistic results of the graphite structure and Fe3O4 magnetic nanoparticles (MNPs) may contribute to the high catalytic activity of the Fe3O4-graphite composite. Compared with pure Fe3O4 MNPs, lesser iron leaching of the Fe3O4-graphite composite was observed during the degradation of LEV. The degradation efficiency of LEV remained approximately 80% at the fifth recycling run, which indicates that the Fe3O4-graphite composite has potential applications in water treatment for removing organic pollutants.

A Lithium-Ion Battery using a 3 D-Array Nanostructured Graphene-Sulfur Cathode and a Silicon Oxide-Based Anode.

PubMed

Benítez, Almudena; Di Lecce, Daniele; Elia, Giuseppe Antonio; Caballero, Álvaro; Morales, Julián; Hassoun, Jusef

2018-05-09

An efficient lithium-ion battery was assembled by using an enhanced sulfur-based cathode and a silicon oxide-based anode and proposed as an innovative energy-storage system. The sulfur-carbon composite, which exploits graphene carbon with a 3 D array (3DG-S), was synthesized by a reduction step through a microwave-assisted solvothermal technique and was fully characterized in terms of structure and morphology, thereby revealing suitable features for lithium-cell application. Electrochemical tests of the 3DG-S electrode in a lithium half-cell indicated a capacity ranging from 1200 to 1000 mAh g -1 at currents of C/10 and 1 C, respectively. Remarkably, the Li-alloyed anode, namely, Li y SiO x -C prepared by the sol-gel method and lithiated by surface treatment, showed suitable performance in a lithium half-cell by using an electrolyte designed for lithium-sulfur batteries. The Li y SiO x -C/3DG-S battery was found to exhibit very promising properties with a capacity of approximately 460 mAh g S -1 delivered at an average voltage of approximately 1.5 V over 200 cycles, suggesting that the characterized materials would be suitable candidates for low-cost and high-energy-storage applications. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Hierarchical FeTiO3-TiO2 hollow spheres for efficient simulated sunlight-driven water oxidation.

PubMed

Han, Taoran; Chen, Yajie; Tian, Guohui; Wang, Jian-Qiang; Ren, Zhiyu; Zhou, Wei; Fu, Honggang

2015-10-14

Oxygen generation is the key step for the photocatalytic overall water splitting and considered to be kinetically more challenging than hydrogen generation. Here, an effective water oxidation catalyst of hierarchical FeTiO3-TiO2 hollow spheres are prepared via a two-step sequential solvothermal processes and followed by thermal treatment. The existence of an effective heterointerface and built-in electric field in the surface space charge region in FeTiO3-TiO2 hollow spheres plays a positive role in promoting the separation of photoinduced electron-hole pairs. Surface photovoltage, transient-state photovoltage, fluorescence and electrochemical characterization are used to investigate the transfer process of photoinduced charge carriers. The photogenerated charge carriers in the hierarchical FeTiO3-TiO2 hollow spheres with a proper molar ratio display much higher separation efficiency and longer lifetime than those in the FeTiO3 alone. Moreover, it is suggested that the hierarchical porous hollow structure can contribute to the enhancement of light utilization, surface active sites and material transportation through the framework walls. This specific synergy significantly contributes to the remarkable improvement of the photocatalytic water oxidation activity of the hierarchical FeTiO3-TiO2 hollow spheres under simulated sunlight (AM1.5).

Evaluation of one-step luminescent cyanoacrylate fuming.

PubMed

Khuu, Alicia; Chadwick, Scott; Spindler, Xanthe; Lam, Rolanda; Moret, Sébastien; Roux, Claude

2016-06-01

One-step luminescent cyanoacrylates have recently been introduced as an alternative to the conventional cyanoacrylate fuming methods. These new techniques do not require the application of a luminescent post-treatment in order to enhance cyanoacrylate-developed fingermarks. In this study, three one-step polymer cyanoacrylates: CN Yellow Crystals (Aneval Inc.), PolyCyano UV (Foster+Freeman Ltd.) and PECA Multiband (BVDA), and one monomer cyanoacrylate: Lumikit™ (Crime Scene Technology), were evaluated against a conventional two-step cyanoacrylate fuming method (Cyanobloom (Foster+Freeman Ltd.) with rhodamine 6G stain). The manufacturers' recommended conditions or conditions compatible with the MVC™ 1000/D (Foster+Freeman Ltd.) were assessed with fingermarks aged for up to 8 weeks on non-porous and semi-porous substrates. Under white light, Cyanobloom generally gave better development than the one-step treatments across the substrates. Similarly when viewed under the respective luminescent conditions, Cyanobloom with rhodamine 6G stain resulted in improved contrast against the one-step treatments except on polystyrene, where PolyCyano UV and PECA Multiband gave better visualisation. Rhodamine 6G post-treatment of one-step samples did not significantly enhance the contrast of any of the one-step treatments against Cyanobloom/rhodamine 6G-treated samples. Copyright © 2016 Elsevier Ireland Ltd. All rights reserved.

Single step synthesis of high-purity CoO nanocrystals.

PubMed

Yang, Huaming; Ouyang, Jing; Tang, Aidong

2007-07-19

Both octahedral and slice-shaped cubic cobalt monoxide (CoO) nanocrystals with narrow size distributions have been successfully synthesized by a simple solvothermal route. It was found that conditions of the solvothermal treatment showed obvious effects on the formation and purity of the as-synthesized CoO nanocrystals, only when cobalt acetate was used as the cobalt source and when temperature reached 190 degrees C could CoO be produced; also, freeze-drying was necessary for obtaining pure CoO. Size of the CoO nanocrystals varied from 30 to 130 nm. Morphology of the products could be controlled by simply changing the type of surfactant in solvent, and the octahedral CoO nanocrystals showed rounded turns. Purity of the products was detected by intensive X-ray photoelectron spectroscopy (XPS) investigation and Fourier transform infrared spectroscopy (FTIR) combined with differential scanning calorimetry/thermal gravity (DSC/TG). The results indicated an absence of unexpected trivalence cobalt series on surface of the samples, thanks to the protection of the surface by trace amount of carbonate ions, adsorbed hydroxylation, and surfactant with a maximum thickness of 2 nm, which were proved by high-resolution transmission electron microscopy (HRTEM). The as-synthesized CoO nanoparticles were added into positive electrode of Ni/MH batteries, and discharge/charge cycling tests were performed under different rates from 0.1C to 5.0C. The results indicated that the specific capacities of batteries with addition of 5% octahedral or slice CoO nanocrystals at 0.1C were 393.3 and 318.1 mAh/g, respectively, which were higher than that without CoO (269.2mAh/g). Specific capacity of battery with addition of 5% octahedral CoO nanocrystals was 40% higher than that without CoO at 5.0C. Octahedral CoO nanocrystals show better electrochemical activity than slice CoO and indicate interesting potential in the field of electrochemical application.

Single-Crystalline Ultrathin Co 3O 4 Nanosheets with Massive Vacancy Defects for Enhanced Electrocatalysis

DOE PAGES

Cai, Zhao; Bi, Yongmin; Hu, Enyuan; ...

2017-09-18

The role of vacancy defects is demonstrated to be positive in various energy-related processes. However, introducing vacancy defects into single-crystalline nanostructures with given facets and studying their defect effect on electrocatalytic properties remains a great challenge. Here this paper deliberately introduces oxygen defects into single-crystalline ultrathin Co 3O 4 nanosheets with O-terminated {111} facets by mild solvothermal reduction using ethylene glycol under alkaline condition. As-prepared defect-rich Co 3O 4 nanosheets show a low overpotential of 220 mV with a small Tafel slope of 49.1 mV dec -1 for the oxygen evolution reaction (OER), which is among the best Co-based OERmore » catalysts to date and even more active than the state-of-the-art IrO 2 catalyst. Such vacancy defects are formed by balancing with reducing environments under solvothermal conditions, but are surprisingly stable even after 1000 cycles of scanning under OER working conditions. Density functional theory plus U calculation attributes the enhanced performance to the oxygen vacancies and consequently exposed second-layered Co metal sites, which leads to the lowered OER activation energy of 2.26 eV and improved electrical conductivity. Finally, this mild solvothermal reduction concept opens a new door for the understanding and future designing of advanced defect-based electrocatalysts.« less

Direct Solvothermal Liquefaction of Pennisetum purpureum Biomass to Produce Biocrude Using Ethanol Solvent

NASA Astrophysics Data System (ADS)

Adriane Ochiai, Mikael; Marrod Cruz, Salvador; Oporto, Louiellyn; de Leon, Rizalinda

2018-03-01

Direct solvothermal liquefaction was used in converting the lignocellulosic biomass, Pennisetum purpureum or Napier grass using ethanol as solvent. Liquefaction of Napier grass resulted in a dark and viscous bio-crude product and exhibited promising yields (34.6377% to 48.6267%). It was determined that the effects of temperature and residence time were statistically significant with the residence time having the greatest positive effect on yield. High yields of bio-crude from Napier grass seem to occur when solvothermal temperature, residence time increased and as solids ratio decreased. However, elemental analysis showed that the bio-crude produced needs to undergo deoxygenation (O: 14.25 - 49.42%) before mixing with petroleum. For the higher heating value (HHV), the parameters observed in the study were statistically insignificant, however, temperature was determined to have the greatest positive effect on HHV. It was observed that high HHV bio-crude were produced at high temperatures, low solids ratio, and low residence times. The acquired averages for the HHV (20.0333 MJ/kg to 29.7744 MJ/kg) were all higher than the HHV of the Napier grass sample used in the study (12.9394 MJ/kg). It was observed in the study, that even though solids ratio has the least effect on both responses, the choice of solids ratio is dependent on its interaction effects with the other parameters as its effects contribute to the observed responses.

The growth of high density network of MOF nano-crystals across macroporous metal substrates - Solvothermal synthesis versus rapid thermal deposition

NASA Astrophysics Data System (ADS)

Maina, James W.; Gonzalo, Cristina Pozo; Merenda, Andrea; Kong, Lingxue; Schütz, Jürg A.; Dumée, Ludovic F.

2018-01-01

Fabrication of metal organic framework (MOF) films and membranes across macro-porous metal substrates is extremely challenging, due to the large pore sizes across the substrates, poor wettability, and the lack of sufficient reactive functional groups on the surface, which prevent high density nucleation of MOF crystals. Herein, macroporous stainless steel substrates (pore size 44 × 40 μm) are functionalized with amine functional groups, and the growth of ZIF-8 crystals investigated through both solvothermal synthesis and rapid thermal deposition (RTD), to assess the role of synthesis routes in the resultant membranes microstructure, and subsequently their performance. Although a high density of well interconnected MOF crystals was observed across the modified substrates following both techniques, RTD was found to be a much more efficient route, yielding high quality membranes under 1 h, as opposed to the 24 h required for solvothermal synthesis. The RTD membranes also exhibited high gas permeance, with He permeance of up to 2.954 ± 0.119 × 10-6 mol m-2 s-1 Pa-1, and Knudsen selectivities for He/N2, Ar/N2 and CO2/N2, suggesting the membranes were almost defect free. This work opens up route for efficient fabrication of MOF films and membranes across macro-porous metal supports, with potential application in electrically mediated separation applications.

Single-Crystalline Ultrathin Co 3O 4 Nanosheets with Massive Vacancy Defects for Enhanced Electrocatalysis

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

Cai, Zhao; Bi, Yongmin; Hu, Enyuan

The role of vacancy defects is demonstrated to be positive in various energy-related processes. However, introducing vacancy defects into single-crystalline nanostructures with given facets and studying their defect effect on electrocatalytic properties remains a great challenge. Here this paper deliberately introduces oxygen defects into single-crystalline ultrathin Co 3O 4 nanosheets with O-terminated {111} facets by mild solvothermal reduction using ethylene glycol under alkaline condition. As-prepared defect-rich Co 3O 4 nanosheets show a low overpotential of 220 mV with a small Tafel slope of 49.1 mV dec -1 for the oxygen evolution reaction (OER), which is among the best Co-based OERmore » catalysts to date and even more active than the state-of-the-art IrO 2 catalyst. Such vacancy defects are formed by balancing with reducing environments under solvothermal conditions, but are surprisingly stable even after 1000 cycles of scanning under OER working conditions. Density functional theory plus U calculation attributes the enhanced performance to the oxygen vacancies and consequently exposed second-layered Co metal sites, which leads to the lowered OER activation energy of 2.26 eV and improved electrical conductivity. Finally, this mild solvothermal reduction concept opens a new door for the understanding and future designing of advanced defect-based electrocatalysts.« less

Highly Efficient Production of Soluble Proteins from Insoluble Inclusion Bodies by a Two-Step-Denaturing and Refolding Method

PubMed Central

Zhang, Yan; Zhang, Ting; Feng, Yanye; Lu, Xiuxiu; Lan, Wenxian; Wang, Jufang; Wu, Houming; Cao, Chunyang; Wang, Xiaoning

2011-01-01

The production of recombinant proteins in a large scale is important for protein functional and structural studies, particularly by using Escherichia coli over-expression systems; however, approximate 70% of recombinant proteins are over-expressed as insoluble inclusion bodies. Here we presented an efficient method for generating soluble proteins from inclusion bodies by using two steps of denaturation and one step of refolding. We first demonstrated the advantages of this method over a conventional procedure with one denaturation step and one refolding step using three proteins with different folding properties. The refolded proteins were found to be active using in vitro tests and a bioassay. We then tested the general applicability of this method by analyzing 88 proteins from human and other organisms, all of which were expressed as inclusion bodies. We found that about 76% of these proteins were refolded with an average of >75% yield of soluble proteins. This “two-step-denaturing and refolding” (2DR) method is simple, highly efficient and generally applicable; it can be utilized to obtain active recombinant proteins for both basic research and industrial purposes. PMID:21829569

Detection of canine distemper virus (CDV) through one step RT-PCR combined with nested PCR.

PubMed

Kim, Y H; Cho, K W; Youn, H Y; Yoo, H S; Han, H R

2001-04-01

A one step reverse transcription PCR (RT-PCR) combined nested PCR was set up to increase efficiency in the diagnosis of canine distemper virus (CDV) infection after developement of nested PCR. Two PCR primer sets were designed based on the sequence of nucleocapsid gene of CDV Onderstepoort strain. One-step RT-PCR with the outer primer pair was revealed to detect 10(2) PFU/ml. The sensitivity was increased hundredfold using the one-step RT-PCR combined with the nested PCR. Specificity of the PCR was also confirmed using other related canine virus and peripheral blood mononuclear cells (PBMC) and body secretes of healthy dogs. Of the 51 blood samples from dogs clinically suspected of CD, 45 samples were revealed as positive by one-step RT-PCR combined with nested PCR. However, only 15 samples were identified as positive with a single one step RT-PCR. Therefore approximately 60% increase in the efficiency of the diagnosis was observed by the combined method. These results suggested that one step RT-PCR combined with nested PCR could be a sensitive, specific, and practical method for diagnosis of CDV infection.

A new member of ferrous sulfates, FeSO{sub 4}·2H{sub 2}O with PtS topology showing spin-canted long-range antiferromagnetic ordering

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

Zhao, Long; Liu, Wei, E-mail: weiliu@ouc.edu.cn; Cao, Lixin

2015-11-15

A sanderite ferrous sulfate FeSO{sub 4}·2H{sub 2}O has been synthesized by the hydro/solvothermal method. Its crystal structure (Pccn, a=6.3160 Å, b=7.7550 Å, c=8.9880 Å, V=440.2 Å{sup 3}, Z=4) can be regarded as the condensation of alternately corner-shared FeO{sub 4}(H{sub 2}O){sub 2} octahedra and SO{sub 4} tetrahedra with a similar topology of PtS. By structural comparison with the known hydrated ferrous sulfates, the structural relation among them has been noted and discussed in detail. A variable temperature magnetic study shows a spin-canted long-range antiferromagnetic ordering in the low temperature regime, which might result from a possible phase transition during the coolingmore » from the high temperature. - Graphical abstract: As a new number of ferrous sulfates, sanderite FeSO{sub 4}·2H{sub 2}O has been synthesized under hydro/solvothermal conditions, which exhibits a similar topology of PtS. - Highlights: • Sanderite ferrous sulfate has been synthesized. • The topology of its structure is similar to that of PtS. • A structural relation between these hydrated ferrous sulfates is discovered.« less

Solvothermal synthesis, electromagnetic and electrochemical properties of jellylike cylinder graphene-Mn3O4 composite with highly coupled effect

NASA Astrophysics Data System (ADS)

Long, Yuting; Xie, Junliang; Li, Hong; Liu, Zirui; Xie, Yahong

2017-12-01

Jellylike cylinder graphene-Mn3O4 composite with highly coupled effect was successfully synthesized by a simple solvothermal process. Without using toxic reducing agent and expensive equipment, this method is environmental compatible and suitable for low cost mass production. High capacitance Mn3O4 nanoparticles are homogeneously anchored on excellent conductivity graphene framework and a growth mechanism is hypothesized. Excellent electron conductivity and unique structure of Mn3O4-graphene composite give rise to various applications such as microwave absorber and electrode material. As a microwave absorber, the composite exhibits lowest reflection loss of -14.2 dB in the frequency range of 2-18 GHz. Good microwave absorption performance is due to the structure of the composite where conductive channels form between nano sized Mn3O4 and high conductivity graphene with defects and dangling bonds. As for electrochemical property, Mn3O4-graphene composite with coupled effect shows excellent performance with highest specific capacitance of 246.7 F g-1 in saturated K2SO4 at a scan rate of 5 mV s-1. Good electrochemical property is also attributed to the structure with high utilization of Mn3O4, fast charge carrier transmission, and excellent electronic conductivity. This composite shows a promising application in absorbing materials and electrodes.

Solvothermal synthesis of platinum alloy nanoparticles for oxygen reduction electrocatalysis.

PubMed

Carpenter, Michael K; Moylan, Thomas E; Kukreja, Ratandeep Singh; Atwan, Mohammed H; Tessema, Misle M

2012-05-23

Platinum alloy nanoparticles show great promise as electrocatalysts for the oxygen reduction reaction (ORR) in fuel cell cathodes. We report here on the use of N,N-dimethylformamide (DMF) as both solvent and reductant in the solvothermal synthesis of Pt alloy nanoparticles (NPs), with a particular focus on Pt-Ni alloys. Well-faceted alloy nanocrystals were generated with this method, including predominantly cubic and cuboctahedral nanocrystals of Pt(3)Ni, and octahedral and truncated octahedral nanocrystals of PtNi. X-ray diffraction (XRD) and high angle annular dark field scanning transmission electron microscopy (HAADF-STEM), coupled with energy dispersive spectroscopy (EDS), were used to characterize crystallite morphology and composition. ORR activities of the alloy nanoparticles were measured with a rotating disk electrode (RDE) technique. While some Pt(3)Ni alloy nanoparticle catalysts showed specific activities greater than 1000 μA/cm(2)(Pt), alloy catalysts prepared with a nominal composition of PtNi displayed activities close to 3000 μA/cm(2)(Pt), or almost 15 times that of a state-of-the-art Pt/carbon catalyst. XRD and EDS confirmed the presence of two NP compositions in this catalyst. HAADF-STEM examination of the PtNi nanoparticle catalyst after RDE testing revealed the development of hollows in a number of the nanoparticles due to nickel dissolution. Continued voltage cycling caused further nickel dissolution and void formation, but significant activity remained even after 20,000 cycles.

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

Polyvinylpyrrolidone adsorption effects on the morphologies of synthesized platinum particles and its catalytic activity

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

Ooi, Mahayatun Dayana Johan; Aziz, Azlan Abdul; Nanobiotechnology Research and Innovation

Flower-like Platinum micro-structures were synthesized from different concentration of the PVP using solvothermal method. At 5.0×10{sup −3} mmol of PVP, well-defined flower-like pattern consists of triangular petals radiating from the centre were produced whereas larger flower network developed at higher PVP concentration. High degree of crystallinity was obtained upon each increment of PVP. The well defined flower like pattern synthesized using 5.0×10{sup −3} mmol PVP exhibit the highest catalytic activity and stability towards electro-oxidation of formic acid.

Comparative studies of electrochemical properties of carbon nanotubes and nanostructured boron carbide

NASA Astrophysics Data System (ADS)

Singh, Paviter; Kaur, Gurpreet; Singh, Kulwinder; Singh, Bikramjeet; Kaur, Manjot; Kumar, Manjeet; Bala, Rajni; Kumar, Akshay

2018-05-01

Boron carbide (B4C) and carbon nanotubes (CNTs) have the potential to act as electrocatalyst as these material show bifunctional behavior. B4C and CNTs were synthesized using solvothermal method. B4C display great catalytic activity as compared to CNTs. Raman spectra confirmed the formation of nanostructured carbon nanotubes. The observed onset potential was smaller 1.58 V in case of B4C as compared to CNTs i.e. 1.96 V in cyclic voltammetry. B4C material can emerge as a promising bifunctional electrocatalyst for battery applications.

Highly reusability surface loaded metal particles magnetic catalyst microspheres (MCM-MPs) for treatment of dye-contaminated water

NASA Astrophysics Data System (ADS)

Liu, Ying; Zhang, Kun; Yin, Xiaoshuang; Yang, Wenzhong; Zhu, Hongjun

2016-04-01

The metal-deposited magnetic catalyst microspheres (MCM-MPs) were successfully synthesized by one facile, high yield and controllable approach. Here, the bare magnetic microspheres were firstly synthesized according to the solvothermal method. Then silica shell were coated on the surface of the magnetic microspheres via sol-gel method, and subsequently with surface modifying with amino in the purpose to form SiO2-NH2 shell. Thus, metal particles were easily adsorbed into the SiO2-NH2 shell and in-situ reduced by NaBH4 solution. All the obtained products (MCM-Cu, MCM-Ag, MCM-Pd) which were monodisperse and constitutionally stable were exhibited high magnetization and excellent catalytic activity towards dyes solution reduction. The catalytic rate ratio of MCM-Pd: MCM-Cu: MCM-Ag could be 10:3:1. Besides, some special coordination compound Cu2(OH)3Br had been generated in the in-situ reduced process of MCM-Cu, which produced superior cyclical stability (>20 times) than that of MCM-Ag and MCM-Pd. In all, those highly reusability and great catalytic efficiency of MCM-MPs show promising and great potential for treatment of dye-contaminated water.

Multiwalled carbon nanotube@a-C@Co9S8 nanocomposites: a high-capacity and long-life anode material for advanced lithium ion batteries

NASA Astrophysics Data System (ADS)

Zhou, Yanli; Yan, Dong; Xu, Huayun; Liu, Shuo; Yang, Jian; Qian, Yitai

2015-02-01

A one-dimensional MWCNT@a-C@Co9S8 nanocomposite has been prepared via a facile solvothermal reaction followed by a calcination process. The amorphous carbon layer between Co9S8 and MWCNT acts as a linker to increase the loading of sulfides on MWCNT. When evaluated as anode materials for lithium ion batteries, the MWCNT@a-C@Co9S8 nanocomposite shows the advantages of high capacity and long life, superior to Co9S8 nanoparticles and MWCNT@Co9S8 nanocomposites. The reversible capacity could be retained at 662 mA h g-1 after 120 cycles at 1 A g-1. The efficient synthesis and excellent performances of this nanocomposite offer numerous opportunities for other sulfides as a new anode for lithium ion batteries.A one-dimensional MWCNT@a-C@Co9S8 nanocomposite has been prepared via a facile solvothermal reaction followed by a calcination process. The amorphous carbon layer between Co9S8 and MWCNT acts as a linker to increase the loading of sulfides on MWCNT. When evaluated as anode materials for lithium ion batteries, the MWCNT@a-C@Co9S8 nanocomposite shows the advantages of high capacity and long life, superior to Co9S8 nanoparticles and MWCNT@Co9S8 nanocomposites. The reversible capacity could be retained at 662 mA h g-1 after 120 cycles at 1 A g-1. The efficient synthesis and excellent performances of this nanocomposite offer numerous opportunities for other sulfides as a new anode for lithium ion batteries. Electronic supplementary information (ESI) available: Infrared spectrogram (IR) of glucose treated MWCNT; TEM images of MWCNT@a-C treated by different concentrations of glucose; SEM and TEM images of the intermediate product obtained from the solvothermal reaction between thiourea and Co(Ac)2; EDS spectrum of MWCNT@a-C@Co9S8 composites; SEM and TEM images of MWCNT@Co9S8 nanocomposites obtained without the hydrothermal treatment by glucose; SEM and TEM images of Co9S8 nanoparticles; Galvanostatic discharge-charge profiles and cycling performance of MWCNT@a-C; TEM images of the anode material at different state of charge (SOC) and depth of discharge (DOD); the comparison of cycling performances of reported cobalt sulfide nanocomposites. See DOI: 10.1039/c4nr07143c

Formation of randomly distributed nano-tubes, -rods and -plates of n-type and p-type bismuth telluride via molecular legation

NASA Astrophysics Data System (ADS)

Ram, Jasa; Ghosal, Partha

2015-08-01

Randomly distributed nanotubes, nanorods and nanoplates of Bi0.5Sb1.5Te3 and Bi2Te2.7Se0.3 ternary compounds have been synthesized via a high yield solvo-thermal process. Prior to solvo-thermal heating at 230 °C for crystallization, we ensured molecular legation in room temperature reaction by complete reduction of precursor materials, dissolved in ethylene glycol and confirmed it by replicating Raman spectra of amorphous and crystalline materials. These nanomaterials have also been characterized using XRD, FE-SEM, EDS and TEM. Possible formation mechanism is also discussed. This single process will enable development of thermoelectric modules and random distribution of diverse morphology will be beneficial in retaining nano-crystallite sizes.

Dependency of magnetic microwave absorption on surface architecture of Co20Ni80 hierarchical structures studied by electron holography

NASA Astrophysics Data System (ADS)

Liu, Qinhe; Xu, Xianhui; Xia, Weixing; Che, Renchao; Chen, Chen; Cao, Qi; He, Jingang

2015-01-01

To design and fabricate rational surface architecture of individual particles is one of the key factors that affect their magnetic properties and microwave absorption capability, which is still a great challenge. Herein, a series of Co20Ni80 hierarchical structures with different surface morphologies, including flower-, urchin-, ball-, and chain-like morphologies, were obtained using structure-directing templates via a facile one-step solvothermal treatment. The microwave reflection loss (RL) of urchin-like Co20Ni80 hierarchical structures reaches as high as -33.5 dB at 3 GHz, with almost twice the RL intensity of the ball- and chain-like structures, and the absorption bandwidth (<-10 dB) is about 5.5 GHz for the flower-like morphology, indicating that the surface nanospikes and nanoflakes on the Co20Ni80 microsphere surfaces have great influences on their magnetic microwave absorption properties. Electron holography analysis reveals that the surface nanospikes and nanoflakes could generate a high density of stray magnetic flux lines and contribute a large saturation magnetization (105.62 emu g-1 for urchin-like and 96.41 emu g-1 for flower-like morphology), leading the urchin-like and flower-like Co20Ni80 to possess stronger microwave RL compared with the ball-like and chain-like Co20Ni80 alloys. The eddy-current absorption mechanism μ''(μ')-2(f)-1 is dominant in the frequency region above 8 GHz, implying that eddy-current loss is a vital factor for microwave RL in the high frequency range. It can be supposed from our findings that different surface morphologies of magnetic hierarchical structures might become an effective path to achieve high-performance microwave absorption for electromagnetic shielding and stealth camouflage applications.To design and fabricate rational surface architecture of individual particles is one of the key factors that affect their magnetic properties and microwave absorption capability, which is still a great challenge. Herein, a series of Co20Ni80 hierarchical structures with different surface morphologies, including flower-, urchin-, ball-, and chain-like morphologies, were obtained using structure-directing templates via a facile one-step solvothermal treatment. The microwave reflection loss (RL) of urchin-like Co20Ni80 hierarchical structures reaches as high as -33.5 dB at 3 GHz, with almost twice the RL intensity of the ball- and chain-like structures, and the absorption bandwidth (<-10 dB) is about 5.5 GHz for the flower-like morphology, indicating that the surface nanospikes and nanoflakes on the Co20Ni80 microsphere surfaces have great influences on their magnetic microwave absorption properties. Electron holography analysis reveals that the surface nanospikes and nanoflakes could generate a high density of stray magnetic flux lines and contribute a large saturation magnetization (105.62 emu g-1 for urchin-like and 96.41 emu g-1 for flower-like morphology), leading the urchin-like and flower-like Co20Ni80 to possess stronger microwave RL compared with the ball-like and chain-like Co20Ni80 alloys. The eddy-current absorption mechanism μ''(μ')-2(f)-1 is dominant in the frequency region above 8 GHz, implying that eddy-current loss is a vital factor for microwave RL in the high frequency range. It can be supposed from our findings that different surface morphologies of magnetic hierarchical structures might become an effective path to achieve high-performance microwave absorption for electromagnetic shielding and stealth camouflage applications. Electronic supplementary information (ESI) available: EDS analysis data, SEM images, electron holography schematic diagram, electron holography and magnetic hysteresis loops. See DOI: 10.1039/c4nr05547k

Enhanced capillary electrophoretic screening of Alzheimer based on direct apolipoprotein E genotyping and one-step multiplex PCR.

PubMed

Woo, Nain; Kim, Su-Kang; Sun, Yucheng; Kang, Seong Ho

2018-01-01

Human apolipoprotein E (ApoE) is associated with high cholesterol levels, coronary artery disease, and especially Alzheimer's disease. In this study, we developed an ApoE genotyping and one-step multiplex polymerase chain reaction (PCR) based-capillary electrophoresis (CE) method for the enhanced diagnosis of Alzheimer's. The primer mixture of ApoE genes enabled the performance of direct one-step multiplex PCR from whole blood without DNA purification. The combination of direct ApoE genotyping and one-step multiplex PCR minimized the risk of DNA loss or contamination due to the process of DNA purification. All amplified PCR products with different DNA lengths (112-, 253-, 308-, 444-, and 514-bp DNA) of the ApoE genes were analyzed within 2min by an extended voltage programming (VP)-based CE under the optimal conditions. The extended VP-based CE method was at least 120-180 times faster than conventional slab gel electrophoresis methods In particular, all amplified DNA fragments were detected in less than 10 PCR cycles using a laser-induced fluorescence detector. The detection limits of the ApoE genes were 6.4-62.0pM, which were approximately 100-100,000 times more sensitive than previous Alzheimer's diagnosis methods In addition, the combined one-step multiplex PCR and extended VP-based CE method was also successfully applied to the analysis of ApoE genotypes in Alzheimer's patients and normal samples and confirmed the distribution probability of allele frequencies. This combination of direct one-step multiplex PCR and an extended VP-based CE method should increase the diagnostic reliability of Alzheimer's with high sensitivity and short analysis time even with direct use of whole blood. Copyright © 2017 Elsevier B.V. All rights reserved.

Surface energy and surface stress on vicinals by revisiting the Shuttleworth relation

NASA Astrophysics Data System (ADS)

Hecquet, Pascal

2018-04-01

In 1998 [Surf. Sci. 412/413, 639 (1998)], we showed that the step stress on vicinals varies as 1/L, L being the distance between steps, while the inter-step interaction energy primarily follows the law as 1/L2 from the well-known Marchenko-Parshin model. In this paper, we give a better understanding of the interaction term of the step stress. The step stress is calculated with respect to the nominal surface stress. Consequently, we calculate the diagonal surface stresses in both the vicinal system (x, y, z) where z is normal to the vicinal and the projected system (x, b, c) where b is normal to the nominal terrace. Moreover, we calculate the surface stresses by using two methods: the first called the 'Zero' method, from the surface pressure forces and the second called the 'One' method, by homogeneously deforming the vicinal in the parallel direction, x or y, and by calculating the surface energy excess proportional to the deformation. By using the 'One' method on the vicinal Cu(0 1 M), we find that the step deformations, due to the applied deformation, vary as 1/L by the same factor for the tensor directions bb and cb, and by twice the same factor for the parallel direction yy. Due to the vanishing of the surface stress normal to the vicinal, the variation of the step stress in the direction yy is better described by using only the step deformation in the same direction. We revisit the Shuttleworth formula, for while the variation of the step stress in the direction xx is the same between the two methods, the variation in the direction yy is higher by 76% for the 'Zero' method with respect to the 'One' method. In addition to the step energy, we confirm that the variation of the step stress must be taken into account for the understanding of the equilibrium of vicinals when they are not deformed.

A comparison of artificial compressibility and fractional step methods for incompressible flow computations

NASA Technical Reports Server (NTRS)

Chan, Daniel C.; Darian, Armen; Sindir, Munir

1992-01-01

We have applied and compared the efficiency and accuracy of two commonly used numerical methods for the solution of Navier-Stokes equations. The artificial compressibility method augments the continuity equation with a transient pressure term and allows one to solve the modified equations as a coupled system. Due to its implicit nature, one can have the luxury of taking a large temporal integration step at the expense of higher memory requirement and larger operation counts per step. Meanwhile, the fractional step method splits the Navier-Stokes equations into a sequence of differential operators and integrates them in multiple steps. The memory requirement and operation count per time step are low, however, the restriction on the size of time marching step is more severe. To explore the strengths and weaknesses of these two methods, we used them for the computation of a two-dimensional driven cavity flow with Reynolds number of 100 and 1000, respectively. Three grid sizes, 41 x 41, 81 x 81, and 161 x 161 were used. The computations were considered after the L2-norm of the change of the dependent variables in two consecutive time steps has fallen below 10(exp -5).

A two-step non-flowcytometry-based naïve B cell isolation method and its application in Staphylococcal enterotoxin B (SEB) presentation.

PubMed

Chokeshai-u-saha, Kaj; Buranapraditkun, Supranee; Jacquet, Alain; Nguyen, Catherine; Ruxrungtham, Kiat

2012-09-01

To study the role of human naïve B cells in antigen presentation and stimulation to naïve CD4+ T cell, a suitable method to reproducibly isolate sufficient naïve B cells is required. To improve the purity of isolated naive B cells obtained from a conventional one-step magnetic bead method, we added a rosetting step to enrich total B cell isolates from human whole blood samples prior to negative cell sorting by magnetic beads. The acquired naïve B cells were analyzed for phenotypes and for their role in Staphylococcal enterotoxin B (SEB) presentation to naïve CD4+ T cells. The mean (SD) naïve B cell (CD19+/CD27-) purity obtained from this two-step method compared with the one-step method was 97% (1.0) versus 90% (1.2), respectively. This two-step method can be used with a sample of whole blood as small as 10 ml. The isolated naive B cells were phenotypically at a resting state and were able to prime naïve CD4+ T cell activation by Staphylococcal enterotoxin B (SEB) presentation. This two-step non-flow cytometry-based approach improved the purity of isolated naïve B cells compared with conventional one-step magnetic bead method. It also worked well with a small blood volume. In addition, this study showed that the isolated naïve B cells can present a super-antigen "SEB" to activate naïve CD4 cells. These methods may thus be useful for further in vitro characterization of human naïve B cells and their roles as antigen presenting cells in various diseases.

Copper-Based Metal-Organic Framework Nanoparticles with Peroxidase-Like Activity for Sensitive Colorimetric Detection of Staphylococcus aureus.

PubMed

Wang, Shuqin; Deng, Wenfang; Yang, Lu; Tan, Yueming; Xie, Qingji; Yao, Shouzhuo

2017-07-26

Cu-MOF nanoparticles with an average diameter of 550 nm were synthesized from 2-aminoterephthalic acid and Cu(NO 3 ) 2 by a mixed solvothermal method. The Cu-MOF nanoparticles can show peroxidase-like activity that can catalyze 3,3',5,5'-tetramethylbenzidine to produce a yellow chromogenic reaction in the presence of H 2 O 2 . The presence of abundant amine groups on the surfaces of Cu-MOF nanoparticles enables facile modification of Staphylococcus aureus (S. aureus) aptamer on Cu-MOF nanoparticles. By combining Cu-MOF-catalyzed chromogenic reaction with aptamer recognition and magnetic separation, a simple, sensitive, and selective colorimetric method for the detection of S. aureus was developed.

Fabrication and applications of copper sulfide (CuS) nanostructures

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

Shamraiz, Umair, E-mail: umairshamraiz@gmail.com; Hussain, Raja Azadar, E-mail: hussainazadar@gamil.com; Badshah, Amin, E-mail: aminbadshah@yahoo.com

2016-06-15

This review article presents different fabrication procedures (under the headlines of solvothermal routes, aerosol methods, solution methods and thermolysis), and applications (photocatalytic degradation, ablation of cancer cells, electrode material in lithium ion batteries and in gas sensing, organic solar cells, field emission properties, super capacitor applications, photoelectrochemical performance of QDSCs, photocatalytic reduction of organic pollutants, electrochemical bio sensing, enhanced PEC characteristics of pre-annealed CuS film electrodes) of copper sulfide (Covellite). - Highlights: • This review article presents the synthesis and applications of copper sulfide. • CuS has been used over the years for different applications in nanoscience. • Different syntheticmore » protocols are followed for their preparation which help in the possible modifications in the morphology of CuS.« less

Facile synthesis of amine-functional reduced graphene oxides as modified quick, easy, cheap, effective, rugged and safe adsorbent for multi-pesticide residues analysis of tea.

PubMed

Ma, Guicen; Zhang, Minglu; Zhu, Li; Chen, Hongping; Liu, Xin; Lu, Chengyin

2018-01-05

Amine-functional reduced graphene oxide (amine-rGO) with different carbon chain length amino groups were successfully synthesized. The graphene oxides (GO) reduction as well as amino grafting were achieved simultaneously in one step via a facile solvothermal synthetic strategy. The obtained materials were characterized by X-ray diffraction, Raman spectroscopy, Fourier-transform infrared spectrometry and X-ray photoelectron spectroscopy to confirm the modification of GO with different amino groups. The adsorption performance of catechins and caffeine from tea acetonitrile extracts on different amine functional rGO samples were evaluated. It was found that tributylamine-functional rGO (tri-BuA-rGO) exhibited the highest adsorption ability for catechins and caffeine compared to GO and other amino group functional rGO samples. It was worth to note that the adsorption capacity of catechins on tri-BuA-rGO was 11 times higher than that of GO (203.7mgg -1 vs 18.7mgg -1 ). Electrostatic interaction, π-π interaction and surface hydrophilic-hydrophobic properties of tri-BuA-rGO played important roles in the adsorption of catechins as well as caffeine. The gravimetric analysis confirmed that the tri-BuA-rGO achieved the highest efficient cleanup preformance compared with traditional dispersive solid phase extraction (dSPE) adsorbents like primary-secondary amine (PSA), graphitized carbon black (GCB) or C18. A multi-pesticides analysis method based on tri-BuA-rGO is validated on 33 representative pesticides in tea using gas chromatography coupled to tandem mass spectrometry or high-performance liquid chromatography coupled with tandem mass spectrometry. The analysis method gave a high coefficient of determination (r 2 >0.99) for each pesticide and satisfactory recoveries in a range of 72.1-120.5%. Our study demonstrated that amine functional rGO as a new type of QuEChERS adsorbent is expected to be widely applied for analysis of pesticides at trace levels. Copyright © 2017 Elsevier B.V. All rights reserved.

Synthesis and magnetic properties of superparamagnetic CoAs nanostructures

NASA Astrophysics Data System (ADS)

Desai, P.; Ashokaan, N.; Masud, J.; Pariti, A.; Nath, M.

2015-03-01

This article provides a comprehensive guide on the synthesis and characterization of superparamagnetic CoAs nanoparticles and elongated nanostructures with high blocking temperature, (TB), via hot-injection precipitation and solvothermal methods. Cobalt arsenides constitute an important family of magnetically active solids that find a variety of applications ranging from magnetic semiconductors to biomedical imaging. While the higher temperature hot-injection precipitation technique (300 °C) yields pure CoAs nanostructures, the lower temperature solvothermal method (200 °C) yields a mixture of CoAs nanoparticles along with other Co-based impurity phases. The synthesis in all these cases involved usage of triphenylarsine ((C6H5)3As) as the As precursor which reacts with solid Co2(CO)8 by ligand displacement to yield a single source precursor. The surfactant, hexadecylamine (HDA) further assists in controlling the morphology of the nanostructures. HDA also provides a basic medium and molten flux-like conditions for the redox chemistry to occur between Co and As at elevated temperatures. The influence of the length of reaction time was investigated by studying the evolution of product morphology over time. It was observed that while spontaneous nucleation at higher temperature followed by controlled growth led to the predominant formation of short nanorods, with longer reaction time, the nanorods were further converted to nanoparticles. The size of the nanoparticles obtained, was mostly in the range of 10-15 nm. The key finding of this work is exceptionally high coercivity in CoAs nanostructures for the first time. Coercivity observed was as high as 0.1 T (1000 Oe) at 2 K. These kinds of magnetic nanostructures find multiple applications in spintronics, whereas the superparamagnetic nanoparticles are viable for use in magnetic storage, ferrofluids and as contrast enhancing agents in MRI.

Photocatalytic study and superparamagnetic nature of Zn-doped MgFe2O4 colloidal size nanocrystals prepared by solvothermal reflux method.

PubMed

Manohar, A; Krishnamoorthi, C

2017-08-01

Biocompatible Mg 1-x Zn x Fe 2 O 4 (x=0.2, 0.4, 0.5, 0.6 & 0.8) nanoparticles were synthesized by solvothermal reflux method. All compounds were crystallized in cubic spinel structure with slightly enhance of lattice parameter with biocompatible substituent Zn 2+ concentration. All compounds were shown spherical geometry with average particle diameter is around 12nm (colloidal size). The spinel structure formation was confirmed by X-ray diffraction,electron diffraction, infrared, Raman shift measurements. Infrared analysis shows oleic acid coating on the surface of nanoparticles and TGA analysis shows that oleic acid desorbs from nanoparticle by decomposition at around 400°C. UV-Vis-NIR spectra show all the compounds show energy band gap in the semiconductor range (≈ 1.9eV). All compounds show superparamagnetic characteristics at room temperature with enhanced saturated mass magnetization (M s ) with Zn 2+ concentration up to x=0.5 and then reduces with further enhance of x up to 0.8. The M s changes were ascribed to occupation of Zn 2+ at tetrahedral sites and proportional enhance of Fe 3+ at octahedral sites. The enhanced Fe 3+ concentration at octahedral sublattice leads to formation Fe 3+ -O 2- -Fe 3+ networks which favor antiferromagnetic interactions due to superexchange phenomenon. Photocatalytic activity of all compounds were studied through methylene blue (MB) degradation analysis. All compounds show ≈ 96% degradation of MB upon 70min irradiation of light on photoreactor vessel. In addition, photocatalytic activity (degradation efficiency) enhances with Zn 2+ concentration in MgFe 2 O 4 . The Zn 2+ substitution enhances both M s and photocatalytic activity biocompatible of MgFe 2 O 4 nanoparticles. Copyright © 2017. Published by Elsevier B.V.

One-step fabrication of multifunctional micromotors

NASA Astrophysics Data System (ADS)

Gao, Wenlong; Liu, Mei; Liu, Limei; Zhang, Hui; Dong, Bin; Li, Christopher Y.

2015-08-01

Although artificial micromotors have undergone tremendous progress in recent years, their fabrication normally requires complex steps or expensive equipment. In this paper, we report a facile one-step method based on an emulsion solvent evaporation process to fabricate multifunctional micromotors. By simultaneously incorporating various components into an oil-in-water droplet, upon emulsification and solidification, a sphere-shaped, asymmetric, and multifunctional micromotor is formed. Some of the attractive functions of this model micromotor include autonomous movement in high ionic strength solution, remote control, enzymatic disassembly and sustained release. This one-step, versatile fabrication method can be easily scaled up and therefore may have great potential in mass production of multifunctional micromotors for a wide range of practical applications.Although artificial micromotors have undergone tremendous progress in recent years, their fabrication normally requires complex steps or expensive equipment. In this paper, we report a facile one-step method based on an emulsion solvent evaporation process to fabricate multifunctional micromotors. By simultaneously incorporating various components into an oil-in-water droplet, upon emulsification and solidification, a sphere-shaped, asymmetric, and multifunctional micromotor is formed. Some of the attractive functions of this model micromotor include autonomous movement in high ionic strength solution, remote control, enzymatic disassembly and sustained release. This one-step, versatile fabrication method can be easily scaled up and therefore may have great potential in mass production of multifunctional micromotors for a wide range of practical applications. Electronic supplementary information (ESI) available: Videos S1-S4 and Fig. S1-S3. See DOI: 10.1039/c5nr03574k

Lightweight reduced graphene oxide-Fe3O4 nanoparticle composite in the quest for an excellent electromagnetic interference shielding material.

PubMed

Singh, Ashwani Kumar; Kumar, Ajit; Haldar, Krishna Kamal; Gupta, Vinay; Singh, Kedar

2018-06-15

This work reports a detailed study of reduced graphene oxide (rGO)-Fe 3 O 4 nanoparticle composite as an excellent electromagnetic (EM) interference shielding material in GHz range. A rGO-Fe 3 O 4 nanoparticle composite was synthesized using a facile, one step, and modified solvothermal method with the reaction of FeCl 3 , ethylenediamine and graphite oxide powder in the presence of ethylene glycol. Various structural, microstructural and optical characterization tools were used to determine its synthesis and various properties. Dielectric, magnetic and EM shielding parameters were also evaluated to estimate its performance as a shielding material for EM waves. X-ray diffraction patterns have provided information about the structural and crystallographic properties of the as-synthesized material. Scanning electron microscopy micrographs revealed the information regarding the exfoliation of graphite into rGO. Well-dispersed Fe 3 O 4 nanoparticles over the surface of the graphene can easily be seen by employing transmission electron microscopy. For comparison, rGO nanosheets and Fe 3 O 4 nanoparticles have also been synthesized and characterized in a similar fashion. A plot of the dielectric and magnetic characterizations provides some useful information related to various losses and the relaxation process. Shielding effectiveness due to reflection (SE R ), shielding effectiveness due to absorption (SE A ), and total shielding effectiveness (SE T ) were also plotted against frequency over a broad range (8-12 GHz). A significant change in all parameters (SE A value from 5 dB to 35 dB for Fe 3 O 4 nanoparticles to rGO-Fe 3 O 4 nanoparticle composite) was found. An actual shielding effectiveness (SE T ) up to 55 dB was found in the rGO-Fe 3 O 4 nanoparticle composite. These graphs give glimpses of how significantly this material shows shielding effectiveness over a broad range of frequency.

Lightweight reduced graphene oxide-Fe3O4 nanoparticle composite in the quest for an excellent electromagnetic interference shielding material

NASA Astrophysics Data System (ADS)

Singh, Ashwani Kumar; Kumar, Ajit; Kamal Haldar, Krishna; Gupta, Vinay; Singh, Kedar

2018-06-01

This work reports a detailed study of reduced graphene oxide (rGO)-Fe3O4 nanoparticle composite as an excellent electromagnetic (EM) interference shielding material in GHz range. A rGO-Fe3O4 nanoparticle composite was synthesized using a facile, one step, and modified solvothermal method with the reaction of FeCl3, ethylenediamine and graphite oxide powder in the presence of ethylene glycol. Various structural, microstructural and optical characterization tools were used to determine its synthesis and various properties. Dielectric, magnetic and EM shielding parameters were also evaluated to estimate its performance as a shielding material for EM waves. X-ray diffraction patterns have provided information about the structural and crystallographic properties of the as-synthesized material. Scanning electron microscopy micrographs revealed the information regarding the exfoliation of graphite into rGO. Well-dispersed Fe3O4 nanoparticles over the surface of the graphene can easily be seen by employing transmission electron microscopy. For comparison, rGO nanosheets and Fe3O4 nanoparticles have also been synthesized and characterized in a similar fashion. A plot of the dielectric and magnetic characterizations provides some useful information related to various losses and the relaxation process. Shielding effectiveness due to reflection (SER), shielding effectiveness due to absorption (SEA), and total shielding effectiveness (SET) were also plotted against frequency over a broad range (8–12 GHz). A significant change in all parameters (SEA value from 5 dB to 35 dB for Fe3O4 nanoparticles to rGO-Fe3O4 nanoparticle composite) was found. An actual shielding effectiveness (SET) up to 55 dB was found in the rGO-Fe3O4 nanoparticle composite. These graphs give glimpses of how significantly this material shows shielding effectiveness over a broad range of frequency.

One-step fabrication of multifunctional micromotors.

PubMed

Gao, Wenlong; Liu, Mei; Liu, Limei; Zhang, Hui; Dong, Bin; Li, Christopher Y

2015-09-07

Although artificial micromotors have undergone tremendous progress in recent years, their fabrication normally requires complex steps or expensive equipment. In this paper, we report a facile one-step method based on an emulsion solvent evaporation process to fabricate multifunctional micromotors. By simultaneously incorporating various components into an oil-in-water droplet, upon emulsification and solidification, a sphere-shaped, asymmetric, and multifunctional micromotor is formed. Some of the attractive functions of this model micromotor include autonomous movement in high ionic strength solution, remote control, enzymatic disassembly and sustained release. This one-step, versatile fabrication method can be easily scaled up and therefore may have great potential in mass production of multifunctional micromotors for a wide range of practical applications.

STEP: What Is It and Should It Be Used for KSC's ISE/CEE Project in the Near Future?

NASA Technical Reports Server (NTRS)

Bareiss, Catherine C.

2000-01-01

The ability to exchange information between different engineering software (i.e, CAD, CAE, CAM) is necessary to aid in collaborative engineering. There are a number of different ways to accomplish this goal. One popular method is to transfer data via different file formats. However this method can lose data and becomes complex as more file formats are added. Another method is to use a standard protocol. STEP is one such standard. This paper gives an overview of STEP, provides a list of where to access more information, and develops guidelines to aid the reader in deciding if STEP is appropriate for his/her use.

Highly biocompatible, nanocrystalline hydroxyapatite synthesized in a solvothermal process driven by high energy density microwave radiation

PubMed Central

Smolen, Dariusz; Chudoba, Tadeusz; Malka, Iwona; Kedzierska, Aleksandra; Lojkowski, Witold; Swieszkowski, Wojciech; Kurzydlowski, Krzysztof Jan; Kolodziejczyk-Mierzynska, Małgorzata; Lewandowska-Szumiel, Małgorzata

2013-01-01

A microwave, solvothermal synthesis of highly biocompatible hydroxyapatite (HAp) nanopowder was developed. The process was conducted in a microwave radiation field having a high energy density of 5 W/mL and over a time less than 2 minutes. The sample measurements included: powder X-ray diffraction, density, specific surface area, and chemical composition. The morphology and structure were investigated by scanning electron microscopy as well as transmission electron microscopy (TEM). The thermal behavior analysis was conducted using a simultaneous thermal analysis technique coupled with quadruple mass spectrometry. Additionally, Fourier transform infrared spectroscopy tests of heated samples were performed. A degradation test and a biocompatibility study in vitro using human osteoblast cells were also conducted. The developed method enables the synthesis of pure, fully crystalline hexagonal HAp nanopowder with a specific surface area close to 240 m2/g and a Ca/P molar ratio equal to 1.57. TEM measurements showed that this method results in particles with an average grain size below 6 nm. A 28-day degradation test conducted according to the ISO standard indicated a 22% loss of initial weight and a calcium ion concentration at 200 μmol/dm3 in the tris(hydroxymethyl)aminomethane hydrochloride test solution. The cytocompatibility of the obtained material was confirmed in a culture of human bone derived cells, both in an indirect test using the material extract, and in direct contact. A quantitative analysis was based on the 2,3-bis-(2-methoxy-4-nitro-5-sulfophenyl)-2H-tetrazolium-5-carboxanilide. Viability assay as well as on DNA content measurements in the PicoGreen test. Indirect observations were performed at one point in time according to the ISO standard for in vitro cytotoxicity (ie, after 24 hours of cell exposure to the extracts). The direct contact tests were completed at three time points: after 24 hours, on day 7, and on day 14 of a culture in an osteogenic medium. All of the tests revealed good tolerance of cells toward the material; this was also shown by means of live/dead fluorescent staining. Both quantitative results and morphological observations revealed much better cell tolerance toward the obtained HAp compared to commercially available HAp NanoXIM, which was used as a reference material. PMID:23431124

Shape-Evolution Control of hybrid perovskite CH3NH3PbI3 crystals via solvothermal synthesis

NASA Astrophysics Data System (ADS)

Zhang, Baohua; Guo, Fuqiang; Yang, Lianhong; Jia, Xiuling; Liu, Bin; Xie, Zili; Chen, Dunjun; Lu, Hai; Zhang, Rong; Zheng, Youdou

2017-02-01

We systematically synthesized CH3NH3PbI3 crystals using solvothermal process, and the reaction conditions such as concentration of the precursor, temperature, time, and lead source have been comprehensively investigated to obtain shape-controlled CH3NH3PbI3 crystals. The results showed that the CH3NH3PbI3 crystals exhibit tetragonal phase and the crystals change from nanoparticles to hopper-faced cuboids. Photoluminescence spectra of the crystals obtained with different lead sources show a blue shift due to the presence of defects in the crystals, and the peak intensity is very sensitive to the lead sources. Moreover, impurities (undesirable byproducts and excess components like HI or CH3NH2) presented during crystal growth can result in hopper growth.

Synthesis of MnFe2O4 magnetic nano hollow spheres by a facile solvothermal route and its characterization

NASA Astrophysics Data System (ADS)

Dey, Chaitali; Chaudhuri, Arka; Goswami, Madhuri Mandal

2018-04-01

Herein, we report the synthesis of manganese ferrite (MnFe2O4) magnetic nano hollow sphere (NHS) by a solvothermal route. Crystalline phase was confirmed by X-ray diffraction (XRD), energy dispersive x-ray (EDX). Magnetic measurements were done in vibrating sample magnetometer (VSM) and morphological structure was analyzed by field emission high resolution scanning electron microscope (FESEM) and structural characterization was confirmed by Fourier transform infrared spectroscopy (FTIR), thermal analysis was performed by thermo-gravimetric analysis-differential thermal analysis (TGA-DTA). The size of the NHS was around 470 nm, this large size may show a potential applicability in industrial application, like dye adsorption, catalysis etc. In addition, because of its ferromagnetic character at room temperature, it can be easily separated by external magnetic field after the application is done.

Solvothermal syntheses and characterization of three new silver(I)/copper(I)-thioarsenates based on As{sup 2+}/As{sup 3+} ions

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

Yao, Hua-Gang, E-mail: hgyao@gdpu.edu.cn; Guangdong Cosmetics Engineering & Technology Research Center, Zhongshan 528458; Tang, Cheng-Fei

2017-02-15

Three new silver(I)/copper(I)-thioarsenates KAgAs{sup II}S{sub 2} (1), RbCu{sub 2}As{sup III}S{sub 3} (2) and RbCu{sub 4}As{sup III}S{sub 4} (3) have been solvothermally synthesized and structurally characterized. 1 exhibits a two-dimensional anionic network built up by As−As bond connecting the left- and right-handed helical [AgS{sub 2}]{sup 4−} chains, and represents the first examples of thioarsenates(II). The structure of 2 consists of two kinds of helical [Cu{sub 2}S{sub 3}]{sup 4–} chains linked by the arsenic atoms to form double layers with rubidium ions between the layers. Compound 3 is built up of infinite [Cu{sub 2}S{sub 2}]{sup 2–} chain and layered [Cu{sub 6}As{sub 2}S{submore » 6}] linked to form a three-dimensional anionic framework, [Cu{sub 4}AsS{sub 4}]{sup –}, and containing channels in which the rubidium cations reside. The optical properties of 1–3 have been investigated by UV–vis spectroscopy. - Graphical abstract: Three new silver(I)/copper(I)-thioarsenates have been solvothermally synthesized and structurally characterized. 1 represents the first examples of thioarsenates(II) while compounds 2 and 3 possess noncondensed pyramidal AsS{sub 3}{sup 3–} unit.« less

Reconstruction of local perturbations in periodic surfaces

NASA Astrophysics Data System (ADS)

Lechleiter, Armin; Zhang, Ruming

2018-03-01

This paper concerns the inverse scattering problem to reconstruct a local perturbation in a periodic structure. Unlike the periodic problems, the periodicity for the scattered field no longer holds, thus classical methods, which reduce quasi-periodic fields in one periodic cell, are no longer available. Based on the Floquet-Bloch transform, a numerical method has been developed to solve the direct problem, that leads to a possibility to design an algorithm for the inverse problem. The numerical method introduced in this paper contains two steps. The first step is initialization, that is to locate the support of the perturbation by a simple method. This step reduces the inverse problem in an infinite domain into one periodic cell. The second step is to apply the Newton-CG method to solve the associated optimization problem. The perturbation is then approximated by a finite spline basis. Numerical examples are given at the end of this paper, showing the efficiency of the numerical method.

Small-sized PdCu nanocapsules on 3D graphene for high-performance ethanol oxidation.

PubMed

Hu, Chuangang; Zhai, Xiangquan; Zhao, Yang; Bian, Ke; Zhang, Jing; Qu, Liangti; Zhang, Huimin; Luo, Hongxia

2014-03-07

A one-pot solvothermal process has been developed for direct preparation of PdCu nanocapsules (with a size of ca. 10 nm) on three-dimensional (3D) graphene. Due to the 3D pore-rich network of graphene and the unique hollow structure of PdCu nanocapsules with a wall thickness of ca. 3 nm, the newly-prepared PdCu/3D graphene hybrids activated electrochemically have great electrocatalytic activity towards ethanol oxidation in alkaline media, much better than single-phase Pd and commercial E-TEK 20% Pt/C catalysts promising for application in direct ethanol fuel cells.

A hybrid Pade-Galerkin technique for differential equations

NASA Technical Reports Server (NTRS)

Geer, James F.; Andersen, Carl M.

1993-01-01

A three-step hybrid analysis technique, which successively uses the regular perturbation expansion method, the Pade expansion method, and then a Galerkin approximation, is presented and applied to some model boundary value problems. In the first step of the method, the regular perturbation method is used to construct an approximation to the solution in the form of a finite power series in a small parameter epsilon associated with the problem. In the second step of the method, the series approximation obtained in step one is used to construct a Pade approximation in the form of a rational function in the parameter epsilon. In the third step, the various powers of epsilon which appear in the Pade approximation are replaced by new (unknown) parameters (delta(sub j)). These new parameters are determined by requiring that the residual formed by substituting the new approximation into the governing differential equation is orthogonal to each of the perturbation coordinate functions used in step one. The technique is applied to model problems involving ordinary or partial differential equations. In general, the technique appears to provide good approximations to the solution even when the perturbation and Pade approximations fail to do so. The method is discussed and topics for future investigations are indicated.

Removal of MCs by Bi2O2CO3: adsorption and the potential of photocatalytic degradation.

PubMed

Wang, Yujiao; Cao, Yanqiu; Li, Hongmei; Gong, Aijun; Han, Jintao; Qian, Zhen; Chao, Wenran

2018-04-01

Microcystins (MCs) is a kind of hepatotoxin, which is the secondary metabolite of cyanobacteria. Bi 2 O 2 CO 3 (BOC) is a kind of cheap and nontoxic semiconductor material. BOC was synthetized by solvothermal method and then microcystin-LR (MC-LR) and microcystin-RR (MC-RR) were removed by BOC, through adsorption and photocatalytic degradation. When the dosage of BOC is 6 g/L, the MC-LR and MC-RR in the natural water sample can be completely adsorbed in 30 min and then after 12 h irradiation, MC-LR and MC-RR were photocatalytically degraded by BOC.

CdS loaded on coal based activated carbon nanofibers with enhanced photocatalytic property

NASA Astrophysics Data System (ADS)

Guo, Jixi; Guo, Mingxi; Jia, Dianzeng; Song, Xianli; Tong, Fenglian

2016-08-01

The coal based activated carbon nanofibers (CBACFs) were prepared by electrospinning a mixture of polyacrylonitrile (PAN) and acid treated coal. Cadmium sulfide (CdS) nanoparticles loaded on CBACFs were fabricated by solvothermal method. The obtained samples were characterized by FESEM, TEM, and XRD. The results reveal that the CdS nanoparticles are homogeneously dispersed on the surfaces of CBACFs. The CdS/CBACFs nanocomposites exhibited higher photoactivity for photodegradation of methyl blue (MB) under visible light irradiation than pure CdS nanoparticles. CBACFs can be used as low cost support materials for the preparation of nanocomposites with high photocatalytic activity.

Ratiometric near infrared luminescent thermometer based on lanthanide metal-organic frameworks

NASA Astrophysics Data System (ADS)

Yue, Dan; Zhang, Jun; Zhao, Dian; Lian, Xiusheng; Cui, Yuanjing; Yang, Yu; Qian, Guodong

2016-09-01

A near infrared luminescent MOFs thermometer (Nd0.676Yb0.324BTC) was prepared via a simple solvothermal method using Ln3+ (Ln=Nd, Yb) ions and 1, 3, 5-benznenetricarboxylic acid (H3BTC), and characterized by PXRD, TGA, ICP, and photoluminescence (PL) spectrum. These results indicate that the Nd0.676Yb0.324BTC displays high relative sensitivity and excellent repeatability in the physiological temperature range (288-323 K), and the maximum relative sensitivity is determined to be 1.187% K-1 at 323 K. These NIR luminescent MOFs may have potential applications in physiological temperature sensing.

Novel multiform morphologies of hydroxyapatite: Synthesis and growth mechanism

NASA Astrophysics Data System (ADS)

Mary, I. Reeta; Sonia, S.; Viji, S.; Mangalaraj, D.; Viswanathan, C.; Ponpandian, N.

2016-01-01

Morphological evolution of materials becomes a prodigious challenge due to their key role in defining their functional properties and desired applications. Herein, we report the synthesis of hydroxyapatite (HAp) microstructures with multiform morphologies, such as spheres, cubes, hexagonal rods and nested bundles constructed from their respective nanoscale building blocks via a simple cost effective hydro/solvothermal method. A possible formation mechanism of diverse morphologies of HAp has been presented. Structural analysis based on X-ray diffraction (XRD) and Fourier transform infrared (FTIR) spectroscopy confirms the purity of the HAp microstructures. The multiform morphologies of HAp were corroborated by using Field emission scanning electron microscope (FESEM).

Parameter analysis of a photonic crystal fiber with raised-core index profile based on effective index method

NASA Astrophysics Data System (ADS)

Seraji, Faramarz E.; Rashidi, Mahnaz; Khasheie, Vajieh

2006-08-01

Photonic crystal fibers (PCFs) with a stepped raised-core profile and one layer equally spaced holes in the cladding are analyzed. Using effective index method and considering a raised step refractive index difference between the index of the core and the effective index of the cladding, we improve the characteristic parameters such as numerical aperture and V-parameter, and reduce its bending loss to about one tenth of a conventional PCF. Implementing such a structure in PCFs may be one step forward to achieve low loss PCFs for communication applications.

Cobalt-Doped Nickel Phosphite for High Performance of Electrochemical Energy Storage.

PubMed

Li, Bing; Shi, Yuxin; Huang, Kesheng; Zhao, Mingming; Qiu, Jiaqing; Xue, Huaiguo; Pang, Huan

2018-03-01

Compared to single metallic Ni or Co phosphides, bimetallic Ni-Co phosphides own ameliorative properties, such as high electrical conductivity, remarkable rate capability, upper specific capacity, and excellent cycle performance. Here, a simple one-step solvothermal process is proposed for the synthesis of bouquet-like cobalt-doped nickel phosphite (Ni 11 (HPO 3 ) 8 (OH) 6 ), and the effect of the structure on the pseudocapacitive performance is investigated via a series of electrochemical measurements. It is found that when the cobalt content is low, the glycol/deionized water ratio is 1, and the reaction is under 200 °C for 20 h, the morphology of the sample is uniform and has the highest specific surface area. The cobalt-doped Ni 11 (HPO 3 ) 8 (OH) 6 electrode presents a maximum specific capacitance of 714.8 F g -1 . More significantly, aqueous and solid-state flexible electrochemical energy storage devices are successfully assembled. The aqueous device shows a high energy density of 15.48 mWh cm -2 at the power density of 0.6 KW cm -2 . The solid-state device shows a high energy density of 14.72 mWh cm -2 at the power density of 0.6 KW cm -2 . These excellent performances confirm that the cobalt-doped Ni 11 (HPO 3 ) 8 (OH) 6 are promising materials for applications in electrochemical energy storage devices. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Electrophoretic deposition of Cu2ZnSn(S0.5Se0.5)4 films using solvothermal synthesized nanoparticles

NASA Astrophysics Data System (ADS)

Badkoobehhezaveh, Amir Masoud; Abdizadeh, Hossein; Golobostanfard, Mohammad Reza

2018-01-01

In this paper, a simple, practical, and fast solvothermal route is presented for synthesizing the Cu2ZnSn(S0.5Se0.5)4 nanoparticles (CZTSSe). In this method, the precursors were dissolved in triethylenetetramine and placed in an autoclave at 240 °C for 1 h under controlled pressure and constant stirring. After washing the samples for several times with absolute ethanol, the obtained CZTSSe nanoparticles were successfully deposited on fluorine doped tin oxide substrates by convenient electrophoretic deposition (EPD) using colloidal nanoparticles. The most appropriate parameters for EPD of pre-synthesized CZTSSe nanoparticles which result in proper surface properties, controlled thickness, and high film quality are investigated by adjusting applied voltage, pH, and deposition time. X-ray diffraction pattern and Raman spectroscopy of the pre-synthesized nanoparticles show kesterite structure formation. The particle size of the CZTSSe nanoparticles is in the range of 100 to 400 nm and for some agglomerates, it is about 2 µm confirmed by scanning electron microscope. The deposited film with optimized parameter has acceptable quality without any crack in it with the thickness of about 4-5 µm. Energy-dispersive X-ray spectroscopy confirms that the chemical composition of the samples is in near stoichiometric Cu-poor and Zn-rich region, which guarantees the p-type character of the film. The diffuse reflectance spectroscopy also demonstrates that the optical band gap of the sample is about 1.2 eV.

Metal-Organic Framework-Derived Hollow Hierarchical Co3O4 Nanocages with Tunable Size and Morphology: Ultrasensitive and Highly Selective Detection of Methylbenzenes.

PubMed

Jo, Young-Moo; Kim, Tae-Hyung; Lee, Chul-Soon; Lim, Kyeorei; Na, Chan Woong; Abdel-Hady, Faissal; Wazzan, Abdulaziz A; Lee, Jong-Heun

2018-03-14

Nearly monodisperse hollow hierarchical Co 3 O 4 nanocages of four different sizes (∼0.3, 1.0, 2.0, and 4.0 μm) consisting of nanosheets were prepared by controlled precipitation of zeolitic imidazolate framework-67 (ZIF-67) rhombic dodecahedra, followed by solvothermal synthesis of Co 3 O 4 nanocages using ZIF-67 self-sacrificial templates, and subsequent heat treatment for the development of high-performance methylbenzene sensors. The sensor based on hollow hierarchical Co 3 O 4 nanocages with the size of ∼1.0 μm exhibited not only ultrahigh responses (resistance ratios) to 5 ppm p-xylene (78.6) and toluene (43.8) but also a remarkably high selectivity to methylbenzene over the interference of ubiquitous ethanol at 225 °C. The unprecedented and high response and selectivity to methylbenzenes are attributed to the highly gas-accessible hollow hierarchical morphology with thin shells, abundant mesopores, and high surface area per unit volume as well as the high catalytic activity of Co 3 O 4 . Moreover, the size, shell thickness, mesopores, and hollow/hierarchical morphology of the nanocages, the key parameters determining the gas response and selectivity, could be well-controlled by tuning the precipitation of ZIF-67 rhombic dodecahedra and solvothermal reaction. This method can pave a new pathway for the design of high-performance methylbenzene sensors for monitoring the quality of indoor air.

Modified solvothermal synthesis of cobalt ferrite (CoFe2O4) magnetic nanoparticles photocatalysts for degradation of methylene blue with H2O2/visible light

NASA Astrophysics Data System (ADS)

Kalam, Abul; Al-Sehemi, Abdullah G.; Assiri, Mohammed; Du, Gaohui; Ahmad, Tokeer; Ahmad, Irfan; Pannipara, M.

2018-03-01

Different grads of magnetic nano-scaled cobalt ferrites (CoFe2O4) photocatalysts were synthesized by modified Solvothermal (MST) process with and without polysaccharide. The indigenously synthesized photocatalysts were characterized by means of X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), thermo gravimetric analysis (TGA), Fourier transform infrared (FT-IR), UV-visible (UV-vis) spectroscopy and N2 adsorption-desorption isotherm method. The Fourier transform infrared spectroscopy study showed the Fe-O stretching vibration 590-619 cm-1, confirming the formation of metal oxide. The crystallite size of the synthesized photocatalysts was found in the range between 20.0 and 30.0 nm. The surface area of obtained magnetic nanoparticles is found to be reasonably high in the range of 63.0-76.0 m2/g. The results shown that only MST-2 is the most active catalyst for photo-Fenton like scheme for fast photodegradation action of methylene blue dye, this is possible due to optical band gap estimated of 2.65 eV. Captivatingly the percentage of degradation efficiency increases up to 80% after 140 min by using MST-2 photocatalyst. Photocatalytic degradation of methylene blue (MB) dye under visible light irradiation with cobalt ferrite magnetic nanoparticles followed first order kinetic constant and rate constant of MST-2 is almost 2.0 times greater than MST-1 photocatalyst.

Engineering 3D bicontinuous hierarchically macro-mesoporous LiFePO4/C nanocomposite for lithium storage with high rate capability and long cycle stability

PubMed Central

Zhang, Qian; Huang, Shao-Zhuan; Jin, Jun; Liu, Jing; Li, Yu; Wang, Hong-En; Chen, Li-Hua; Wang, Bin-Jie; Su, Bao-Lian

2016-01-01

A highly crystalline three dimensional (3D) bicontinuous hierarchically macro-mesoporous LiFePO4/C nanocomposite constructed by nanoparticles in the range of 50~100 nm via a rapid microwave assisted solvothermal process followed by carbon coating have been synthesized as cathode material for high performance lithium-ion batteries. The abundant 3D macropores allow better penetration of electrolyte to promote Li+ diffusion, the mesopores provide more electrochemical reaction sites and the carbon layers outside LiFePO4 nanoparticles increase the electrical conductivity, thus ultimately facilitating reverse reaction of Fe3+ to Fe2+ and alleviating electrode polarization. In addition, the particle size in nanoscale can provide short diffusion lengths for the Li+ intercalation-deintercalation. As a result, the 3D macro-mesoporous nanosized LiFePO4/C electrode exhibits excellent rate capability (129.1 mA h/g at 2 C; 110.9 mA h/g at 10 C) and cycling stability (87.2% capacity retention at 2 C after 1000 cycles, 76.3% at 5 C after 500 cycles and 87.8% at 10 C after 500 cycles, respectively), which are much better than many reported LiFePO4/C structures. Our demonstration here offers the opportunity to develop nanoscaled hierarchically porous LiFePO4/C structures for high performance lithium-ion batteries through microwave assisted solvothermal method. PMID:27181195

Engineering 3D bicontinuous hierarchically macro-mesoporous LiFePO4/C nanocomposite for lithium storage with high rate capability and long cycle stability.

PubMed

Zhang, Qian; Huang, Shao-Zhuan; Jin, Jun; Liu, Jing; Li, Yu; Wang, Hong-En; Chen, Li-Hua; Wang, Bin-Jie; Su, Bao-Lian

2016-05-16

A highly crystalline three dimensional (3D) bicontinuous hierarchically macro-mesoporous LiFePO4/C nanocomposite constructed by nanoparticles in the range of 50~100 nm via a rapid microwave assisted solvothermal process followed by carbon coating have been synthesized as cathode material for high performance lithium-ion batteries. The abundant 3D macropores allow better penetration of electrolyte to promote Li(+) diffusion, the mesopores provide more electrochemical reaction sites and the carbon layers outside LiFePO4 nanoparticles increase the electrical conductivity, thus ultimately facilitating reverse reaction of Fe(3+) to Fe(2+) and alleviating electrode polarization. In addition, the particle size in nanoscale can provide short diffusion lengths for the Li(+) intercalation-deintercalation. As a result, the 3D macro-mesoporous nanosized LiFePO4/C electrode exhibits excellent rate capability (129.1 mA h/g at 2 C; 110.9 mA h/g at 10 C) and cycling stability (87.2% capacity retention at 2 C after 1000 cycles, 76.3% at 5 C after 500 cycles and 87.8% at 10 C after 500 cycles, respectively), which are much better than many reported LiFePO4/C structures. Our demonstration here offers the opportunity to develop nanoscaled hierarchically porous LiFePO4/C structures for high performance lithium-ion batteries through microwave assisted solvothermal method.

Solvothermal synthesis of Mg-doped Li2FeSiO4/C nanocomposite cathode materials for lithium-ion batteries

NASA Astrophysics Data System (ADS)

Kumar, Ajay; Jayakumar, O. D.; Naik, V. M.; Nazri, G. A.; Naik, R.

Lithium transition metal orthosilicates, such as Li2FeSiO4 and Li2MnSiO4, as cathode material have attracted much attention lately due to their high theoretical capacity ( 330 mAh/g), low cost, and environmental friendliness. However, they suffer from poor electronic conductivity and slow lithium ion diffusion in the solid phase. Several cation-doped orthosilicates have been studied to improve their electrochemical performance. We have synthesized partially Mg-substituted Li2Mgx Fe1-x SiO4-C, (x = 0.0, 0.01, 0.02, and 0.04) nano-composites by solvothermal method followed by annealing at 600oC in argon flow. The structure and morphology of the composites were characterized by XRD, SEM and TEM. The surface area and pore size distribution were measured by using N2 adsorption/desorption curves. The electrochemical performance of the Li2MgxFe1-x SiO4-C composites was evaluated by Galvanostatic cycling against metallic lithium anode, electrochemical impedance spectroscopy, and cyclic voltammetry. Li2Mg0.01Fe0.99SiO4-C sample shows a capacity of 278 mAh/g (at C/30 rate in the 1.5-4.6 V voltage window) with an excellent rate capability and stability, compared to the other samples. We attribute this observation to its higher surface area, enhanced electronic conductivity and higher lithium ion diffusion coefficient.

Synthesis of a Ni2P/Ni12P5 bi-phase nanocomposite for the efficient catalytic reduction of 4-nitrophenol based on the unique n-n heterojunction effects.

PubMed

Tian, Feng-Yu; Hou, Dongfang; Zhang, Wei-Min; Qiao, Xiu-Qing; Li, Dong-Sheng

2017-10-24

A novel heterostructure catalyst of Ni 2 P/Ni 12 P 5 has been fabricated through a simple solvothermal method by modifying the molar ratio of the initial raw materials. The products are characterized by X-ray powder diffraction (XRD), field emission scanning electron microscopy (FE-SEM), high-resolution transmission electron microscopy (HRTEM), nitrogen adsorption and X-ray photoelectron spectroscopy (XPS). It is found that the two phases, Ni 2 P and Ni 12 P 5 , are interlaced with one another in the as-formed nanocomposite, resulting in more interfaces. The bi-phase catalyst exhibits a markedly enhanced catalytic activity in the reduction of 4-nitrophenol, as compared to that of single Ni 2 P or Ni 12 P 5 . The enhanced catalytic activity can be attributed to the unique n-n series effects, which result in the increased ease of electron transfer over the Ni 2 P/Ni 12 P 5 bi-phase catalyst.

Facile Synthesis of Mixed Metal Organic Frameworks: Electrode Materials for Supercapacitor with Excellent Areal Capacitance and Operational Stability.

PubMed

Kazemi, Sayed Habib; Hosseinzadeh, Batoul; Kazemi, Hojjat; Kiani, Mohammad Ali; Hajati, Shaaker

2018-06-08

Electrode materials with high surface area, tailored pore size and efficient capability for ion insertion and enhanced transport of electrons and ions are needed for advanced supercapacitors. In the present study, a mixed metal organic framework (cobalt and manganese based MOF) was synthesized through a simple one pot solvothermal method and employed as the electrode material for supercapacitor. Notably, Co-Mn MOF electrode displayed a large surface area and excellent cycling stability (over 95% capacitance retention after 1500 cycles). Also, superior pseudocapacitive behavior was observed for Co-Mn MOF electrode in KOH electrolyte with an exceptional areal capacitance of 1.318 F cm-2. Moreover, an asymmetric supercapacitor was assembled using Co-Mn MOF and activated carbon electrode as positive and negative electrodes, respectively. The fabricated supercapacitor showed specific capacitances of 106.7 F g-1 at a scan rate of 10 mV s-1 and delivered maximum energy density of 30 Wh kg-1 at 2285.7 W kg-1. Our studies suggest the Co-Mn MOF as promising electrode materials for supercapacitor applications.

Solvothermal synthesis of ZnO nanoparticles and anti-infection application in vivo.

PubMed

Bai, Xiangyang; Li, Linlin; Liu, Huiyu; Tan, Longfei; Liu, Tianlong; Meng, Xianwei

2015-01-21

Zinc oxide nanoparticles (ZnONPs) have been widely studied as the bacteriostatic reagents. However, synthesis of small ZnO nanoparticles with good monodispersion and stability in aqueous solution is still a challenge. Anti-infection research of ZnONPs used as antibacterial agent in vivo is rare. In this paper, a novel, sustainable, and simple method to synthesize ZnO nanoparticles with good monodispersion in aqueous low-temperature conditions and with a small molecule agent is reported. Inhibition zone test and the minimum inhibitory concentration test were performed to examine the antibacterial activity of ZnONPs against bacteria Staphylococcus aureus and Escherichia coli in vitro. For further application in vivo, low cytotoxicity and low acute toxicity in mice of ZnO were demonstrated. Finally, 4 nm ZnONPs combined with poly(vinyl alcohol) gel was used as antibacterial agent in rodent elytritis model, and significant anti-infection effect was proven. In one word, the present research would shed new light on the designing of antibacterial materials like ZnO with promising application in disinfection.

Facile synthesis of high-temperature (1000 °C) phase-stable rice-like anatase TiO2 nanocrystals

NASA Astrophysics Data System (ADS)

Lv, Lizhen; Chen, Qirong; Liu, Xiuyun; Wang, Miaomiao; Meng, Xiangfu

2015-05-01

High-temperature phase-stable rice-like anatase TiO2 nanocrystals were synthesized by one-pot solvothermal method using soluble titania xerogel and isopropyl alcohol (IPA) as the precursor and the solvent, respectively. Sample characterization was carried out by powder X-ray diffraction, high-resolution transmission electron microscopy, field emission scanning electron microscope, X-ray photoelectron spectroscopy, and N2 adsorption-desorption isotherms. The results showed that TiO2 nanocrystals had rice-like shapes with an average size of 5 nm in width and 35 nm in length. The BET surface area was 153 m2/g. Unexpectedly, the rice-like TiO2 nanocrystals exhibited high-temperature phase stability, which could remain as pure anatase phase after calcinations at 1000 °C. Growth mechanism investigation revealed that the IPA solvent played a key role in nucleation and growth of rice-like anatase TiO2 nanocrystals. The photodegradation of rhodamine B demonstrated that rice-like anatase TiO2 nanocrystals exhibited enhanced photocatalytic activity under visible light irradiation.

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

Liu, Shuling, E-mail: liusl8888@yahoo.com.cn; Li, Honglin; Yan, Lu

Graphical abstract: - Highlights: • 3D urchin-like ZnS/CdS composites were synthesized via a two-step method. • The CdS nanoparticles were assembled on the thorns of 3D ZnS urchins. • The ZnS/CdS composites show excellent photocatalytic degradation activities. • The modification of CdS on ZnS is responsible for the enhanced property. - Abstract: Urchin-like ZnS/CdS semiconductor composites were successfully synthesized by combining solvothermal route with homogeneous precipitation process. The as-obtained samples were characterized by means of XRD, EDX, TEM, HR-TEM, ED and FE-SEM techniques. The results show that the as-obtained composites were comprised of the hexagonal structure ZnS and CdS, andmore » CdS nanoparticles were assembled on the surfaces of the thorns of urchin-like ZnS. In addition, the optical properties and photocatalytic activities of the as-prepared ZnS/CdS composites toward some organic dyes (such as Methyl Orange, Pyronine B, Rhodamine B and Methylene Blue) were separately investigated. It is found that the ZnS/CdS composites exhibit excellent photocatalytic degradation activity for these dyes under UV irradiation, as compared to corresponding pure ZnS urchins and commercial anatase TiO{sub 2} (P-25). This enhanced activity may be related to the modification of CdS nanoparticles on the surfaces of thorns of ZnS urchins and a tentative mechanism for the enhanced photocatalytic degradation activities of the ZnS/CdS composite catalyst was proposed.« less

Structure tracking aided design and synthesis of Li 3V 2(PO 4) 3 nanocrystals as high-power cathodes for lithium ion batteries

DOE PAGES

Wang, Liping; Bai, Jianming; Gao, Peng; ...

2015-07-30

In this study, preparing new electrode materials with synthetic control of phases and electrochemical properties is desirable for battery applications but hardly achievable without knowing how the synthesis reaction proceeds. Herein, we report on structure tracking-aided design and synthesis of single-crystalline Li 3V 2(PO 4) 3 (LVP) nanoparticles with extremely high rate capability. A comprehensive investigation was made to the local structural orderings of the involved phases and their evolution toward forming LVP phase using in situ/ex situ synchrotron X-ray and electron-beam diffraction, spectroscopy, and imaging techniques. The results shed light on the thermodynamics and kinetics of synthesis reactions andmore » enabled the design of a cost-efficient synthesis protocol to make nanocrystalline LVP, wherein solvothermal treatment is a crucial step leading to an amorphous intermediate with local structural ordering resembling that of LVP, which, upon calcination at moderate temperatures, rapidly transforms into the desired LVP phase. The obtained LVP particles are about 50 nm, coated with a thin layer of amorphous carbon and featured with excellent cycling stability and rate capability – 95% capacity retention after 200 cycles and 66% theoretical capacity even at a current rate of 10 C. The structure tracking based method we developed in this work offers a new way of designing battery electrodes with synthetic control of material phases and properties.« less

Preparation of Nickel Cobalt Sulfide Hollow Nanocolloids with Enhanced Electrochemical Property for Supercapacitors Application

PubMed Central

Chen, Zhenhua; Wan, Zhanghui; Yang, Tiezhu; Zhao, Mengen; Lv, Xinyan; Wang, Hao; Ren, Xiuli; Mei, Xifan

2016-01-01

Nanostructured functional materials with hollow interiors are considered to be good candidates for a variety of advanced applications. However, synthesis of uniform hollow nanocolloids with porous texture via wet chemistry method is still challenging. In this work, nickel cobalt precursors (NCP) in sub-micron sized spheres have been synthesized by a facile solvothermal method. The subsequent sulfurization process in hydrothermal system has changed the NCP to nickel cobalt sulfide (NCS) with porous texture. Importantly, the hollow interiors can be tuned through the sulfurization process by employing different dosage of sulfur source. The derived NCS products have been fabricated into supercapacitor electrodes and their electrochemical performances are measured and compared, where promising results were found for the next-generation high-performance electrochemical capacitors. PMID:27114165

Synthesis of magnetic mesoporous metal-organic framework-5 for the effective enrichment of malachite green and crystal violet in fish samples.

PubMed

Zhou, Zhihui; Fu, Yanqing; Qin, Qian; Lu, Xin; Shi, Xianzhe; Zhao, Chunxia; Xu, Guowang

2018-07-27

A novel, magnetic and mesoporous Fe 3 O 4 @PEI-MOF-5 material was synthesized for the effective enrichment of malachite green (MG) and crystal violet (CV) in fish samples. The Fe 3 O 4 @PEI-MOF-5 material was prepared by a facile two-step solvothermal approach in which Fe 3 O 4 @PEI and MOF-5 were connected through chemical bonds. Characterization of the newly synthesized Fe 3 O 4 @PEI-MOF-5 material was performed by Fourier transform infrared spectroscopy, X-ray diffractometry, vibrating sample magnetometry, scanning electron microscopy, transmission electron microscopy, thermogravimetric analysis and X-ray photoelectron spectroscopy. This new material was determined to have high magnetization and chemical stability, a large surface area and a distinctive morphology. An effective enrichment and detection method for MG and CV was subsequently developed by combining the Fe 3 O 4 @PEI-MOF-5 material with ultra-high-performance liquid chromatography-tandem mass spectrometry. The linearity ranges of this approach for MG and CV were 1-500ng/mL and 0.25-500ng/mL, respectively, with correlation coefficients (R 2 ) of 0.999. The limits of detection (LODs) of the method for MG and CV were 0.30ng/mL and 0.08ng/mL, respectively, indicating that the Fe 3 O 4 @PEI-MOF-5 material had good adsorption properties for MG and CV. Fe 3 O 4 @PEI-MOF-5 can be expected to also provide efficient enrichment of MG and CV in other complex matrices. Copyright © 2018 Elsevier B.V. All rights reserved.

Towards "Inverse" Character Tables? A One-Step Method for Decomposing Reducible Representations

ERIC Educational Resources Information Center

Piquemal, J.-Y.; Losno, R.; Ancian, B.

2009-01-01

In the framework of group theory, a new procedure is described for a one-step automated reduction of reducible representations. The matrix inversion tool, provided by standard spreadsheet software, is applied to the central part of the character table that contains the characters of the irreducible representation. This method is not restricted to…

Calcite phase determination of CaCO3 nanoparticles synthesized by one step drying method

NASA Astrophysics Data System (ADS)

Sulimai, N. H.; Rani, Rozina Abdul; Khusaimi, Z.; Abdullah, S.; Salifairus, M. J.; Alrokayan, Salman; Khan, Haseeb; Rusop, M.

2018-05-01

Calcium Carbonate (CaCO3) is a type of carbonic salt. It exist naturally as white odourless solid and may also be synthesized by chemical reactions. This work studies one-step precipitation of CaCO3 that was prepared by novel method of one-step precipitation method. The method was then proceeded by different types of drying. The first type is by normal drying in oven whereas the second type is with the presence of hydrothermal influence. From the results, precipitated CaCO3 dried by normal drying method produces CaCO3 with two polymorphs present; calcite and vaterite. Normal drying at 500°C has no vaterite phase left. Drying by hydrothermal precipitated CaCO3 has Nitrogen (N) left on the surfaces of the precipitated CaCO3. This work successfully identified calcite phase in the precipitated CaCO3.

Thin single-crystalline Bi2(Te1-xSex)3 ternary nanosheets synthesized by a solvothermal technique

NASA Astrophysics Data System (ADS)

Guo, Jing; Jian, Jikang; Zhang, Zhihua; Wu, Rong; Li, Jin; Sun, Yanfei

2016-01-01

Bi2(Te1-xSex)3 ternary nanosheets have been successfully synthesized through a facile solvothermal technique using diethylenetriamine as solvent, where x can vary from 0 to 1. X-ray diffraction (XRD) and Scanning electron microscopy (SEM) indicate that the as-synthesized Bi2(Te1-xSex)3 samples are nanosheets with rhombohedral structure, and the thickness of the nanosheets can be as thin as several nanometers. High resolution transmission electron microscopy (HRTEM) and selected area electron diffraction (SAED) reveal that the nanosheets are single crystalline with a rhombohedral structure. Energy disperse spectroscopy (EDS) and XRD analysis by Vegard's law confirm that the ternary Bi2(Te1-xSex)3 nanosheets have been obtained here. The growth of the nanosheets is discussed based on an amine-based molecular template mechanism that has been employed to synthesize some other metal chalcogenides.

Ga2O3 and GaN nanocrystalline film: reverse micelle assisted solvothermal synthesis and characterization.

PubMed

Sinha, Godhuli; Ganguli, Dibyendu; Chaudhuri, Subhadra

2008-03-01

Gallium oxide (beta-Ga2O3) nanoparticles were successfully deposited on quartz glass substrates using sodium bis(2-ethylhexyl) sulfosuccinate (AOT)/n-hexane/ethylene glycol monomethyl ether (EGME) reverse micelle-mediated solvothermal process with different omega values. The mean diameter of Ga2O3 particles was approximately 2-3 nm and found to be approximately independent of omega values of the reverse micelles. However, when the Ga2O3 nanocrystalline films were nitrided at 900 degrees C under flowing NH3 atmosphere for 1 h, the mean diameter of the resulted gallium nitride (wurtzite-GaN) nanoparticles varied from 3-9 nm. Both nanocrystalline films of Ga2O3 and GaN were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), Fourier transform infrared (FTIR) spectroscopy, UV-vis spectroscopy and photoluminescence in order to study their chemical and physical properties explicitly.

Natural sunlight irradiated flower-like CuS synthesized from DMF solvothermal treatment

NASA Astrophysics Data System (ADS)

Zhao, Wei; Wang, Zihao; Zhou, Lei; Liu, Nianqi; Wang, Hongxing

2016-09-01

Three-dimensional CuS hierarchical crystals with high catalytic activity had been successfully fabricated using a facile solvothermal process. The CuS microparticles showed different flower-like morphology and good dispersion by optimizing reaction conditions. It was found that using N,N-dimethylformamide (DMF) as the solvent reagent in the proper temperature conditions was favorable for the growth of hierarchically structured CuS. The hexagonal flower-like CuS synthesized at 170°C for 60 min displayed broad-spectrum photocatalytic properties under ultraviolet (UV) and visible irradiation. The as-prepared CuS crystals exhibited good performance to decolorize methylene blue (MB) solution under visible light irradiation. The total organic carbon (TOC) removal of rhodamine B (RhB) solution was nearly 60% after 5 h of the natural sunlight irradiation, and the property was stable after testing over four recycles, demonstrating a potential application in waster water treatment.

Innovative biofilm inhibition and anti-microbial behavior of molybdenum sulfide nanostructures generated by microwave-assisted solvothermal route

NASA Astrophysics Data System (ADS)

Qureshi, Nilam; Patil, Rajendra; Shinde, Manish; Umarji, Govind; Causin, Valerio; Gade, Wasudev; Mulik, Uttam; Bhalerao, Anand; Amalnerkar, Dinesh P.

2015-03-01

The incessant use of antibiotics against infectious diseases has translated into a vicious circle of developing new antibiotic drug and its resistant strains in short period of time due to inherent nature of micro-organisms to alter their genes. Many researchers have been trying to formulate inorganic nanoparticles-based antiseptics that may be linked to broad-spectrum activity and far lower propensity to induce microbial resistance than antibiotics. The way-out approaches in this direction are nanomaterials based (1) bactericidal and (2) bacteriostatic activities. We, herein, present hitherto unreported observations on microbial abatement using non-cytotoxic molybdenum disulfide nanostructures (MSNs) which are synthesized using microwave assisted solvothermal route. Inhibition of biofilm formation using MSNs is a unique feature of our study. Furthermore, this study evinces antimicrobial mechanism of MSNs by reactive oxygen species (ROS) dependent generation of superoxide anion radical via disruption of cellular functions.

Torque Characteristics Analysis of Hybrid Stepping Motor Using 3-D Finite Element Method

NASA Astrophysics Data System (ADS)

Kawase, Yoshihiro; Yamaguchi, Tadashi; Masuda, Tatsuya; Domeki, Hideo; Kobori, Masaru

Hybrid stepping motors are widely used for various electric instruments because of high torque, high accuracy and small step angle. It is necessary for the optimum design of hybrid stepping motors to analyze torque characteristics accurately. In this paper, a hybrid stepping motor is analyzed using the 3-D finite element method taking into account the rotation of the armature. The effects of the interlaminar gap in the core on the torque characteristics are clarified using the gap elements. The validity of our method is clarified by comparison between the calculated results and measured ones.

Construction and optical properties of infinite Cd and finite Cu molecules stairs

NASA Astrophysics Data System (ADS)

Zhao, Qiang; Mao, Wutao; Shen, Zhi; Wang, Qinghong; Zhou, Qian

2017-02-01

Two coordination complexes, namely [(hpdq)(pta)Cd]n (1) and [(pptp)(pta)Cu2Cl] (2) have been synthesized by solvothermal method based on two polypyridyl ligands, 2,3,6,7,10,11-hexakis- (2-pyridyl)dipyrazino[2,3-f:2‧,3‧-h]quinoxaline) (hpdq), 4‧-(4- (3H-pyrrol-3-yl)phenyl)- 2,2‧:6‧,2″- terpyridine (pptp) and auxiliary ligand p-phthalic acid (pta), respectively. Single crystal x-ray diffraction analyses reveal that complexes 1 and 2 assembled based on distinct asymmetric unit comprising one and two respective polypyridyl ligands but one Cd(II) and two Cu(I)ions, respectively. Among them, The asymmetric units in 1 was extended to one dimensional chain via the link of auxiliary ligand pta, just like infinite layers of stairs that connected by cadmium ions as the node. While that in 2 to Zero dimensional tetranuclear structure via the link of auxiliary ligand pta, just like finite four layers of stairs that Copper ion as the node connection. Furthermore, solid fluorescence spectra properties of two complexes were also investigated, and the result shows the fluorescence intensity of complex 1 is stronger than that of the hpdq ligand, but the fluorescence intensity of complex 2 is weaker than that of the pptp ligand. CCDC number of 1and 2 are 1483301 and 1483302.

Enhanced removal of bisphenol-AF by activated carbon-alginate beads with cetyltrimethyl ammonium bromide.

PubMed

Tang, Zheng; Peng, Sha; Hu, Shuya; Hong, Song

2017-06-01

Adsorption removal of bisphenol-AF (BPAF) from aqueous solutions by synthesized activated carbon-alginate beads (AC-AB) with cetyltrimethyl ammonium bromide (CTAB) has been studied using two ways. The traditional method (two-step) first synthesized CTAB-modified AC-AB (AC-AB-CTAB), then used it to remove BPAF by adsorption. And one-step method dispersed AC-AB and CTAB in wastewater, followed by the removal of BPAF accompanied with the synthesis of AC-AB-CTAB. The one-step method showed a better performance than the two-step method, achieving a maximum removal of BPAF with 284.6mg/g. Kinetic studies and adsorption isotherms indicated that adsorption process of BPAF on AC-AB by the one-step method could be expressed by a pseudo-second-order model and a Dubinin-Ashtakhov (D-A) isotherm, respectively. The effects of pH, ionic strength, and inorganic ions on BPAF adsorption were also investigated. Furthermore, hydrophobic interactions, hydrogen bonds, and π-π electron donor-acceptor (EDA) interactions were discussed to explain the enhanced adsorption behavior of BPAF on AC-AB with CTAB. The findings verified the effectiveness of AC-AB for the removal of BPAF from wastewater and its high stability within five regeneration cycles. Copyright © 2017 Elsevier Inc. All rights reserved.

Improved perovskite phototransistor prepared using multi-step annealing method

NASA Astrophysics Data System (ADS)

Cao, Mingxuan; Zhang, Yating; Yu, Yu; Yao, Jianquan

2018-02-01

Organic-inorganic hybrid perovskites with good intrinsic physical properties have received substantial interest for solar cell and optoelectronic applications. However, perovskite film always suffers from a low carrier mobility due to its structural imperfection including sharp grain boundaries and pinholes, restricting their device performance and application potential. Here we demonstrate a straightforward strategy based on multi-step annealing process to improve the performance of perovskite photodetector. Annealing temperature and duration greatly affects the surface morphology and optoelectrical properties of perovskites which determines the device property of phototransistor. The perovskite films treated with multi-step annealing method tend to form highly uniform, well-crystallized and high surface coverage perovskite film, which exhibit stronger ultraviolet-visible absorption and photoluminescence spectrum compare to the perovskites prepared by conventional one-step annealing process. The field-effect mobilities of perovskite photodetector treated by one-step direct annealing method shows mobility as 0.121 (0.062) cm2V-1s-1 for holes (electrons), which increases to 1.01 (0.54) cm2V-1s-1 for that treated with muti-step slow annealing method. Moreover, the perovskite phototransistors exhibit a fast photoresponse speed of 78 μs. In general, this work focuses on the influence of annealing methods on perovskite phototransistor, instead of obtains best parameters of it. These findings prove that Multi-step annealing methods is feasible to prepared high performance based photodetector.

One-pot synthesis of CoNiO2 single-crystalline nanoparticles as high-performance electrode materials of asymmetric supercapacitors

NASA Astrophysics Data System (ADS)

Du, Weimin; Gao, Yanping; Tian, Qingqing; Li, Dan; Zhang, Zhenhu; Guo, Jiaojiao; Qian, Xuefeng

2015-09-01

A facile one-pot solvothermal method has been developed to synthesize CoNiO2 single-crystalline nanoparticles. Crystal phase, morphology, crystal lattice, and composition of the obtained products were characterized by X-ray diffraction, scanning electron microscope, high-resolution transmission electron microscopy, and energy-dispersive X-ray analysis, respectively. Results revealed that the as-synthesized CoNiO2 nanoparticles belong to cubic structure with narrow size-distribution (8-10 nm). Subsequently, new asymmetric supercapacitors were successfully assembled with CoNiO2 nanoparticles as positive electrode and activated carbon as negative electrode. The electrochemical results show that asymmetric supercapacitors based on CoNiO2 nanoparticles possess excellent supercapacitor properties, i.e., a stable electrochemical window of 0-1.7 V, higher energy density of 24.0 Wh/kg at a power density of 415.4 W/kg, and excellent cycling stability (96.8 % capacitance retention after 5000 charge-discharge cycles). Meanwhile, both a light-emitting diode and a mini fan can be powered by two series connection asymmetric supercapacitors. These results imply that the present asymmetric supercapacitors based on CoNiO2 nanoparticles possess the promising potential application in the field of high-performance energy storage.

Crystal Phase and Architecture Engineering of Lotus-Thalamus-Shaped Pt-Ni Anisotropic Superstructures for Highly Efficient Electrochemical Hydrogen Evolution.

PubMed

Zhang, Zhicheng; Liu, Guigao; Cui, Xiaoya; Chen, Bo; Zhu, Yihan; Gong, Yue; Saleem, Faisal; Xi, Shibo; Du, Yonghua; Borgna, Armando; Lai, Zhuangchai; Zhang, Qinghua; Li, Bing; Zong, Yun; Han, Yu; Gu, Lin; Zhang, Hua

2018-06-07

The rational design and synthesis of anisotropic 3D nanostructures with specific composition, morphology, surface structure, and crystal phase is of significant importance for their diverse applications. Here, the synthesis of well-crystalline lotus-thalamus-shaped Pt-Ni anisotropic superstructures (ASs) via a facile one-pot solvothermal method is reported. The Pt-Ni ASs with Pt-rich surface are composed of one Ni-rich "core" with face-centered cubic (fcc) phase, Ni-rich "arms" with hexagonal close-packed phase protruding from the core, and facet-selectively grown Pt-rich "lotus seeds" with fcc phase on the end surfaces of the "arms." Impressively, these unique Pt-Ni ASs exhibit superior electrocatalytic activity and stability toward the hydrogen evolution reaction under alkaline conditions compared to commercial Pt/C and previously reported electrocatalysts. The obtained overpotential is as low as 27.7 mV at current density of 10 mA cm -2 , and the turnover frequency reaches 18.63 H 2 s -1 at the overpotential of 50 mV. This work provides a new strategy for the synthesis of highly anisotropic superstructures with a spatial heterogeneity to boost their promising application in catalytic reactions. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Core-shell structured MnSiO3 supported with CNTs as a high capacity anode for lithium-ion batteries.

PubMed

Feng, Jing; Li, Qin; Wang, Huijun; Zhang, Min; Yang, Xia; Yuan, Ruo; Chai, Yaqin

2018-04-17

Metal silicates are good candidates for use in lithium ion batteries (LIBs), however, their electrochemical performance is hindered by their poor electrical conductivity and volume expansion during Li+ insertion/desertion. In this work, one-dimensional core-shell structured MnSiO3 supported with carbon nanotubes (CNTs) (referred to as CNT@MnSiO3) with good conductivity and electrochemical performance has been successfully synthesized using a solvothermal process under moderate conditions. In contrast to traditional composites of CNTs and nanoparticles, the CNT@MnSiO3 composite in this work is made up of CNTs with a layer of MnSiO3 on the surface. The one-dimensional CNT@MnSiO3 nanotubes provide a useful channel for transferring Li+ ions during the discharge/charge process, which accelerates the Li+ diffusion speed. The CNTs inside the structure not only enhance the conductivity of the composite, but also prevent volume expansion. A high reversible capacity (920 mA h g-1 at 500 mA g-1 over 650 cycles) and good rate performance were obtained for CNT@MnSiO3, showing that this strategy of synthesizing coaxial CNT@MnSiO3 nanotubes offers a promising method for preparing other silicates for LIBs or other applications.

Solution of elliptic partial differential equations by fast Poisson solvers using a local relaxation factor. 2: Two-step method

NASA Technical Reports Server (NTRS)

Chang, S. C.

1986-01-01

A two-step semidirect procedure is developed to accelerate the one-step procedure described in NASA TP-2529. For a set of constant coefficient model problems, the acceleration factor increases from 1 to 2 as the one-step procedure convergence rate decreases from + infinity to 0. It is also shown numerically that the two-step procedure can substantially accelerate the convergence of the numerical solution of many partial differential equations (PDE's) with variable coefficients.

Solvothermal fabrication of TiO2/sepiolite composite gel with exposed {0 0 1} and {1 0 1} facets and its enhanced photocatalytic activity

NASA Astrophysics Data System (ADS)

Liu, Ruirui; Ji, Zhijiang; Wang, Jing; Zhang, Jinjun

2018-05-01

A novel TiO2/sepiolite composite gel (TiSG) was fabricated in the presence of cetyltrimethylammonium bromide (CTAB) through a simple solvothermal reaction in an acetic acid-water solvent. A homogeneous anchoring of TiO2 nanoparticles with exposed {0 0 1} and {1 0 1} facets on sepiolite nanofibers was achieved. CTAB content, solvothermal temperature/time, and HAc content play crucial roles in the morphological and facet formation of TiSG. A possible mechanism for the formation of TiSG was further proposed. CTAB as capping/shape-controlling agent can strongly bind to the more reactive (0 0 1) facet of TiO2 and then mitigate the thermodynamically favored (0 0 1) plane growth. Eventually, the truncated octahedral TiO2 was obtained by controlling the growth rates in 〈0 0 1〉 and 〈1 0 1〉 directions. Sepiolite as a cross-linking agent provides sufficient crosslinking sites for TiO2 to induce three-dimensional (3D) network formation, thereby generating the composite gel. The synthesized TiSG samples were then used as photocatalysts, which exhibited increased methyl orange removal under UV-vis light (350-780 nm) by the synergistic effect of adsorption and in-situ photocatalytic degradation as compared to P25 and bare TiO2. The excellent photocatalytic performance of TiSG was mainly ascribed to the formations of 3D gel structure and surface heterojunctions between (0 0 1) and (1 0 1) facets.

Accuracy of Multiple Pour Cast from Various Elastomer Impression Methods

PubMed Central

Saad Toman, Majed; Ali Al-Shahrani, Abdullah; Ali Al-Qarni, Abdullah

2016-01-01

The accurate duplicate cast obtained from a single impression reduces the profession clinical time, patient inconvenience, and extra material cost. The stainless steel working cast model assembly consisting of two abutments and one pontic area was fabricated. Two sets of six each custom aluminum trays were fabricated, with five mm spacer and two mm spacer. The impression methods evaluated during the study were additional silicone putty reline (two steps), heavy-light body (one step), monophase (one step), and polyether (one step). Type IV gypsum casts were poured at the interval of one hour, 12 hours, 24 hours, and 48 hours. The resultant cast was measured with traveling microscope for the comparative dimensional accuracy. The data obtained were subjected to Analysis of Variance test at significance level <0.05. The die obtained from two-step putty reline impression techniques had the percentage of variation for the height −0.36 to −0.97%, while diameter was increased by 0.40–0.90%. The values for one-step heavy-light body impression dies, additional silicone monophase impressions, and polyether were −0.73 to −1.21%, −1.34%, and −1.46% for the height and 0.50–0.80%, 1.20%, and −1.30% for the width, respectively. PMID:28096815

Two-Dimensional Wavelike Spinel Lithium Titanate for Fast Lithium Storage

PubMed Central

Liu, Jiehua; Wei, Xiangfeng; Liu, Xue-Wei

2015-01-01

Safe fast-charging lithium-ion batteries (LIBs) have huge potential market size on demand according to their shortened charging time for high-power devices. Zero-strain spinel Li4Ti5O12 is one of ideal candidates for safe high-power batteries owing to its good cycling performance, low cost and safety. However, the inherent insulating characteristic of LTO seriously limits its high-rate capability. In this work, we successfully synthesize novel wavelike spinel LTO nanosheets using a facile ‘co-hydrolysis’ method, which is superior to molten-salt approach and traditional solvothermal method in some respects. The unique 2D structures have single-crystal framework with shortened path for Li ion transport. As a result, the N-doped 2D wavelike LTO with 0.6 wt.% of ‘carbon joint’ not only exhibits exciting capacity of ~180 and ~150 mA h g−1 for fast lithium storage at high discharge/charge rates of 1.7 and 8.5 A g−1 (10C and 50C) respectively, but also shows excellent low-temperature performance at −20°C. In addition, the cost may be further decreased due to recycled functional reagents. This novel nanostructured 2D LTO anode material makes it possible to develop safe fast-charging high-power lithium ion batteries. PMID:25985465

One-step methods for the prediction of orbital motion, taking its periodic components into account

NASA Astrophysics Data System (ADS)

Lavrov, K. N.

1988-03-01

The paper examines the design and analysis of the properties of implicit one-step integration methods which use the trigonometric approximation of ordinary differential equations containing periodic components. With reference to an orbital-motion prediction example, it is shown that the proposed schemes are more efficient in terms of computer memory than Everhart's (1974) approach. The results obtained make it possible to improve Everhart's method.

Methods, systems and devices for detecting and locating ferromagnetic objects

DOEpatents

Roybal, Lyle Gene [Idaho Falls, ID; Kotter, Dale Kent [Shelley, ID; Rohrbaugh, David Thomas [Idaho Falls, ID; Spencer, David Frazer [Idaho Falls, ID

2010-01-26

Methods for detecting and locating ferromagnetic objects in a security screening system. One method includes a step of acquiring magnetic data that includes magnetic field gradients detected during a period of time. Another step includes representing the magnetic data as a function of the period of time. Another step includes converting the magnetic data to being represented as a function of frequency. Another method includes a step of sensing a magnetic field for a period of time. Another step includes detecting a gradient within the magnetic field during the period of time. Another step includes identifying a peak value of the gradient detected during the period of time. Another step includes identifying a portion of time within the period of time that represents when the peak value occurs. Another step includes configuring the portion of time over the period of time to represent a ratio.

One-Step Extraction and Hydrolysis of Flavonoid Glycosides in Rape Bee Pollen Based on Soxhlet-Assisted Matrix Solid Phase Dispersion.

PubMed

Tu, Xijuan; Ma, Shuangqin; Gao, Zhaosheng; Wang, Jing; Huang, Shaokang; Chen, Wenbin

2017-11-01

Flavonoids are frequently found as glycosylated derivatives in plant materials. To determine contents of flavonoid aglycones in these matrices, procedures for the extraction and hydrolysis of flavonoid glycosides are required. The current sample preparation method is both labour and time consuming. Develop a modified matrix solid phase dispersion (MSPD) procedure as an alternative methodology for the one-step extraction and hydrolysis of flavonoid glycosides. HPLC-DAD was applied for demonstrating the one-step extraction and hydrolysis of flavonoids in rape bee pollen. The obtained contents of flavonoid aglycones (quercetin, kaempferol, isorhamnetin) were used for the optimisation and validation of the method. The extraction and hydrolysis were accomplished in one step. The procedure completes in 2 h with silica gel as dispersant, a 1:2 ratio of sample to dispersant, and 60% aqueous ethanol with 0.3 M hydrochloric acid as the extraction solution. The relative standard deviations (RSDs) of repeatability were less than 5%, and the recoveries at two fortified levels were between 88.3 and 104.8%. The proposed methodology is simple and highly efficient, with good repeatability and recovery. Compared with currently available methods, the present work has advantages of using less time and labour, higher extraction efficiency, and less consumption of the acid catalyst. This method may have applications for the one-step extraction and hydrolysis of bioactive compounds from plant materials. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

A Step Circuit Program.

ERIC Educational Resources Information Center

Herman, Susan

1995-01-01

Aerobics instructors can use step aerobics to motivate students. One creative method is to add the step to the circuit workout. By incorporating the step, aerobic instructors can accommodate various fitness levels. The article explains necessary equipment and procedures, describing sample stations for cardiorespiratory fitness, muscular strength,…

Methods of operation of apparatus measuring formation resistivity from within a cased well having one measurement and two compensation steps

DOEpatents

Vail, III, William B.

1993-01-01

Methods of operation of an apparatus having at least two pairs of voltage measurement electrodes vertically disposed in a cased well to measure the resistivity of adjacent geological formations from inside the cased well. During stationary measurements with the apparatus at a fixed vertical depth within the cased well, the invention herein discloses methods of operation which include a measurement step and subsequent first and second compensation steps respectively resulting in improved accuracy of measurement. First and second order errors of measurement are identified, and the measurement step and two compensation steps provide methods to substantially eliminate their influence on the results. A multiple frequency apparatus adapted to movement within the well is described which simultaneously provide the measurement and two compensation steps.

Voting strategy for artifact reduction in digital breast tomosynthesis.

PubMed

Wu, Tao; Moore, Richard H; Kopans, Daniel B

2006-07-01

Artifacts are observed in digital breast tomosynthesis (DBT) reconstructions due to the small number of projections and the narrow angular range that are typically employed in tomosynthesis imaging. In this work, we investigate the reconstruction artifacts that are caused by high-attenuation features in breast and develop several artifact reduction methods based on a "voting strategy." The voting strategy identifies the projection(s) that would introduce artifacts to a voxel and rejects the projection(s) when reconstructing the voxel. Four approaches to the voting strategy were compared, including projection segmentation, maximum contribution deduction, one-step classification, and iterative classification. The projection segmentation method, based on segmentation of high-attenuation features from the projections, effectively reduces artifacts caused by metal and large calcifications that can be reliably detected and segmented from projections. The other three methods are based on the observation that contributions from artifact-inducing projections have higher value than those from normal projections. These methods attempt to identify the projection(s) that would cause artifacts by comparing contributions from different projections. Among the three methods, the iterative classification method provides the best artifact reduction; however, it can generate many false positive classifications that degrade the image quality. The maximum contribution deduction method and one-step classification method both reduce artifacts well from small calcifications, although the performance of artifact reduction is slightly better with the one-step classification. The combination of one-step classification and projection segmentation removes artifacts from both large and small calcifications.

Searching for Sustainable and "Greener" Li-ion Batteries

ScienceCinema

Tarascon, Jean-Marie [University of Picardie at Aimens, France

2017-12-09

Lithium-ion batteries are strong candidates for powering upcoming generations of hybrid electric vehicles and plug-in hybrid electric vehicles. But improvements in safety must be achieved while keeping track of materials resources and abundances, as well as materials synthesis and recycling processes, all of which could inflict a heavy energy cost. Thus, electrode materials that have a minimum footprint in nature and are made via eco-efficient processes are sorely needed. The arrival of electrode materials based on minerals such as LiFePO4 (tryphilite) is a significant, but not sufficient, step toward the long-term demand for materials sustainability. The eco-efficient synthesis of LiFePO4 nanopowders via hydrothermal/ solvo-thermal processes using latent bases, structure directing templates, or other bio-related approaches will be presented in this talk. However, to secure sustainability and greeness, organic electrodes appear to be ideal candidates.... We took a fresh look at organic based electrodes; the results of this research into sequentially metal-organic-framework electrodes and Li-based organic electrodes (LixCyOz) will be reported and discussed.

Synthesis and properties of transition-metal arsenide nanostructures: From superparamagnetism to superconductivity

NASA Astrophysics Data System (ADS)

Desai, Prachi

This dissertation study focuses on developing new protocols for synthesis of nanostructured transition-metal pnictides including superconducting LiFeAs and studying their structure- property relationship. Nanostructured materials are known to differ in properties compared to their bulk counterparts owing to enhanced surface area and increased packing efficiency in devices. Synthetic chemistry skills and nanofabrication techniques like wet chemistry, electrodeposition, solvothermal, hydrothermal and lithography, are extremely useful for creating nanostructures of these functional materials. This is a challenging task simply because maintaining the phase composition same as that of the bulk material along with achieving nanostructures (nanoparticles, nanowires, nanopillars etc.) simultaneously is not easy. Papers I and II showcase novel synthesis methods for E based pnictides [EPn where E = 1st row transition elements and Pn = P, As etc.]. The superparamagnetism of transition-metal pnictides (e.g. FeAs, CoAs) nanomaterials obtained by this method have interesting magnetic features like high blocking temperatures and inter-particle magnetic exchange. Paper III, shows the concept of generalized protocol of EAs synthesis and discusses the principles behind this method. This protocol has been tested for applicability to not only FeAs, but also MnAs, CoAs and CrAs systems. Generalization of this method along with the discovery of superparamagnetic behavior in FeAs is one of the key findings of this research work. Alongside, paper IV shows the formation of Co3O4 nanowires through solid-solid conversion route aided by sacrificial templates.

Resonant frequency calculations using a hybrid perturbation-Galerkin technique

NASA Technical Reports Server (NTRS)

Geer, James F.; Andersen, Carl M.

1991-01-01

A two-step hybrid perturbation Galerkin technique is applied to the problem of determining the resonant frequencies of one or several degree of freedom nonlinear systems involving a parameter. In one step, the Lindstedt-Poincare method is used to determine perturbation solutions which are formally valid about one or more special values of the parameter (e.g., for large or small values of the parameter). In step two, a subset of the perturbation coordinate functions determined in step one is used in Galerkin type approximation. The technique is illustrated for several one degree of freedom systems, including the Duffing and van der Pol oscillators, as well as for the compound pendulum. For all of the examples considered, it is shown that the frequencies obtained by the hybrid technique using only a few terms from the perturbation solutions are significantly more accurate than the perturbation results on which they are based, and they compare very well with frequencies obtained by purely numerical methods.

Influence of the Preparation Method on Planar Perovskite CH3NH3PbI3-xClx Solar Cell Performance and Hysteresis

NASA Astrophysics Data System (ADS)

Ivanova, A.; Tokmakov, A.; Lebedeva, K.; Roze, M.; Kaulachs, I.

2017-08-01

Organometal halide perovskites are promising materials for lowcost, high-efficiency solar cells. The method of perovskite layer deposition and the interfacial layers play an important role in determining the efficiency of perovskite solar cells (PSCs). In the paper, we demonstrate inverted planar perovskite solar cells where perovskite layers are deposited by two-step modified interdiffusion and one-step methods. We also demonstrate how PSC parameters change by doping of charge transport layers (CTL). We used dimethylsupoxide (DMSO) as dopant for the hole transport layer (PEDOT:PSS) but for the electron transport layer [6,6]-phenyl C61 butyric acid methyl ester (PCBM)) we used N,N-dimethyl-N-octadecyl(3-aminopropyl)trimethoxysilyl chloride (DMOAP). The highest main PSC parameters (PCE, EQE, VOC) were obtained for cells prepared by the one-step method with fast crystallization and doped CTLs but higher fill factor (FF) and shunt resistance (Rsh) values were obtained for cells prepared by the two-step method with undoped CTLs.

Thiazolothiazole-linked porous organic polymers

DOE PAGES

Zhu, Xiang; Tian, Chengcheng; Jin, Tian; ...

2014-10-07

In this study, thiazolothiazole-linked porous organic polymers have been synthesized from a facile catalyst-free condensation reaction between aldehydes and dithiooxamide under solvothermal conditions. The resultant porous frameworks exhibit a highly selective uptake of CO 2 over N 2 under ambient conditions.

Systems and methods for short range RF communication

NASA Technical Reports Server (NTRS)

Hershey, John Erik (Inventor); Tomlinson, Harold Woodruff (Inventor); DeCristofaro, Richard Anthony (Inventor); Ross, John Anderson Fergus (Inventor); Sexton, Daniel White (Inventor)

2012-01-01

A method transmitting a message over at least one of a plurality of channels of a communications network is provided. The method comprises the steps of detecting a presence of jamming pulses in the at least one of the plurality of channels. The characteristics of the jamming pulses in the at least one of the plurality of channels is determined wherein the determined characteristics define at least interstices between the jamming pulses. The message is transmitted over the at least one of the plurality of channels wherein the message is transmitted within the interstices of the jamming pulse determined from the step of determining characteristics of the jamming pulses.

Defect engineering of two-dimensional WO3 nanosheets for enhanced electrochromism and photoeletrochemical performance

NASA Astrophysics Data System (ADS)

Zhou, Xiaofang; Zheng, Xiaoli; Yan, Bo; Xu, Tao; Xu, Qun

2017-04-01

The capability of introduction of oxygen vacancies in a controlled way has emerged as the heart of modern transition metal oxide semiconductor chemistry. As chemical defects, the oxygen vacancies have been proposed as electron donors, which are prone to increase carrier density and promote charge carrier separation. Herein, we have successfully prepared 2D WO3 ultrathin nanosheets with abundant surface oxygen vacancies by a combination of facile solvothermal reaction and hydrogenation method. The resultant hydrogenated WO3 ultrathin nanosheets exhibit remarkable electrochromism and photocatalytic performances compared with the non-hydrogenated samples, mainly due to their increased oxygen vacancies, narrowed band gap coupled with fast charge transfer and enhanced adsorption of visible light.

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

Photo-Fenton Degradation of Organic Dyes Based on a Fe₃O₄ Nanospheres/Biomass Composite Loaded Column.

PubMed

Zheng, Kai; Zhang, Jubo; Wang, Yan; Gao, Longxue; Di, Mingyu; Yuan, Fang; Bao, Wenhui; Yang, Tao; Liang, Daxin

2018-06-01

In order to deal with pollution of organic dyes, magnetic Fe3O4 nanospheres (NPs) with an average diameter of 202 ± 0.5 nm were synthesized by a solvothermal method at 200 °C, and they can efficiently degrade organic dyes (methylene blue (MB), rhodamine B (RhB) and xylenol orange (XO)) aqueous solutions (20 mg/L) within 1 min. Based on this Fenton reagent, Fe3O4 NPs/biomass composite degradation column was made using sawdust as substrate, and it can efficiently degrade organic dyes continually. More importantly, the composite can be regenerated just by an ultrasonic treatment, and its degradation performance almost remains the same.

Improved Reproducibility for Perovskite Solar Cells with 1 cm2 Active Area by a Modified Two-Step Process.

PubMed

Shen, Heping; Wu, Yiliang; Peng, Jun; Duong, The; Fu, Xiao; Barugkin, Chog; White, Thomas P; Weber, Klaus; Catchpole, Kylie R

2017-02-22

With rapid progress in recent years, organohalide perovskite solar cells (PSC) are promising candidates for a new generation of highly efficient thin-film photovoltaic technologies, for which up-scaling is an essential step toward commercialization. In this work, we propose a modified two-step method to deposit the CH 3 NH 3 PbI 3 (MAPbI 3 ) perovskite film that improves the uniformity, photovoltaic performance, and repeatability of large-area perovskite solar cells. This method is based on the commonly used two-step method, with one additional process involving treating the perovskite film with concentrated methylammonium iodide (MAI) solution. This additional treatment is proved to be helpful for tailoring the residual PbI 2 level to an optimal range that is favorable for both optical absorption and inhibition of recombination. Scanning electron microscopy and photoluminescence image analysis further reveal that, compared to the standard two-step and one-step methods, this method is very robust for achieving uniform and pinhole-free large-area films. This is validated by the photovoltaic performance of the prototype devices with an active area of 1 cm 2 , where we achieved the champion efficiency of ∼14.5% and an average efficiency of ∼13.5%, with excellent reproducibility.

One‐dimensional TiO2 Nanotube Photocatalysts for Solar Water Splitting

PubMed Central

Ge, Mingzheng; Li, Qingsong; Cao, Chunyan; Huang, Jianying; Li, Shuhui; Zhang, Songnan; Chen, Zhong; Zhang, Keqin; Al‐Deyab, Salem S.

2016-01-01

Hydrogen production from water splitting by photo/photoelectron‐catalytic process is a promising route to solve both fossil fuel depletion and environmental pollution at the same time. Titanium dioxide (TiO2) nanotubes have attracted much interest due to their large specific surface area and highly ordered structure, which has led to promising potential applications in photocatalytic degradation, photoreduction of CO2, water splitting, supercapacitors, dye‐sensitized solar cells, lithium‐ion batteries and biomedical devices. Nanotubes can be fabricated via facile hydrothermal method, solvothermal method, template technique and electrochemical anodic oxidation. In this report, we provide a comprehensive review on recent progress of the synthesis and modification of TiO2 nanotubes to be used for photo/photoelectro‐catalytic water splitting. The future development of TiO2 nanotubes is also discussed. PMID:28105391

Controllable synthesis of layered Co-Ni hydroxide hierarchical structures for high-performance hybrid supercapacitors

NASA Astrophysics Data System (ADS)

Yuan, Peng; Zhang, Ning; Zhang, Dan; Liu, Tao; Chen, Limiao; Ma, Renzhi; Qiu, Guanzhou; Liu, Xiaohe

2016-01-01

A facile solvothermal method is developed for synthesizing layered Co-Ni hydroxide hierarchical structures by using hexamethylenetetramine (HMT) as alkaline reagent. The electrochemical measurements reveal that the specific capacitances of layered bimetallic (Co-Ni) hydroxides are generally superior to those of layered monometallic (Co, Ni) hydroxides. The as-prepared Co0.5Ni0.5 hydroxide hierarchical structures possesses the highest specific capacitance of 1767 F g-1 at a galvanic current density of 1 A g-1 and an outstanding specific capacitance retention of 87% after 1000 cycles. In comparison with the dispersed nanosheets of Co-Ni hydroxide, layered hydroxide hierarchical structures show much superior electrochemical performance. This study provides a promising method to construct hierarchical structures with controllable transition-metal compositions for enhancing the electrochemical performance in hybrid supercapacitors.

Contact formation and gettering of precipitated impurities by multiple firing during semiconductor device fabrication

DOEpatents

Sopori, Bhushan

2014-05-27

Methods for contact formation and gettering of precipitated impurities by multiple firing during semiconductor device fabrication are provided. In one embodiment, a method for fabricating an electrical semiconductor device comprises: a first step that includes gettering of impurities from a semiconductor wafer and forming a backsurface field; and a second step that includes forming a front contact for the semiconductor wafer, wherein the second step is performed after completion of the first step.

One-step formation of w/o/w multiple emulsions stabilized by single amphiphilic block copolymers.

PubMed

Hong, Liangzhi; Sun, Guanqing; Cai, Jinge; Ngai, To

2012-02-07

Multiple emulsions are complex polydispersed systems in which both oil-in-water (O/W) and water-in-oil (W/O) emulsion exists simultaneously. They are often prepared accroding to a two-step process and commonly stabilized using a combination of hydrophilic and hydrophobic surfactants. Recently, some reports have shown that multiple emulsions can also be produced through one-step method with simultaneous occurrence of catastrophic and transitional phase inversions. However, these reported multiple emulsions need surfactant blends and are usually described as transitory or temporary systems. Herein, we report a one-step phase inversion process to produce water-in-oil-in-water (W/O/W) multiple emulsions stabilized solely by a synthetic diblock copolymer. Unlike the use of small molecule surfactant combinations, block copolymer stabilized multiple emulsions are remarkably stable and show the ability to separately encapsulate both polar and nonpolar cargos. The importance of the conformation of the copolymer surfactant at the interfaces with regards to the stability of the multiple emulsions using the one-step method is discussed.

Trimming Line Design using New Development Method and One Step FEM

NASA Astrophysics Data System (ADS)

Chung, Wan-Jin; Park, Choon-Dal; Yang, Dong-yol

2005-08-01

In most of automobile panel manufacturing, trimming is generally performed prior to flanging. To find feasible trimming line is crucial in obtaining accurate edge profile after flanging. Section-based method develops blank along section planes and find trimming line by generating loop of end points. This method suffers from inaccurate results for regions with out-of-section motion. On the other hand, simulation-based method can produce more accurate trimming line by iterative strategy. However, due to limitation of time and lack of information in initial die design, it is still not widely accepted in the industry. In this study, new fast method to find feasible trimming line is proposed. One step FEM is used to analyze the flanging process because we can define the desired final shape after flanging and most of strain paths are simple in flanging. When we use one step FEM, the main obstacle is the generation of initial guess. Robust initial guess generation method is developed to handle bad-shaped mesh, very different mesh size and undercut part. The new method develops 3D triangular mesh in propagational way from final mesh onto the drawing tool surface. Also in order to remedy mesh distortion during development, energy minimization technique is utilized. Trimming line is extracted from the outer boundary after one step FEM simulation. This method shows many benefits since trimming line can be obtained in the early design stage. The developed method is successfully applied to the complex industrial applications such as flanging of fender and door outer.

Stability analysis of Eulerian-Lagrangian methods for the one-dimensional shallow-water equations

USGS Publications Warehouse

Casulli, V.; Cheng, R.T.

1990-01-01

In this paper stability and error analyses are discussed for some finite difference methods when applied to the one-dimensional shallow-water equations. Two finite difference formulations, which are based on a combined Eulerian-Lagrangian approach, are discussed. In the first part of this paper the results of numerical analyses for an explicit Eulerian-Lagrangian method (ELM) have shown that the method is unconditionally stable. This method, which is a generalized fixed grid method of characteristics, covers the Courant-Isaacson-Rees method as a special case. Some artificial viscosity is introduced by this scheme. However, because the method is unconditionally stable, the artificial viscosity can be brought under control either by reducing the spatial increment or by increasing the size of time step. The second part of the paper discusses a class of semi-implicit finite difference methods for the one-dimensional shallow-water equations. This method, when the Eulerian-Lagrangian approach is used for the convective terms, is also unconditionally stable and highly accurate for small space increments or large time steps. The semi-implicit methods seem to be more computationally efficient than the explicit ELM; at each time step a single tridiagonal system of linear equations is solved. The combined explicit and implicit ELM is best used in formulating a solution strategy for solving a network of interconnected channels. The explicit ELM is used at channel junctions for each time step. The semi-implicit method is then applied to the interior points in each channel segment. Following this solution strategy, the channel network problem can be reduced to a set of independent one-dimensional open-channel flow problems. Numerical results support properties given by the stability and error analyses. ?? 1990.

Deferred discrimination algorithm (nibbling) for target filter management

NASA Astrophysics Data System (ADS)

Caulfield, H. John; Johnson, John L.

1999-07-01

A new method of classifying objects is presented. Rather than trying to form the classifier in one step or in one training algorithm, it is done in a series of small steps, or nibbles. This leads to an efficient and versatile system that is trained in series with single one-shot examples but applied in parallel, is implemented with single layer perceptrons, yet maintains its fully sequential hierarchical structure. Based on the nibbling algorithm, a basic new method of target reference filter management is described.

One step linear reconstruction method for continuous wave diffuse optical tomography

NASA Astrophysics Data System (ADS)

Ukhrowiyah, N.; Yasin, M.

2017-09-01

The method one step linear reconstruction method for continuous wave diffuse optical tomography is proposed and demonstrated for polyvinyl chloride based material and breast phantom. Approximation which used in this method is selecting regulation coefficient and evaluating the difference between two states that corresponding to the data acquired without and with a change in optical properties. This method is used to recovery of optical parameters from measured boundary data of light propagation in the object. The research is demonstrated by simulation and experimental data. Numerical object is used to produce simulation data. Chloride based material and breast phantom sample is used to produce experimental data. Comparisons of results between experiment and simulation data are conducted to validate the proposed method. The results of the reconstruction image which is produced by the one step linear reconstruction method show that the image reconstruction almost same as the original object. This approach provides a means of imaging that is sensitive to changes in optical properties, which may be particularly useful for functional imaging used continuous wave diffuse optical tomography of early diagnosis of breast cancer.

Optimization of one-step in situ transesterification method for accurate quantification of EPA in Nannochloropsis gaditana

DOE PAGES

Tang, Yuting; Zhang, Yue; Rosenberg, Julian N.; ...

2016-11-08

Microalgae are a valuable source of lipid feedstocks for biodiesel and valuable omega-3 fatty acids. Nannochloropsis gaditana has emerged as a promising producer of eicosapentaenoic acid (EPA) due to its fast growth rate and high EPA content. In the present study, the fatty acid profile of Nannochloropsis gaditana was found to be naturally high in EPA and devoid of docosahexaenoic acid (DHA), thereby providing an opportunity to maximize the efficacy of EPA production. Using an optimized one-step in situ transesterification method (methanol:biomass = 90 mL/g; HCl 5% by vol.; 70 °C; 1.5 h), the maximum fatty acid methyl ester (FAME)more » yield of Nannochloropsis gaditana cultivated under rich condition was quantified as 10.04% ± 0.08% by weight with EPA-yields as high as 4.02% ± 0.17% based on dry biomass. The total FAME and EPA yields were 1.58- and 1.23-fold higher separately than that obtained using conventional two-step method (solvent system: methanol and chloroform). Furthermore, this one-step in situ method provides a fast and simple method to measure fatty acid methyl ester (FAME) yields and could serve as a promising method to generate eicosapentaenoic acid methyl ester from microalgae.« less

Optimization of one-step in situ transesterification method for accurate quantification of EPA in Nannochloropsis gaditana

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

Tang, Yuting; Zhang, Yue; Rosenberg, Julian N.

Microalgae are a valuable source of lipid feedstocks for biodiesel and valuable omega-3 fatty acids. Nannochloropsis gaditana has emerged as a promising producer of eicosapentaenoic acid (EPA) due to its fast growth rate and high EPA content. In the present study, the fatty acid profile of Nannochloropsis gaditana was found to be naturally high in EPA and devoid of docosahexaenoic acid (DHA), thereby providing an opportunity to maximize the efficacy of EPA production. Using an optimized one-step in situ transesterification method (methanol:biomass = 90 mL/g; HCl 5% by vol.; 70 °C; 1.5 h), the maximum fatty acid methyl ester (FAME)more » yield of Nannochloropsis gaditana cultivated under rich condition was quantified as 10.04% ± 0.08% by weight with EPA-yields as high as 4.02% ± 0.17% based on dry biomass. The total FAME and EPA yields were 1.58- and 1.23-fold higher separately than that obtained using conventional two-step method (solvent system: methanol and chloroform). Furthermore, this one-step in situ method provides a fast and simple method to measure fatty acid methyl ester (FAME) yields and could serve as a promising method to generate eicosapentaenoic acid methyl ester from microalgae.« less

Aluminum-doped ceria-zirconia solid solutions with enhanced thermal stability and high oxygen storage capacity.

PubMed

Dong, Qiang; Yin, Shu; Guo, Chongshen; Sato, Tsugio

2012-10-01

A facile solvothermal method to synthesize aluminum-doped ceria-zirconia (Ce0.5Zr0.5-xAlxO2-x/2, x = 0.1 to 0.4) solid solutions was carried out using Ce(NH4)2(NO3)6, Zr(NO3)3·2H2O Al(NO3)3·9H2O, and NH4OH as the starting materials at 200°C for 24 h. The obtained solid solutions from the solvothermal reaction were calcined at 1,000°C for 20 h in air atmosphere to evaluate the thermal stability. The synthesized Ce0.5Zr0.3Al0.2O1.9 particle was characterized for the oxygen storage capacity (OSC) in automotive catalysis. For the characterization, X-ray diffraction, transmission electron microscopy, and the Brunauer-Emmet-Teller (BET) technique were employed. The OSC values of all samples were measured at 600°C using thermogravimetric-differential thermal analysis. Ce0.5Zr0.3Al0.2O1.9 solid solutions calcined at 1,000°C for 20 h with a BET surface area of 18 m2 g-1 exhibited a considerably high OSC of 427 μmol-O g-1 and good OSC performance stability. The same synthesis route was employed for the preparation of the CeO2 and Ce0.5Zr0.5O2. The incorporation of aluminum ion in the lattice of ceria-based catalyst greatly enhanced the thermal stability and OSC.

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

Yao, Kaisheng; Henan Normal University, School of Chemistry and Environmental Science, Key Laboratory of Green Chemical Media and Reactions, Xin xiang, Henan 453007; Lu, Weiwei

A novel method was proposed for successful fabrication of CuS nanostructures with various morphologies. At the ionic liquids (ILs)-modulated CHCl{sub 3}-H{sub 2}O interface, copper cupferronate [Cu(cup){sub 2}] in CHCl{sub 3} reacted with thiourea in water to generate CuS nanostructures via a solvothermal reaction process. The effects of alkyl chain length of imidazolium cations and nature of anions of the ILs, molar ratio of Cu(cup){sub 2} to thiourea, the reaction temperature and time on the morphology of the products were studied systematically. It was shown that by changing alkyl chain length of imidazolium cations and nature of anions of the ILs,more » CuS nanostructures with various morphologies, including flowers, urchins, large nanodisks and nanoparticles, could be obtained at the liquid-liquid interface, and the ILs played important template roles in directing the formation of CuS nanostructures. Furthermore, the as-prepared CuS samples exhibited high catalytic activity for photodegradation of methyl orange and thermal decomposition of ammonium perchlorate. - Graphical abstract: At the ionic liquids-modulated CHCl{sub 3}-H{sub 2}O interface, the CuS nanostructures with the various morphologies of flowers, urchins, large nanodisks and nanoparticles have been successfully prepared via a solvothermal reaction process. Highlights: Black-Right-Pointing-Pointer The properties of oil-H{sub 2}O interface can be modulated by employing different ILs. Black-Right-Pointing-Pointer The modulated interface has been used to prepare CuS nanostructures with various morphologies. Black-Right-Pointing-Pointer The CuS samples exhibited high catalytic activity for the photodegradation of methyl orange.« less

The influence of tightening sequence and method on screw preload in implant superstructures.

PubMed

Al-Sahan, Maha M; Al Maflehi, Nassr S; Akeel, Riyadh F

2014-01-01

This study evaluated the effect of six screw-tightening sequences and two tightening methods on the screw preload in implant-supported superstructures. The preload was measured using strain gauges following the screw tightening of a metal framework connected to four implants. The experiment included six sequences ([1] 1-2-3-4, [2] 4-2-3-1, [3] 4-3-1-2, [4] 1-4-2-3, [5] 2-3-4-1, and [6] 3-2-4-1), two methods (onestep, three-step), and five replications. Significant differences were found between tightening sequences and methods. In the three-step method, a higher total preload was found in sequences 2 (312 ± 85 N), 3 (246 ± 54 N), and 4 (310 ± 96 N). In the one-step method, a higher total preload was found in sequences 1 (286 ± 94 N), 5 (764 ± 142 N), and 6 (350 ± 69 N). It is concluded that the highest total screw preload was achieved when anterior implants of the superstructure were first tightened in one step, followed by posterior implants.

Method and system for determining the torque required to launch a vehicle having a hybrid drive-train

DOEpatents

Hughes, Douglas A.

2006-04-04

A method and system are provided for determining the torque required to launch a vehicle having a hybrid drive-train that includes at least two independently operable prime movers. The method includes the steps of determining the value of at least one control parameter indicative of a vehicle operating condition, determining the torque required to launch the vehicle from the at least one determined control parameter, comparing the torque available from the prime movers to the torque required to launch the vehicle, and controlling operation of the prime movers to launch the vehicle in response to the comparing step. The system of the present invention includes a control unit configured to perform the steps of the method outlined above.

Solvothermal synthesis of Zn{sub 2}GeO{sub 4}:Mn{sup 2+} nanophosphor in water/diethylene glycol system

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

Takeshita, Satoru; Honda, Joji; Isobe, Tetsuhiko, E-mail: isobe@applc.keio.ac.jp

2012-05-15

The influence of aging of the suspension containing the amorphous precusors on structural, compositional and photoluminescent properties is studied to understand the mechanism on the formation of Zn{sub 2}GeO{sub 4}:Mn{sup 2+} nanoparticles during the solvothermal reaction in the water/diethylene glycol mixed solvent. Aging at 200 Degree-Sign C for 20 min forms the crystalline Zn{sub 2}GeO{sub 4} nanorods and then they grow up to {approx} 50 nm in mean length after aging for 240 min. Their interplanar spacing of (410) increases with increasing the aging time. The photoluminescence intensity corresponding to the d-d transition of Mn{sup 2+} increases with increasing themore » aging time up to 120 min, and then decreases after aging for 240 min. The photoluminescence lifetime decreases with increasing the aging time, indicating the locally concentrated Mn{sup 2+} ions. These results reveal that Mn{sup 2+} ions gradually replace Zn{sup 2+} ions near surface through repeating dissolusion and precipitation processes during prolonged aging after the complete crystallization of Zn{sub 2}GeO{sub 4}. - Graphical abstract: TEM images of Zn{sub 2}GeO{sub 4}:Mn{sup 2+} nanoparticles aged at 200 Degree-Sign C for different aging times in the mixed solvent of water and diethylene glycol. Highlights: Black-Right-Pointing-Pointer Mechanism on formation of Zn{sub 2}GeO{sub 4}:Mn{sup 2+} nanophosphor under solvothermal condition. Black-Right-Pointing-Pointer Zn{sub 2}GeO{sub 4} nanorods crystallize via amorphous precursors. Black-Right-Pointing-Pointer Gradual substitution of Mn{sup 2+} during prolonged aging. Black-Right-Pointing-Pointer Such an inhomogeneous Mn{sup 2+} doping process results in concentration quenching.« less

Scheduled Peripheral Component Interconnect Arbiter

NASA Technical Reports Server (NTRS)

Nixon, Scott Alan (Inventor)

2015-01-01

Systems and methods are described for arbitrating access of a communication bus. In one embodiment, a method includes performing steps on one or more processors. The steps include: receiving an access request from a device of the communication bus; evaluating a bus schedule to determine an importance of the device based on the access request; and selectively granting access of the communication bus to the device based on the importance of the device.

Accurate upwind methods for the Euler equations

NASA Technical Reports Server (NTRS)

Huynh, Hung T.

1993-01-01

A new class of piecewise linear methods for the numerical solution of the one-dimensional Euler equations of gas dynamics is presented. These methods are uniformly second-order accurate, and can be considered as extensions of Godunov's scheme. With an appropriate definition of monotonicity preservation for the case of linear convection, it can be shown that they preserve monotonicity. Similar to Van Leer's MUSCL scheme, they consist of two key steps: a reconstruction step followed by an upwind step. For the reconstruction step, a monotonicity constraint that preserves uniform second-order accuracy is introduced. Computational efficiency is enhanced by devising a criterion that detects the 'smooth' part of the data where the constraint is redundant. The concept and coding of the constraint are simplified by the use of the median function. A slope steepening technique, which has no effect at smooth regions and can resolve a contact discontinuity in four cells, is described. As for the upwind step, existing and new methods are applied in a manner slightly different from those in the literature. These methods are derived by approximating the Euler equations via linearization and diagonalization. At a 'smooth' interface, Harten, Lax, and Van Leer's one intermediate state model is employed. A modification for this model that can resolve contact discontinuities is presented. Near a discontinuity, either this modified model or a more accurate one, namely, Roe's flux-difference splitting. is used. The current presentation of Roe's method, via the conceptually simple flux-vector splitting, not only establishes a connection between the two splittings, but also leads to an admissibility correction with no conditional statement, and an efficient approximation to Osher's approximate Riemann solver. These reconstruction and upwind steps result in schemes that are uniformly second-order accurate and economical at smooth regions, and yield high resolution at discontinuities.

Method for non-referential defect characterization using fractal encoding and active contours

DOEpatents

Gleason, Shaun S [Knoxville, TN; Sari-Sarraf, Hamed [Lubbock, TX

2007-05-15

A method for identification of anomalous structures, such as defects, includes the steps of providing a digital image and applying fractal encoding to identify a location of at least one anomalous portion of the image. The method does not require a reference image to identify the location of the anomalous portion. The method can further include the step of initializing an active contour based on the location information obtained from the fractal encoding step and deforming an active contour to enhance the boundary delineation of the anomalous portion.

Solution of elliptic PDEs by fast Poisson solvers using a local relaxation factor

NASA Technical Reports Server (NTRS)

Chang, Sin-Chung

1986-01-01

A large class of two- and three-dimensional, nonseparable elliptic partial differential equations (PDEs) is presently solved by means of novel one-step (D'Yakanov-Gunn) and two-step (accelerated one-step) iterative procedures, using a local, discrete Fourier analysis. In addition to being easily implemented and applicable to a variety of boundary conditions, these procedures are found to be computationally efficient on the basis of the results of numerical comparison with other established methods, which lack the present one's: (1) insensitivity to grid cell size and aspect ratio, and (2) ease of convergence rate estimation by means of the coefficient of the PDE being solved. The two-step procedure is numerically demonstrated to outperform the one-step procedure in the case of PDEs with variable coefficients.

[Application of ordinary Kriging method in entomologic ecology].

PubMed

Zhang, Runjie; Zhou, Qiang; Chen, Cuixian; Wang, Shousong

2003-01-01

Geostatistics is a statistic method based on regional variables and using the tool of variogram to analyze the spatial structure and the patterns of organism. In simulating the variogram within a great range, though optimal simulation cannot be obtained, the simulation method of a dialogue between human and computer can be used to optimize the parameters of the spherical models. In this paper, the method mentioned above and the weighted polynomial regression were utilized to simulate the one-step spherical model, the two-step spherical model and linear function model, and the available nearby samples were used to draw on the ordinary Kriging procedure, which provided a best linear unbiased estimate of the constraint of the unbiased estimation. The sum of square deviation between the estimating and measuring values of varying theory models were figured out, and the relative graphs were shown. It was showed that the simulation based on the two-step spherical model was the best simulation, and the one-step spherical model was better than the linear function model.

Theory and computation of optimal low- and medium-thrust transfers

NASA Technical Reports Server (NTRS)

Chuang, C.-H.

1994-01-01

This report describes the current state of development of methods for calculating optimal orbital transfers with large numbers of burns. Reported on first is the homotopy-motivated and so-called direction correction method. So far this method has been partially tested with one solver; the final step has yet to be implemented. Second is the patched transfer method. This method is rooted in some simplifying approximations made on the original optimal control problem. The transfer is broken up into single-burn segments, each single-burn solved as a predictor step and the whole problem then solved with a corrector step.

Synthesis, structural characterization and high pressure phase transitions of monolithium hydronium sulfate

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

Banerjee, Debasis, E-mail: debasis.banerjee@stonybrook.edu; Plonka, Anna M.; Kim, Sun Jin

2013-01-15

A three dimensional lithium hydronium sulfate LiSO{sub 4}{center_dot}H{sub 3}O [1], [space group Pna2{sub 1}a=8.7785(12) A, b=9.1297(12) A, c=5.2799(7) A, V=423.16(10) A{sup 3}] was synthesized via solvothermal methods using 1,5-naphthalenedisulfonic acid (1,5-NSA) as the source of sulfate ions. The structure of [1], determined by single crystal X-ray diffraction techniques, consists of corner sharing LiO{sub 4} and SO{sub 4} tetrahedra, forming an anionic 3-D open framework that is charge balanced by hydronium ions positioned within channels running along [001] and forming strong H-bonding with the framework oxygen atoms. Compound [1] undergoes two reversible phase transitions, involving reorientation of SO{sub 4}{sup 2-} ionsmore » at pressures of approximately 2.5 and 5 GPa at room temperature, as evident from characteristic discontinuous frequency drops in the {nu}{sub 1} mode of the Raman spectra. Additionally, compound [1] forms dense {beta}-lithium sulfate at 300 Degree-Sign C, as evident from temperature dependent powder XRD and combined reversible TGA-DSC experiments. - Graphical abstract: Left: View of corner-shared LiO{sub 4} and SO{sub 4} tetrahedra along [001] direction with hydronium ions situated in the channels. Right: (a) Photograph of the loaded DAC (b) Ambient pressure Raman spectrum of compound [1] (c) Evolution of the {nu}{sub 1} mode with the increasing and decreasing pressure indicating transitions to high-pressure phases at {approx}2.5 (red curves) and {approx}5 GPa (blue curves) and at {approx}3.5 GPa upon decompression. Highlights: Black-Right-Pointing-Pointer A 3-D lithium hydronium sulfate is synthesized by solvothermal methods. Black-Right-Pointing-Pointer Two high pressure phase transition occurs due to rotation of sulfate groups. Black-Right-Pointing-Pointer The framework undergoes a high temperature structural transformation, to form {beta}-Li{sub 2}SO{sub 4} phase.« less

Agarose encapsulated mesoporous carbonated hydroxyapatite nanocomposites powder for drug delivery.

PubMed

Kolanthai, Elayaraja; Abinaya Sindu, P; Thanigai Arul, K; Sarath Chandra, V; Manikandan, E; Narayana Kalkura, S

2017-01-01

The powder composites are predominantly used for filling of voids in bone and as drug delivery carrier to prevent the infection or inflammatory reaction in the damaged tissues. The objective of this work was to study the synthesis of agarose encapsulation on carbonated hydroxyapatite powder and their biological and drug delivery properties. Mesoporous, nanosized carbonated hydroxyapatite/agarose (CHAp/agarose) powder composites were prepared by solvothermal method and subsequently calcined to study the physico-chemical changes, if it subjected to thermal exposure. The phase of the as-synthesized powder was CHAp/agarose whereas the calcinated samples were non-stoichiometric HAp. The CHAp/agarose nanorods were of length 10-80nm and width 40-190nm for the samples synthesized at temperatures 120°C (ST120) and 150°C (ST150). The calcination process produced spheres (10-50nm) and rods with reduced size (40-120nm length and 20-30nm width). Composites were partially dissolved in SBF solution followed by exhibited better bioactivity than non-stoichiometric HAp confirmed by gravimetric method. Hemo and biocompatibility remained unaffected by presence of agarose or carbonate in the HAp. Specific surface area of the composites was high and exhibited an enhanced amoxicillin and 5-fluorouracil release than the calcined samples. The composites demonstrated a strong antimicrobial activity against E. coli, S. aureus and S. epidermidis. The ST120 showed prolonged drug (AMX and 5-Fcil) release and antimicrobial efficacy than ST150 and calcined samples. This technique would be simple and rapid for composites preparation, to produce high quality crystalline, resorbable, mesoporous and bioactive nanocomposite (CHAp/agarose) powders. This work provides new insight into the role of agarose coated on bioceramics by solvothermal technique and suggests that CHAp/agarose composites powders are promising materials for filling of void in bone and drug delivery applications. Copyright © 2016 Elsevier B.V. All rights reserved.

Assessing the foundation of the Trojan Horse Method

NASA Astrophysics Data System (ADS)

Bertulani, C. A.; Hussein, M. S.; Typel, S.

2018-01-01

We discuss the foundation of the Trojan Horse Method (THM) within the Inclusive Non-Elastic Breakup (INEB) theory. We demonstrate that the direct part of the INEB cross section, which is of two-step character, becomes, in the DWBA limit of the three-body theory with appropriate approximations and redefinitions, similar in structure to the one-step THM cross section. We also discuss the connection of the THM to the Surrogate Method (SM), which is a genuine two-step process.

Synthesis, characterization and photocatalytic activity of magnetically separable hexagonal Ni/ZnO nanostructure

NASA Astrophysics Data System (ADS)

Senapati, Samarpita; Srivastava, Suneel K.; Singh, Shiv B.

2012-09-01

The hexagonal zinc oxide coated nickel (Ni/ZnO) nanostructure photocatalyst has successfully been prepared by the reduction of nickel chloride hexahydrate using hydrazine hydrate through the solvothermal process at 140 °C followed by surface modification of the product by the reflux method at 110 °C for 1 h. The X-ray diffraction (XRD) pattern showed that the `as prepared' sample consists of face centered cubic Ni and hexagonal wurtzite ZnO without any traces of impurity. Field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM) images confirmed the formation of nickel nanoparticles under solvothermal conditions. These nickel nanoparticles, when subjected to reflux, formed the hexagonal zinc oxide coated nickel nanostructure. Fourier transform infrared (FTIR) spectra, photoluminescence (PL) and Raman studies also confirmed the presence of zinc oxide in the hybrid nanostructure. The growth mechanism for the development of the hexagonal zinc oxide coated nickel (Ni/ZnO) nanostructure has also been proposed. The appearance of the hysteresis loop, in the as-prepared Ni/ZnO hybrid nanostructure, demonstrated its ferromagnetic character at room temperature. The hexagonal Ni/ZnO nanostructure also acts as an efficient photocatalyst in the degradation of methylene blue under ultraviolet light irradiation. It is observed that the catalytic efficiency of the hybrid nanocatalyst is better compared to pure zinc oxide. Most importantly, the Ni/ZnO catalyst could also be easily separated, simply by applying an external magnetic field, and reused.The hexagonal zinc oxide coated nickel (Ni/ZnO) nanostructure photocatalyst has successfully been prepared by the reduction of nickel chloride hexahydrate using hydrazine hydrate through the solvothermal process at 140 °C followed by surface modification of the product by the reflux method at 110 °C for 1 h. The X-ray diffraction (XRD) pattern showed that the `as prepared' sample consists of face centered cubic Ni and hexagonal wurtzite ZnO without any traces of impurity. Field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM) images confirmed the formation of nickel nanoparticles under solvothermal conditions. These nickel nanoparticles, when subjected to reflux, formed the hexagonal zinc oxide coated nickel nanostructure. Fourier transform infrared (FTIR) spectra, photoluminescence (PL) and Raman studies also confirmed the presence of zinc oxide in the hybrid nanostructure. The growth mechanism for the development of the hexagonal zinc oxide coated nickel (Ni/ZnO) nanostructure has also been proposed. The appearance of the hysteresis loop, in the as-prepared Ni/ZnO hybrid nanostructure, demonstrated its ferromagnetic character at room temperature. The hexagonal Ni/ZnO nanostructure also acts as an efficient photocatalyst in the degradation of methylene blue under ultraviolet light irradiation. It is observed that the catalytic efficiency of the hybrid nanocatalyst is better compared to pure zinc oxide. Most importantly, the Ni/ZnO catalyst could also be easily separated, simply by applying an external magnetic field, and reused. Electronic supplementary information (ESI) available: Fig. S1 Ni/ZnO hybrid nanostructure prepared using (a) 0.195 and (b) 0.25 M [Zn2+] at 90 °C Fig. S2 FTIR spectra of nickel nanoparticles prepared at 140 °C (a), and Ni/ZnO hybrid nanostructure prepared using (b) 0.063, (c) 0.125, (d) 0.195 and (e) 0.25 M [Zn2+]; Fig. S3 Raman spectra of Ni/ZnO nanostructure prepared using (a) 0.063, (b) 0.125, (c) 0.195 and (d) 0.25 M [Zn2+]; Fig. S4 Room temperature PL spectra of (a) ZnO and (b) Ni/ZnO nanostructure prepared using 0.25 M [Zn2+]. See DOI: 10.1039/c2nr31831h

The effect of different screw-tightening techniques on the stress generated on an internal-connection implant superstructure.

PubMed

Choi, Jung-Han; Lim, Young-Jun; Kim, Chang-Whe; Kim, Myung-Joo

2009-01-01

This study evaluated the effect of different screw-tightening sequences, forces, and methods on the stresses generated on a well-fitting internal-connection implant (Astra Tech) superstructure. A metal framework directly connected to four parallel implants was fabricated on a fully edentulous mandibular resin model. Six stone casts with four implant replicas were made from a pickup impression of the superstructure to represent a "well-fitting" situation. Stresses generated by four screw-tightening sequences (1-2-3-4, 4-3-2-1, 2-4-3-1, and 2-3-1-4), two forces (10 and 20 Ncm), and two methods (one-step and two-step) were evaluated. In the two-step method, screws were tightened to the initial torque (10 Ncm) in a predetermined screw-tightening sequence and then to the final torque (20 Ncm) in the same sequence. Stresses were recorded twice by three strain gauges attached to the framework (superior face midway between abutments). Deformation data were analyzed using multiple analysis of variance at a .05 level of statistical significance. In all stone casts, stresses were produced by the superstructure connection, regardless of screw-tightening sequence, force, and method. No statistically significant differences for superstructure preload stresses were found based on screw-tightening sequences (-180.0 to -181.6 microm/m) or forces (-163.4 and -169.2 microm/m) (P > .05). However, different screw-tightening methods induced different stresses on the superstructure. The two-step screw-tightening method (-180.1 microm/m) produced significantly higher stress than the one-step method (-169.2 microm/m) (P = .0457). Within the limitations of this in vitro study, screw-tightening sequence and force were not critical factors in the stress generated on a well-fitting internal-connection implant superstructure. The stress caused by the two-step method was greater than that produced using the one-step method. Further studies are needed to evaluate the effect of screw-tightening techniques on preload stress in various different clinical situations.

A [Ce21] keplerate.

PubMed

Canaj, Angelos B; Siczek, Milosz; Lis, Tadeusz; Murrie, Mark; Brechin, Euan K; Milios, Constantinos J

2017-06-28

The solvothermal reaction between Ce(NO 3 ) 3 ·6H 2 O, 2-amino-isobutyric acid, 2-hydroxy-1-naphthaldehyde and 2-amino-2-methyl-1,3-propanediol in MeOH, in the presence of base, leads to the formation of a unique [CeCe ] keplerate cage.

Comparison of IMRT planning with two-step and one-step optimization: a strategy for improving therapeutic gain and reducing the integral dose

NASA Astrophysics Data System (ADS)

Abate, A.; Pressello, M. C.; Benassi, M.; Strigari, L.

2009-12-01

The aim of this study was to evaluate the effectiveness and efficiency in inverse IMRT planning of one-step optimization with the step-and-shoot (SS) technique as compared to traditional two-step optimization using the sliding windows (SW) technique. The Pinnacle IMRT TPS allows both one-step and two-step approaches. The same beam setup for five head-and-neck tumor patients and dose-volume constraints were applied for all optimization methods. Two-step plans were produced converting the ideal fluence with or without a smoothing filter into the SW sequence. One-step plans, based on direct machine parameter optimization (DMPO), had the maximum number of segments per beam set at 8, 10, 12, producing a directly deliverable sequence. Moreover, the plans were generated whether a split-beam was used or not. Total monitor units (MUs), overall treatment time, cost function and dose-volume histograms (DVHs) were estimated for each plan. PTV conformality and homogeneity indexes and normal tissue complication probability (NTCP) that are the basis for improving therapeutic gain, as well as non-tumor integral dose (NTID), were evaluated. A two-sided t-test was used to compare quantitative variables. All plans showed similar target coverage. Compared to two-step SW optimization, the DMPO-SS plans resulted in lower MUs (20%), NTID (4%) as well as NTCP values. Differences of about 15-20% in the treatment delivery time were registered. DMPO generates less complex plans with identical PTV coverage, providing lower NTCP and NTID, which is expected to reduce the risk of secondary cancer. It is an effective and efficient method and, if available, it should be favored over the two-step IMRT planning.

Solvothermal syntheses and characterization of three new silver(I)/copper(I)-thioarsenates based on As2+/As3+ ions

NASA Astrophysics Data System (ADS)

Yao, Hua-Gang; Tang, Cheng-Fei; An, Yong-Lin; Ou, Zi-Jian; Wu, Guo-Hao; Lan, Pei; Zheng, Yi-Long

2017-02-01

Three new silver(I)/copper(I)-thioarsenates KAgAsIIS2 (1), RbCu2AsIIIS3 (2) and RbCu4AsIIIS4 (3) have been solvothermally synthesized and structurally characterized. 1 exhibits a two-dimensional anionic network built up by As-As bond connecting the left- and right-handed helical [AgS2]4- chains, and represents the first examples of thioarsenates(II). The structure of 2 consists of two kinds of helical [Cu2S3]4- chains linked by the arsenic atoms to form double layers with rubidium ions between the layers. Compound 3 is built up of infinite [Cu2S2]2- chain and layered [Cu6As2S6] linked to form a three-dimensional anionic framework, [Cu4AsS4]-, and containing channels in which the rubidium cations reside. The optical properties of 1-3 have been investigated by UV-vis spectroscopy.

Positron annihilation spectroscopic studies of solvothermally synthesized ZnO nanobipyramids and nanoparticles

NASA Astrophysics Data System (ADS)

Ghoshal, Tandra; Biswas, Subhajit; Kar, Soumitra; Chaudhuri, Subhadra; Nambissan, P. M. G.

2008-02-01

Zinc oxide (ZnO) samples in the form of hexagonal-based bipyramids and particles of nanometer dimensions were synthesized through solvothermal route and characterized by x-ray diffraction and transmission electron microscopy. Positron annihilation experiments were performed to study the structural defects such as vacancies and surfaces in these nanosystems. From coincidence Doppler broadening measurements, the positron trapping sites were identified as Zn vacancies or Zn-O-Zn trivacancy clusters. The positron lifetimes, their relative intensities, and the Doppler broadened lineshape parameter S all showed characteristic changes across the nanobipyramid size corresponding to the thermal diffusion length of positrons. In large nanobipyramids, vacancies within the crystallites also trapped positrons and the effects of agglomeration of such vacancies due to increased temperatures of synthesis were reflected in the variation of the annihilation parameters with their base diameters. The sizes of the nanoparticles used were all in the limit of thermal diffusion length of positrons and the annihilation characteristics were in accordance with the decreasing contribution from surfaces with increasing particle size.

Positron annihilation spectroscopic studies of solvothermally synthesized ZnO nanobipyramids and nanoparticles.

PubMed

Ghoshal, Tandra; Biswas, Subhajit; Kar, Soumitra; Chaudhuri, Subhadra; Nambissan, P M G

2008-02-21

Zinc oxide (ZnO) samples in the form of hexagonal-based bipyramids and particles of nanometer dimensions were synthesized through solvothermal route and characterized by x-ray diffraction and transmission electron microscopy. Positron annihilation experiments were performed to study the structural defects such as vacancies and surfaces in these nanosystems. From coincidence Doppler broadening measurements, the positron trapping sites were identified as Zn vacancies or Zn-O-Zn trivacancy clusters. The positron lifetimes, their relative intensities, and the Doppler broadened lineshape parameter S all showed characteristic changes across the nanobipyramid size corresponding to the thermal diffusion length of positrons. In large nanobipyramids, vacancies within the crystallites also trapped positrons and the effects of agglomeration of such vacancies due to increased temperatures of synthesis were reflected in the variation of the annihilation parameters with their base diameters. The sizes of the nanoparticles used were all in the limit of thermal diffusion length of positrons and the annihilation characteristics were in accordance with the decreasing contribution from surfaces with increasing particle size.

Solvothermal-induced phase transition and visible photocatalytic activity of nitrogen-doped titania.

PubMed

Liu, Jianjun; Qin, Wei; Zuo, Shengli; Yu, Yingchun; Hao, Zhengping

2009-04-15

Nitrogen-doped titania nanoparticles consisting of pure anatase, pure rutile and bicrystallites (anatase+rutile and anatase+brookite) have been prepared in TiCl(3)-HMT (hexamethylene tetramine)-alcohol solution under solvothermal process. The effect of the solvent type and amount of HMT as pH adjuster on the phase composition of titania and its visible photocatalytic activity for degradation to MO (methyl orange) was investigated. It is found that anatase gradually transferred to rutile with increase of carbon chain using methanol, ethanol, 1-propanol and 1-butanol as solvent. The pure anatase formed at the pH value of 1-2, while bicrystalline titania (anatase+rutile and anatase+brookite) at that of 7-10 in the presence of methanol. The bicrystalline (anatase+brookite) titania have the best visible photocatalytic activity among all the samples. The -(NO) and -(NH) dopants with an N (1s) binding energy of 400 eV may have positive effects on the visible light photocatalytic activity.

Trinuclear organooxotin assemblies from solvothermal synthesis reaction: Crystal structure, hydrogen bonding and π π stacking interaction

NASA Astrophysics Data System (ADS)

Ma, Chunlin; Sun, Junshan; Zhang, Rufen

2007-05-01

Two new trinuclear mono-organooxotin(IV) complexes with 2,3,4,5-tetrafluorobenzoic acid and sodium perchlorate of the types: [(SnR) 3(OH)(2,3,4,5-F 4C 6HCO 2) 4 · ClO 4] · [O 2CC 6HF 4](R = PhCH 2, 1; o- F-PhCH 2 for 2), have been solvothermally synthesized and structurally characterized by elemental, IR, 1H, 13C and 119Sn NMR and X-ray crystallography diffraction analyses. Complex 2 is also characterized by X-ray crystallography diffraction analyses. In complex 2, four carboxyl groups and a perchlorate bridged three tin atoms in a cyclohexane chair arrangement and form the basic framework. A hydroxyl group comprises the oxygen components of the stannoxane ring system. In these complexes, weak but significant intramolecular hydrogen bonding and π-π stacking interaction are also shown. These contacts lead to aggregation and supramolecular assembly of complexes 1 and 2 into 1D or 2D framework.

Solvothermal synthesis and structure of coordination polymers of Nd(III) and Dy(III) with rigid isophthalic acid derivatives and flexible adipic acid

NASA Astrophysics Data System (ADS)

Kariem, Mukaddus; Kumar, Manesh; Yawer, Mohd; Sheikh, Haq Nawaz

2017-12-01

Two new coordination polymers (CPs) with the formula [Nd(hip)(adip) 0.5(H2O)2]n.nH2O (1) and [Dy(aip)(adip)0.5(H2O)2]n.nH2O (2) were synthesized by self-assembly of lanthanide salts with rigid [5-hydroxyisophthalic acid (H2hip)], [5-aminoisophthalic acid (H2aip)] and flexible [adipic acid (H2adip)] linkers under solvothermal conditions. The CPs 1 &2 crystallize in monoclinic C2/c space group. Both the CPs have 1D linear ladder shaped extension with the linkages having the backbone of hip2-, aip2- and adip2- ligands. The 1D linear ladder chains generate three dimensional (3D) supramolecular frameworks via significant π-π and hydrogen bonding interactions. The CP 2 (Dy) emit strong ligand sensitized characteristic f-f luminescence emission. The CP 2 also exhibit weak ferromagnetic interactions at low temperatures.

Solvothermal synthesis and structural characterization of a three-dimensional metal organic polymer [NaZn(1,2,4-BTC)] (1,2,4-BTC=1,2,4-benzenetricarboxylate)

NASA Astrophysics Data System (ADS)

Wang, Lei; Shi, Zhan; Li, Guanghua; Fan, Yong; Fu, Wensheng; Feng, Shouhua

2004-01-01

A new three-dimensional metal-organic polymer, [NaZn(1,2,4-BTC)] (where 1,2,4-BTC=1,2,4-benzenetricarboxylate), has been prepared under solvothermal conditions and characterized by single crystal X-ray diffraction. The compound crystallizes in the monoclinic space group P2 1/ c, with cell parameters: a=9.7706(4) Å, b=12.3549(5) Å, c=6.8897(3) Å, β=91.640(2)°, V=831.35(6) Å 3 and Z=4. In the three-dimensional structure of the compound, each Zn atom is five-coordinated in distorted trigonal bipyramidal geometry, while the sixfold coordination of Na corresponds to a slightly distorted triangular prism. The organic ligand, 1,2,4-BTC, shows a novel and unprecedented coordination mode: 11 bonds to 10 metals with each carboxylate function exhibiting different linkages. It remains stable when desolvated and when heated up to 410 °C.

A two steps solution approach to solving large nonlinear models: application to a problem of conjunctive use.

PubMed

Vieira, J; Cunha, M C

2011-01-01

This article describes a solution method of solving large nonlinear problems in two steps. The two steps solution approach takes advantage of handling smaller and simpler models and having better starting points to improve solution efficiency. The set of nonlinear constraints (named as complicating constraints) which makes the solution of the model rather complex and time consuming is eliminated from step one. The complicating constraints are added only in the second step so that a solution of the complete model is then found. The solution method is applied to a large-scale problem of conjunctive use of surface water and groundwater resources. The results obtained are compared with solutions determined with the direct solve of the complete model in one single step. In all examples the two steps solution approach allowed a significant reduction of the computation time. This potential gain of efficiency of the two steps solution approach can be extremely important for work in progress and it can be particularly useful for cases where the computation time would be a critical factor for having an optimized solution in due time.

Surface-Engineered Multifunctional Eu:Gd2O3 Nanoplates for Targeted and pH-Responsive Drug Delivery and Imaging Applications.

PubMed

Saha, Arindam; Mohanta, Subas Chandra; Deka, Kashmiri; Deb, Pritam; Devi, Parukuttyamma Sujatha

2017-02-01

In this paper, we report the synthesis of surface-engineered multifunctional Eu:Gd 2 O 3 triangular nanoplates with small size and uniform shape via a high-temperature solvothermal technique. Surface engineering has been performed by a one-step polyacrylate coating, followed by controlled conjugation chemistry. This creates the desired number of surface functional groups that can be used to attach folic acid as a targeting ligand on the nanoparticle surface. To specifically deliver the drug molecules in the nucleus, the folate density on the nanoparticle surface has been kept low. We have also modified the drug molecules with terminal double bond and ester linkage for the easy conjugation of nanoparticles. The nanoparticle surface was further modified with free thiols to specifically attach the modified drug molecules with a pH-responsive feature. High drug loading has been encountered for both hydrophilic drug daunorubicin (∼69% loading) and hydrophobic drug curcumin (∼75% loading) with excellent pH-responsive drug release. These nanoparticles have also been used as imaging probes in fluorescence imaging. Some preliminary experiments to evaluate their application in magnetic resonance imaging have also been explored. A detailed fluorescence imaging study has confirmed the efficient delivery of drugs to the nuclei of cancer cells with a high cytotoxic effect. Synthesized surface-engineered nanomaterials having small hydrodynamic size, excellent colloidal stability, and high drug-loading capacity, along with targeted and pH-responsive delivery of dual drugs to the cancer cells, will be potential nanobiomaterials for various biomedical applications.

Designed Single-Step Synthesis, Structure, and Derivative Textural Properties of Well-Ordered Layered Penta-Coordinate Silicon Alcoholate Complexes

PubMed Central

Li, Xiansen; Michaelis, Vladimir K.; Ong, Ta-Chung; Smith, Stacey J.; Griffin, Robert G.; Wang, Evelyn N.

2014-01-01

The controllable synthesis of well-ordered layered materials with specific nanoarchitecture poses a grand challenge in materials chemistry. We report the solvothermal synthesis of two structurally analogous 5-coordinate organosilicate complexes via a novel transesterification mechanism. Since the polycrystalline nature of the intrinsic hypervalent Si complex thwarts the endeavor in determining its structure, a novel strategy concerning the elegant addition of a small fraction of B species as an effective crystal growth mediator and a sacrificial agent is proposed to directly prepare diffraction-quality single crystals without disrupting the intrinsic elemental type. In the determined crystal structure, two monomeric primary building units (PBUs) self-assemble into a dimeric asymmetric secondary BU via strong Na+-O2− ionic bonds. The designed one-pot synthesis is straightforward, robust, and efficient, leading to a well-ordered (10ī)-parallel layered Si complex with its principal interlayers intercalated with extensive van der Waals gaps in spite of the presence of substantial Na+ counterions as a result of unique atomic arrangement in its structure. On the other hand, upon fast pyrolysis, followed by acid leaching, both complexes are converted into two SiO2 composites bearing BET surface areas of 163.3 and 254.7 m2 g−1 for the pyrolyzed intrinsic and B-assisted Si complexes, respectively. The transesterification methodology merely involving alcoholysis but without any hydrolysis side reaction is designed to have generalized applicability for use in synthesizing new layered metal-organic compounds with tailored PBUs and corresponding metal oxide particles with hierarchical porosity. PMID:24737615

System and method for chromatography and electrophoresis using circular optical scanning

DOEpatents

Balch, Joseph W.; Brewer, Laurence R.; Davidson, James C.; Kimbrough, Joseph R.

2001-01-01

A system and method is disclosed for chromatography and electrophoresis using circular optical scanning. One or more rectangular microchannel plates or radial microchannel plates has a set of analysis channels for insertion of molecular samples. One or more scanning devices repeatedly pass over the analysis channels in one direction at a predetermined rotational velocity and with a predetermined rotational radius. The rotational radius may be dynamically varied so as to monitor the molecular sample at various positions along a analysis channel. Sample loading robots may also be used to input molecular samples into the analysis channels. Radial microchannel plates are built from a substrate whose analysis channels are disposed at a non-parallel angle with respect to each other. A first step in the method accesses either a rectangular or radial microchannel plate, having a set of analysis channels, and second step passes a scanning device repeatedly in one direction over the analysis channels. As a third step, the scanning device is passed over the analysis channels at dynamically varying distances from a centerpoint of the scanning device. As a fourth step, molecular samples are loaded into the analysis channels with a robot.

Development of a modularized two-step (M2S) chromosome integration technique for integration of multiple transcription units in Saccharomyces cerevisiae.

PubMed

Li, Siwei; Ding, Wentao; Zhang, Xueli; Jiang, Huifeng; Bi, Changhao

2016-01-01

Saccharomyces cerevisiae has already been used for heterologous production of fuel chemicals and valuable natural products. The establishment of complicated heterologous biosynthetic pathways in S. cerevisiae became the research focus of Synthetic Biology and Metabolic Engineering. Thus, simple and efficient genomic integration techniques of large number of transcription units are demanded urgently. An efficient DNA assembly and chromosomal integration method was created by combining homologous recombination (HR) in S. cerevisiae and Golden Gate DNA assembly method, designated as modularized two-step (M2S) technique. Two major assembly steps are performed consecutively to integrate multiple transcription units simultaneously. In Step 1, Modularized scaffold containing a head-to-head promoter module and a pair of terminators was assembled with two genes. Thus, two transcription units were assembled with Golden Gate method into one scaffold in one reaction. In Step 2, the two transcription units were mixed with modules of selective markers and integration sites and transformed into S. cerevisiae for assembly and integration. In both steps, universal primers were designed for identification of correct clones. Establishment of a functional β-carotene biosynthetic pathway in S. cerevisiae within 5 days demonstrated high efficiency of this method, and a 10-transcriptional-unit pathway integration illustrated the capacity of this method. Modular design of transcription units and integration elements simplified assembly and integration procedure, and eliminated frequent designing and synthesis of DNA fragments in previous methods. Also, by assembling most parts in Step 1 in vitro, the number of DNA cassettes for homologous integration in Step 2 was significantly reduced. Thus, high assembly efficiency, high integration capacity, and low error rate were achieved.

Brain tissue segmentation in 4D CT using voxel classification

NASA Astrophysics Data System (ADS)

van den Boom, R.; Oei, M. T. H.; Lafebre, S.; Oostveen, L. J.; Meijer, F. J. A.; Steens, S. C. A.; Prokop, M.; van Ginneken, B.; Manniesing, R.

2012-02-01

A method is proposed to segment anatomical regions of the brain from 4D computer tomography (CT) patient data. The method consists of a three step voxel classification scheme, each step focusing on structures that are increasingly difficult to segment. The first step classifies air and bone, the second step classifies vessels and the third step classifies white matter, gray matter and cerebrospinal fluid. As features the time averaged intensity value and the temporal intensity change value were used. In each step, a k-Nearest-Neighbor classifier was used to classify the voxels. Training data was obtained by placing regions of interest in reconstructed 3D image data. The method has been applied to ten 4D CT cerebral patient data. A leave-one-out experiment showed consistent and accurate segmentation results.

Intrinsically water-repellent copper oxide surfaces; An electro-crystallization approach

NASA Astrophysics Data System (ADS)

Akbari, Raziyeh; Ramos Chagas, Gabriela; Godeau, Guilhem; Mohammadizadeh, Mohammadreza; Guittard, Frédéric; Darmanin, Thierry

2018-06-01

Use of metal oxide thin layers is increased due to their good durability under environmental conditions. In this work, the repeatable nanostructured crystalite Cu2O thin films, developed by electrodeposition method without any physical and chemical modifications, demonstrate good hydrophobicity. Copper (I) oxide (Cu2O) layers were fabricated on gold/Si(1 0 0) substrates by different electrodeposition methods i.e. galvanostatic deposition, cyclic voltammetry, and pulse potentiostatic deposition and using copper sulfate (in various concentrations) as a precursor. The greatest crystalline face on prepared Cu2O samples is (1 1 1) which is the most hydrophobic facet of Cu2O cubic structure. Indeed, different crystallite structures such as nanotriangles and truncated octahedrons were formed on the surface for various electrodeposition methods. The increase of the contact angle (θw) measured by the rest time, reaching to about 135°, was seen at different rates and electrodeposition methods. In addition, two-step deposition surfaces were also prepared by applying two of the mentioned methods, alternatively. In general, the morphology of the two-step deposition surfaces showed some changes compared to that of one-step samples, allowing the formation of different crystallite shapes. Moreover, the wettability behavior showd the larger θw of the two-step deposition layers compared to the related one-step deposition layers. Therefore, the highest observed θw was related to the one of two-step deposition layers due to the creation of small octahedral structures on the surface, having narrow and deep valleys. However, there was an exception which was due to the resulted big structures and broad valleys on the surface. So, it is possible to engineer different crystallites shapes using the proposed two-step deposition method. It is expected that hydrophobic crystallite thin films can be used in environmental and electronic applications to save energy and materials properties.

Synthesis of Fe3O4/Polyacrylonitrile Composite Electrospun Nanofiber Mat for Effective Adsorption of Tetracycline.

PubMed

Liu, Qing; Zhong, Lu-Bin; Zhao, Quan-Bao; Frear, Craig; Zheng, Yu-Ming

2015-07-15

Novel Fe3O4/polyacrylonitrile (PAN) composite nanofibers (NFs) were prepared by a simple two-step process, an electrospinning and solvothermal method. Characterization by field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM) demonstrated formation of a uniform nanoparticles coating (about 20 nm in thickness) on the PAN nanofiber backbone. The coating was constructed by well-crystallized cubic phase Fe3O4 nanoparticles as examined by X-ray diffraction spectroscopy (XRD). The coating doubled the specific surface area of NFs, from 8.4 to 17.8 m2 g(-1), as confirmed by nitrogen sorption isotherm analysis. To evaluate the feasibility of Fe3O4/PAN composite NFs as a potential adsorbent for antibiotic removal, batch adsorption experiments were conducted using tetracycline (TC) as the model antibiotic molecule. The results showed that Fe3O4/PAN composite NFs were effective in removing TC with no impactful loss of Fe in the pH regime of environmental interest (5-8). The adsorption of TC onto Fe3O4/PAN composite NFs better fitted the pseudo-second-order kinetics model, and the maximum adsorption capacity calculated from Langmuir isotherm model was 257.07 mg g(-1) at pH 6. The composite NFs also exhibited good regenerability over repeated adsorption/desorption cycles. Surface complexation between TC and the composite NFs contributed most to the adsorption as elucidated by X-ray photoelectron spectroscopy (XPS). This highly effective and novel adsorbent can be easily modularized and separated, promising its huge potential in drinking and wastewater treatment for antibiotic removal.

Overview of fast algorithm in 3D dynamic holographic display

NASA Astrophysics Data System (ADS)

Liu, Juan; Jia, Jia; Pan, Yijie; Wang, Yongtian

2013-08-01

3D dynamic holographic display is one of the most attractive techniques for achieving real 3D vision with full depth cue without any extra devices. However, huge 3D information and data should be preceded and be computed in real time for generating the hologram in 3D dynamic holographic display, and it is a challenge even for the most advanced computer. Many fast algorithms are proposed for speeding the calculation and reducing the memory usage, such as:look-up table (LUT), compressed look-up table (C-LUT), split look-up table (S-LUT), and novel look-up table (N-LUT) based on the point-based method, and full analytical polygon-based methods, one-step polygon-based method based on the polygon-based method. In this presentation, we overview various fast algorithms based on the point-based method and the polygon-based method, and focus on the fast algorithm with low memory usage, the C-LUT, and one-step polygon-based method by the 2D Fourier analysis of the 3D affine transformation. The numerical simulations and the optical experiments are presented, and several other algorithms are compared. The results show that the C-LUT algorithm and the one-step polygon-based method are efficient methods for saving calculation time. It is believed that those methods could be used in the real-time 3D holographic display in future.

Sensing cocaine in saliva with attenuated total reflection infrared (ATR-IR) spectroscopy combined with a one-step extraction method

NASA Astrophysics Data System (ADS)

Hans, Kerstin M.-C.; Gianella, Michele; Sigrist, Markus W.

2012-03-01

On-site drug tests have gained importance, e.g., for protecting the society from impaired drivers. Since today's drug tests are majorly only positive/negative, there is a great need for a reliable, portable and preferentially quantitative drug test. In the project IrSens we aim to bridge this gap with the development of an optical sensor platform based on infrared spectroscopy and focus on cocaine detection in saliva. We combine a one-step extraction method, a sample drying technique and infrared attenuated total reflection (ATR) spectroscopy. As a first step we have developed an extraction technique that allows us to extract cocaine from saliva to an almost infrared-transparent solvent and to record ATR spectra with a commercially available Fourier Transform-infrared spectrometer. To the best of our knowledge this is the first time that such a simple and easy-to-use one-step extraction method is used to transfer cocaine from saliva into an organic solvent and detect it quantitatively. With this new method we are able to reach a current limit of detection around 10 μg/ml. This new extraction method could also be applied to waste water monitoring and controlling caffeine content in beverages.

Stability with large step sizes for multistep discretizations of stiff ordinary differential equations

NASA Technical Reports Server (NTRS)

Majda, George

1986-01-01

One-leg and multistep discretizations of variable-coefficient linear systems of ODEs having both slow and fast time scales are investigated analytically. The stability properties of these discretizations are obtained independent of ODE stiffness and compared. The results of numerical computations are presented in tables, and it is shown that for large step sizes the stability of one-leg methods is better than that of the corresponding linear multistep methods.

A rapid, one step molecular identification of Trichoderma citrinoviride and Trichoderma reesei.

PubMed

Saroj, Dina B; Dengeti, Shrinivas N; Aher, Supriya; Gupta, Anil K

2015-06-01

Trichoderma species are widely used as production hosts for industrial enzymes. Identification of Trichoderma species requires a complex molecular biology based identification involving amplification and sequencing of multiple genes. Industrial laboratories are required to run identification tests repeatedly in cell banking procedures and also to prove absence of production host in the product. Such demands can be fulfilled by a brief method which enables confirmation of strain identity. This communication describes one step identification method for two common Trichoderma species; T. citrinoviride and T. reesei, based on identification of polymorphic region in the nucleotide sequence of translation elongation factor 1 alpha. A unique forward primer and common reverse primer resulted in 153 and 139 bp amplicon for T. citrinoviride and T. reesei, respectively. Simplification was further introduced by using mycelium as template for PCR amplification. Method described in this communication allows rapid, one step identification of two Trichoderma species.

Method for forming a thermocouple

DOEpatents

Metz, Hugh J.

1979-01-01

A method is provided for producing a fast response, insulated junction thermocouple having a uniform diameter outer sheath in the region of the measuring junction. One step is added to the usual thermocouple fabrication process that consists in expanding the thermocouple sheath following the insulation removal step. This makes it possible to swage the sheath back to the original diameter and compact the insulation to the desired high density in the final fabrication step.

Nanofiber electrode and method of forming same

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

Pintauro, Peter N.; Zhang, Wenjing

In one aspect, a method of forming an electrode for an electrochemical device is disclosed. In one embodiment, the method includes the steps of mixing at least a first amount of a catalyst and a second amount of an ionomer or uncharged polymer to form a solution and delivering the solution into a metallic needle having a needle tip. The method further includes the steps of applying a voltage between the needle tip and a collector substrate positioned at a distance from the needle tip, and extruding the solution from the needle tip at a flow rate such as tomore » generate electrospun fibers and deposit the generated fibers on the collector substrate to form a mat with a porous network of fibers. Each fiber in the porous network of the mat has distributed particles of the catalyst. The method also includes the step of pressing the mat onto a membrane.« less

Fabrication of flower-like Ni{sub 3}(NO{sub 3}){sub 2}(OH){sub 4} and their electrochemical properties evaluation

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

Kong, Ling-Bin, E-mail: konglb@lut.cn; School of Materials Science and Engineering, Lanzhou University of Technology, Lanzhou 730050; Deng, Li

Graphical abstract: Ni{sub 3}(NO{sub 3}){sub 2}(OH){sub 4} nano-flakes materials, which have a flower-like structure, were successfully synthesized by a facile solvothermal method without adding any surfactant. The as-prepared Ni{sub 3}(NO{sub 3}){sub 2}(OH){sub 4} possesses a maximum specific capacitance of 2212.5 F g{sup −1} at the current density of 5 mA, suggesting its potential application in electrode material for secondary batteries and electrochemical capacitors. Highlights: ► Flower-like Ni{sub 3}(NO{sub 3}){sub 2}(OH){sub 4} materials were fabricated in a simple method. ► High specific capacitance of 2212.5 F g{sup −1} has been achieved. ► For the first time the effects of concentration andmore » temperature on its specific capacitance has been studied. -- Abstract: Flower-like Ni{sub 3}(NO{sub 3}){sub 2}(OH){sub 4} was successfully synthesized by a facile solvothermal method. The microstructure and surface morphology of prepared Ni{sub 3}(NO{sub 3}){sub 2}(OH){sub 4} were physically characterized by X-ray diffraction (XRD) analysis, scanning electron microscopy (SEM) and transmission electron microscope (TEM). The electrochemical properties studies were carried out using cyclic voltammetry (CV), chronopotentiometry technology and AC impedance spectroscopy, respectively. The results indicate that the flower-like structure has a profound impact on electrode performance at high discharge capacitance. A maximum specific capacitance of 2212.5 F g{sup −1} at the current density of 5 mA could be achieved, suggesting its potential application in electrode material for secondary batteries and electrochemical capacitors. Furthermore, the effects of Ni(NO{sub 3}){sub 2}·6H{sub 2}O concentration and temperature on the microstructure and specific capacitance of prepared Ni{sub 3}(NO{sub 3}){sub 2}(OH){sub 4} have also been systematically studied. The results show that flower-like structure can be formed when the concentration is appropriate, while the temperature has just little effect on its electrochemical properties.« less

Two-step method for creating a gastric tube during laparoscopic-thoracoscopic Ivor-Lewis esophagectomy.

PubMed

Liu, Yu; Li, Ji-Jia; Zu, Peng; Liu, Hong-Xu; Yu, Zhan-Wu; Ren, Yi

2017-12-07

To introduce a two-step method for creating a gastric tube during laparoscopic-thoracoscopic Ivor-Lewis esophagectomy and assess its clinical application. One hundred and twenty-two patients with middle or lower esophageal cancer who underwent laparoscopic-thoracoscopic Ivor-Lewis esophagectomy at Liaoning Cancer Hospital and Institute from March 2014 to March 2016 were included in this study, and divided into two groups based on the procedure used for creating a gastric tube. One group used a two-step method for creating a gastric tube, and the other group used the conventional method. The two groups were compared regarding the operating time, surgical complications, and number of stapler cartridges used. The mean operating time was significantly shorter in the two-step method group than in the conventional method group [238 (179-293) min vs 272 (189-347) min, P < 0.01]. No postoperative death occurred in either group. There was no significant difference in the rate of complications [14 (21.9%) vs 13 (22.4%), P = 0.55] or mean number of stapler cartridges used [5 (4-6) vs 5.2 (5-6), P = 0.007] between the two groups. The two-step method for creating a gastric tube during laparoscopic-thoracoscopic Ivor-Lewis esophagectomy has the advantages of simple operation, minimal damage to the tubular stomach, and reduced use of stapler cartridges.

A neutral molecular-based layered magnet [Fe(C2O4)(CH3OH)]n exhibiting magnetic ordering at TN approximately 23 K.

PubMed

Zhang, Bin; Zhang, Yan; Zhang, Jinbiao; Li, Junchao; Zhu, Daoben

2008-10-07

Solvothermal synthesis of FeCl(2).4H2O and H2C2O(4).2H2O in methanol at 120 degrees C yielded yellow plate-like crystals of [Fe(C2O4)(CH3OH)]n. Each iron atom is in a distorted octahedral environment, being bonded to four oxygen atoms from two bisbidentate oxalate anions, one O atom of a chelating oxalate anion and one O atom from a methanol molecule as an oxalate group bridging ligand in a five-coordination mode. The neutral layer of [Fe(C2O4)(CH3OH)]n with a [4,4] net along the ac plane. There is no interaction between layers. A long range magnetic ordering with spin canting at TN approximately 23 K was observed and confirmed by AC susceptibility measurements.

Rare Earth Ion-Doped Upconversion Nanocrystals: Synthesis and Surface Modification

PubMed Central

Chang, Hongjin; Xie, Juan; Zhao, Baozhou; Liu, Botong; Xu, Shuilin; Ren, Na; Xie, Xiaoji; Huang, Ling; Huang, Wei

2014-01-01

The unique luminescent properties exhibited by rare earth ion-doped upconversion nanocrystals (UCNPs), such as long lifetime, narrow emission line, high color purity, and high resistance to photobleaching, have made them widely used in many areas, including but not limited to high-resolution displays, new-generation information technology, optical communication, bioimaging, and therapy. However, the inherent upconversion luminescent properties of UCNPs are influenced by various parameters, including the size, shape, crystal structure, and chemical composition of the UCNPs, and even the chosen synthesis process and the surfactant molecules used. This review will provide a complete summary on the synthesis methods and the surface modification strategies of UCNPs reported so far. Firstly, we summarize the synthesis methodologies developed in the past decades, such as thermal decomposition, thermal coprecipitation, hydro/solvothermal, sol-gel, combustion, and microwave synthesis. In the second part, five main streams of surface modification strategies for converting hydrophobic UCNPs into hydrophilic ones are elaborated. Finally, we consider the likely directions of the future development and challenges of the synthesis and surface modification, such as the large-scale production and actual applications, stability, and so on, of the UCNPs. PMID:28346995

Construction of two microporous metal-organic frameworks with flu and pyr topologies based on Zn4(μ3-OH)2(CO2)6 and Zn6(μ6-O)(CO2)6 secondary building units.

PubMed

Li, Xing-Jun; Jiang, Fei-Long; Wu, Ming-Yan; Chen, Lian; Qian, Jin-Jie; Zhou, Kang; Yuan, Da-Qiang; Hong, Mao-Chun

2014-01-21

By employment of a tripodal phosphoric carboxylate ligand, tris(4-carboxylphenyl)phosphine oxide (H3TPO), two novel porous metal-organic frameworks, namely, [Zn4(μ3-OH)2(TPO)2(H2O)2] (1) and [Zn6(μ6-O)(TPO)2](NO3)4·3H2O (2), have been synthesized by solvothermal methods. Complexes 1 and 2 exhibit three-dimensional microporous frameworks with flu and pyr topologies and possess rare butterfly-shaped Zn4(μ3-OH)2(CO2)6 and octahedral Zn6(μ6-O)(CO2)6 secondary building units, respectively. Large cavities and one-dimensional channels are observed in these two frameworks. Gas-sorption measurements indicate that complex 2 has a good H2 uptake capacity of 171.9 cm(3) g(-1) (1.53 wt %) at 77 K and 1.08 bar, and its ideal adsorbed solution theory calculation predicts highly selective adsorption of CO2 over N2 and CH4. Furthermore, complexes 1 and 2 exhibit excellent blue emission at room temperature.

In-situ preparation of hierarchical flower-like TiO2/carbon nanostructures as fillers for polymer composites with enhanced dielectric properties

PubMed Central

Xu, Nuoxin; Zhang, Qilong; Yang, Hui; Xia, Yuting; Jiang, Yongchang

2017-01-01

Novel three-dimensional hierarchical flower-like TiO2/carbon (TiO2/C) nanostructures were in-situ synthesized via a solvothermal method involving calcination of organic precursor under inert atmosphere. The composite films comprised of P (VDF-HFP) and as-prepared hierarchical flower-like TiO2/C were fabricated by a solution casting and hot-pressing approach. The results reveal that loading the fillers with a small amount of carbon is an effective way to improve the dielectric constant and suppress the dielectric loss. In addition, TiO2/C particles with higher carbon contents exhibit superiority in promoting the dielectric constants of composites when compared with their noncarbon counterparts. For instance, the highest dielectric constant (330.6) of the TiO2/C composites is 10 times over that of noncarbon-TiO2-filled ones at the same filler volume fraction, and 32 times over that of pristine P (VDF-HFP). The enhancement in the dielectric constant can be attributed to the formation of a large network, which is composed of local micro-capacitors with carbon particles as electrodes and TiO2 as the dielectric in between. PMID:28262766

Synthesis of UiO-66-OH zirconium metal-organic framework and its application for selective extraction and trace determination of thorium in water samples by spectrophotometry

NASA Astrophysics Data System (ADS)

Moghaddam, Zahra Safaei; Kaykhaii, Massoud; Khajeh, Mostafa; Oveisi, Ali Reza

2018-04-01

In this study, a zirconium-based metal-organic framework (Zr-MOF), named UiO-66-OH, was synthesized by the solvo-thermal method and characterized by Fourier transform-infrared spectroscopy (FTIR), powder X-ray diffraction (PXRD), and scanning electron microscopy (SEM). This Zr-MOF was then employed as a sorbent for selective extraction and preconcentration of thorium ions after their complexation with 2-(2,4-dihydroxyphenyl)-3,5,7-trihydroxychromen-4-one (morin) from environmental water samples prior to its spectrophotometrical determination. The experimental parameters affecting extraction, such as pH of sample solution, amount of Zr-MOF, type and volume of eluting solvent, adsorption and desorption time, and concentration of complexing agent were evaluated and optimized. Under the optimized conditions, an enrichment factor of 250 was achieved. The limit of detection was calculated to be 0.35 μg·L- 1 with a linear range between 10 and 2000 μg·L- 1of thorium. The maximum sorption capacity of MOF toward thorium was found to be 47.5 mg·g- 1. The proposed procedure was successfully applied to the analysis of real water samples.

A composite step conjugate gradients squared algorithm for solving nonsymmetric linear systems

NASA Astrophysics Data System (ADS)

Chan, Tony; Szeto, Tedd

1994-03-01

We propose a new and more stable variant of the CGS method [27] for solving nonsymmetric linear systems. The method is based on squaring the Composite Step BCG method, introduced recently by Bank and Chan [1,2], which itself is a stabilized variant of BCG in that it skips over steps for which the BCG iterate is not defined and causes one kind of breakdown in BCG. By doing this, we obtain a method (Composite Step CGS or CSCGS) which not only handles the breakdowns described above, but does so with the advantages of CGS, namely, no multiplications by the transpose matrix and a faster convergence rate than BCG. Our strategy for deciding whether to skip a step does not involve any machine dependent parameters and is designed to skip near breakdowns as well as produce smoother iterates. Numerical experiments show that the new method does produce improved performance over CGS on practical problems.

Modeling behavior dynamics using computational psychometrics within virtual worlds.

PubMed

Cipresso, Pietro

2015-01-01

In case of fire in a building, how will people behave in the crowd? The behavior of each individual affects the behavior of others and, conversely, each one behaves considering the crowd as a whole and the individual others. In this article, I propose a three-step method to explore a brand new way to study behavior dynamics. The first step relies on the creation of specific situations with standard techniques (such as mental imagery, text, video, and audio) and an advanced technique [Virtual Reality (VR)] to manipulate experimental settings. The second step concerns the measurement of behavior in one, two, or many individuals focusing on parameters extractions to provide information about the behavior dynamics. Finally, the third step, which uses the parameters collected and measured in the previous two steps in order to simulate possible scenarios to forecast through computational models, understand, and explain behavior dynamics at the social level. An experimental study was also included to demonstrate the three-step method and a possible scenario.

An ingenious one-dimensional zirconium phosphonate with efficient strontium exchange capability and moderate proton conductivity.

PubMed

Zhang, Jiarong; Chen, Lanhua; Gui, Daxiang; Zhang, Haowen; Zhang, Duo; Liu, Wei; Huang, Guolin; Diwu, Juan; Chai, Zhifang; Wang, Shuao

2018-04-17

A new 1-D zirconium phosphonate [(CH3)2NH2]2[Zr(CH2(HPO3)(PO3))2] (SZ-5) was synthesized via a solvothermal reaction and its single crystal structure was elucidated. SZ-5 exhibits efficient strontium exchange capability with high uptake capacity and selectivity, as further demonstrated by the radioactive Sr-90 removal from a real contaminated seawater sample with an extremely high ionic strength. In addition, the measured proton conductivity at 90 °C and 90% relative humidity (RH) is 5.65 × 10-4 S cm-1. The efficient ion-exchange ability and the moderate proton conductivity suggest the potential applications of SZ-5 in fuel cells or in the remediation of contaminated water.

Carbon Nanosheets: Synthesis and Application.

PubMed

Fan, Huailin; Shen, Wenzhong

2015-06-22

Carbon nanosheets (CNSs) with tunable sizes, morphologies, and pore structures have been synthesized through several chemical routes. Graphitized CNSs have been synthesized through exfoliation, chemical vapor deposition, or high-temperature carbonization. Porous CNSs have been synthesized by using various methods, including pyrolysis, self-assembly, or a solvothermal method in connection with carbonization. These CNSs have successfully been used as detectors for metal ions, as cathodes for field electron emissions, as electrodes for supercapacitors and fuel cells, and as supports for photocatalytic and catalytic oxygen reduction. Therefore, the synthesis and application of CNSs are receiving increasing levels of interest, particularly as application benefits, in the context of future energy/chemical industry, are becoming recognized. This review provides a summary of the most recent and important progress in the production of CNSs and highlights their application in environmental and energy-related fields. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Uniform Fe3O4 microflowers hierarchical structures assembled with porous nanoplates as superior anode materials for lithium-ion batteries

NASA Astrophysics Data System (ADS)

Wang, Xiaoliang; Liu, Yanguo; Arandiyan, Hamidreza; Yang, Hongping; Bai, Lu; Mujtaba, Jawayria; Wang, Qingguo; Liu, Shanghe; Sun, Hongyu

2016-12-01

Uniform Fe3O4 microflowers assembled with porous nanoplates were successfully synthesized by a solvothermal method and subsequent annealing process. The structural and compositional analysis of the Fe3O4 microflowers were studied by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and X-ray photoelectron spectroscopy (XPS). The Bruauer-Emmett-Teller (BET) specific surface area was calculated by the nitrogen isotherm curve and pore size distribution of Fe3O4 microflowers was determined by the Barret-Joyner-Halenda (BJH) method. When evaluated as anode material for lithium-ion batteries, the as-prepared Fe3O4 microflowers electrodes delivered superior capacity, better cycling stability and rate capability than that of Fe3O4 microspheres electrodes. The improved electrochemical performance was attributed to the microscale flowerlike architecture and the porous sheet structural nature.

Sandwiched Thin-Film Anode of Chemically Bonded Black Phosphorus/Graphene Hybrid for Lithium-Ion Battery.

PubMed

Liu, Hanwen; Zou, Yuqin; Tao, Li; Ma, Zhaoling; Liu, Dongdong; Zhou, Peng; Liu, Hongbo; Wang, Shuangyin

2017-09-01

A facile vacuum filtration method is applied for the first time to construct sandwich-structure anode. Two layers of graphene stacks sandwich a composite of black phosphorus (BP), which not only protect BP from quickly degenerating but also serve as current collector instead of copper foil. The BP composite, reduced graphene oxide coated on BP via chemical bonding, is simply synthesized by solvothermal reaction at 140 °C. The sandwiched film anode used for lithium-ion battery exhibits reversible capacities of 1401 mAh g -1 during the 200th cycle at current density of 100 mA g -1 indicating superior cycle performance. Besides, this facile vacuum filtration method may also be available for other anode material with well dispersion in N-methyl pyrrolidone (NMP). © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Direct chemiluminescence of carbon dots induced by potassium ferricyanide and its analytical application

NASA Astrophysics Data System (ADS)

Amjadi, Mohammad; Manzoori, Jamshid L.; Hallaj, Tooba; Sorouraddin, Mohammad H.

2014-03-01

The chemiluminescence (CL) of water-soluble fluorescent carbon dots (C-dots) induced by direct chemical oxidation was investigated. C-dots were prepared by solvothermal method and characterized by fluorescence spectra and transmission electron microscopy. It was found that K3Fe(CN)6 could directly oxidize C-dots to produce a relatively intense CL emission. The mechanism of CL generation was investigated based on the fluorescence and CL emission spectra and the effect of radical scavengers on the CL intensity. The inhibitive effect of some metal ions and biologically important molecules on the CL intensity of the system was examined and the potential of the system for the determination of these species at trace levels was studied. In order to evaluate the capability of method to real sample analysis, it was applied to the determination of Cr(VI) and adrenaline in water and injection samples, respectively.

Operator Approach to the Master Equation for the One-Step Process

NASA Astrophysics Data System (ADS)

Hnatič, M.; Eferina, E. G.; Korolkova, A. V.; Kulyabov, D. S.; Sevastyanov, L. A.

2016-02-01

Background. Presentation of the probability as an intrinsic property of the nature leads researchers to switch from deterministic to stochastic description of the phenomena. The kinetics of the interaction has recently attracted attention because it often occurs in the physical, chemical, technical, biological, environmental, economic, and sociological systems. However, there are no general methods for the direct study of this equation. The expansion of the equation in a formal Taylor series (the so called Kramers-Moyal's expansion) is used in the procedure of stochastization of one-step processes. Purpose. However, this does not eliminate the need for the study of the master equation. Method. It is proposed to use quantum field perturbation theory for the statistical systems (the so-called Doi method). Results: This work is a methodological material that describes the principles of master equation solution based on quantum field perturbation theory methods. The characteristic property of the work is that it is intelligible for non-specialists in quantum field theory. Conclusions: We show the full equivalence of the operator and combinatorial methods of obtaining and study of the one-step process master equation.

Synthesis of reticulated hollow spheres structure NiCo2S4 and its application in organophosphate pesticides biosensor.

PubMed

Peng, Lei; Dong, Sheying; Wei, Wenbo; Yuan, Xiaojing; Huang, Tinglin

2017-06-15

Electrode materials play a key role in the development of electrochemical sensors, particularly enzyme-based biosensors. Here, a novel NiCo 2 S 4 with reticulated hollow spheres assembled from rod-like structures was prepared by a one-pot solvothermal method and its formation mechanism was discussed. Moreover, comparison of NiCo 2 S 4 materials from different experiment conditions as biosensors was investigated by electrochemical impedance spectroscopy (EIS) and differential pulse voltammetry (DPV), and the best one that was reticulated hollow spheres assembled from rod-like structures NiCo 2 S 4 has been successfully employed as a matrix of AChE immobilization for the special structure, superior conductivity and rich reaction active sites. When using common two kinds of organophosphate pesticides (OPs) as model analyte, the biosensors demonstrated a wide linear range of 1.0×10 -12 -1.0×10 -8 gmL -1 with the detection limit of 4.2×10 -13 gmL -1 for methyl parathion, and 1.0×10 -13 -1.0×10 -10 gmL -1 with the detection limit of 3.5×10 -14 gmL -1 for paraoxon, respectively. The proposed biosensors exhibited many advantages such as acceptable stability and low cost, providing a promising tool for analysis of OPs. Copyright © 2016 Elsevier B.V. All rights reserved.

High Curie temperature Bi(1.85)Mn(0.15)Te3 nanoplates.

PubMed

Cheng, Lina; Chen, Zhi-Gang; Ma, Song; Zhang, Zhi-dong; Wang, Yong; Xu, Hong-Yi; Yang, Lei; Han, Guang; Jack, Kevin; Lu, Gaoqing Max; Zou, Jin

2012-11-21

Bi(1.85)Mn(0.15)Te(3) hexagonal nanoplates with a width of ~200 nm and a thickness of ~20 nm were synthesized using a solvothermal method. According to the structural characterization and compositional analysis, the Mn(2+) and Mn(3+) ions were found to substitute Bi(3+) ions in the lattice. High-level Mn doping induces significant lattice distortion and decreases the crystal lattice by 1.07% in the a axis and 3.18% in the c axis. A high ferromagnetic state with a Curie temperature of ~45 K is observed in these nanoplates due to Mn(2+) and Mn(3+) ion doping, which is a significant progress in the field of electronics and spintronics.

Synthesis and electrochemical characterization of Ni-B/ZIF-8 as electrode materials for supercapacitors

NASA Astrophysics Data System (ADS)

Li, Zhen; Gao, Yilong; Wu, Jianxiang; Zhang, Wei; Tan, Yueyue; Tang, Bohejin

2016-09-01

Ni-B/Zeolitic Imidazolate Frameworks-8 (Ni-B/ZIF-8) is synthesized via a series of solvothermal, incipient wetness impregnation and chemical reduction methods. The ZIF-8 serves as the host for the growth of Ni-B forming a Ni-B/ZIF-8 composite. Characterization by X-ray diffraction and Transmission electron microscope reveals the dispersion of Ni-B in ZIF-8. As electrode materials for supercapacitors, ZIF-8, Ni-B and Ni-B/ZIF-8 electrodes exhibit specific capacitances of 147, 563 and 866 F g-1, respectively at a scan rate of 5 mV s-1 and good stability over 500 cycles. In particular, Ni-B/ZIF-8 is a promising material for supercapacitors.

Application of Two Cobalt-Based Metal-Organic Frameworks as Oxidative Desulfurization Catalysts.

PubMed

Masoomi, Mohammad Yaser; Bagheri, Minoo; Morsali, Ali

2015-12-07

Two new porous cobalt-based metal-organic frameworks, [Co6(oba)5(OH)2(H2O)2(DMF)4]n · 5DMF (TMU-10) and [Co3(oba)3(O) (Py)0.5] n · 4DMF · Py (TMU-12) have been synthesized by solvothermal method using a nonlinear dicarboxylate ligand. Under mild reaction conditions, these compounds exhibited good catalytic activity and reusability in oxidative desulfurization (ODS) reaction of model oil which was prepared by dissolving dibenzothiophene (DBT) in n-hexane. FT-IR and Mass analysis showed that the main product of DBT oxidation is its corresponding sulfone, which was adsorbed on the surfaces of catalysts. The activation energy was obtained as 13.4 kJ/mol.

Surface-enhanced Raman scattering from silver nanostructures with different morphologies

NASA Astrophysics Data System (ADS)

Zhang, W. C.; Wu, X. L.; Kan, C. X.; Pan, F. M.; Chen, H. T.; Zhu, J.; Chu, Paul K.

2010-07-01

Scanning electron microscopy and X-ray diffraction reveal that four different types of crystalline silver nanostructures including nanoparticles, nanowires, nanocubes, and bipyramids are synthesized by a solvothermal method by reducing silver nitrate with ethylene glycol using poly(vinylpyrrolidone) as an adsorption agent and adding different quantities of sodium chloride to the solution. These nanostructures which exhibit different surface plasma resonance properties in the ultraviolet-visible region are shown to be good surface-enhanced Raman scattering (SERS) substrates using rhodamine 6G molecules. Our results demonstrate that the silver nanocubes, bipyramids with sharp corners and edges, and aggregated silver nanoparticles possess better SERS properties than the silver nanowires, indicating that they can serve as high-sensitivity substrates in SERS-based measurements.

Surfactant-free synthesis of octahedral ZnO/ZnFe2O4 heterostructure with ultrahigh and selective adsorption capacity of malachite green

NASA Astrophysics Data System (ADS)

Liu, Jue; Zeng, Min; Yu, Ronghai

2016-05-01

A new octahedral ZnO/ZnFe2O4 heterostructure has been fabricated through a facile surfactant-free solvothermal method followed by thermal treatment. It exhibits a record-high adsorption capacity (up to 4983.0 mg·g-1) of malachite green (MG), which is a potentially harmful dye in prevalence and should be removed from wastewater and other aqueous solutions before discharging into the environment. The octahedral ZnO/ZnFe2O4 heterostructure also demonstrates strong selective adsorption towards MG from two kinds of mixed solutions: MG/methyl orange (MO) and MG/rhodamine B (RhB) mixtures, indicating its promise in water treatment.

Surfactant-free synthesis of octahedral ZnO/ZnFe2O4 heterostructure with ultrahigh and selective adsorption capacity of malachite green

PubMed Central

Liu, Jue; Zeng, Min; Yu, Ronghai

2016-01-01

A new octahedral ZnO/ZnFe2O4 heterostructure has been fabricated through a facile surfactant-free solvothermal method followed by thermal treatment. It exhibits a record-high adsorption capacity (up to 4983.0 mg·g−1) of malachite green (MG), which is a potentially harmful dye in prevalence and should be removed from wastewater and other aqueous solutions before discharging into the environment. The octahedral ZnO/ZnFe2O4 heterostructure also demonstrates strong selective adsorption towards MG from two kinds of mixed solutions: MG/methyl orange (MO) and MG/rhodamine B (RhB) mixtures, indicating its promise in water treatment. PMID:27142194

Self-Assembled Cu-Sn-S Nanotubes with High (De)Lithiation Performance.

PubMed

Lin, Jie; Lim, Jin-Myoung; Youn, Duck Hyun; Kawashima, Kenta; Kim, Jun-Hyuk; Liu, Yang; Guo, Hang; Henkelman, Graeme; Heller, Adam; Mullins, Charles Buddie

2017-10-24

Through a gelation-solvothermal method without heteroadditives, Cu-Sn-S composites self-assemble to form nanotubes, sub-nanotubes, and nanoparticles. The nanotubes with a Cu 3-4 SnS 4 core and Cu 2 SnS 3 shell can tolerate long cycles of expansion/contraction upon lithiation/delithiation, retaining a charge capacity of 774 mAh g -1 after 200 cycles with a high initial Coulombic efficiency of 82.5%. The importance of the Cu component for mitigation of the volume expansion and structural evolution upon lithiation is informed by density functional theory calculations. The self-generated template and calculated results can inspire the design of analogous Cu-M-S (M = metal) nanotubes for lithium batteries or other energy storage systems.

Development of a One-Step Duplex RT-PCR Method for the Simultaneous Detection of VP3/VP1 and VP1/P2B Regions of the Hepatitis A Virus.

PubMed

Kim, Mi-Ju; Lee, Shin-Young; Kim, Hyun-Joong; Lee, Jeong Su; Joo, In Sun; Kwak, Hyo Sun; Kim, Hae-Yeong

2016-08-28

The simultaneous detection and accurate identification of hepatitis A virus (HAV) is critical in food safety and epidemiological studies to prevent the spread of HAV outbreaks. Towards this goal, a one-step duplex reverse-transcription (RT)-PCR method was developed targeting the VP1/P2B and VP3/VP1 regions of the HAV genome for the qualitative detection of HAV. An HAV RT-qPCR standard curve was produced for the quantification of HAV RNA. The detection limit of the duplex RT-PCR method was 2.8 × 10(1) copies of HAV. The PCR products enabled HAV genotyping analysis through DNA sequencing, which can be applied for epidemiological investigations. The ability of this duplex RT-PCR method to detect HAV was evaluated with HAV-spiked samples of fresh lettuce, frozen strawberries, and oysters. The limit of detection of the one-step duplex RT-PCR for each food model was 9.4 × 10(2) copies/20 g fresh lettuce, 9.7 × 10(3) copies/20 g frozen strawberries, and 4.1 × 10(3) copies/1.5 g oysters. Use of a one-step duplex RT-PCR method has advantages such as shorter time, decreased cost, and decreased labor owing to the single amplification reaction instead of four amplifications necessary for nested RT-PCR.

Methods for dispersing hydrocarbons using autoclaved bacteria

DOEpatents

Tyndall, Richard L.

1996-01-01

A method of dispersing a hydrocarbon includes the steps: providing a bacterium selected from the following group: ATCC 85527, ATCC 75529, and ATCC 55638, a mutant of any one of these bacteria possessing all the identifying characteristics of any one of these bacteria, and mixtures thereof; autoclaving the bacterium to derive a dispersant solution therefrom; and contacting the dispersant solution with a hydrocarbon to disperse the hydrocarbon. Moreover, a method for preparing a dispersant solution includes the following steps: providing a bacterium selected from the following group: ATCC 75527, ATCC 75529, and ATCC 55638, a mutant of any one of these bacteria possessing all the identifying characteristics of any one of these bacteria, and mixtures thereof; and autoclaving the bacterium to derive a dispersant solution therefrom.

Methods for dispersing hydrocarbons using autoclaved bacteria

DOEpatents

Tyndall, R.L.

1996-11-26

A method of dispersing a hydrocarbon includes the following steps: providing a bacterium selected from the following group: ATCC 85527, ATCC 75529, and ATCC 55638, a mutant of any one of these bacteria possessing all the identifying characteristics of any one of these bacteria, and mixtures; autoclaving the bacterium to derive a dispersant solution; and contacting the dispersant solution with a hydrocarbon to disperse the hydrocarbon. Moreover, a method for preparing a dispersant solution includes the following steps: providing a bacterium selected from the following group: ATCC 75527, ATCC 75529, and ATCC 55638, a mutant of any one of these bacteria possessing all the identifying characteristics of any one of these bacteria, and mixtures; and autoclaving the bacterium to derive a dispersant solution.

A Modified Method for Isolation of Rhein from Senna

PubMed Central

Mehta, Namita; Laddha, K. S.

2009-01-01

A simple and efficient method for the isolation of rhein from Cassia angustifolia (senna) leaves is described in which the hydrolysis of the sennosides and extraction of the hydrolysis products (free anthraquinones) is carried out in one step. Further isolation of rhein is achieved from the anthraquinone mixture. This method reduces the number of steps required for isolation of rhein as compared to conventional methods. PMID:20336207

Thermoelectric properties of bismuth telluride nanoplate thin films determined using combined infrared spectroscopy and first-principles calculation

NASA Astrophysics Data System (ADS)

Wada, Kodai; Tomita, Koji; Takashiri, Masayuki

2018-06-01

The thermoelectric properties of bismuth telluride (Bi2Te3) nanoplate thin films were estimated using combined infrared spectroscopy and first-principles calculation, followed by comparing the estimated properties with those obtained using the standard electrical probing method. Hexagonal single-crystalline Bi2Te3 nanoplates were first prepared using solvothermal synthesis, followed by preparing Bi2Te3 nanoplate thin films using the drop-casting technique. The nanoplates were joined by thermally annealing them at 250 °C in Ar (95%)–H2 (5%) gas (atmospheric pressure). The electronic transport properties were estimated by infrared spectroscopy using the Drude model, with the effective mass being determined from the band structure using first-principles calculations based on the density functional theory. The electrical conductivity and Seebeck coefficient obtained using the combined analysis were higher than those obtained using the standard electrical probing method, probably because the contact resistance between the nanoplates was excluded from the estimation procedure of the combined analysis method.

Research on the range side lobe suppression method for modulated stepped frequency radar signals

NASA Astrophysics Data System (ADS)

Liu, Yinkai; Shan, Tao; Feng, Yuan

2018-05-01

The magnitude of time-domain range sidelobe of modulated stepped frequency radar affects the imaging quality of inverse synthetic aperture radar (ISAR). In this paper, the cause of high sidelobe in modulated stepped frequency radar imaging is analyzed first in real environment. Then, the chaos particle swarm optimization (CPSO) is used to select the amplitude and phase compensation factors according to the minimum sidelobe criterion. Finally, the compensated one-dimensional range images are obtained. Experimental results show that the amplitude-phase compensation method based on CPSO algorithm can effectively reduce the sidelobe peak value of one-dimensional range images, which outperforms the common sidelobe suppression methods and avoids the coverage of weak scattering points by strong scattering points due to the high sidelobes.

A Review of High-Order and Optimized Finite-Difference Methods for Simulating Linear Wave Phenomena

NASA Technical Reports Server (NTRS)

Zingg, David W.

1996-01-01

This paper presents a review of high-order and optimized finite-difference methods for numerically simulating the propagation and scattering of linear waves, such as electromagnetic, acoustic, or elastic waves. The spatial operators reviewed include compact schemes, non-compact schemes, schemes on staggered grids, and schemes which are optimized to produce specific characteristics. The time-marching methods discussed include Runge-Kutta methods, Adams-Bashforth methods, and the leapfrog method. In addition, the following fourth-order fully-discrete finite-difference methods are considered: a one-step implicit scheme with a three-point spatial stencil, a one-step explicit scheme with a five-point spatial stencil, and a two-step explicit scheme with a five-point spatial stencil. For each method studied, the number of grid points per wavelength required for accurate simulation of wave propagation over large distances is presented. Recommendations are made with respect to the suitability of the methods for specific problems and practical aspects of their use, such as appropriate Courant numbers and grid densities. Avenues for future research are suggested.

Purification of anti-Japanese encephalitis virus monoclonal antibody by ceramic hydroxyapatite chromatography without proteins A and G.

PubMed

Saito, Maiko; Kurosawa, Yae; Okuyama, Tsuneo

2012-02-01

Antibody purification using proteins A and G has been a standard method for research and industrial processes. The conventional method, however, includes a three-step process, including buffer exchange, before chromatography. In addition, proteins A and G require low pH elution, which causes antibody aggregation and inactivates the antibody's immunity. This report proposes a two-step method using hydroxyapatite chromatography and membrane filtration, without proteins A and G. This novel method shortens the running time to one-third the conventional method for each cycle. Using our two-step method, 90.2% of the monoclonal antibodies purified were recovered in the elution fraction, the purity achieved was >90%, and most of the antigen-specific activity was retained. This report suggests that the two-step method using hydroxyapatite chromatography and membrane filtration should be considered as an alternative to purification using proteins A and G.

Synthesis, structure and characterization of two new copper(I)-thioarsenates (III) constructed by the [AsS{sub 3}]{sup 3-} and CuS{sub x} units

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

Yao, Hua-Gang; Ji, Min; Ji, Shou-Hua

2013-02-15

Two new copper(I)-thioarsenates(III), CsCu{sub 2}AsS{sub 3}(1) and KCu{sub 4}AsS{sub 4}(2), have been synthesized solvothermally in the presence of copper powder. Compound 1 is built up of trigonal AsS{sub 3} pyramid, tetrahedral CuAsS{sub 3} and CuS{sub 3} moieties forming 4-membered, 5-membered and 6-membered rings. The fusion of these rings produces layered anions [Cu{sub 2}AsS{sub 3}]{sup -}, and cesium cations are located between metal-sulfide layers. The structure of 2 consists of infinite [Cu{sub 2}S{sub 2}]{sup 2-} chain and layered [Cu{sub 6}As{sub 2}S{sub 6}] linked to form a three-dimensional anionic framework, [Cu{sub 4}AsS{sub 4}]{sup -}, and containing channels in which the potassium cationsmore » reside. - Graphical abstract: Qne layered CsCu{sub 2}AsS{sub 3} and one framework KCu{sub 4}AsS{sub 4} possessing noncondensed [AsS{sub 3}]{sup 3-} unit have been synthesized solvothermally. The optical band gaps of the two compounds are 2.3 and 1.8 eV, respectively. Highlights: Black-Right-Pointing-Pointer We obtained two new copper(I)-thioarsenate(III), CsCu{sub 2}AsS{sub 3} and KCu{sub 4}AsS{sub 4}. Black-Right-Pointing-Pointer Both compounds possess noncondensed [AsS{sub 3}]{sup 3-} unit and represent new structure types. Black-Right-Pointing-Pointer The optical band gaps of the two compounds are 2.3 eV and 1.8 eV, respectively.« less

Comparison of step-down and binary search algorithms for determination of defibrillation threshold in humans.

PubMed

Shorofsky, Stephen R; Peters, Robert W; Rashba, Eric J; Gold, Michael R

2004-02-01

Determination of DFT is an integral part of ICD implantation. Two commonly used methods of DFT determination, the step-down method and the binary search method, were compared in 44 patients undergoing ICD testing for standard clinical indications. The step-down protocol used an initial shock of 18 J. The binary search method began with a shock energy of 9 J and successive shock energies were increased or decreased depending on the success of the previous shock. The DFT was defined as the lowest energy that successfully terminated ventricular fibrillation. The binary search method has the advantage of requiring a predetermined number of shocks, but some have questioned its accuracy. The study found that (mean) DFT obtained by the step-down method was 8.2 +/- 5.0, whereas by the binary search method DFT was 8.1 +/- 0.7 J, P = NS. DFT differed by no more than one step between methods in 32 (71%) of patients. The number of shocks required to determine DFT by the step-down method was 4.6 +/- 1.4, whereas by definition, the binary search method always required three shocks. In conclusion, the binary search method is preferable because it is of comparable efficacy and requires fewer shocks.

The effect of glycerol-related osmotic changes on post-thaw motility and acrosomal integrity of ram spermatozoa.

PubMed

Fiser, P S; Fairfull, R W

1989-02-01

Ram semen, collected by artificial vagina, was diluted and processed for long-term storage as described by P. S. Fiser, L. Ainsworth, and R. W. Fairfull (Canad. J. Anim. Sci. 62, 425-428, 1982). The concentration of the cryoprotectant, glycerol, was adjusted to 4% in the diluted semen prior to freezing by a one-step addition at 30 degrees C (Method 1), by cooling the semen to 5 degrees C and addition of the glycerol gradually over 30 min (Method 2), by one-step addition of glycerol prior to equilibration for 2 hr (Method 3), or by cooling to 5 degrees C, followed by a holding period of 2 hr at 5 degrees C, and the one-step addition of glycerol just prior to freezing (Method 4). After thawing, the glycerol concentration of the semen was reduced by stepwise dilution from 4 to 0.4% over 15 or 30 min or by a one-step ten-fold dilution. The average post-thaw percentage of motile spermatozoa was significantly lower after addition of glycerol by Method 1 (39.9%) than when the glycerol was added by the other three methods (range, 44.0-46.4% averaged over the glycerol dilution). The average post-thaw percentage of intact acrosomes (61.2%), highest in semen in which the glycerol was added by Method 2, was not significantly different from those in which glycerol was added to semen by Methods 3 and 4, but it was significantly higher than that found in semen in which the glycerol was added by Method 1 (54.4%). However, when averaged over the method of glycerolation, the post-thaw percentage of motile spermatozoa (range, 43.7-44.2%) and the percentage of intact acrosomes (range, 56.8-59.5%) did not differ significantly in semen subjected to gradual decrease in glycerol concentration and diluent osmolality (over 15 and 30 min) or by a one-step, 10-fold dilution. These data indicate that post-thaw survival of spermatozoa can be influenced by the way in which glycerol is added prior to freezing. However, post-thaw spermatozoa motility and acrosomal integrity can be maintained even after a rapid decrease in glycerol concentration such as that which accompanies insemination or dilution of semen for assessment of motility.

One-step synthesis of 2D-layered carbon wrapped transition metal nitrides from transition metal carbides (MXenes) for supercapacitors with ultrahigh cycling stability.

PubMed

Yuan, Wenyu; Cheng, Laifei; Wu, Heng; Zhang, Yani; Lv, Shilin; Guo, Xiaohui

2018-03-13

A novel one-step method to synthesize 2D carbon wrapped TiN (C@TiN) was proposed via using 2D metal carbides (MXenes) as precursors. This study provides a novel approach to synthesize carbon wrapped metal nitrides.

One-step purification of nisin A by immunoaffinity chromatography.

PubMed

Suárez, A M; Azcona, J I; Rodríguez, J M; Sanz, B; Hernández, P E

1997-12-01

The lantibiotic nisin A was purified to homogeneity by a single-step immunoaffinity chromatography method. An immunoadsorption matrix was developed by direct binding of anti-nisin A monoclonal antibodies to N-hydroxysuccinimide-activated Sepharose. The purification procedure was rapid and reproducible and rendered much higher final yields of nisin than any other described method.

Microwave-assisted solvothermal synthesis of hierarchical TiO2 microspheres for efficient electro-field-assisted-photocatalytic removal of tributyltin in tannery wastewater.

PubMed

Zhao, Yang; Huang, Zhiding; Chang, Wenkai; Wei, Chao; Feng, Xugen; Ma, Lin; Qi, Xiaoxia; Li, Zenghe

2017-07-01

Organotin compounds have been widely used in recent decades, however, the residential tributyltin (TBT) in environment has potential harmful effects on human health due to the disruption of endocrine system even at trace level. Herein, this work reports on an effective electro-field-assisted-photocatalytic technique for removal of TBT by applying an electric field to photocatalysis of as-prepared hierarchical TiO 2 microspheres. The synthesis of catalytic materials is based on a self-assembly process induced by microwave-assisted solvothermal reaction. Hierarchical TiO 2 microspheres consisting of nanowires can be obtained in short time with this facile method and possess high surface area and superior optical properties. As the catalyst, it was found that the reaction rate constant of electro-field-assisted-photocatalytic removal (0.0488 min -1 ) of TBT exhibited almost a 9 fold improvement as compared to that of photocatalysis (0.0052 min -1 ). The proposed mechanism of electro-field-assisted-photocatalytic removal of TBT was verified by using 117 Sn-enriched TBT spike solution as an isotopic tracer. In addition, varying impacts from some key reaction conditions, such as voltage of potential, pH value and the presence of Cr and formaldehyde were also discussed. The overall satisfactory TBT removal performance of the proposed electro-field-assisted-photocatalysis procedure with hierarchical TiO 2 microspheres, which was validated using actual tannery wastewater samples from three different kinds of tanning procedures. These attributes suggest that this electro-field-assisted-photocatalysis may have broad applications for the treatment of tannery wastewater. Copyright © 2017 Elsevier Ltd. All rights reserved.

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

Zhang, Ren-Chun; Zhang, You-Juan; Yuan, Bai-Qing

A new three-dimensional framework iodide, (DabcoH){sub 2}[(Dabco){sub 2}Ag{sub 14}I{sub 16}] (1), was solvothermal synthesized by transformation of dense AgI using p-methylthiophenol as mineralizer, and characterized by elemental analysis, single-crystal and powder X-ray diffraction, thermogravimetric analysis, differential scanning calorimetry analysis, UV–vis diffuse reflectance spectroscopy and fluorescence spectroscopy. Compound 1 crystallizes in the trigonal space group R-3c, a=13.4452(2) Å, c=63.725(2) Å, V=9976.5(4) Å{sup 3}, Z=6. It features a 3D silver-rich [(Dabco){sub 2}Ag{sub 14}I{sub 16}]{sup 2−} anionic framework built up from corner-sharing of hybrid [(Dabco){sub 2}Ag{sub 14}I{sub 19}]{sup 5−} clusters, with protonated DabcoH{sup +} as counterions residing in the channels. UV–vis reflectance spectroscopymore » reveals the band gap of 1 is 3.3 eV. Compound 1 exhibits a strong photoluminescent emission band at 567 nm upon excitation at 489 nm. - Graphical abstract: A new 3-D iodoargentate was synthesized by transformation of dense AgI in I{sup −}-deficient system using thiophenol as mineralizer. - Highlights: • We have developed a new method to synthesize iodide using thiophenol as mineralizer. • A new 3D iodide, (DabcoH){sub 2}[(Dabco){sub 2}Ag{sub 14}I{sub 16}], was synthesized by transformation of dense AgI under solvothermal condition. • The compound features a 3D Ag–I framework with highest Ag/I ratio. • Compound 1 is a semiconductor with the band gap of 3.3 eV. • Compound 1 exhibits a strong photoluminescent emission band at 567 nm upon excitation at 489 nm.« less

Na1.25Ni1.25Fe1.75(PO4)3 nanoparticles as a janus electrode material for Li-ion batteries

NASA Astrophysics Data System (ADS)

Karegeya, Claude; Mahmoud, Abdelfattah; Hatert, Frédéric; Vertruyen, Bénédicte; Cloots, Rudi; Lippens, Pierre-Emmanuel; Boschini, Frédéric

2018-06-01

A solvothermal method was used to prepare Na1.25Ni1.25Fe1.75(PO4)3 nanoparticles, a new promising electrode material for lithium-ion batteries. The composition and the crystal structure were determined by 57Fe Mössbauer spectroscopy and powder X-ray diffraction Rietveld refinements and confirmed by magnetic measurements. The structural formula □0.75Na1.25Ni1.25Fe1.75(PO4)3 was obtained showing a significant amount of Na vacancies, which enhances Li diffusion. Na1.25Ni1.25Fe1.75(PO4)3 was used as negative and positive electrode material and shows excellent electrochemical performances. As negative electrode in the voltage range 0.03-3.5 V vs. Li+/Li, the first discharge at current density of 40 mA g-1 delivers a specific capacity of 1186 mAh g-1, which is almost three times its theoretical capacity (428 mAh g-1). Then, reversible capacity of 550 mAh g-1 was obtained at 50 mA g-1 with high rate capability (150 mAh g-1 at 500 mA g-1) and capacity retention of 350 cycles. As positive electrode material, specific capacities of about 145 and 99 mAh g-1 were delivered at current densities of 5 and 50 mA g-1, respectively, in the voltage range of 1.5-4.5 V vs. Li+/Li. In addition, we show that the use of solvothermal synthesis contributes to the synthesis of small sized particles leading to good electrochemical performances.

Synthesis and characterization of pharmaceutical surfactant templated mesoporous silica: Its application to controlled delivery of duloxetine

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

Mani, Ganesh; Pushparaj, Hemalatha; Peng, Mei Mei

2014-03-01

Graphical abstract: - Highlights: • Usefulness of dual pharmaceutical surfactants in silica synthesis was evaluated. • Effects of concentration of secondary template (Tween-40) were studied. • Effects of fixed solvothermal condition on mesostructure formation were studied. • Duloxetine drug loading capability was studied. • Sustained release of duloxetine was evaluated. - Abstract: A new group of mesoporous silica nanoparticles (MSNs) were synthesized using combination pharmaceutical surfactants, Triton X-100 and Tween-40 as template and loaded with duloxetine hydrochloride (DX), for improving the sustained release of DX and patterns with high drug loading. Agglomerated spherical silica MSNs were synthesized by sol–gel andmore » solvothermal methods. The calcined and drug loaded MSNs were characterized using X-ray diffraction (XRD), Braunner–Emmett–Teller (BET), thermogravimetric analysis (TGA), Fourier-transform infrared (FT-IR) spectroscopy, scanning electron microscopy (SEM), differential scanning calorimetry (DSC), diffuse reflectance ultraviolet–visible (DRS-UV–vis) spectroscopy. MSNs with high surface area and pore volume were selected and studied for their DX loading and release. The selected MSNs can accommodate a maximum of 34% DX within it. About 90% was released at 200 h and hence, the synthesized MSNs were capable of engulfing DX and sustain its release. Further form the Ritger and Peppas, Higuchi model for mechanism drug release from all the MSN matrices follows anomalous transport or Non-Fickian diffusion with the ‘r’ and ‘n’ value 0.9 and 0.45 < n < 1, respectively. So, from this study it could be concluded that the MSNs synthesized using pharmaceutical templates were better choice of reservoir for the controlled delivery of drug which requires sustained release.« less

Adaptive step-size algorithm for Fourier beam-propagation method with absorbing boundary layer of auto-determined width.

PubMed

Learn, R; Feigenbaum, E

2016-06-01

Two algorithms that enhance the utility of the absorbing boundary layer are presented, mainly in the framework of the Fourier beam-propagation method. One is an automated boundary layer width selector that chooses a near-optimal boundary size based on the initial beam shape. The second algorithm adjusts the propagation step sizes based on the beam shape at the beginning of each step in order to reduce aliasing artifacts.

Adaptive step-size algorithm for Fourier beam-propagation method with absorbing boundary layer of auto-determined width

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

Learn, R.; Feigenbaum, E.

Two algorithms that enhance the utility of the absorbing boundary layer are presented, mainly in the framework of the Fourier beam-propagation method. One is an automated boundary layer width selector that chooses a near-optimal boundary size based on the initial beam shape. Furthermore, the second algorithm adjusts the propagation step sizes based on the beam shape at the beginning of each step in order to reduce aliasing artifacts.

Adaptive step-size algorithm for Fourier beam-propagation method with absorbing boundary layer of auto-determined width

DOE PAGES

Learn, R.; Feigenbaum, E.

2016-05-27

Two algorithms that enhance the utility of the absorbing boundary layer are presented, mainly in the framework of the Fourier beam-propagation method. One is an automated boundary layer width selector that chooses a near-optimal boundary size based on the initial beam shape. Furthermore, the second algorithm adjusts the propagation step sizes based on the beam shape at the beginning of each step in order to reduce aliasing artifacts.

Development and evaluation of polyvinyl-alcohol blend polymer films as battery separators

NASA Technical Reports Server (NTRS)

Manzo, M. A.

1982-01-01

Several dialdehydes and epoxies were evaluated for their suitability as cross-linkers. Optium concentrations of several cross-linking reagents were determined. A two-step method of cross-linking, which involves treatment of the film in an acid or acid periodate bath, was investigated and dropped in favor of a one-step method in which the acid catalyst, which initiates cross-linking, is added to the PVA - cross-linker solution before casting. The cross-linking was thus achieved during the drying step. This one-step method was much more adaptable to commercial processing. Cross-linked films were characterized as alkaline battery separators. Films were prepared in the lab and tested in cells in order to evaluate the effect of film composition and a number of processing parameters on cell performance. These tests were conducted in order to provide a broader data base from which to select optimum processing parameters. Results of the separator screening tests and the cell tests are discussed.

Dependence of microwave dielectric properties on crystallization behaviour of CaMgSi{sub 2}O{sub 6} glass-ceramics

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

Choi, Bo Kyeong; Jang, Sung Wook; Kim, Eung Soo, E-mail: eskim@kyonggi.ac.kr

2015-07-15

The effects of the crystallization behaviour of CaMgSi{sub 2}O{sub 6} (diopside) glass-ceramics on their microwave dielectric properties were investigated as functions of the Cr{sub 2}O{sub 3} content and heat-treatment method used (one or two steps). The crystallization behaviours of the specimens were affected by the Cr{sub 2}O{sub 3} content as well as by the heat-treatment method employed, and were evaluated using X-ray diffraction and the combined Rietveld and reference intensity ratio (RIR) method. The dielectric constants (K) of the specimens did not change significantly with an increase in the Cr{sub 2}O{sub 3} content. The quality factor (Qf) of the specimensmore » increased for Cr{sub 2}O{sub 3} contents of up to 0.5 wt% Cr{sub 2}O{sub 3}, but then decreased for higher contents. These results could be attributed to the degree of crystallization. For the same Cr{sub 2}O{sub 3} content, the specimens that underwent a two-step heat treatment showed lower K values and higher Qf values than those heat-treated in one-step. These results could be attributed to the smaller crystallite size and higher degree of crystallization in the specimens obtained from the two-step heat treatment compared with those of the specimens heat-treated in one-step method.« less

Methods and apparatus for managing corrosion in buildings

DOEpatents

Chey, S Jay; Hamann, Hendrik F; Klein, Levente Ioan; Schappert, Michael Alan; Stepanchuk, Andriy

2015-02-03

Principles of the invention provide methods and apparatus for providing corrosion management in buildings. In one aspect, an exemplary method includes the step of receiving first data relating corrosion rate to a plurality of environmental conditions. This first data is subsequently utilized to determine a quantitative relationship between corrosion rate and the plurality of environmental conditions. In another step, second data indicative of one or more environmental conditions within a building is received. A corrosion rate in the building is then determined at least in part by applying the determined quantitative relationship to this second data.

Algorithm-enabled partial-angular-scan configurations for dual-energy CT.

PubMed

Chen, Buxin; Zhang, Zheng; Xia, Dan; Sidky, Emil Y; Pan, Xiaochuan

2018-05-01

We seek to investigate an optimization-based one-step method for image reconstruction that explicitly compensates for nonlinear spectral response (i.e., the beam-hardening effect) in dual-energy CT, to investigate the feasibility of the one-step method for enabling two dual-energy partial-angular-scan configurations, referred to as the short- and half-scan configurations, on standard CT scanners without involving additional hardware, and to investigate the potential of the short- and half-scan configurations in reducing imaging dose and scan time in a single-kVp-switch full-scan configuration in which two full rotations are made for collection of dual-energy data. We use the one-step method to reconstruct images directly from dual-energy data through solving a nonconvex optimization program that specifies the images to be reconstructed in dual-energy CT. Dual-energy full-scan data are generated from numerical phantoms and collected from physical phantoms with the standard single-kVp-switch full-scan configuration, whereas dual-energy short- and half-scan data are extracted from the corresponding full-scan data. Besides visual inspection and profile-plot comparison, the reconstructed images are analyzed also in quantitative studies based upon tasks of linear-attenuation-coefficient and material-concentration estimation and of material differentiation. Following the performance of a computer-simulation study to verify that the one-step method can reconstruct numerically accurately basis and monochromatic images of numerical phantoms, we reconstruct basis and monochromatic images by using the one-step method from real data of physical phantoms collected with the full-, short-, and half-scan configurations. Subjective inspection based upon visualization and profile-plot comparison reveals that monochromatic images, which are used often in practical applications, reconstructed from the full-, short-, and half-scan data are largely visually comparable except for some differences in texture details. Moreover, quantitative studies based upon tasks of linear-attenuation-coefficient and material-concentration estimation and of material differentiation indicate that the short- and half-scan configurations yield results in close agreement with the ground-truth information and that of the full-scan configuration. The one-step method considered can compensate effectively for the nonlinear spectral response in full- and partial-angular-scan dual-energy CT. It can be exploited for enabling partial-angular-scan configurations on standard CT scanner without involving additional hardware. Visual inspection and quantitative studies reveal that, with the one-step method, partial-angular-scan configurations considered can perform at a level comparable to that of the full-scan configuration, thus suggesting the potential of the two partial-angular-scan configurations in reducing imaging dose and scan time in the standard single-kVp-switch full-scan CT in which two full rotations are performed. The work also yields insights into the investigation and design of other nonstandard scan configurations of potential practical significance in dual-energy CT. © 2018 American Association of Physicists in Medicine.

On the Development of Multi-Step Inverse FEM with Shell Model

NASA Astrophysics Data System (ADS)

Huang, Y.; Du, R.

2005-08-01

The inverse or one-step finite element approach is increasingly used in the sheet metal stamping industry to predict strain distribution and the initial blank shape in the preliminary design stage. Based on the existing theory, there are two types of method: one is based on the principle of virtual work and the other is based on the principle of extreme work. Much research has been conducted to improve the accuracy of simulation results. For example, based on the virtual work principle, Batoz et al. developed a new method using triangular DKT shell elements. In this new method, the bending and unbending effects are considered. Based on the principle of extreme work, Majlessi and et al. proposed the multi-step inverse approach with membrane elements and applied it to an axis-symmetric part. Lee and et al. presented an axis-symmetric shell element model to solve the similar problem. In this paper, a new multi-step inverse method is introduced with no limitation on the workpiece shape. It is a shell element model based on the virtual work principle. The new method is validated by means of comparing to the commercial software system (PAMSTAMP®). The comparison results indicate that the accuracy is good.

Electrochemical and diffusional insights of combustion synthesized SrLi2Ti6O14 negative insertion material for Li-ion Batteries

NASA Astrophysics Data System (ADS)

Dayamani, Allumolu; Shinde, Ganesh S.; Chaupatnaik, Anshuman; Rao, R. Prasada; Adams, Stefan; Barpanda, Prabeer

2018-05-01

Solvothermal synthetic routes can provide energy-savvy platforms to fabricate battery anode materials involving relatively milder annealing steps vis-à-vis the conventional solid-state synthesis. These energy efficient routes in turn restrict aggressive grain growth to form nanoscale particles favouring efficient Li+ diffusion. Here, we report an economic solution combustion synthesis of SrLi2Ti6O14 anode involving nitrate-urea complexation with a short annealing duration of only 2 h (900 °C). Rietveld refinement confirms the phase purity of target product assuming an orthorhombic framework (Cmca symmetry). It delivers reversible capacity of ∼125 mAh.g-1 at a rate of C/20 involving a 1.38 V Ti4+/Ti3+ redox activity with excellent rate kinetics and cycling stability. Bond valence site energy (BVSE) calculations gauge SrLi2Ti6O14 to be an anisotropic 3D Li+ ion conductor with the highest ionic conductivity along the c direction. The electrochemical and diffusional pathways have been elucidated for combustion prepared SrLi2Ti6O14 as an efficient and safe negative electrode candidate for Li-ion batteries.

C(3i)-symmetric octanuclear cadmium cages: double-anion-templated synthesis, formation mechanism, and properties.

PubMed

Sun, Jie; Sun, Di; Yuan, Shuai; Tian, Dongxu; Zhang, Liangliang; Wang, Xingpo; Sun, Daofeng

2012-12-14

A series of C(3i)-symmetric bicapped trigonal antiprismatic Cd(8) cages [2X@Cd(8)L(6)(H(2)O)(6)]⋅n Y⋅solvents (X = Cl(-), Y = NO(3)(-), n = 2: MOCC-4; X = Br(-), Y = NO(3)(-), n = 2: MOCC-5; X = NO(3)(-), Y = NO(3)(-), n = 2: MOCC-6; X = NO(3)(-), Y = BF(4)(-), n = 2: MOCC-7; X = NO(3)(-), Y = ClO(4)(-), n = 2: MOCC-8; X = CO(3)(2-), n = 0: MOCC-9), doubly anion templated by different anions, were solvothermally synthesized by means of a flexible ligand. Interestingly, the CO(3)(2-) template for MOCC-9 was generated in situ by two-step decomposition of DMF solvent. For other MOCCs, spherical or trigonal monovalent anions could also play the role of template in their formation. The template abilities of these anions in the formation of the cages were experimentally studied and are discussed for the first time. Anion exchange of MOCC-8 was carried out and showed anion-size selectivity. All of the cage-like compounds emit strong luminescence at room temperature. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Bonding effectiveness of self-etch adhesives to dentin after 24 h water storage

PubMed Central

Sarr, Mouhamed; Benoist, Fatou Leye; Bane, Khaly; Aidara, Adjaratou Wakha; Seck, Anta; Toure, Babacar

2018-01-01

Purpose: This study evaluated the immediate bonding effectiveness of five self-etch adhesive systems bonded to dentin. Materials and Methods: The microtensile bond strength of five self-etch adhesives systems, including one two-step and four one-step self-etch adhesives to dentin, was measured. Human third molars had their superficial dentin surface exposed, after which a standardized smear layer was produced using a medium-grit diamond bur. The selected adhesives were applied according to their respective manufacturer's instructions for μTBS measurement after storage in water at 37°C for 24 h. Results: The μTBS varied from 11.1 to 44.3 MPa; the highest bond strength was obtained with the two-step self-etch adhesive Clearfil SE Bond and the lowest with the one-step self-etch adhesive Adper Prompt L-Pop. Pretesting failures mainly occurring during sectioning with the slow-speed diamond saw were observed only with the one-step self-etch adhesive Adper Prompt L-Pop (4 out of 18). Conclusions: When bonded to dentin, the self-etch adhesives with simplified application procedures (one-step self-etch adhesives) still underperform as compared to the two-step self-etch adhesive Clearfil SE Bond. PMID:29674814

Method for the simultaneous preparation of radon-211, xenon-125, xenon-123, astatine-211, iodine-125 and iodine-123

DOEpatents

Mirzadeh, S.; Lambrecht, R.M.

1985-07-01

The invention relates to a practical method for commercially producing radiopharmaceutical activities and, more particularly, relates to a method for the preparation of about equal amount of Radon-211 (/sup 211/Rn) and Xenon-125 (/sup 125/Xe) including a one-step chemical procedure following an irradiation procedure in which a selected target of Thorium (/sup 232/Th) or Uranium (/sup 238/U) is irradiated. The disclosed method is also effective for the preparation in a one-step chemical procedure of substantially equal amounts of high purity /sup 123/I and /sup 211/At. In one preferred arrangement of the invention almost equal quantities of /sup 211/Rn and /sup 125/Xe are prepared using a onestep chemical procedure in which a suitably irradiated fertile target material, such as thorium-232 or uranium-238, is treated to extract those radionuclides from it. In the same one-step chemical procedure about equal quantities of /sup 211/At and /sup 123/I are prepared and stored for subsequent use. In a modified arrangement of the method of the invention, it is practiced to separate and store about equal amounts of only /sup 211/Rn and /sup 125/Xe, while preventing the extraction or storage of the radionuclides /sup 211/At and /sup 123/I.

A high-order relaxation method with projective integration for solving nonlinear systems of hyperbolic conservation laws

NASA Astrophysics Data System (ADS)

Lafitte, Pauline; Melis, Ward; Samaey, Giovanni

2017-07-01

We present a general, high-order, fully explicit relaxation scheme which can be applied to any system of nonlinear hyperbolic conservation laws in multiple dimensions. The scheme consists of two steps. In a first (relaxation) step, the nonlinear hyperbolic conservation law is approximated by a kinetic equation with stiff BGK source term. Then, this kinetic equation is integrated in time using a projective integration method. After taking a few small (inner) steps with a simple, explicit method (such as direct forward Euler) to damp out the stiff components of the solution, the time derivative is estimated and used in an (outer) Runge-Kutta method of arbitrary order. We show that, with an appropriate choice of inner step size, the time step restriction on the outer time step is similar to the CFL condition for the hyperbolic conservation law. Moreover, the number of inner time steps is also independent of the stiffness of the BGK source term. We discuss stability and consistency, and illustrate with numerical results (linear advection, Burgers' equation and the shallow water and Euler equations) in one and two spatial dimensions.

Lignocellulosic Biomass Transformations via Greener Oxidative Pretreatment Processes: Access to Energy and Value-Added Chemicals

PubMed Central

Den, Walter; Sharma, Virender K.; Lee, Mengshan; Nadadur, Govind; Varma, Rajender S.

2018-01-01

Anthropogenic climate change, principally induced by the large volume of carbon dioxide emission from the global economy driven by fossil fuels, has been observed and scientifically proven as a major threat to civilization. Meanwhile, fossil fuel depletion has been identified as a future challenge. Lignocellulosic biomass in the form of organic residues appears to be the most promising option as renewable feedstock for the generation of energy and platform chemicals. As of today, relatively little bioenergy comes from lignocellulosic biomass as compared to feedstock such as starch and sugarcane, primarily due to high cost of production involving pretreatment steps required to fragment biomass components via disruption of the natural recalcitrant structure of these rigid polymers; low efficiency of enzymatic hydrolysis of refractory feedstock presents a major challenge. The valorization of lignin and cellulose into energy products or chemical products is contingent on the effectiveness of selective depolymerization of the pretreatment regime which typically involve harsh pyrolytic and solvothermal processes assisted by corrosive acids or alkaline reagents. These unselective methods decompose lignin into many products that may not be energetically or chemically valuable, or even biologically inhibitory. Exploring milder, selective and greener processes, therefore, has become a critical subject of study for the valorization of these materials in the last decade. Efficient alternative activation processes such as microwave- and ultrasound irradiation are being explored as replacements for pyrolysis and hydrothermolysis, while milder options such as advanced oxidative and catalytic processes should be considered as choices to harsher acid and alkaline processes. Herein, we critically abridge the research on chemical oxidative techniques for the pretreatment of lignocellulosics with the explicit aim to rationalize the objectives of the biomass pretreatment step and the problems associated with the conventional processes. The mechanisms of reaction pathways, selectivity and efficiency of end-products obtained using greener processes such as ozonolysis, photocatalysis, oxidative catalysis, electrochemical oxidation, and Fenton or Fenton-like reactions, as applied to depolymerization of lignocellulosic biomass are summarized with deliberation on future prospects of biorefineries with greener pretreatment processes in the context of the life cycle assessment. PMID:29755972

Lignocellulosic Biomass Transformations via Greener Oxidative Pretreatment Processes: Access to Energy and Value-Added Chemicals.

PubMed

Den, Walter; Sharma, Virender K; Lee, Mengshan; Nadadur, Govind; Varma, Rajender S

2018-01-01

Anthropogenic climate change, principally induced by the large volume of carbon dioxide emission from the global economy driven by fossil fuels, has been observed and scientifically proven as a major threat to civilization. Meanwhile, fossil fuel depletion has been identified as a future challenge. Lignocellulosic biomass in the form of organic residues appears to be the most promising option as renewable feedstock for the generation of energy and platform chemicals. As of today, relatively little bioenergy comes from lignocellulosic biomass as compared to feedstock such as starch and sugarcane, primarily due to high cost of production involving pretreatment steps required to fragment biomass components via disruption of the natural recalcitrant structure of these rigid polymers; low efficiency of enzymatic hydrolysis of refractory feedstock presents a major challenge. The valorization of lignin and cellulose into energy products or chemical products is contingent on the effectiveness of selective depolymerization of the pretreatment regime which typically involve harsh pyrolytic and solvothermal processes assisted by corrosive acids or alkaline reagents. These unselective methods decompose lignin into many products that may not be energetically or chemically valuable, or even biologically inhibitory. Exploring milder, selective and greener processes, therefore, has become a critical subject of study for the valorization of these materials in the last decade. Efficient alternative activation processes such as microwave- and ultrasound irradiation are being explored as replacements for pyrolysis and hydrothermolysis, while milder options such as advanced oxidative and catalytic processes should be considered as choices to harsher acid and alkaline processes. Herein, we critically abridge the research on chemical oxidative techniques for the pretreatment of lignocellulosics with the explicit aim to rationalize the objectives of the biomass pretreatment step and the problems associated with the conventional processes. The mechanisms of reaction pathways, selectivity and efficiency of end-products obtained using greener processes such as ozonolysis, photocatalysis, oxidative catalysis, electrochemical oxidation, and Fenton or Fenton-like reactions, as applied to depolymerization of lignocellulosic biomass are summarized with deliberation on future prospects of biorefineries with greener pretreatment processes in the context of the life cycle assessment.

Lignocellulosic Biomass Transformations via Greener Oxidative Pretreatment Processes: Access to Energy and Value-Added Chemicals

NASA Astrophysics Data System (ADS)

Den, Walter; Sharma, Virender K.; Lee, Mengshan; Nadadur, Govind; Varma, Rajender S.

2018-04-01

Anthropogenic climate change, principally induced by the large volume of carbon dioxide emission from the global economy driven by fossil fuels, has been observed and scientifically proven as a major threat to civilization. Meanwhile, fossil fuel depletion has been identified as a future challenge. Lignocellulosic biomass in the form of organic residues appears to be the most promising option as renewable feedstock for the generation of energy and platform chemicals. As of today, relatively little bioenergy comes from lignocellulosic biomass as compared to feedstock such as starch and sugarcane, primarily due to high cost of production involving pretreatment steps required to fragment biomass components via disruption of the natural recalcitrant structure of these rigid polymers; low efficiency of enzymatic hydrolysis of refractory feedstock presents a major challenge. The valorization of lignin and cellulose into energy products or chemical products is contingent on the effectiveness of selective depolymerization of the pretreatment regime which typically involve harsh pyrolytic and solvothermal processes assisted by corrosive acids or alkaline reagents. These unselective methods decompose lignin into many products that may not be energetically or chemically valuable, or even biologically inhibitory. Exploring milder, selective and greener processes, therefore, has become a critical subject of study for the valorization of these materials in the last decade. Efficient alternative activation processes such as microwave- and ultrasound irradiation are being explored as replacements for pyrolysis and hydrothermolysis, while milder options such as advanced oxidative and catalytic processes should be considered as choices to harsher acid and alkaline processes. Herein, we critically abridge the research on chemical oxidative techniques for the pretreatment of lignocellulosics with the explicit aim to rationalize the objectives of the biomass pretreatment step and the problems associated with the conventional processes. The mechanisms of reaction pathways, selectivity and efficiency of end-products obtained using greener processes such as ozonolysis, photocatalysis, oxidative catalysis, electrochemical oxidation, and Fenton or Fenton-like reactions, as applied to depolymerization of lignocellulosic biomass are summarized with deliberation on future prospects of biorefineries with greener pretreatment processes in the context of the life cycle assessment.

A two-step, fourth-order method with energy preserving properties

NASA Astrophysics Data System (ADS)

Brugnano, Luigi; Iavernaro, Felice; Trigiante, Donato

2012-09-01

We introduce a family of fourth-order two-step methods that preserve the energy function of canonical polynomial Hamiltonian systems. As is the case with linear mutistep and one-leg methods, a prerogative of the new formulae is that the associated nonlinear systems to be solved at each step of the integration procedure have the very same dimension of the underlying continuous problem. The key tools in the new methods are the line integral associated with a conservative vector field (such as the one defined by a Hamiltonian dynamical system) and its discretization obtained by the aid of a quadrature formula. Energy conservation is equivalent to the requirement that the quadrature is exact, which turns out to be always the case in the event that the Hamiltonian function is a polynomial and the degree of precision of the quadrature formula is high enough. The non-polynomial case is also discussed and a number of test problems are finally presented in order to compare the behavior of the new methods to the theoretical results.

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

NASA Astrophysics Data System (ADS)

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

2016-09-01

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

Preschool Teachers' Skills in Teaching Music: Two Steps Forward One Step Back

ERIC Educational Resources Information Center

Ehrlin, Anna; Wallerstedt, Cecilia

2014-01-01

This study investigates through observations and interviews what importance further education has for preschool teachers' practice in two music-profiled preschool and their way of conceptualising it. A distinction between music as a method for teaching, on the one hand, and as a content of knowledge, on the other, is used in the analysis. The…

Studying the Global Bifurcation Involving Wada Boundary Metamorphosis by a Method of Generalized Cell Mapping with Sampling-Adaptive Interpolation

NASA Astrophysics Data System (ADS)

Liu, Xiao-Ming; Jiang, Jun; Hong, Ling; Tang, Dafeng

In this paper, a new method of Generalized Cell Mapping with Sampling-Adaptive Interpolation (GCMSAI) is presented in order to enhance the efficiency of the computation of one-step probability transition matrix of the Generalized Cell Mapping method (GCM). Integrations with one mapping step are replaced by sampling-adaptive interpolations of third order. An explicit formula of interpolation error is derived for a sampling-adaptive control to switch on integrations for the accuracy of computations with GCMSAI. By applying the proposed method to a two-dimensional forced damped pendulum system, global bifurcations are investigated with observations of boundary metamorphoses including full to partial and partial to partial as well as the birth of fully Wada boundary. Moreover GCMSAI requires a computational time of one thirtieth up to one fiftieth compared to that of the previous GCM.

The Synthesis of LiMnxFe1−xPO4/C Cathode Material through Solvothermal Jointed with Solid-State Reaction

PubMed Central

He, Xiangming; Wang, Jixian; Dai, Zhongjia; Wang, Li; Tian, Guangyu

2016-01-01

LiMnxFe1−xPO4/C material has been synthesized through a facile solid-state reaction under the condition of carbon coating, using solvothermal-prepared LiMnPO4 and LiFePO4 as precursors and sucrose as a carbon resource. XRD and element distribution analysis reveal completed solid-state reaction of precursors. LiMnxFe1−xPO4/C composites inherit the morphology of precursors after heat treatment without obvious agglomeration and size increase. LiMnxFe1−xPO4 solid solution forms at low temperature around 350 °C, and Mn2+/Fe2+ diffuse completely within 1 h at 650 °C. The LiMnxFe1−xPO4/C (x < 0.8) composite exhibits a high-discharge capacity of over 120 mAh·g−1 (500 Wh·kg−1) at low C-rates. This paves a way to synthesize the crystal-optimized LiMnxFe1−xPO4/C materials for high performance Li-ion batteries. PMID:28773887

Influence of Reduced Graphene Oxide on Effective Absorption Bandwidth Shift of Hybrid Absorbers.

PubMed

Ameer, Shahid; Gul, Iftikhar Hussain

2016-01-01

The magnetic nanoparticle composite NiFe2O4 has traditionally been studied for high-frequency microwave absorption with marginal performance towards low-frequency radar bands (particularly L and S bands). Here, NiFe2O4 nanoparticles and nanohybrids using large-diameter graphene oxide (GO) sheets are prepared via solvothermal synthesis for low-frequency wide bandwidth shielding (L and S radar bands). The synthesized materials were characterized using XRD, SEM, FTIR and microwave magneto dielectric spectroscopy. The dimension of these solvothermally synthesized pristine particles and hybrids lies within 30-58 nm. Microwave magneto-dielectric spectroscopy was performed in the low-frequency region in the 1 MHz-3 GHz spectrum. The as-synthesized pristine nanoparticles and hybrids were found to be highly absorbing for microwaves throughout the L and S radar bands (< -10 dB from 1 MHz to 3 GHz). This excellent microwave absorbing property induced by graphene sheet coupling shows application of these materials with absorption bandwidth which is tailored such that these could be used for low frequency. Previously, these were used for high frequency absorptions (typically > 4 GHz) with limited selective bandwidth.

Fabrication and luminescent properties of Al2O3:Cr3 + microspheres via a microwave solvothermal route followed by heat treatment

NASA Astrophysics Data System (ADS)

Zhu, Zhenfeng; Liu, Dianguang; Liu, Hui; Du, Juan; Yu, Hongguang; Deng, Jie

2012-06-01

AlOOH:Cr3 + powders were synthesized via a microwave solvothermal route at 433 K for 30 min and were used as the precursor and template for the preparation of γ-Al2O3:Cr3 + by thermal transformation at 773 K for 2 h in air. The obtained γ-Al2O3 based powders were microspheres with an average diameter about 1.9 μm. Photoluminescence (PL) spectra showed that the Al2O3:Cr3 + particles presented a symmetric broad R band at 696 nm without appreciable splitting when excited at 462 nm. It is shown that the 0.04 mol% of doping concentration of Cr3 + ions in γ-Al2O3:Cr3 + is optimum. According to Dexter's theory, the critical distance between Cr3 + ions for energy transfer was determined to be 47.54 Å. Based on the corresponding PL spectrum, full width at half maximum (FWHM) of Al2O3:Cr3 + (0.04 mol%) was calculated to be 3.35 nm.

Novel hedgehog-like 5 V LiCoPO4 positive electrode material for rechargeable lithium battery

NASA Astrophysics Data System (ADS)

Wang, Fei; Yang, Jun; NuLi, Yanna; Wang, Jiulin

2011-05-01

Hedgehog-like LiCoPO4 with hierarchical microstructures is first synthesized via a simple solvothermal process in water-benzyl alcohol mixed solvent at 200 °C. Morphology and crystalline structure of the samples are characterized by scanning electron microscope, transmission electron microscopy and X-ray diffraction. The hedgehog-like LiCoPO4 microstructures in the size of about 5-8 μm are composed of large numbers of nanorods in diameter of ca. 40 nm and length of ca. 1 μm, which are coated with a carbon layer of ca. 8 nm in thickness by in situ carbonization of glucose during the solvothermal reaction. As a 5 V positive electrode material for rechargeable lithium battery, the hedgehog-like LiCoPO4 delivers an initial discharge capacity of 136 mAh g-1 at 0.1 C rate and retains its 91% after 50 cycles, showing much better electrochemical performances than sub-micrometer LiCoPO4 synthesized by conventional high-temperature solid-state reaction.

Solvothermal synthesis of well-dispersed MF2 (M = Ca,Sr,Ba) nanocrystals and their optical properties

NASA Astrophysics Data System (ADS)

Zhang, Xiaoming; Quan, Zewei; Yang, Jun; Yang, Piaoping; Lian, Hongzhou; Lin, Jun

2008-02-01

MF2 (M = Ca,Sr,Ba) nanocrystals (NCs) were synthesized via a solvothermal process in the presence of oleic acid and characterized by x-ray diffraction (XRD), transmission electron microscopy (TEM), Fourier transform infrared (FT-IR) spectra, UV/vis absorption spectra, photoluminescence (PL) excitation and emission spectra, and lifetimes, respectively. In the synthetic process, oleic acid as a surfactant played a crucial role in confining the growth and solubility of the MF2 NCs. The as-prepared CaF2, SrF2 and BaF2 NCs present morphologies of truncated octahedron, cube and sheet in a narrow distribution, respectively. Possible growth mechanisms were proposed to explain these results. The as-prepared NCs are highly crystalline and can be well dispersed in cyclohexane to form stable and clear colloidal solutions, which demonstrate strong emission bands centred at 400 nm in photoluminescence (PL) spectra compared with the cyclohexane solvent. The PL properties of the colloidal solutions of the as-prepared NCs can be ascribed to the trap states of surface defects.

Reduced graphene oxide supported highly porous V2O5 spheres as a high-power cathode material for lithium ion batteries.

PubMed

Rui, Xianhong; Zhu, Jixin; Sim, Daohao; Xu, Chen; Zeng, Yi; Hng, Huey Hoon; Lim, Tuti Mariana; Yan, Qingyu

2011-11-01

Reduced graphene oxide (rGO) supported highly porous polycrystalline V(2)O(5) spheres (V(2)O(5)/rGO) were prepared by using a solvothermal approach followed by an annealing process. Initially, reduced vanadium oxide (rVO) nanoparticles with sizes in the range of 10-50 nm were formed through heterogeneous nucleation on rGO sheets during the solvothermal process. These rVO nanoparticles were oxidized to V(2)O(5) after the annealing process in air at 350 °C and assembled into polycrystalline porous spheres with sizes of 200-800 nm. The weight ratio between the rGO and V(2)O(5) is tunable by changing the weight ratio of the precursors, which in turn affects the morphology of V(2)O(5)/rGO composites. The V(2)O(5)/rGO composites display superior cathode performances with highly reversible specific capacities, good cycling stabilities and excellent rate capabilities (e.g. 102 mA h g(-1) at 19 C).