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.

Facile Synthesis of Novel Networked Ultralong Cobalt Sulfide Nanotubes and Its Application in Supercapacitors.

PubMed

Liu, Sangui; Mao, Cuiping; Niu, Yubin; Yi, Fenglian; Hou, Junke; Lu, Shiyu; Jiang, Jian; Xu, Maowen; Li, Changming

2015-11-25

Ultralong cobalt sulfide (CoS(1.097)) nanotube networks are synthesized by a simple one-step solvothermal method without any surfactant or template. A possible formation mechanism for the growth processes is proposed. Owing to the hollow structure and large specific area, the novel CoS(1.097) materials present outstanding electrochemical properties. Electrochemical measurements for supercapacitors show that the as-prepared ultralong CoS(1.097) nanotube networks exhibit high specific capacity, good capacity retention, and excellent Coulombic efficiency.

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

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.

LiFePO4 mesocrystals for lithium-ion batteries.

PubMed

Popovic, Jelena; Demir-Cakan, Rezan; Tornow, Julian; Morcrette, Mathieu; Su, Dang Sheng; Schlögl, Robert; Antonietti, Markus; Titirici, Maria-Magdalena

2011-04-18

Olivine LiFePO(4) is considered one of the most promising cathode materials for Li-ion batteries. A simple one-step, template-free, low-temperature solvothermal method is developed for the synthesis of urchinlike hierarchical mesocrystals of pristine LiFePO(4) as well as carbon-coated LiFePO(4) composites. Each urchinlike mesocrystal consists of LiFePO(4) sheets self-assembled via a dipolar field in spheres during a solvothermal process under the influence of Cl(-) anions. The obtained primary sheets of LiFePO(4) are single crystalline in nature and can be coated in situ with an amorphous nitrogen-doped carbonaceous layer several nanometers in thickness. To increase the conductivity of the carbon coating, the materials are subjected to further temperature treatment (700 °C) under an inert atmosphere. The lithium storage performance of the pure LiFePO(4) is compared with that of its carbon-coated counterparts. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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.

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.

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.

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.

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.

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

[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.

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.

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.

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.

Facile fabrication of plate-shaped hydrohausmannite as electrode material for supercapacitors

NASA Astrophysics Data System (ADS)

Liang, Jun; Chai, Yao; Li, Deli; Li, Meng; Lu, Jiaxue; Li, Li; Luo, Min

2017-08-01

A simple and one-step solvothermal synthesis method has been developed to prepare two-dimensional (2-D) hydrohausmannite ((Mn4-2xMnx)Mn8O16-x(OH)x) nanoplates with radial length of 300 nm and thickness of about 25 nm in a binary ethanediamine/water solvent system. The formation mechanism of hydrohausmannite is suggested. As an anode material for electrochemical capacitors, the plate-shaped hydrohausmannite not only displays a high specific capacity (215 at 0.1 A g-1) and good rate capability, but also shows good stable performance along with 94% specific capacity retained after 3000 cycle tests. The method can be easily controlled and expected to be applicable for the large-scale preparation of the 2-D hydrohausmannite.

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).

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

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

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.

One-Pot Solvothermal in Situ Growth of 1D Single-Crystalline NiSe on Ni Foil as Efficient and Stable Transparent Conductive Oxide Free Counter Electrodes for Dye-Sensitized Solar Cells.

PubMed

Bao, Chao; Li, Faxin; Wang, Jiali; Sun, Panpan; Huang, Niu; Sun, Yihua; Fang, Liang; Wang, Lei; Sun, Xiaohua

2016-12-07

One-dimensional single-crystal nanostructural nickel selenides were successfully in situ grown on metal nickel foils by two simple one-step solvothermal methods, which formed NiSe/Ni counter electrodes (CEs) for dye-sensitized solar cells (DSSCs). The nickel foil acted as the nickel source in the reaction process, a supporting substrate, and an electron transport "speedway". Electrochemical testing indicated that the top 1D single-crystal NiSe exhibited prominent electrocatalytic activity for I 3 - reduction. Due to the metallic conductivity of Ni substrate and the outstanding electrocatalytic activity of single-crystal NiSe, the DSSC based on a NiSe/Ni CE exhibited higher fill factor (FF) and larger short-circuit current density (J sc ) than the DSSC based on Pt/FTO CE. The corresponding power conversion efficiency (6.75%) outperformed that of the latter (6.18%). Moreover, the NiSe/Ni CEs also showed excellent electrochemical stability in the I - /I 3 - redox electrolyte. These findings indicated that single-crystal NiSe in situ grown on Ni substrate was a potential candidate to replace Pt/TCO as a cheap and highly efficient counter electrode of DSSC.

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.

One-pot solvothermal synthesis of ordered intermetallic Pt{sub 2}In{sub 3} as stable and efficient electrocatalyst towards direct alcohol fuel cell application

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

Jana, Rajkumar; Peter, Sebastian C., E-mail: sebastiancp@jncasr.ac.in

Ordered intermetallic Pt{sub 2}In{sub 3} nanoparticles have been synthesized by superhydride reduction of K{sub 2}PtCl{sub 4} and InCl{sub 3}.xH{sub 2}O precursors using facile, one-pot solvothermal method. We report surfactant free solvothermal synthesis of a novel ordered Pt{sub 2}In{sub 3} 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 Pt{sub 2}In{sub 3} catalyst exhibit far superior electrocatalytic activity andmore » 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 Pt{sub 2}In{sub 3} nanoparticles can make the catalyst an ideal catalyst candidate for direct alcohol fuel cell. - Graphical abstract: The ordered structure of Pt{sub 2}In{sub 3} nanoparticles synthesized by solvothermal method has confirmed through XRD and TEM. Cyclic voltametry and chronoamperometry showed improved catalytic activity and stability compared to commercial Pt/C. - Highlights: • Ordered Pt{sub 2}In{sub 3} nanoparticles were synthesized by solvothermal method. • Electrooxidation of alcohols on Pt{sub 2}In{sub 3} catalyst was investigated in acidic medium. • Pt{sub 2}In{sub 3} catalyst has superior catalytic activity compared to commercial Pt/C. • Pt{sub 2}In{sub 3} catalyst exhibited much higher stability than commercial Pt/C.« 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.

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.

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.

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.

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 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.

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.

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.

A One-Step, Solvothermal Reduction Method for Producing Reduced Graphene Oxide Dispersions in Organic Solvents

PubMed Central

Dubin, Sergey; Gilje, Scott; Wang, Kan; Tung, Vincent C.; Cha, Kitty; Hall, Anthony S.; Farrar, Jabari; Varshneya, Rupal; Yang, Yang; Kaner, Richard B.

2014-01-01

Refluxing graphene oxide (GO) in N-methyl-2-pyrrolidinone (NMP) results in deoxygenation and reduction to yield a stable colloidal dispersion. The solvothermal reduction is accompanied by a color change from light brown to black. Atomic force microscopy (AFM) and scanning electron microscopy (SEM) images of the product confirm the presence of single sheets of the solvothermally reduced graphene oxide (SRGO). X-ray photoelectron spectroscopy (XPS) of SRGO indicates a significant increase in intensity of the C=C bond character, while the oxygen content decreases markedly after the reduction is complete. X-ray diffraction analysis of SRGO shows a single broad peak at 26.24° 2θ (3.4 Å), confirming the presence of graphitic stacking of reduced sheets. SRGO sheets are redispersible in a variety of organic solvents, which may hold promise as an acceptor material for bulk heterojunction photovoltaic cells, or electromagnetic interference shielding applications. PMID:20586422

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.

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.

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.

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 fabrication and enhanced visible light photocatalytic activity of Cu2O-reduced graphene oxide composite microspheres for photodegradation of Rhodamine B

NASA Astrophysics Data System (ADS)

Sun, Lingling; Wang, Guohong; Hao, Ruirui; Han, Deyan; Cao, Sheng

2015-12-01

The addition of graphene oxide (GO) in the semiconductors has been regarded as one of the effective methods to enhance their photocatalytic activity. In this study, Cu2O-reduced graphene oxide (Cu2O-rGO) composites with low loading (0-0.5 wt.%) of graphene oxide (GO) were produced by a one-step green solvothermal method in ethanol system by using Cu(NO3)2·3H2O and glutamic acid as copper precursor and reducing agent, respectively. During the solvothermal treatment, GO was reduced to rGO. The as-prepared Cu2O-reduced graphene oxide composite microspheres exhibited enhanced photocatalytic activity toward the degradation of RhB aqueous solution under visible light irradiation. At the optimal loading of graphene oxide (0.05 wt.%), Cu2O-rGO composites showed the highest photocatalytic activity, exceeding that of pure Cu2O and commercial Degussa P25 by a factor of 2.9 and 7.9, respectively. The enhanced photocatalytic activity may be ascribed to the strong coupling interaction between Cu2O particles and rGO nanosheets, which reduces the recombination of charge carriers.

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.

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.

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.

Electrochemical and XPS study of LiFePO4 cathode nanocomposite with PPy/PEG conductive network

NASA Astrophysics Data System (ADS)

Fedorková, A.; Oriňáková, R.; Oriňák, A.; Kupková, M.; Wiemhöfer, H.-D.; Audinot, J. N.; Guillot, J.

2012-08-01

High performance PPy/PEG-LiFePO4 nanocomposites as cathode materials were synthesized by solvothermal method and simple chemical oxidative polymerization of pyrrole (Py) monomer on the surface of LiFePO4 particles. The samples were characterized by scanning electron microscope (SEM), energy dispersive X-ray spectroscopy (EDX), X-ray photoelectron spectrometry (XPS) and charge-discharge tests. PPyPEG hybrid layers decrease particle to particle contact resistance while the impedance measurements confirmed that the coating of PPy-PEG significantly decreases the charge transfer resistance of the electrode material. The initial discharge capacities of this sample at C/5 and 1C are 150 and 128 mAh/g, respectively. The results show that PPy/PEGLiFePO4 composites are more effective than bare LiFePO4 as cathode material.

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 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.

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

Simple and efficient synthesis of copper(II)-modified uniform magnetic Fe3O4@SiO2 core/shell microspheres for immobilization of cellulase

NASA Astrophysics Data System (ADS)

Li, Shi-Kuo; Hou, Xiao-Cheng; Huang, Fang-Zhi; Li, Chuan-Hao; Kang, Wen-Juan; Xie, An-Jian; Shen, Yu-Hua

2013-11-01

In this paper, we reported a simple and efficient protocol for preparation of Cu2+-modified magnetic Fe3O4@SiO2 core/shell microspheres for immobilization of cellulase. The uniform magnetic Fe3O4@SiO2 core/shell microspheres with a thin shell of 20 nm were synthesized through a solvothermal method followed by a sol-gel process. An amino-terminated silane coupling agent of (3-aminopropyl)triethoxysilane (APTS) was then grafted on them for capturing Cu2+ ions. The reaction process is very simple, efficient, and economical. Noticeably, the content of Cu2+ ions on the magnetic core/shell microspheres can reach 4.6 Wt%, endowing them possess as high immobilization capacity as 225.5 mg/g for cellulase. And the immobilized cellulase can be retained over 90 % on the magnetic microspheres after six cycles. Meanwhile, the magnetic microspheres decorated with Cu2+ ions show a superparamagnetic character with a high magnetic saturation of 58.5 emu/g at room temperature, suggesting conveniently and rapidly recycle the enzyme from solution. This facile, recyclable, high immobilization capacity and activity strategy may find potential applications in enzyme catalytic reactions with low cost.

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.

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.

Template-free synthesis of mesoporous nanoring-like Zn-Co mixed oxides with high lithium storage performance

NASA Astrophysics Data System (ADS)

Lu, Lun; Gao, Yan-Li; Yang, Zhi-Zheng; Wang, Cheng; Wang, Jin-Guo; Wang, Hui-Yuan; Jiang, Qi-Chuan

2018-04-01

Mesoporous nanoring-like Zn-Co mixed oxides are synthesized via a simple template-free solvothermal method with a subsequent annealing process. The ring-like nanostructures with hollow interiors are formed under the complexing effects of potassium sodium tartrate. Numerous mesopores are generated after the precursor is annealed at 500 °C. When applied as anode materials, the mesoporous nanoring-like Zn-Co mixed oxides can deliver a high discharge capacity of 1102 mAh g-1 after 200 cycles at 500 mA g-1. Even when the current density is increased to 2 A g-1, the mixed oxides can still retain a reversible capacity of 761 mAh g-1. Such high cycling stability and rate capability are mainly derived from the unique mesoporous ring-like nanostructures and the synergistic effects between Zn and Co based oxides.

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.

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.

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.

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

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.

Synthesis of flower-like BaTiO3/Fe3O4 hierarchically structured particles and their electrorheological and magnetic properties.

PubMed

Wang, Baoxiang; Yin, Yichao; Liu, Chenjie; Yu, Shoushan; Chen, Kezheng

2013-07-21

Flower-like BaTiO3/Fe3O4 hierarchically structured particles composed of nano-scale structures on micro-scale materials were synthesized by a simple solvothermal approach and characterized by the means of X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), magnetic testing and rotary viscometer. The influences on the morphology and structure of solvothermal times, type and amount of surfactant, EG : H2O ratio, etc. were studied. Magnetic testing results show that the samples have strong magnetism and they exhibit superparamagnetic behavior, as evidenced by no coercivity and the remanence at room temperature, due to their very small sizes, observed on the M-H loop. The saturation magnetization (M(s)) value can achieve 18.3 emu g(-1). The electrorheological (ER) effect was investigated using a suspension of the flower-like BaTiO3/Fe3O4 hierarchically structured particles dispersed in silicone oil. We can observe a slight shear-thinning behavior of shear viscosity at a low shear rate region even at zero applied electric field and a Newtonian fluid behavior at high shear rate regions.

Microemulsion-mediated solvothermal synthesis of tin(IV) hydrogen phosphate rose-like three-dimensional nanostructures and their electrochemical properties

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

Yang Hui; He Xiaoyan; Cao Minhua

2009-03-05

Novel rose-like three-dimensional Sn(HPO{sub 4}){sub 2}.H{sub 2}O nanostructures self-assembled by tightly stacked nanopetals were successfully synthesized by a simple cetyltrimethylammonium bromide (CTAB)/water/cyclohexane/n-pentanol microemulsion system under solvothermal conditions for the first time. A series of compared experiments were carried out to investigate the factors that influence the morphology and size of the products. It was found that the molar ratio of water to CTAB and the concentration of SnCl{sub 4} aqueous solution play important roles in the formation of the rose-like nanostructures. A possible formation mechanism of rose-like nanostructures was proposed, which may be related to the crystal structure of Sn(HPO{submore » 4}){sub 2}.H{sub 2}O and the spherical micelles formed by the microemulsion. The electrochemical properties of Sn(HPO{sub 4}){sub 2}.H{sub 2}O were investigated through cyclic voltammetry (CV) measurements. X-ray powder diffraction (XRD), transmission electron microscopy (TEM), and field-emission scanning electron microscope (FE-SEM) were used to characterize the products.« 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.

Removal of methylene blue from aqueous solution by a solvothermal-synthesized graphene/magnetite composite.

PubMed

Ai, Lunhong; Zhang, Chunying; Chen, Zhonglan

2011-09-15

In this study, we have demonstrated a facile one-step solvothermal method for the synthesis of the graphene nanosheet (GNS)/magnetite (Fe(3)O(4)) composite. During the solvothermal treatment, in situ conversion of FeCl(3) to Fe(3)O(4) and simultaneous reduction of graphene oxide (GO) into graphene in ethylene glycol solution were achieved. Electron microscopy study suggests the Fe(3)O(4) spheres with a size of about 200 nm are uniformly distributed and firmly anchored on the wrinkled graphene layers with a high density. The resulting GNS/Fe(3)O(4) composite shows extraordinary adsorption capacity and fast adsorption rates for removal of organic dye, methylene blue (MB), in water. The adsorption kinetics, isotherms and thermodynamics were investigated in detail to reveal that the kinetics and equilibrium adsorptions are well-described by pseudo-second-order kinetic and Langmuir isotherm model, respectively. The thermodynamic parameters reveal that the adsorption process is spontaneous and endothermic in nature. This study shows that the as-prepared GNS/Fe(3)O(4) composite could be utilized as an efficient, magnetically separable adsorbent for the environmental cleanup. Copyright © 2011 Elsevier B.V. All rights reserved.

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.

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

Development of magnetic graphene @hydrophilic polydopamine for the enrichment and analysis of phthalates in environmental water samples.

PubMed

Wang, Xianying; Song, Guoxin; Deng, Chunhui

2015-01-01

Magnetic graphene @hydrophilic polydopamine composites were successfully fabricated via a simple solvothermal reaction and self-polymerization of dopamine. Benefit from the excellent characteristics of strong magnetic responsivity, super-hydrophilicity and abundant π-electron system, the prepared material showed great potential as a magnetic solid phase extraction (MSPE) sorbent. In this work, six kinds of phthalates (PAEs) were selected as the target analytes to evaluate the extraction ability of the adsorbents combined with MSPE-GC-MS. And various extraction parameters were optimized by selecting the pH value of samples, the amount of sorbents, adsorption and desorption time, the type and volume of eluting solution. Meanwhile, the whole extraction process could be finished in 30 min. Under the optimized conditions, validations of the method were evaluated as well. And the results presented excellent linearity with a wide range of 50-20,000 μg/L (R(2)>0.9991). The detection of limits were in the range from 0.05-5 μg/L (S/N=3). Therefore, the novel magnetic graphene@polydopamine composites were successfully used as the sorbents for the enrichment and analysis of PAEs in real water samples. This proposed method provided a simple, efficient and sensitive approach for the determination of aromatic compounds in real environmental samples. Copyright © 2014 Elsevier B.V. All rights reserved.

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

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.

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

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.

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

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

Surfactant-assisted growth and optical properties of ZnO hexagonal bilayer disk-like microstructures

NASA Astrophysics Data System (ADS)

Zhu, Q. P.; Shen, X. Y.; Wang, L. L.; Zhu, L. P.; Wang, L. J.; Liao, G. H.

2018-01-01

ZnO hexagonal bilayer disk-like microstructures are successfully fabricated using a simple solvothermal method assisted with surfactant. The structure and morphology were investigated by XRD, SEM, and EDS. XRD result indicated that the as-obtained samples were well-crystallized wurtzite hexagonal ZnO structure. SEM images showed that the ZnO hexagonal bilayer disk-like assembles consist of two uniform and smooth disks with an average edge length of 6 μm and thickness of ˜4 μm. UV-vis spectrum reveals that ZnO sampls show an appreciable red shift and the band gap energy of the obtained ZnO samples were about 3.15 eV. A very strong UV emission at the ultraviolet (UV) region was observed in the photoluminescence (PL) spectrum of the as-prepared ZnO samples tested at room-temperature. A possible growth process of the ZnO hexagonal bilayer disk-like microstructures was schematically illustrated.

MoS2 /Carbon Nanotube Core-Shell Nanocomposites for Enhanced Nonlinear Optical Performance.

PubMed

Zhang, Xiaoyan; Selkirk, Andrew; Zhang, Saifeng; Huang, Jiawei; Li, Yuanxin; Xie, Yafeng; Dong, Ningning; Cui, Yun; Zhang, Long; Blau, Werner J; Wang, Jun

2017-03-08

Nanocomposites of layered MoS 2 and multi-walled carbon nanotubes (CNTs) with core-shell structure were prepared by a simple solvothermal method. The formation of MoS 2 nanosheets on the surface of coaxial CNTs has been confirmed by scanning electron microscopy, transmission electron microscopy, absorption spectrum, Raman spectroscopy, and X-ray photoelectron spectroscopy. Enhanced third-order nonlinear optical performances were observed for both femtosecond and nanosecond laser pulses over a broad wavelength range from the visible to the near infrared, compared to those of MoS 2 and CNTs alone. The enhancement can be ascribed to the strong coupling effect and the photoinduced charge transfer between MoS 2 and CNTs. This work affords an efficient way to fabricate novel CNTs based nanocomposites for enhanced nonlinear light-matter interaction. The versatile nonlinear properties imply a huge potential of the nanocomposites in the development of nanophotonic devices, such as mode-lockers, optical limiters, or optical switches. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

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.

Controllable construction of flower-like FeS/Fe2O3 composite for lithium storage

NASA Astrophysics Data System (ADS)

Wang, Jie; He, Huan; Wu, Zexing; Liang, Jianing; Han, Lili; Xin, Huolin L.; Guo, Xuyun; Zhu, Ye; Wang, Deli

2018-07-01

Transitions metal sulfides/oxides have been considered as promising anode candidates for next generation lithium-ion batteries (LIBs) due to high theoretical capacities. However, the large volume change during lithiation/delithiation process and poor electronic conductivity often result in a poor charging/discharging performance. Herein, we design a flower-like FeS/Fe2O3 composite via a simple "solvothermal-oxidation" method, in which the Fe2O3 is most distributed on the surface of the flower. The unique porous structure and synergistic effect between FeS and Fe2O3 not only accommodate the large volume expansion, but also facilitate Li ion and electron transport. The Fe2O3 shell effectively reduce the dissolution of Li2Sx during discharge/charge process. When serving as the anode material in lithium ion battery, FeS/Fe2O3 exhibits superior specific capacity, rate capacity and cycling stability compared with pure FeS and Fe2O3.

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.

In-situ preparation and unique electrochemical behavior of pore-embedding CoO/Co3O4 intermixed composite for Li+ rechargeable battery electrodes

NASA Astrophysics Data System (ADS)

Kim, Jin Kyu; Ju, Ji Young; Choi, Seul Ki; Unithrattil, Sanjith; Lee, Sun Sook; Kang, Yongku; Kim, Yongseon; Im, Won Bin; Choi, Sungho

2018-02-01

Electrochemically active CoO/Co3O4 co-existing microspheres with morphology-inherited porous particles is successfully synthesized via a simple solvothermal method. The as-prepared intermixed composite undergoes a monoxide CoO-preferred conversion reaction with an extremely enhanced capacity retention, ∼905 mA h g-1 after 250 cycles for discharge state, which is 1.6 times higher than the conventional CoOx-based anodes. Moreover, stable catalytic behavior of the electrocatalysts in Li-air cathodes of the given composites is also demonstrated. We believe that the extraordinarily enhanced electrode performance might be due to the novel pore-tempered microspheres packed with double electrochemically active centers of the CoO/Co3O4 composite effectively confine the detrimental volume exchange during the reversible cyclic reactions as well as the preserved multiple reactive sites for a reversible Li+ ⇄ LiOx reaction, which is advantageous for advanced Li rechargeable battery.

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

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.

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.

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

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.

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

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 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.

[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.

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.

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.

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.

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

Fabrication and Electromagnetic Properties of Conjugated NH2-CuPc@Fe3O4

NASA Astrophysics Data System (ADS)

Yan, Liang; Pu, Zejun; Xu, Mingzhen; Wei, Renbo; Liu, Xiaobo

2017-10-01

Conjugated amino-phthalocyanine copper containing carboxyl groups/magnetite (NH2-CuPc@Fe3O4) has been fabricated from FeCl3·6H2O and NH2-CuPc via a simple solvothermal method and its electromagnetic properties investigated. Scanning electron microscopy and transmission electron microscopy revealed that the NH2-CuPc@Fe3O4 was a waxberry-like nanomaterial with NH2-CuPc molecules effectively embedded in the interior of Fe3O4 particles in the form of beads. Introduction of NH2-CuPc effectively improved the complementarity between the dielectric and magnetic losses of the system, resulting in excellent electromagnetic performance. The minimum reflection loss of the as-prepared composite reached -33.4 dB at 7.0 GHz for coating layer thickness of 4.0 mm and bandwidth below -10.0 dB (90% absorption) of up to 3.8 GHz. These results indicate that introduction of NH2-CuPc results in a composite with potential for use as an electromagnetic microwave absorption material.

Research Update: Facile synthesis of CoFe2O4 nano-hollow spheres for efficient bilirubin adsorption

NASA Astrophysics Data System (ADS)

Rakshit, Rupali; Pal, Monalisa; Chaudhuri, Arka; Mandal, Madhuri; Mandal, Kalyan

2015-11-01

Herein, we report an unprecedented bilirubin (BR) adsorption efficiency of CoFe2O4 (CFO) nanostructures in contrast to the commercially available activated carbon and resin which are generally used for haemoperfusion and haemodialysis. We have synthesized CFO nanoparticles of diameter 100 nm and a series of nano-hollow spheres of diameter 100, 160, 250, and 350 nm using a simple template free solvothermal technique through proper variation of reaction time and capping agent, oleylamine (OLA), respectively, and carried out SiO2 coating by employing Stöber method. The comparative BR adsorption study of CFO and SiO2 coated CFO nanostructures indicates that apart from porosity and hollow configuration of nanostructures, the electrostatic affinity between anionic carboxyl group of BR and cationic amine group of OLA plays a significant role in adsorbing BR. Finally, we demonstrate that the BR adsorption capacity of the nanostructures can be tailored by varying the morphology as well as size of the nanostructures. We believe that our developed magnetic nanostructures could be considered as a potential material towards therapeutic applications against hyperbilirubinemia.

Highly exposed {001} facets of titanium dioxide modified with reduced graphene oxide for dopamine sensing.

PubMed

How, Gregory Thien Soon; Pandikumar, Alagarsamy; Ming, Huang Nay; Ngee, Lim Hong

2014-05-23

Titanium dioxide (TiO2) with highly exposed {001} facets was synthesized through a facile solvo-thermal method and its surface was decorated by using reduced graphene oxide (rGO) sheets. The morphology and chemical composition of the prepared rGO/TiO2 {001} nanocomposite were examined by using suitable characterization techniques. The rGO/TiO2 {001} nanocomposite was used to modify glassy carbon electrode (GCE), which showed higher electrocatalytic activity towards the oxidation of dopamine (DA) and ascorbic acid (AA), when compared to unmodified GCE. The differential pulse voltammetric studies revealed good sensitivity and selectivity nature of the rGO/TiO2 {001} nanocomposite modified GCE for the detection of DA in the presence of AA. The modified GCE exhibited a low electrochemical detection limit of 6 μM over the linear range of 2-60 μM. Overall, this work provides a simple platform for the development of GCE modified with rGO/TiO2 {001} nanocomposite with highly exposed {001} facets for potential electrochemical sensing applications.

Highly exposed {001} facets of titanium dioxide modified with reduced graphene oxide for dopamine sensing

NASA Astrophysics Data System (ADS)

How, Gregory Thien Soon; Pandikumar, Alagarsamy; Ming, Huang Nay; Ngee, Lim Hong

2014-05-01

Titanium dioxide (TiO2) with highly exposed {001} facets was synthesized through a facile solvo-thermal method and its surface was decorated by using reduced graphene oxide (rGO) sheets. The morphology and chemical composition of the prepared rGO/TiO2 {001} nanocomposite were examined by using suitable characterization techniques. The rGO/TiO2 {001} nanocomposite was used to modify glassy carbon electrode (GCE), which showed higher electrocatalytic activity towards the oxidation of dopamine (DA) and ascorbic acid (AA), when compared to unmodified GCE. The differential pulse voltammetric studies revealed good sensitivity and selectivity nature of the rGO/TiO2 {001} nanocomposite modified GCE for the detection of DA in the presence of AA. The modified GCE exhibited a low electrochemical detection limit of 6 μM over the linear range of 2-60 μM. Overall, this work provides a simple platform for the development of GCE modified with rGO/TiO2 {001} nanocomposite with highly exposed {001} facets for potential electrochemical sensing applications.

Highly exposed {001} facets of titanium dioxide modified with reduced graphene oxide for dopamine sensing

PubMed Central

How, Gregory Thien Soon; Pandikumar, Alagarsamy; Ming, Huang Nay; Ngee, Lim Hong

2014-01-01

Titanium dioxide (TiO2) with highly exposed {001} facets was synthesized through a facile solvo-thermal method and its surface was decorated by using reduced graphene oxide (rGO) sheets. The morphology and chemical composition of the prepared rGO/TiO2 {001} nanocomposite were examined by using suitable characterization techniques. The rGO/TiO2 {001} nanocomposite was used to modify glassy carbon electrode (GCE), which showed higher electrocatalytic activity towards the oxidation of dopamine (DA) and ascorbic acid (AA), when compared to unmodified GCE. The differential pulse voltammetric studies revealed good sensitivity and selectivity nature of the rGO/TiO2 {001} nanocomposite modified GCE for the detection of DA in the presence of AA. The modified GCE exhibited a low electrochemical detection limit of 6 μM over the linear range of 2–60 μM. Overall, this work provides a simple platform for the development of GCE modified with rGO/TiO2 {001} nanocomposite with highly exposed {001} facets for potential electrochemical sensing applications. PMID:24853929

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.

Improving cycle stability of SnS anode for sodium-ion batteries by limiting Sn agglomeration

NASA Astrophysics Data System (ADS)

Wang, Wenhui; Shi, Liang; Lan, Danni; Li, Quan

2018-02-01

Flower-like SnS nanostructures are obtained by a simple solvothermal method for anode applications in Na-ion batteries. We show experimental evidence of progressive Sn agglomeration and crystalline Na2S enrichment at the end of de-sodiation process of the SnS electrode, both of which contribute to the capacity decay of the electrode upon repeated cycles. By replacing the commonly adopted acetylene black conductive additive with multi-wall carbon nanotubes (MWCNT), the cycle stability of the SnS electrode is largely improved, which correlates well with the observed suppression of both Sn agglomeration and Na2S enrichment at the end of de-sodiation cycle. A full cell is assembled with the SnS/MWCNT anode and the P2-Na2/3Ni1/3Mn1/2Ti1/6O2 cathode. An initial energy density of 262 Wh/kg (normalized to the total mass of cathode and anode) is demonstrated for the full cell, which retains 71% of the first discharge capacity after 40 cycles.

Preparation and performance study of MgFe2O4/metal-organic framework composite for rapid removal of organic dyes from water

NASA Astrophysics Data System (ADS)

Tian, Huairu; Peng, Jun; Lv, Tingting; Sun, Chen; He, Hua

2018-01-01

In present study, a stable and magnetic metal-organic framework (MOF) material was synthesized by simple solvothermal method as adsorbent to rapid removal of two organic dyes, the Rhodamine B (RB) and Rhodamine 6G (Rh6G), in water samples. The prepared material showed great characteristics of large surface area (519.86 m2 g-1), excellent magnetic responsivity (35.00 emu g-1) and rapid removal (within 5 min). Maximum adsorption capacities of the magnetic material toward RB and Rh6G were up to 219.78 and 306.75 mg g-1, respectively. Adsorption kinetics suggested the adsorption process met the pseudo-second-order kinetic model. The prepared material could be reused at least 10 times by washing with acetonitrile solution, the relative standard deviation (RSD) of these ten cycles removal efficiency was 4.8%. In conclusion, good chemical inertness, a mechanical/water stability and super-hydrophilicity feature made this MOF a promising adsorbent for targets removal from environmental water sample.

Enhanced electrochemical performance of a ZnO-MnO composite as an anode material for lithium ion batteries.

PubMed

Song, Min Seob; Nahm, Sahn; Cho, Won Il; Lee, Chongmok

2015-09-28

A ZnO-MnO composite was synthesized using a simple solvothermal method combined with a high-temperature treatment. To observe the phase change during the heating process, in situ high-temperature XRD analysis was performed under vacuum conditions. The results indicated that ZnMn2O4 transformed into the ZnO-MnO composite phase starting from 500 °C and that this composite structure was retained until 700 °C. The electrochemical performances of the ZnO-MnO composite electrode were evaluated through galvanostatic discharge-charge tests and cyclic voltammetry analysis. Its initial coulombic efficiency was significantly improved to 68.3% compared to that of ZnMn2O4 at 54.7%. Furthermore, the ZnO-MnO composite exhibited improved cycling performance and enhanced rate capability compared with untreated ZnMn2O4. To clarify the discharge-charge mechanism of the ZnO-MnO composite electrode, the structural changes during the charge and discharge processes were also investigated using ex situ XRD and TEM.

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

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.

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.

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.

One-step solvothermal deposition of ZnO nanorod arrays on a wood surface for robust superamphiphobic performance and superior ultraviolet resistance

PubMed Central

Yao, Qiufang; Wang, Chao; Fan, Bitao; Wang, Hanwei; Sun, Qingfeng; Jin, Chunde; Zhang, Hong

2016-01-01

In the present paper, uniformly large-scale wurtzite-structured ZnO nanorod arrays (ZNAs) were deposited onto a wood surface through a one-step solvothermal method. The as-prepared samples were characterized by X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FTIR), thermogravimetry (TG), and differential thermal analysis (DTA). ZNAs with a diameter of approximately 85 nm and a length of approximately 1.5 μm were chemically bonded onto the wood surface through hydrogen bonds. The superamphiphobic performance and ultraviolet resistance were measured and evaluated by water or oil contact angles (WCA or OCA) and roll-off angles, sand abrasion tests and an artificially accelerated ageing test. The results show that the ZNA-treated wood demonstrates a robust superamphiphobic performance under mechanical impact, corrosive liquids, intermittent and transpositional temperatures, and water spray. Additionally, the as-prepared wood sample shows superior ultraviolet resistance. PMID:27775091

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.

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.

One-step solvothermal deposition of ZnO nanorod arrays on a wood surface for robust superamphiphobic performance and superior ultraviolet resistance

NASA Astrophysics Data System (ADS)

Yao, Qiufang; Wang, Chao; Fan, Bitao; Wang, Hanwei; Sun, Qingfeng; Jin, Chunde; Zhang, Hong

2016-10-01

In the present paper, uniformly large-scale wurtzite-structured ZnO nanorod arrays (ZNAs) were deposited onto a wood surface through a one-step solvothermal method. The as-prepared samples were characterized by X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FTIR), thermogravimetry (TG), and differential thermal analysis (DTA). ZNAs with a diameter of approximately 85 nm and a length of approximately 1.5 μm were chemically bonded onto the wood surface through hydrogen bonds. The superamphiphobic performance and ultraviolet resistance were measured and evaluated by water or oil contact angles (WCA or OCA) and roll-off angles, sand abrasion tests and an artificially accelerated ageing test. The results show that the ZNA-treated wood demonstrates a robust superamphiphobic performance under mechanical impact, corrosive liquids, intermittent and transpositional temperatures, and water spray. Additionally, the as-prepared wood sample shows superior ultraviolet resistance.

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

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.

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

Facile solvothermal synthesis of cube-like Ag@AgCl: a highly efficient visible light photocatalyst

NASA Astrophysics Data System (ADS)

Han, Lei; Wang, Ping; Zhu, Chengzhou; Zhai, Yueming; Dong, Shaojun

2011-07-01

In this paper, a stable and highly efficient plasmonic photocatalyst, Ag@AgCl, with cube-like morphology, has been successfully prepared via a simple hydrothermal method. Using methylene dichloride as chlorine source in the synthesis can efficiently control the morphology of Ag@AgCl, due to the low release rate of chloride ions. Scanning electron microscopy (SEM), X-ray powder diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and UV-vis diffuse reflectance spectra were used to characterize the obtained product. The photocatalytic activity of the obtained product was evaluated by the photodegradation of methyl orange (MO) under visible light irradiation, and it was found, interestingly, that Ag@AgCl exhibits high visible light photocatalytic activity and good stability.In this paper, a stable and highly efficient plasmonic photocatalyst, Ag@AgCl, with cube-like morphology, has been successfully prepared via a simple hydrothermal method. Using methylene dichloride as chlorine source in the synthesis can efficiently control the morphology of Ag@AgCl, due to the low release rate of chloride ions. Scanning electron microscopy (SEM), X-ray powder diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and UV-vis diffuse reflectance spectra were used to characterize the obtained product. The photocatalytic activity of the obtained product was evaluated by the photodegradation of methyl orange (MO) under visible light irradiation, and it was found, interestingly, that Ag@AgCl exhibits high visible light photocatalytic activity and good stability. Electronic supplementary information (ESI) available: SEM images of the AgCl samples synthesized by changing the addition amount of PVP and AgNO3. See DOI: 10.1039/c1nr10247h

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.

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.

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

Interesting electron storage phenomenon in the spherical Ag/TiO{sub 2} nanocomposites and its application for the decomposition of acetaldehyde in the dark

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

Wang, Xinyan; State Key Laboratory of Electroanalytical Chemistry, c/o Engineering Laboratory for Modern Analytical Techniques, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, Changchun 130022; Wu, Tongshun

2016-01-15

Highlights: • The Ag/TiO{sub 2} composites have been prepared by a facile solvothermal method. • The photogenerated charges transfer behaviors between the Ag and TiO{sub 2}. • The Ag/TiO{sub 2} composites can store photogenerated electrons for a relative long time. • The Ag/TiO{sub 2} composite could be further used to decompose acetaldehyde in the dark. - Abstract: Ag/TiO{sub 2} nanocomposite has been prepared by a facile one-step low-temperature solvothermal method. The powder X-ray diffraction (XRD) and transmission electron microscopy (TEM) measurements have been used to characterize the detailed structure of the as-synthesized nanocomposite and the results indicate that the nanocompoistemore » is with the spherical structure and Ag and TiO{sub 2} nanoparticles are homogeneously dispersed in the sphere. Surface photovoltage (SPV) and transient photovoltage (TPV) techniques were used to further investigate the charge transfer behavior between the TiO{sub 2} and Ag in this composite material, and the results reveal that the nanocomposites could store the electrons for a relative long time even under air. Furthermore, these stored electrons in the nanocomposites have been successfully applied to decompose the acetaldehyde in the dark.« less

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.

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

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 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.

Synthesis optimisation and characterisation of the organic-inorganic layered materials ZnS(m-xylylenediamine){sub 1/2} and ZnS(p-xylylenediamine){sub 1/2}

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

Luberda-Durnaś, K.; Guillén, A. González; Łasocha, W., E-mail: lasocha@chemia.uj.edu.pl

2016-06-15

Hybrid organic-inorganic layered materials of the type ZnS(amine){sub 1/2}, where amine=m-xylylenediamine (MXDA) or p-xylylenediamine (PXDA), were synthesised using a simple solvothermal method. Since the samples crystallised in the form of very fine powder, X-ray powder diffraction techniques were used for structural characterisation. The crystal structure studies, involving direct methods, show that both compounds crystallised in the orthorhombic crystal system, but in different space groups: ZnS(MXDA){sub 1/2} in non-centrosymmetric Ccm2{sub 1}, ZnS(PXDA){sub 1/2} in centrosymmetric Pcab. The obtained materials are built according to similar orders: semiconducting monolayers with the formula ZnS, parallel to the (010) plane, are separated by diamines. Themore » organic and inorganic fragments are connected by covalent bonds between metal atoms of the layers and nitrogen atoms of the amino groups. The optical properties of the hybrid materials differ from those of their bulk counterpart. In both compounds a blue-shift of about 0.8 or 0.9 eV was observed with reference to the bulk phase of ZnS. - Highlights: • New hybrid compounds: ZnS(MXDA){sub 1/2} and ZnS(PXDA){sub 1/2} were obtained. • Hybrids were studied using XRD, TG/DSC, XRK, SEM, UV–vis spectroscopy. • Structures of both materials were solved by powder diffraction methods.« less

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.

Facile Synthesis of V₂O₅ Hollow Spheres as Advanced Cathodes for High-Performance Lithium-Ion Batteries.

PubMed

Zhang, Xingyuan; Wang, Jian-Gan; Liu, Huanyan; Liu, Hongzhen; Wei, Bingqing

2017-01-18

Three-dimensional V₂O₅ hollow structures have been prepared through a simple synthesis strategy combining solvothermal treatment and a subsequent thermal annealing. The V₂O₅ materials are composed of microspheres 2-3 μm in diameter and with a distinct hollow interior. The as-synthesized V₂O₅ hollow microspheres, when evaluated as a cathode material for lithium-ion batteries, can deliver a specific capacity as high as 273 mAh·g -1 at 0.2 C. Benefiting from the hollow structures that afford fast electrolyte transport and volume accommodation, the V₂O₅ cathode also exhibits a superior rate capability and excellent cycling stability. The good Li-ion storage performance demonstrates the great potential of this unique V₂O₅ hollow material as a high-performance cathode for lithium-ion batteries.

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

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.

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

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.

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.

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

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.

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.

Solvothermal one-step synthesis of Ni-Al layered double hydroxide/carbon nanotube/reduced graphene oxide sheet ternary nanocomposite with ultrahigh capacitance for supercapacitors.

PubMed

Yang, Wanlu; Gao, Zan; Wang, Jun; Ma, Jing; Zhang, Milin; Liu, Lianhe

2013-06-26

A Ni-Al layered double hydroxide (LDH), mutil-wall carbon nanotube (CNT), and reduced graphene oxide sheet (GNS) ternary nanocomposite electrode material has been developed by a facile one-step ethanol solvothermal method. The obtained LDH/CNT/GNS composite displayed a three-dimensional (3D) architecture with flowerlike Ni-Al LDH/CNT nanocrystallites gradually self-assembled on GNS nanosheets. GNS was used as building blocks to construct 3D nanostructure, and the LDH/CNT nanoflowers in turn separated the two-dimensional (2D) GNS sheets, which preserved the high surface area of GNSs. Furthermore, the generated porous networks with a narrow pore size distribution in the LDH/CNT/GNS composite were also demonstrated by the N2 adsorption/desorption experiment. Such morphology would be favorable to improve the mass transfer and electrochemical action of the electrode. As supercapacitor electrode material, the LDH/CNT/GNS hybrid exhibited excellent electrochemical performance, including ultrahigh specific capacitance (1562 F/g at 5 mA/cm(2)), excellent rate capability, and long-term cycling performance, which could be a promising energy storage/conversion material for supercapacitor application.

Morphology controlled synthesis of nanoporous Co3O4 nanostructures and their charge storage characteristics in supercapacitors.

PubMed

Deori, Kalyanjyoti; Ujjain, Sanjeev Kumar; Sharma, Raj Kishore; Deka, Sasanka

2013-11-13

Cubic spinel Co3O4 nanoparticles with spherical (0D) and hexagonal platelet (2D) morphologies were synthesized using a simple solvothermal method by tuning the reaction time. XRD and HRTEM analyses revealed pure phase with growth of Co3O4 particles along [111] and [110] directions. UV-vis studies showed two clear optical absorption peaks corresponding to two optical band gaps in the range of 400-500 nm and 700-800 nm, respectively, related to the ligand to metal charge transfer events (O(2-) → Co(2+,3+)). Under the electrochemical study in two electrode assembly system (Co3O4/KOH/Co3O4) without adding any large area support or a conductive filler, the hexagonal platelet Co3O4 particles exhibited comparatively better characteristics with high specific capacitance (476 F g(-1)), energy density 42.3 Wh kg(-1) and power density 1.56 kW kg(-1) at current density of 0.5 Ag(-1), that suited for potential applications in supercapacitors. The observed better electrochemical properties of the nanoporous Co3O4 particles is attributed to the layered platelet structural arrangement of the hexagonal platelet and the presence of exceptionally high numbers of regularly ordered pores.

Pyrrolic-N-doped graphene oxide/Fe2O3 mesocrystal nanocomposite: Efficient charge transfer and enhanced photo-Fenton catalytic activity

NASA Astrophysics Data System (ADS)

Liu, Bing; Tian, Lihong; Wang, Ran; Yang, Jinfeng; Guan, Rong; Chen, Xiaobo

2017-11-01

Though α-Fe2O3 has attracted much attention in photocatalytic or Fenton-catalytic degradation of organic contaminants, its performance is still unsatisfactory due to fast recombination of electrons and holes in photocatalytic process and the difficult conversion of Fe(II) and Fe(III) in Fenton reaction. Herein, a pyrrolic N-doped graphene oxide/Fe2O3 mesocrystal (NG-Fe2O3) nanocomposite with good distribution is synthesized by a simple solvothermal method and adjusting the oxygen-containing groups on graphene oxide. The morphology of NG-Fe2O3 contributes to a relatively large BET surface area and an intimate contact between NG and Fe2O3. These two important factors along with the excellent electro-conductivity of pyrrolic-N doped GO result in the efficient separation of electron-hole pairs and fast conversion of Fe(II)and Fe(III) in photo-Fenton synergistic reaction. Thus, a remarkably improved photo-Fenton catalytic activity of NG-Fe2O3 is obtained. The degrading rate on methyl blue increases by 1.5 times and the conversion rate of glyphosate increases by 2.3 times under visible light irradiation, compared to pristine α-Fe2O3 mesocrystals.

Novel approach for removing brominated flame retardant from aquatic environments using Cu/Fe-based metal-organic frameworks: A case of hexabromocyclododecane (HBCD).

PubMed

Li, Xiang; Liu, Hongli; Jia, Xiaoshan; Li, Guiying; An, Taicheng; Gao, Yanpeng

2018-04-15

Cu and Fe based metal-organic frameworks (Cu-BTC and Fe-BTC) were synthesized via a simple solvothermal method and innovatively utilized to remove a typical nonionic brominated flame retardant, hexabromocyclododecane (HBCD), from aquatic environment. Results show that over 80% of HBCD was removed by Cu-BTC within 5h, which is 1.3 times higher than removal by Fe-BTC. Thermodynamic analysis confirms spontaneous adsorption of HBCD onto the metal-organic frameworks (MOFs). Furthermore, the Gibbs free energy of Cu-BTC (-9.11kJ/mol) is more negative than that of Fe-BTC (-5.04kJ/mol). Both adsorption isotherms of HBCD onto Cu-BTC and Fe-BTC followed the Langmuir model, indicating a typical monomolecular-layer adsorption mechanism. In addition, the water stability test of these MOFs shows that the collapse of the Cu-BTC crystal structure is significantly hindered in the aquatic environment due to adsorption of the hydrophobic HBCD. The proposed adsorption mechanism includes van der Waals and hydrophobic interactions. These findings demonstrate that Cu/Fe-BTC are promising adsorbents for the removal of hydrophobic organic pollutants from aquatic environments, and may further improve the understanding of MOF materials for environmental applications. Copyright © 2017 Elsevier B.V. All rights reserved.

Synthesis and photocatalytic performance of reduced graphene oxide-TiO2 nanocomposites for orange II degradation under UV light irradiation.

PubMed

Li, Tengfei; Wang, Tiecheng; Qu, Guangzhou; Liang, Dongli; Hu, Shibin

2017-05-01

To enhance the photocatalytic activity of TiO 2 , reduced graphene oxide-TiO 2 (RGO-TiO 2 ) composites with sandwich-like structure were synthesized using a simple solvothermal method. The morphology, crystalline information, and structural property of the photocatalyst were characterized by field emission scanning electron microscopy, transmission electron microscopy, X-ray diffraction, and Fourier transmission infrared spectroscopy. The photocatalytic performances of the RGO-TiO 2 composites were evaluated by the degradation of orange II (AO7) in water under UV light irradiation. The results showed that the RGO-TiO 2 composites exhibited much higher photocatalytic activity than TiO 2 and that the removal efficiency of AO7 could reach above 95% only after 20 min of UV light irradiation under the optimum condition. The improved photocatalytic activity might be attributed to the improved charge transfer and significant separation of the photoinduced electrons and holes in the presence of a two-dimensional graphene network. The results of recycling experiments show that RGO-TiO 2 composites have a high photostability, which is expected in the practical application. Radical trapping experiments indicated that ·OH plays a crucial role in the process of AO7 degradation.

Hollow mesoporous TiO2 microspheres for enhanced photocatalytic degradation of acetaminophen in water.

PubMed

Lin, Chin Jung; Yang, Wen-Ta; Chou, Chen-Yi; Liou, Sofia Ya Hsuan

2016-06-01

Hollow core-shell mesoporous TiO2 microspheres were synthesized by a template-free solvothermal route for efficient photocatalytic degradation of acetaminophen. X-ray diffraction, scanning electron microscopy, transmission electron microscopy, and Barrett-Joyner-Halenda data revealed a micrometer-sized mesoporous anatase TiO2 hollow sphere with large surface area and efficient light harvesting. For the photocatalytic degradation of acetaminophen in 60 min, the conversion fraction of the drug increased from 88% over commercial Degussa P25 TiO2 to 94% over hollow spheres with about 25% increase in the initial reaction rate. Even after 10 repeated runs, the recycled hollow spheres showed good photodegradation activity. The intermediates generated in the photocatalytic reactions were eventually converted into molecules that are easier to handle. The simple fabrication route would facilitate the development of photocatalysts for the decomposition of environmental contaminants. Copyright © 2016 Elsevier Ltd. All rights reserved.

Synthesis and Characteristics of Large-Area and High-Filling CdS Nanowire Arrays in AAO Template.

PubMed

Lv, Xiao-Yi; Hou, Jun-Wei; Gao, Zhi-Xian; Liu, Hong-Fei

2018-05-01

CdS nanowires arrays were successfully synthesized by a simple solvothermal process using AAO as templates. The phase structures, morphologies, and optical properties of the products were investigated by X-ray diffraction, scanning electron microscopy, high-resolution transmission electron microscopy, Raman spectroscopy, and photoluminescence spectroscopy. It was found that the nanowires were composed of hexagonal structure CdS nanoparticles and the average diameters is about 60-70 nm. A strong green emission with a maximum around 505 nm was observed from the synthesized CdS nanowires at room temperature, which was attributed to near-band-edge emission. A 3D self-seed nucleation coalescent process was proposed for the formation of CdS nanowires structures. The present synthetic route is expected to be applied to the synthesis of other II-VI groups or other group's 1D semiconducting materials.

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.

A novel metal-organic framework composite MIL-101(Cr)@GO as an efficient sorbent in dispersive micro-solid phase extraction coupling with UHPLC-MS/MS for the determination of sulfonamides in milk samples.

PubMed

Jia, Xiuna; Zhao, Pan; Ye, Xiu; Zhang, Lianjun; Wang, Ting; Chen, Qinyu; Hou, Xiaohong

2017-07-01

As a novel material, metal-organic framework/graphite oxide (MIL-101(Cr)@GO) has great potential for the pretreatment of trace analytes. In the present study, MIL-101(Cr)@GO was synthesized using a solvothermal synthesis method at the nanoscale and was applied as sorbent in the dispersive micro-solid phase extraction (DMSPE) for the enrichment of the trace sulfonamides (SAs) from milk samples for the first time. Several experimental parameters including kinds of sorbents, the effect of pH, the amount of MIL-101(Cr)@GO, ionic strength, adsorption time, desorption solvent and desorption time were investigated. Under the optimal conditions, the linear ranges were from 0.1 to 10μg/L, 0.2-20μg/L or 0.5-50μg/L for the analytes with regression coefficients (r) from 0.9942 to 0.9999. The limits of detection were between 0.012 and 0.145μg/L. The recoveries ranged from 79.83% to 103.8% with relative standard deviations (RSDs)<10% (n=3). MIL-101(Cr)@GO exhibited remarkable advantages compared to MIL-101(Cr), MIL-100(Fe), activated carbon and other sorbent materials used in pretreatment methods. A simple, rapid, sensitive, inexpensive and less solvent consuming method of DMSPE-ultra-high performance liquid chromatography-tandem mass spectrometry (DMSPE-UHPLC-MS/MS) was successfully applied to the pre-concentration and determination of twelve SAs in milk samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Preparation of C₁₈-functionalized magnetic polydopamine microspheres for the enrichment and analysis of alkylphenols in water samples.

PubMed

Wang, Xianying; Deng, Chunhui

2016-02-01

In this work, C18-functionalized magnetic polydopamine microspheres (Fe3O4@PDA@C18) were successfully synthesized and applied to the analysis of alkylphenols in water samples. The magnetic Fe3O4 particles coated with hydrophilic surface were synthesized via a solvothermal reaction and the self-polymerization of dopamine. And then the C18 groups were fabricated by a silylanization method. Benefit from the merits of Fe3O4 particles, polydopamine coating and C18 groups, the Fe3O4@PDA@C18 material possessed several properties of super magnetic responsiviness, good water dispersibility, π-electron system and hydrophobic C18 groups. Thus, the materials had great potential to be developed as the adsorbent for the magnetic solid-phase extraction (MSPE) technique. Here, we selected three kinds of alkylphenols (4-tert-octylphenol, 4-n-nonylphenol, 4-n-octylphenol) to be the target analyst for evaluating the performance of the prepared material. In this study, various extraction parameters were investigated and optimized, such as pH values of water sample solution, amount of adsorbents, adsorption and desorption time, the species of desorption solution. Meanwhile, the method validations were studied, including linearity, limit of detection and method precision. From the results, Fe3O4@PDA@C18 composites were successfully applied as the adsorbents for the extraction of alkylphenols in water samples. The proposed material provided an approach for a simple, rapid magnetic solid-phase extraction for hydrophobic compounds in environmental samples. Copyright © 2015 Elsevier B.V. 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

Centrosymmetric [N(CH3)4]2TiF6 vs. noncentrosymmetric polar [C(NH2)3]2TiF6: A hydrogen-bonding effect on the out-of-center distortion of TiF6 octahedra

NASA Astrophysics Data System (ADS)

Kim, Eun-ah; Lee, Dong Woo; Ok, Kang Min

2012-11-01

The syntheses, structures, and characterization of organically templated zero-dimensional titanium fluoride materials, A2TiF6 (A[N(CH3)4] or [C(NH2)3]), are reported. Phase pure samples of A2TiF6 were synthesized by either solvothermal reaction method or a simple mixing method. While [N(CH3)4]2TiF6 crystallizes in a centrosymmetric space group, R-3, [C(NH2)3]2TiF6 crystallizes in a noncentrosymmetric polar space group, Cm. The asymmetric out-of-center distortion of TiF6 octahedra in polar [C(NH2)3]2TiF6 are attributable to the hydrogen-bonding interactions between the fluorine atoms in TiF6 octahedra and the nitrogen atoms in the [C(NH2)3]+ cation. Powder second-harmonic generation (SHG) measurements on the [C(NH2)3]2TiF6, using 1064 nm radiation, indicate the material has SHG efficiency of 25× that of α-SiO2, which indicates an average nonlinear optical susceptibility, exp of 2.8 pm/V. Additional SHG measurements reveal that the material is not phase-matchable (Type 1). The magnitudes of out-of-center distortions and dipole moment calculations for TiF6 octahedra will be also reported.

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.

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.

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

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.

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.

Graphene Oxide Directed One-Step Synthesis of Flowerlike Graphene@HKUST-1 for Enzyme-Free Detection of Hydrogen Peroxide in Biological Samples.

PubMed

Wang, Qingxiang; Yang, Yizhen; Gao, Feng; Ni, Jiancong; Zhang, Yanhui; Lin, Zhenyu

2016-11-30

A novel metal-organic framework (MOF)-based electroactive nanocomposite containing graphene fragments and HKUST-1 was synthesized via a facile one-step solvothermal method using graphene oxide (GO), benzene-1,3,5-tricarboxylic acid (BTC), and copper nitrate (Cu(NO 3 ) 2 ) as the raw materials. The morphology and structure characterization revealed that the GO could induce the transformation of HKUST-1 from octahedral structure to the hierarchical flower shape as an effective structure-directing agent. Also, it is interesting to find out that the GO was torn into small fragments to participate in the formation of HKUST-1 and then transformed into the reduction form during the solvothermal reaction process, which dramatically increased the surface area, electronic conductivity, and redox-activity of the material. Electrochemical assays showed that the synergy of graphene and HKUST-1 in the nanocomposite leaded to high electrocatalysis, fast response, and excellent selectivity toward the reduction of hydrogen peroxide (H 2 O 2 ). Based on these remarkable advantages, satisfactory results were obtained when the nanocomposite was used as a sensing material for electrochemical determination of H 2 O 2 in the complex biological samples such as human serum and living Raw 264.7 cell fluids.

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.

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

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.

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.

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

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.

A facile approach to fabricate flexible all-solid-state supercapacitors based on MnFe2O4/graphene hybrids

NASA Astrophysics Data System (ADS)

Cai, Weihua; Lai, Ting; Dai, Wanlin; Ye, Jianshan

2014-06-01

A critical challenge for the construction of flexible electrochemical capacitors is the preparation of flexible electrodes with large specific capacitance and robust mechanical strength. Here, we demonstrate a facile approach to make high performance and flexible electrodes by dropping MnFe2O4/graphene hybrid inks onto flexible graphite sheets (as current collectors and substrates) and drying under an infrared lamp. MnFe2O4/graphene hybrid inks are synthesized by immobilizing the MnFe2O4 microspheres on the graphene nanosheets via a simple solvothermal route. Electrochemical studies show that MnFe2O4/graphene exhibits a high capacitance of 300 F g-1 at a current density of 0.3 A g-1. In addition, the excellent electrochemical performance of a supercapacitor consisting of a sandwich structure of two pieces of MnFe2O4/graphene hybrids modified electrodes separated by polyvinyl alcohol (PVA)-H2SO4 gel electrolyte is further explored. Our studies reveal that the flexible supercapacitor device with 227 μm thickness can achieve a maximum specific capacitance of 120 F g-1 at a current density of 0.1 A g-1 and excellent cycle performance retaining 105% capacitance after 5000 cycles. This research may offer a method for the fabrication of lightweight, stable, flexible and high performance energy storage devices.

Photocatalytic degradation of pentachlorophenol in aqueous solution by visible light sensitive N-F-codoped TiO{sub 2} photocatalyst

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

Govindan, Kadarkarai, E-mail: govindanmu@gmail.com; Water Chemistry Lab, Water Institute, Karunya University, Coimbatore 641 114; Murugesan, Sepperumal

Graphical abstract: Schematic representation for the visible light photocatalytic process of N and F codoped TiO{sub 2}. Highlights: ► Visible light sensitive N-F-codoped TiO{sub 2}. ► Photocatalytic degradation of pentachlorophenol. ► Effect of oxidants on photocatalytic degradation of pentachlorophenol. ► PMS is a more efficient oxidant for the photodegradation of PCP. - Abstract: In this present study, N-F-codoped titanium dioxide nanocatalyst (NFTO) has been synthesized by simple sol–gel assisted solvothermal method for the effective utilization of visible light in photocatalytic reactions. Structural characterization of the photocatalyst is analyzed by XRD, UV–vis diffuse reflectance spectra (DRS), SEM and TEM. Moreover themore » chemical statuses of NFTO are gathered by X-ray photoelectron spectroscopy (XPS). The results show that a high surface area with photoactive anatase phase crystalline is obtained. In addition, nitrogen and fluorine atoms are doped into TiO{sub 2} crystal lattice to extend the visible light absorption and higher photocatalytic activity. The photocatalytic degradation of pentachlorophenol in aqueous solution is examined under visible light irradiation, the addition of oxidants such as PMS, PDS and H{sub 2}O{sub 2} is analyzed in detail. The rate of photocatalytic degradation of pentachlorophenol is obtained in the following order: PMS > PDS > H{sub 2}O{sub 2}.« less

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.

One-step synthesis of hierarchically porous hybrid TiO2 hollow spheres with high photocatalytic activity

NASA Astrophysics Data System (ADS)

Liu, Ruiping; Ren, Feng; Yang, Jinlin; Su, Weiming; Sun, Zhiming; Zhang, Lei; Wang, Chang-an

2016-03-01

Hierarchically porous hybrid TiO2 hollow spheres were solvothermally synthesized successfully by using tetrabutyl titanate as titanium precursor and hydrated metal sulfates as soft templates. The as-prepared TiO2 spheres with hierarchically pore structures and high specific surface area and pore volume consisted of highly crystallized anatase TiO2 nanocrystals hybridized with a small amount of metal oxide from the hydrated sulfate. The proposed hydrated-sulfate assisted solvothermal (HAS) synthesis strategy was demonstrated to be widely applicable to various systems. Evaluation of the hybrid TiO2 hollow spheres for the photo-decomposition of methyl orange (MO) under visible-light irradiation revealed that they exhibited excellent photocatalytic activity and durability.

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 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

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

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.

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.

Solvothermal synthesis and controlled self-assembly of monodisperse titanium-based perovskite colloidal nanocrystals

NASA Astrophysics Data System (ADS)

Caruntu, Daniela; Rostamzadeh, Taha; Costanzo, Tommaso; Salemizadeh Parizi, Saman; Caruntu, Gabriel

2015-07-01

The rational design of monodisperse ferroelectric nanocrystals with controlled size and shape and their organization into hierarchical structures has been a critical step for understanding the polar ordering in nanoscale ferroelectrics, as well as the design of nanocrystal-based functional materials which harness the properties of individual nanoparticles and the collective interactions between them. We report here on the synthesis and self-assembly of aggregate-free, single-crystalline titanium-based perovskite nanoparticles with controlled morphology and surface composition by using a simple, easily scalable and highly versatile colloidal route. Single-crystalline, non-aggregated BaTiO3 colloidal nanocrystals, used as a model system, have been prepared under solvothermal conditions at temperatures as low as 180 °C. The shape of the nanocrystals was tuned from spheroidal to cubic upon changing the polarity of the solvent, whereas their size was varied from 16 to 30 nm for spheres and 5 to 78 nm for cubes by changing the concentration of the precursors and the reaction time, respectively. The hydrophobic, oleic acid-passivated nanoparticles exhibit very good solubility in non-polar solvents and can be rendered dispersible in polar solvents by a simple process involving the oxidative cleavage of the double bond upon treating the nanopowders with the Lemieux-von Rudloff reagent. Lattice dynamic analysis indicated that regardless of their size, BaTiO3 nanocrystals present local disorder within the perovskite unit cell, associated with the existence of polar ordering. We also demonstrate for the first time that, in addition to being used for fabricating large area, crack-free, highly uniform films, BaTiO3 nanocubes can serve as building blocks for the design of 2D and 3D mesoscale structures, such as superlattices and superparticles. Interestingly, the type of superlattice structure (simple cubic or face centered cubic) appears to be determined by the type of solvent in which the nanocrystals were dispersed. This approach provides an excellent platform for the synthesis of other titanium-based perovskite colloidal nanocrystals with controlled chemical composition, surface structure and morphology and for their assembly into complex architectures, therefore opening the door for the design of novel mesoscale functional materials/nanocomposites with potential applications in energy conversion, data storage and the biomedical field.The rational design of monodisperse ferroelectric nanocrystals with controlled size and shape and their organization into hierarchical structures has been a critical step for understanding the polar ordering in nanoscale ferroelectrics, as well as the design of nanocrystal-based functional materials which harness the properties of individual nanoparticles and the collective interactions between them. We report here on the synthesis and self-assembly of aggregate-free, single-crystalline titanium-based perovskite nanoparticles with controlled morphology and surface composition by using a simple, easily scalable and highly versatile colloidal route. Single-crystalline, non-aggregated BaTiO3 colloidal nanocrystals, used as a model system, have been prepared under solvothermal conditions at temperatures as low as 180 °C. The shape of the nanocrystals was tuned from spheroidal to cubic upon changing the polarity of the solvent, whereas their size was varied from 16 to 30 nm for spheres and 5 to 78 nm for cubes by changing the concentration of the precursors and the reaction time, respectively. The hydrophobic, oleic acid-passivated nanoparticles exhibit very good solubility in non-polar solvents and can be rendered dispersible in polar solvents by a simple process involving the oxidative cleavage of the double bond upon treating the nanopowders with the Lemieux-von Rudloff reagent. Lattice dynamic analysis indicated that regardless of their size, BaTiO3 nanocrystals present local disorder within the perovskite unit cell, associated with the existence of polar ordering. We also demonstrate for the first time that, in addition to being used for fabricating large area, crack-free, highly uniform films, BaTiO3 nanocubes can serve as building blocks for the design of 2D and 3D mesoscale structures, such as superlattices and superparticles. Interestingly, the type of superlattice structure (simple cubic or face centered cubic) appears to be determined by the type of solvent in which the nanocrystals were dispersed. This approach provides an excellent platform for the synthesis of other titanium-based perovskite colloidal nanocrystals with controlled chemical composition, surface structure and morphology and for their assembly into complex architectures, therefore opening the door for the design of novel mesoscale functional materials/nanocomposites with potential applications in energy conversion, data storage and the biomedical field. Electronic supplementary information (ESI) available: FE-SEM image of 12 nm BaTiO3 nanocubes deposited onto a silicon wafer (Fig. SI1), the X-ray diffraction pattern of a superlattice structure formed by monodisperse 10 nm BaTiO3 cuboidal nanocrystals (Fig. SI2) and TEM images of a BaTiO3 superparticle (Fig. SI3). See DOI: 10.1039/c5nr00737b

Biphase-Interface Enhanced Sodium Storage and Accelerated Charge Transfer: Flower-Like Anatase/Bronze TiO2/C as an Advanced Anode Material for Na-Ion Batteries.

PubMed

Chu, Chenxiao; Yang, Jing; Zhang, Qianqian; Wang, Nana; Niu, Feier; Xu, Xuena; Yang, Jian; Fan, Weiliu; Qian, Yitai

2017-12-20

Flower-like assembly of ultrathin nanosheets composed of anatase and bronze TiO 2 embedded in carbon is successfully synthesized by a simple solvothermal reaction, followed with a high-temperature annealing. As an anode material in sodium-ion batteries, this composite exhibits outstanding electrochemical performances. It delivers a reversible capacity of 120 mA h g -1 over 6000 cycles at 10 C. Even at 100 C, there is still a capacity of 104 mA h g -1 . Besides carbon matrix and hierarchical structure, abundant interfaces between anatase and bronze greatly enhance the performance by offering additional sites for reversible Na + storage and improving the charge-transfer kinetics. The interface enhancements are confirmed by discharge/charge profiles, rate performances, electrochemical impedance spectra, and first-principle calculations. These results offer a new pathway to upgrade the performances of anode materials in sodium-ion batteries.

Upconversion fluorescent strip sensor for rapid determination of Vibrio anguillarum

NASA Astrophysics Data System (ADS)

Zhao, Peng; Wu, Yuanyuan; Zhu, Yihua; Yang, Xiaoling; Jiang, Xin; Xiao, Jingfan; Zhang, Yuanxing; Li, Chunzhong

2014-03-01

Here, we report a simple and ultrasensitive upconversion fluorescent strip sensor based on NaYF4:Yb,Er nanoparticles (NPs) and the lateral flow immunochromatographic assay (LFIA). Carboxyl-modified β-NaYF4:Yb,Er NPs were successfully synthesized by a facile one-pot solvothermal approach, upon further coupling with monoclonal antibody, the resultant UCNPs-antibody conjugates probes were used in LFIA and served as signal vehicles for the fluorescent reporters. V. anguillarum was used as a model analyte to demonstrate the use of this strip sensor. The limit of the detection for the fluorescent strip was determined as 102 CFU mL-1, which is 100 times lower than those displayed by enzyme-linked immunosorbent assays, while the time needed for the detection was only 15 min. Furthermore, no cross-reaction with other eight pathogens was found, indicating the good specificity of the strip. This developed LFIA would offer the potential as a useful tool for the quantification of pathogens analysis in the future.

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.

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.

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

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

One-step solvothermal synthesis of carnation flower-like SnS2 as superior electrodes for supercapacitor applications

NASA Astrophysics Data System (ADS)

Mishra, Rajneesh Kumar; Baek, Geun Woo; Kim, Kyuwon; Kwon, Hyuck-In; Jin, Sung Hun

2017-12-01

We report the synthesis of carnation flower-like SnS2 (CF-SnS2) via a one-step solvothermal method for potential application as supercapacitor electrodes in energy storage devices. The structural and morphological properties of CF-SnS2 were characterized by X-ray diffraction, Raman analysis, and field-emission scanning and transmission electron microscopies. X-ray photoelectron spectroscopy and scanning tunneling electron microscopy with color mapping verified the distribution of Sn and S, and depicted the successful formation of SnS2. Electrochemical studies were performed to explore the supercapacitive nature of CF-SnS2. Supercapacitors with CF-SnS2 electrodes delivered excellent cyclic voltammetry performances, superior gravimetric specific capacitances, and high power densities. The evaluated specific capacitance and power density reached ∼524.5 F/g and 12.3 W/kg, respectively, at a current density of 0.08 A/g, and ∼215.9 F/g and 61.4 W/kg, respectively, at a current density of 0.38 A/g. These values are at least two times higher than those previously reported. The long-term cyclic stability was also tested to demonstrate the endurance of the CF-SnS2-based supercapacitor, with a 66% rate retention and galvanostatic charge/discharge reversibility. These electrochemical findings indicate that CF-SnS2 is a promising candidate for electrode materials in supercapacitor applications.

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

One-step solvothermal synthesis of TiO2-reduced graphene oxide nanocomposites with enhanced visible light photoreduction of Cr(VI)

NASA Astrophysics Data System (ADS)

Shaikh, Aasiya; Mishra, Shailendra Prasad; Mohapatra, Priyabrata; Parida, Smrutiranjan

2017-06-01

Hexavalent chromium, Cr(VI), is a mutagenic and carcinogenic heavy metal environmental pollutant. Photoreduction is one of the remediation methods of the hexavalent chromium Cr(VI), which necessitates design of an efficient catalyst for visible light performance. Here, we report a one-step solvothermal synthesis of TiO2-reduced graphene oxide (TiO2- xRGO) composite catalysts using a mild reducing agent, dimethylformamide (DMF). Nanoscale TiO2 particles in the size range of 4-9 nm were formed on the reduced graphene sheets. The formation of the composite catalysts was accompanied by the appearance of a large fluorescence quenching, which indicates an efficient separation of photogenerated electrons and holes. The composites displayed excellent photoreduction of Cr(VI) in the visible light, which was found to be a function of the weight percentage of RGO in the composite. At the optimum composition of TiO2- xRGO, a maximum removal rate of 96% was recorded, which was higher than that of the pristine TiO2, which showed no appreciable catalytic activity under the same condition. The performance degraded with increasing RGO content in the composite, which can be attributed to the higher electron-hole recombination on the RGO surface. The Cr(VI) photoreduction also exhibited a pH dependence. The highest removal rate was observed in the acidic medium.

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.

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.

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.

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.

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.

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

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.

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.

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

A magnetic nanoscale Fe₃O₄/Pβ-CD composite as an efficient peroxidase mimetic for glucose detection.

PubMed

Shi, Yun; Huang, Jun; Wang, Jiangning; Su, Ping; Yang, Yi

2015-10-01

Magnetic polymer particles with different surface functionalizations were prepared by a simple one-pot solvothermal method and characterized as peroxidase mimetics. The fluorescence enhancement obtained by attaching a β-cyclodextrin polymer (Pβ(-CD)) to the surfaces of Fe3O4 magnetic microspheres (Fe3O4 MMs) to generate a Fe3O4/P(β-CD) composite allowed the rapid, sensitive and selective analysis of glucose. The catalytic activity of the Fe3O4/P(β-CD) composite was evaluated with regard to the effects of catalyst particle size and species, pH value, level of catalyst, benzoic acid concentration and reaction time. Detection limits of 0.015 μM for H2O2 and 0.03 μM for glucose were determined when measuring at the 10-min mark. The presence of other saccharides, ion species, amino acids and proteins, had little effect on the results, and this technique was found to allow the analysis of glucose in human serum with high accuracy. The reusability of the Fe3O4/P(β-CD) composite was also investigated after 10 successive runs. A possible mechanism is proposed in which Fe3O4 plays a significant role in inducing fluorescence and P(β-CD) enhances the fluorescence signal, acting as both a stabilizer and a phase transfer agent. Copyright © 2015 Elsevier B.V. All rights reserved.

Alternate current magnetic property characterization of nonstoichiometric zinc ferrite nanocrystals for inductor fabrication via a solution based process

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

Yun, Hongseok; Kim, Jungkwun; Allen, Mark G.

2016-03-21

We investigate the ac magnetic behavior of solution processable, non-stoichiometric zinc ferrite nanocrystals with a series of sizes and zinc concentrations. Nearly monodisperse Zn{sub x}Fe{sub 3−x}O{sub 4} nanocrystals (x = 0–0.25) with an average size ranging from 7.4 nm to 13.8 nm are synthesized by using a solvothermal method. All the nanocrystals are in a superparamagnetic state at 300 K, which is confirmed by Superconductive Quantum Interference Device magnetometry. Due to the doping of non-magnetic Zn{sup 2+} into A site of ferrite, the saturation magnetization of nanocrystals increases as the size and Zn concentration increases. The ac magnetic permeability measurements at radio frequencies reveal thatmore » the real part of the magnetic permeability of similarly sized ferrite nanocrystals can be enhanced by almost twofold as the Zn{sup 2+} doping level increases from 0 to 0.25. The integration of 12.3 nm Zn{sub 0.25}Fe{sub 2.75}O{sub 4} nanocrystals into a toroidal inductor and a solenoid inductor prepared via a simple solution cast process yields a higher quality factors than air core inductors with the same geometries up to 5 MHz and 9 MHz, respectively, which is in the regime of the switching frequencies for the advanced integrated power converters.« less

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

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.

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.

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.

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.

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.

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.

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.

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

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

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.

Improvement of the photovoltaic parameters of perovskite solar cells using a reduced-graphene-oxide-modified titania layer and soluble copper phthalocyanine as a hole transporter.

PubMed

Nouri, Esmaiel; Mohammadi, Mohammad Reza; Xu, Zong-Xiang; Dracopoulos, Vassilios; Lianos, Panagiotis

2018-01-24

Functional perovskite solar cells can be made by using a simple, inexpensive and stable soluble tetra-n-butyl-substituted copper phthalocyanine (CuBuPc) as a hole transporter. In the present study, TiO 2 /reduced graphene oxide (T/RGO) hybrids were synthesized via an in situ solvothermal process and used as electron acceptor/transport mediators in mesoscopic perovskite solar cells based on soluble CuBuPc as a hole transporter and on graphene oxide (GO) as a buffer layer. The impact of the RGO content on the optoelectronic properties of T/RGO hybrids and on the solar cell performance was studied, suggesting improved electron transport characteristics and photovoltaic parameters. An enhanced electron lifetime and recombination resistance led to an increase in the short circuit current density, open circuit voltage and fill factor. The device based on a T/RGO mesoporous layer with an optimal RGO content of 0.2 wt% showed 22% higher photoconversion efficiency and higher stability compared with pristine TiO 2 -based devices.

Insight into the core-shell structures of Cu-In-S microspheres

NASA Astrophysics Data System (ADS)

Wochnik, Angela S.; Frank, Anna; Heinzl, Christoph; Häusler, Jonas; Schneider, Julian; Hoffmann, Ramona; Matich, Sonja; Scheu, Christina

2013-12-01

In this study we report about the inner and outer structure of CuInS2 microspheres which might be used e.g. in pastes for simple, low-cost solar cell preparation, as well as in electrodes for light-driven water splitting. The microspheres are synthesized via a mild, template-free solvothermal synthesis route and characterised by electron and focused ion beam microscopy, X-ray diffraction, inductively coupled plasma atomic emission and energy dispersive X-ray spectroscopy. The investigations of cross sections prepared by focused ion beam showed that the spheres consist of compact cores and flaky surface structures. Depending on the reaction time, the core possesses a stoichiometric or Cu-rich chemical composition surrounded by an In-rich shell. The flaky surface always comprises a stoichiometric composition in tetragonal chalcopyrite crystal structure, whereas the other areas additionally show minor contributions of CuS, and CuInS2 in hexagonal wurtzite structure. The presence of different phases can be beneficial for future applications since they offer different absorption behaviour in the visible range.

Synthesis and characterization of metastable, 20 nm-sized Pna21-LiCoPO4 nanospheres

NASA Astrophysics Data System (ADS)

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

2017-04-01

The majority of research activities on LiCoPO4 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 Pna21 modification. Herein, we present a comprehensive study on the structure-property relationships of 15-20 nm Pna21-LiCoPO4 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 L2,3-edge X-ray absorption spectroscopic data confirm the local tetrahedral symmetry of Co2+. 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-LiCoPO4 at 527 °C. The influence of the atmosphere and the particle size on the thermal stability is also investigated.

Graphene-like boron nitride modified bismuth phosphate materials for boosting photocatalytic degradation of enrofloxacin.

PubMed

Chen, Zhigang; Chen, Xiaoliu; Di, Jun; Liu, Yiling; Yin, Sheng; Xia, Jiexiang; Li, Huaming

2017-04-15

A novel graphene-like BN modified BiPO 4 material was prepared for the first time via a simple solvothermal process with the assistance of reactable ionic liquid 1-decyl-3-methylimidazolium dihydrogen phosphate ([Omim]H 2 PO 4 ). The as-prepared photocatalyst was characterized by XRD, FT-IR, Raman, XPS, TEM, DRS, BET, PL, EIS and ESR to investigate the structure, morphology, optical property, surface area, electrical property and active species. The photocatalytic activities of graphene-like BN/BiPO 4 materials were evaluated by the degradation of antibiotic enrofloxacin (ENR) under UV light irradiation and the 1wt% graphene-like BN/BiPO 4 displayed the best activity among the BN/BiPO 4 composites. The enhanced photocatalytic activity for the removal of enrofloxacin was attributed to higher separation efficiency of photogenerated electron-hole pairs, and the generated more O 2 - and OH radicals when the BN was modified on BiPO 4 . Moreover, a probable degradation mechanism was proposed for the improved photocatalytic activity of BN modified BiPO 4 . Copyright © 2016 Elsevier Inc. All rights reserved.

One-step solvothermal synthesis, a worm-shaped morphology and luminescence properties of green-emitting Y2O2S:Tb3+ nanophosphors

NASA Astrophysics Data System (ADS)

Liu, Fan; Lian, Jingbao; Wu, Nianchu; He, Jiao; Zhang, Xue; Liu, Feng

2018-02-01

The worm-shaped Y2O2S:Tb3+ nanophosphors have been successfully prepared via one-step solvothermal synthesis, using ethanediamine as the main solvent and sublimed sulfur powder as the source of sulfur without adding additional structure-directing reagents. XRD, FT-IR, FESEM, PL and CIE chromaticity diagram were used to characterize the obtained products. XRD results demonstrate that all diffraction peaks of the sample can be well indexed to pure hexagonal phase of Y2O2S with optimal condition, i.e. the molar ration of S/Y3+m = 10, solvothermal temperature T = 220 °C and synthetic time t = 24 h. When t varies from 2 h to 24 h, the morphology of Y2O2S transforms from cauliflower-like structure to worm-shaped nanoparticles with the length of ∼80 nm. The formation mechanism depending on t has also been proposed. Upon 250 nm ultraviolet (UV) light excitation, the worm-shaped Y2O2S:Tb3+ nanophosphors exhibit green emissions, corresponding to the 5D4 → 7FJ (J = 6, 5, 4, 3) transitions of Tb3+ions. The quenching concentration is 7% and its corresponding lifetime is 1216 μs. The CIE chromaticity coordinates show the tuneable emission shifting from yellow green to yellowish green with increasing concentration of Tb3+ions from 1% to 7%. Those results suggest that the worm-shaped Y2O2S:Tb3+ nanophosphors may have potential applications in X-ray intensifying screens, fluorescence and biomedical fields.

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.

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.

Ultrafine cobalt nanoparticles supported on reduced graphene oxide: Efficient catalyst for fast reduction of hexavalent chromium at room temperature

NASA Astrophysics Data System (ADS)

Xu, Tingting; Xue, Jinjuan; Zhang, Xiaolei; He, Guangyu; Chen, Haiqun

2017-04-01

A novel composite ultrafine cobalt nanoparticles-reduced graphene oxide (Co-RGO) was firstly synthesized through a modified one-step solvothermal method with Co(OH)2 as the precursor. The prepared low-cost Co-RGO composite exhibited excellent catalytic activity for the reduction of highly toxic Cr(VI) to nontoxic Cr(III) at room temperature when formic acid (HCOOH) was employed as the reductant, and its catalytic performance was even comparable with that of noble metal-based catalysts in the same reduction reaction. Moreover, Co-RGO composite could be readily recovered under an external magnetic field and efficiently participated in recycled reaction for Cr(VI) reduction.

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.

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.

Preparation of anatase TiO2 thin film by low temperature annealing as an electron transport layer in inverted polymer solar cells

NASA Astrophysics Data System (ADS)

Noh, Hongche; Oh, Seong-Geun; Im, Seung Soon

2015-04-01

To prepare the anatase TiO2 thin films on ITO glass, amorphous TiO2 colloidal solution was synthesized through the simple sol-gel method by using titanium (IV) isopropoxide as a precursor. This amorphous TiO2 colloidal solution was spread on ITO glass by spin-coating, then treated at 450 °C to obtain anatase TiO2 film (for device A). For other TiO2 films, amorphous TiO2 colloidal solution was treated through solvothermal process at 180 °C to obtain anatase TiO2 colloidal solution. This anatase TiO2 colloidal solution was spread on ITO glass by spin coating, and then annealed at 200 °C (for device B) and 130 °C (for device C), respectively. The average particle size of amorphous TiO2 colloidal solution was about 1.0 nm and that of anatase TiO2 colloidal solution was 10 nm. The thickness of TiO2 films was about 15 nm for all cases. When inverted polymer solar cells were fabricated by using these TiO2 films as an electron transport layer, the device C showed the highest PCE (2.6%) due to the lack of defect, uniformness and high light absorbance of TiO2 films. The result of this study can be applied for the preparation of inverted polymer solar cell using TiO2 films as a buffer layer at low temperature on plastic substrate by roll-to roll process.

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

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

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

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

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

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.

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

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.

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.

High-surface-area mesoporous TiO2 microspheres via one-step nanoparticle self-assembly for enhanced lithium-ion storage

NASA Astrophysics Data System (ADS)

Wang, Hsin-Yi; Chen, Jiazang; Hy, Sunny; Yu, Linghui; Xu, Zhichuan; Liu, Bin

2014-11-01

Mesoporous TiO2 microspheres assembled from TiO2 nanoparticles with specific surface areas as high as 150 m2 g-1 were synthesized via a facile one-step solvothermal reaction of titanium isopropoxide and anhydrous acetone. Aldol condensation of acetone gradually releases structural H2O, which hydrolyzes and condenses titanium isopropoxide, forming TiO2 nanocrystals. Simultaneous growth and aggregation of TiO2 nanocrystals leads to the formation of high-surface-area TiO2 microspheres under solvothermal conditions. After a low-temperature post-synthesis calcination, carbonate could be incorporated into TiO2 as a dopant with the carbon source coming from the organic byproducts during the synthesis. Carbonate doping modifies the electronic structure of TiO2 (e.g., Fermi level, Ef), and thus influences its electrochemical properties. Solid electrolyte interface (SEI) formation, which is not common for titania, could be initiated in carbonate-doped TiO2 due to elevated Ef. After removing carbonate dopants by high-temperature calcination, the mesoporous TiO2 microspheres showed much improved performance in lithium insertion and stability at various current rates, attributed to a synergistic effect of high surface area, large pore size and good anatase crystallinity.Mesoporous TiO2 microspheres assembled from TiO2 nanoparticles with specific surface areas as high as 150 m2 g-1 were synthesized via a facile one-step solvothermal reaction of titanium isopropoxide and anhydrous acetone. Aldol condensation of acetone gradually releases structural H2O, which hydrolyzes and condenses titanium isopropoxide, forming TiO2 nanocrystals. Simultaneous growth and aggregation of TiO2 nanocrystals leads to the formation of high-surface-area TiO2 microspheres under solvothermal conditions. After a low-temperature post-synthesis calcination, carbonate could be incorporated into TiO2 as a dopant with the carbon source coming from the organic byproducts during the synthesis. Carbonate doping modifies the electronic structure of TiO2 (e.g., Fermi level, Ef), and thus influences its electrochemical properties. Solid electrolyte interface (SEI) formation, which is not common for titania, could be initiated in carbonate-doped TiO2 due to elevated Ef. After removing carbonate dopants by high-temperature calcination, the mesoporous TiO2 microspheres showed much improved performance in lithium insertion and stability at various current rates, attributed to a synergistic effect of high surface area, large pore size and good anatase crystallinity. Electronic supplementary information (ESI) available. See DOI: 10.1039/c4nr04729j

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.

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.

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.

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.

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.

Enhanced lithium storage performances of hierarchical hollow MoS₂ nanoparticles assembled from nanosheets.

PubMed

Wang, Meng; Li, Guangda; Xu, Huayun; Qian, Yitai; Yang, Jian

2013-02-01

MoS(2), because of its layered structure and high theoretical capacity, has been regarded as a potential candidate for electrode materials in lithium secondary batteries. But it suffers from the poor cycling stability and low rate capability. Here, hierarchical hollow nanoparticles of MoS(2) nanosheets with an increased interlayer distance are synthesized by a simple solvothermal reaction at a low temperature. The formation of hierarchical hollow nanoparticles is based on the intermediate, K(2)NaMoO(3)F(3), as a self-sacrificed template. These hollow nanoparticles exhibit a reversible capacity of 902 mA h g(-1) at 100 mA g(-1) after 80 cycles, much higher than the solid counterpart. At a current density of 1000 mA g(-1), the reversible capacity of the hierarchical hollow nanoparticles could be still maintained at 780 mAh g(-1). The enhanced lithium storage performances of the hierarchical hollow nanoparticles in reversible capacities, cycling stability and rate performances can be attributed to their hierarchical surface, hollow structure feature and increased layer distance of S-Mo-S. Hierarchical hollow nanoparticles as an ensemble of these features, could be applied to other electrode materials for the superior electrochemical performance.

Alkaline earth metal doped tin oxide as a novel oxygen storage material

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

Dong, Qiang, E-mail: dong@tagen.tohoku.ac.jp; Yin, Shu; Yoshida, Mizuki

2015-09-15

Alkaline earth metal doped tin oxide (SnO{sub 2}) hollow nanospheres with a diameter of 50 nm have been synthesized successfully via a facial solvothermal route in a very simple system composed of only ethanol, acetic acid, SnCl{sub 4}·5H{sub 2}O and A(NO{sub 3}){sub 2}·xH{sub 2}O (A = Mg, Ca, Sr, Ba). The synthesized undoped SnO{sub 2} and A-doped SnO{sub 2} hollow nanospheres were characterized by the oxygen storage capacity (OSC), X-ray diffraction, transmission electron microscopy and the Brunauer–Emmet–Teller (BET) technique. The OSC values of all samples were measured using thermogravimetric-differential thermal analysis. The incorporation of alkaline earth metal ion into tinmore » oxide greatly enhanced the thermal stability and OSC. Especially, Ba-doped SnO{sub 2} hollow nanospheres calcined at 1000 °C for 20 h with a BET surface area of 61 m{sup 2} g{sup −1} exhibited the considerably high OSC of 457 μmol-O g{sup −1} and good thermal stability. Alkaline earth metal doped tin oxide has the potential to be a novel oxygen storage material.« less

Cobalt doping of the MOF-5 framework and its effect on gas-adsorption properties.

PubMed

Botas, Juan A; Calleja, Guillermo; Sánchez-Sánchez, Manuel; Orcajo, M Gisela

2010-04-20

Partial isomorphic substitution of Zn in IRMOF metal clusters by cobalt ions is described for the first time. Specifically, different numbers of Co(2+) ions have been incorporated during solvothermal crystallization into the Zn-based MOF-5 (IRMOF-1) framework, which is one of the most studied MOF materials. The amount of Zn that can be substituted seems to be limited, being no more than 25% of total metal content, that is, no more than one Co atom inside every metal cluster formed by four transition-metal ions, on average. Several characterization techniques, including X-ray diffraction, DR UV-visible spectroscopy, N(2) adsorption isotherms, and thermogravimetrical analysis, strongly support the effective incorporation of Co into the material framework. As-synthesized CoMOF-5 has cobalt ions in octahedral coordination, changing to tetrahedral by simple evacuation, presumably by the removal of two diethylformamide molecules per Co ion. Moreover, the H(2), CH(4), and CO(2) uptake of MOF-5 materials systematically increases with the Co content, particularly at high pressure. Such an increase is moderate anyway, considering that Co is incorporated into unexposed metal sites that are less accessible to gas molecules.

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.

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.

One-pot synthesis of hierarchical Cu{sub 2}O/Cu hollow microspheres with enhanced visible-light photocatalytic activity

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

Hong, Tianjie; Tao, Feifei, E-mail: feifeitao@usx.edu.cn; Lin, Jiudong

2015-08-15

The hierarchical Cu{sub 2}O/Cu hollow microspheres have been fabricated by the one-pot solvothermal redox method, which is one-step approach without any surfactant and template. By using the HRTEM, XRD, XPS and UV–vis spectroscopy, the as-prepared product is composed of Cu{sub 2}O and Cu with energy band gap of 1.72 eV. Based on the time-dependent experiments, the content of Cu{sub 2}O and Cu compositions can be effectively controlled by adjusting the reaction time and a possible mechanism is proposed. In addition, using various dye molecules to stimulate pollutants, the hierarchical Cu{sub 2}O/Cu hollow microspheres reacted for 8 h exhibit excellent visible-lightmore » photocatalytic activities, which is much higher than those of the Cu{sub 2}O/Cu catalysts formed at the shorter reaction time, commercial Cu{sub 2}O powder and the mixture of alone Cu{sub 2}O and Cu. This enhanced photocatalytic performance makes these hierarchical Cu{sub 2}O/Cu hollow microspheres a kind of efficient visible-light photocatalyst in removing some organic compounds in wastewater. - Graphical abstract: The hierarchical Cu{sub 2}O/Cu hollow microspheres with adjustable components have been synthesized by one-step solvothermal redox approach. The special structures and composition lead to the excellent visible-light photocatalytic activity. - Highlights: • The hierarchical Cu{sub 2}O/Cu hollow microspheres are fabricated by one-step approach. • The content of Cu{sub 2}O and Cu can be controlled by adjusting the reaction time. • The material exhibits a better visible-light photocatalytic activity and stability. • Degradation kinetics of MO by Cu{sub 2}O/Cu fits the pseudo first-order model.« less

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.

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.

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

Simple route to (NH4)xWO3 nanorods for near infrared absorption

NASA Astrophysics Data System (ADS)

Guo, Chongshen; Yin, Shu; Dong, Qiang; Sato, Tsugio

2012-05-01

Described here is how to synthesize one-dimensional ammonium tungsten bronze ((NH4)xWO3) by a facile solvothermal approach in which ethylene glycol and acetic acid were employed as solvents and ammonium paratungstate was used as a starting material, as well as how to develop the near infrared absorption properties of (NH4)xWO3 nanorods for application as a solar light control filter. The as-obtained product was characterized by field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), thermogravimetry (TG), atomic force microscope (AFM) and UV-Vis-NIR spectra. The SEM and TEM images clearly revealed that the obtained sample possessed rod/fiber-like morphologies with diameters around 120 nm. As determined by UV-Vis-NIR optical measurement, the thin film consisted of (NH4)xWO3 nanoparticles, which can selectively transmit most visible lights, but strongly absorb the near-infrared (NIR) lights and ultraviolet rays. These interesting optical properties make the (NH4)xWO3 nanorods suitable for the solar control windows.Described here is how to synthesize one-dimensional ammonium tungsten bronze ((NH4)xWO3) by a facile solvothermal approach in which ethylene glycol and acetic acid were employed as solvents and ammonium paratungstate was used as a starting material, as well as how to develop the near infrared absorption properties of (NH4)xWO3 nanorods for application as a solar light control filter. The as-obtained product was characterized by field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), thermogravimetry (TG), atomic force microscope (AFM) and UV-Vis-NIR spectra. The SEM and TEM images clearly revealed that the obtained sample possessed rod/fiber-like morphologies with diameters around 120 nm. As determined by UV-Vis-NIR optical measurement, the thin film consisted of (NH4)xWO3 nanoparticles, which can selectively transmit most visible lights, but strongly absorb the near-infrared (NIR) lights and ultraviolet rays. These interesting optical properties make the (NH4)xWO3 nanorods suitable for the solar control windows. Electronic supplementary information (ESI) available. See DOI: 10.1039/c2nr30612c

Amino acid based MOFs: synthesis, structure, single crystal to single crystal transformation, magnetic and related studies in a family of cobalt and nickel aminoisophthales.

PubMed

Sarma, Debajit; Ramanujachary, K V; Lofland, S E; Magdaleno, Travis; Natarajan, Srinivasan

2009-12-21

Four new 5-aminoisophthalates of cobalt and nickel have been prepared employing hydro/solvothermal methods: [Co(2)(C(8)H(5)NO(4))(2)(C(4)H(4)N(2))(H(2)O)(2)].3H(2)O (I), [Ni(2)(C(8)H(5)NO(4))(2)(C(4)H(4)N(2))(H(2)O)(2)].3H(2)O (II), [Co(2)(H(2)O)(mu(3)-OH)(2)(C(8)H(5)NO(4))] (III), and [Ni(2)(H(2)O)(mu(3)-OH)(2)(C(8)H(5)NO(4))] (IV). Compounds I and II are isostructural, having anion-deficient CdCl(2) related layers bridged by a pyrazine ligand, giving rise to a bilayer arrangement. Compounds III and IV have one-dimensional M-O(H)-M chains connected by the 5-aminoisophthalate units forming a three-dimensional structure. The coordinated as well as the lattice water molecules of I and II could be removed and inserted by simple heating-cooling cycles under the atmospheric conditions. The removal of the coordinated water molecule is accompanied by changes in the coordination environment around the M(2+) (M = Co, Ni) and color of the samples (purple to blue, Co; green to dark yellow, Ni). This change has been examined by a variety of techniques that include in situ single crystal to single crystal transformation studies and in situ IR and UV-vis spectroscopic studies. Magnetic studies indicate antiferromagnetic behavior in I and II, a field-induced magnetism in III, and a canted antiferromagnetic behavior in IV.

Synthesis and characterization of mesoporous and hollow-mesoporous MxFe3-xO4 (M=Mg, Mn, Fe, Co, Ni, Cu, Zn) microspheres for microwave-triggered controllable drug delivery

NASA Astrophysics Data System (ADS)

Chen, Ping; Cui, Bin; Bu, Yumei; Yang, Zhenfeng; Wang, Yaoyu

2017-12-01

Spinel ferrites can be used in magnetic targeting and microwave heating and can therefore be used for targeted and controllable drug delivery. We used the cetyltrimethylammonium bromide-assisted solvothermal method to synthesize a series of spinel ferrites (MxFe3-xO4, M=Mg, Mn, Fe, Co, Ni, Cu, Zn) with a mesoporous or hollow-mesoporous structure suitable for direct drug loading and the particle diameters ranging from 200 to 350 nm. We investigated the effects of M2+ cation on the morphology and properties of these products by analyzing their transmission electron microscopy images, mesoporous properties, magnetic properties, and microwave responses. We chose hollow-mesoporous MxFe3-xO4 (M=Fe, Co, Zn) nanoparticles, which had better overall properties, for the drug VP16 (etoposide) loading and microwave-controlled release. The CoxFe3-xO4 and Fe3O4 particles trapped 61.5 and 64.8%, respectively, of the VP16, which were higher than that (60.4%) of ZnxFe3-xO4. Controllable drug release by these simple magnetic nanocarriers can be achieved by microwave irradiation, and VP16-loaded CoxFe3-xO4 released the most VP16 molecules (more than 50% after 1 h and 69.1% after 6 h) under microwave irradiation. Our results confirm the favorable drug loading and microwave-controlled delivery by these ferrites, and lay a theoretical foundation to promote clinical application of the targeted controllable drug delivery system. [Figure not available: see fulltext.

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.

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.

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).

Two new Cu{sup I} compounds with zwitterionic tetrazolate ligand: In situ synthesis, crystal structures, luminescence and photocatalytic properties

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

Zhang, Jian-Yong; Xing, Yuan-Yuan; Wang, Qing-Wei

2015-12-15

Two 2D new Cu(I) coordination polymers, namely [Cu{sub 2}(mpTZ){sub 2}Br{sub 2}]·H{sub 2}O (1), and [Cu{sub 2}(mpTZ){sub 2}N{sub 3}]ClO{sub 4} (2) (mpTZ=N-methyl-4-pyridinium tetrazolate) have been synthesized under solvothermal conditions, in which the mpTZ ligands and Cu{sup I} ions were obtained through in situ [2+3] cycloaddition reaction and reduction reaction of Cu{sup II} salts, respectively. Both compounds have been structural characterized by single crystal X-ray diffraction, FT-IR, PXRD and EA. Compound 1 exhibits a 2D neutral coordination network, in which the Cu{sup I} ions are bridged by η{sub 3}−1, 2, 4-tetrazolate into 2D sheet. In compound 2, the Cu{sup I} ions aremore » linked by azide (in µ{sub 3}−1, 1, 3 bridging mode) and tetrazolate (in η{sub 3}−1, 2, 3 bridging mode) anions into 2D positively charged sheet, extended along the bc plane. Both compounds 1 and 2 exhibit intense bluish green luminescence in the solid state. Photocatalytic performances of the two compounds for the degradation of methylene blue (MB) under visible light were also investigated and the MB degradation in the presence of 1 was nearly complete (99%) after 150 min. - Graphical abstract: Two Cu{sup I}CPs have been solvothermally synthesized through the in situ [2+3] cycloaddition and metal reduction reaction. Both compounds exhibit intense luminescence and high photocatalytic degradation under visible light. - Highlights: • Two new Cu{sup I}-based CPs are solvothermally synthesized through in situ [2+3] cycloaddition reaction and metal reduction reaction. • Both compounds exhibit strong luminescence and photocatalytic degradation of methylene blue (MB) under visible light. • The MB degradation in the presence of 1 is nearly complete (99%) after 150 min.« less

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.

Synthesis of ultrathin mesoporous NiCo2O4 nanosheets on carbon fiber paper as integrated high-performance electrodes for supercapacitors

NASA Astrophysics Data System (ADS)

Deng, Fangze; Yu, Lin; Cheng, Gao; Lin, Ting; Sun, Ming; Ye, Fei; Li, Yongfeng

2014-04-01

Two-dimensional ultrathin mesoporous NiCo2O4 nanosheets on carbon fiber paper (CFP) are synthesized through a facile solvothermal method combined with a post thermal treatment. The well interconnected ultrathin NiCo2O4 nanosheets directly grown on the carbon nanofibers could allow for easy diffusion of the electrolyte, shorten the transport path of ion and electron and accommodate the strain during cycling. As a result, superior pseudocapacitive performance is achieved with large specific capacitance of 999 F g-1 at a high current density of 20 A g-1. The capacitance loss is 15.6% after 3000 cycles at a current density of 10 A g-1, displaying good cycle ability and high rate capability.

In vitro genotoxicity and cytotoxicity of polydopamine-coated magnetic nanostructures.

PubMed

Woźniak, Anna; Walawender, Magdalena; Tempka, Dominika; Coy, Emerson; Załęski, Karol; Grześkowiak, Bartosz F; Mrówczyński, Radosław

2017-10-01

Synthesis of magnetic nanoparticles and magnetic nanoclusters was performed by the co-precipitation method or solvothermal synthesis, respectively, followed by oxidative polymerization of dopamine, resulting in a polydopamine (PDA) shell. The nanomaterials obtained were described using TEM, FTIR and magnetic measurements. For the first time, cyto- and genotoxicity studies of polydopamine-coated nanostructures were performed on cancer and normal cell lines, providing in-depth insight into the toxicity of such materials. The tests conducted, e.g. ROS, apoptosis and DNA double-break of the nanomaterials obtained revealed the low toxicity of these structures. Thus, these results prove the biocompatibility and low genotoxicity of these materials and provide new data on the toxicity of PDA-coated materials, which is of great importance for their biomedical application. Copyright © 2017 Elsevier Ltd. All rights reserved.

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.

Cost-effective fabrication of thermal- and chemical-stable ZIF-9 nanocrystals at ammonia atmosphere

NASA Astrophysics Data System (ADS)

Ebrahimi, Arash; Mansournia, Mohammadreza

2017-12-01

In this study, room temperature synthesis of zeolitic imidazolate framework-9 (ZIF-9) nanocrystals is reported for the first time at ammonia atmosphere in the absence of any organic additive. High thermal stability of the as-fabricated ZIF-9 up to 300 °C is illustrated by TG and XRD data. Also, the chemical resistance of product to harsh and severe solvothermal conditions introduces it to be an objective as potential material in many applications. Besides, the modest microporosity of the as-obtained ZIF-9 materials attracts more attentions for further investigation compared to those fabricated in organic solvents. By and large, the represented low-cost and room temperature synthetic method can be applicable in the large scale preparation of ZIF-9 for potentially practical utilization.

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.

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.

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

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

Nonlinear optical and multi-photon absorption properties in graphene-ZnO nanocomposites

NASA Astrophysics Data System (ADS)

Tong, Qing; Wang, Yu-Hua; Yu, Xiang-Xiang; Wang, Bo; Liang, Zhuang; Tang, Meng; Wu, An-Shun; Zhang, Hai-Jun; Liang, Feng; Xie, Ya-Feng; Wang, Jun

2018-04-01

Graphene-ZnO (GZO) nanocomposites were synthesized by a modified solvothermal method, and characterized by transmission electron microscopy, x-ray diffraction, Raman spectra, and UV-vis absorption spectra. The controllable nonlinear optical (NLO) properties of as-prepared GZO nanocomposites were tested by an open-aperture Z-scan method with 1030 nm fs laser pulses; the tested results showed that there were five-photon absorption (5PA) at 46.8 GW cm-2, 3PA at 28.1 GW cm-2, 2PA at 18.7 GW cm-2, and a vital change from saturable absorption (SA) to reverse SA (RSA) with the increase of incident intensity. This was the first time that 5PA was found in GZO nanocomposites at such a low intensity, 46.8 GW cm-2. The tunable NLO property from SA to RSA and controllable multi-photon absorption provided a facile approach for their applications in optical, optoelectronic devices, and information storage.

Hexagonal-like Nb2O5 Nanoplates-Based Photodetectors and Photocatalyst with High Performances

NASA Astrophysics Data System (ADS)

Liu, Hui; Gao, Nan; Liao, Meiyong; Fang, Xiaosheng

2015-01-01

Ultraviolet (UV) photodetectors are important tools in the fields of optical imaging, environmental monitoring, and air and water sterilization, as well as flame sensing and early rocket plume detection. Herein, hexagonal-like Nb2O5 nanoplates are synthesized using a facile solvothermal method. UV photodetectors based on single Nb2O5 nanoplates are constructed and the optoelectronic properties have been probed. The photodetectors show remarkable sensitivity with a high external quantum efficiency (EQE) of 9617%, and adequate wavelength selectivity with respect to UV-A light. In addition, the photodetectors exhibit robust stability and strong dependence of photocurrent on light intensity. Also, a low-cost drop-casting method is used to fabricate photodetectors based on Nb2O5 nanoplate film, which exhibit singular thermal stability. Moreover, the hexagonal-like Nb2O5 nanoplates show significantly better photocatalytic performances in decomposing Methylene-blue and Rhdamine B dyes than commercial Nb2O5.

Booming Development of Group IV–VI Semiconductors: Fresh Blood of 2D Family

PubMed Central

Zhou, Xing; Zhang, Qi; Gan, Lin; Li, Huiqiao; Xiong, Jie

2016-01-01

As an important component of 2D layered materials (2DLMs), the 2D group IV metal chalcogenides (GIVMCs) have drawn much attention recently due to their earth‐abundant, low‐cost, and environmentally friendly characteristics, thus catering well to the sustainable electronics and optoelectronics applications. In this instructive review, the booming research advancements of 2D GIVMCs in the last few years have been presented. First, the unique crystal and electronic structures are introduced, suggesting novel physical properties. Then the various methods adopted for synthesis of 2D GIVMCs are summarized such as mechanical exfoliation, solvothermal method, and vapor deposition. Furthermore, the review focuses on the applications in field effect transistors and photodetectors based on 2D GIVMCs, and extends to flexible devices. Additionally, the 2D GIVMCs based ternary alloys and heterostructures have also been presented, as well as the applications in electronics and optoelectronics. Finally, the conclusion and outlook have also been presented in the end of the review. PMID:27981008

Synthesis and spectral studies on Cd(II) dithiocarbamate complexes and their use as precursors for CdS nanoparticles

NASA Astrophysics Data System (ADS)

Sathiyaraj, Ethiraj; Padmavathy, Krishnaraj; Kumar, Chandran Udhaya; Krishnan, Kannan Gokula; Ramalingan, Chennan

2017-11-01

Bis(N-cyclopropyl-N-4-chlorobenzyldithiocarbamato-S,S‧)cadmium(II) (1) and (2,2‧-bipyridine) bis(N-cyclopropyl-N-4-chlorobenzyldithiocarbamato-S,S‧)cadmium(II) (2) have been synthesized and characterized by FT-IR, 1HNMR and 13C NMR analyses. For the complex 2, single crystal X-ray diffraction analysis and computational studies (optimized geometry, HOMO-LUMO and MEP) have been executed employing DFT/B3LYP method with LANL 2DZ basic set. The optimized bond lengths and bond angles agree well with the experimental results. The complexes 1 and 2 have been used as single source precursors for the synthesis of ethyleneglycol capped CdS1 and CdS2 nanoparticles, respectively. CdS1 and CdS2 nanoparticles have been synthesized by solvothermal method. PXRD, SEM, Elemental colour mapping, EDAX, TEM and UV-Vis spectroscopy have been used to characterize the as-prepared CdS nanoparticles. The X-ray diffraction pattern confirms both their hexagonal structures.

Band-gap engineering and comparative investigation of Ti2Nb10O29 photocatalysts obtained by Various synthetic routes

NASA Astrophysics Data System (ADS)

Xie, Meiling; Zhu, Hekai; Fang, Minghao; Huang, Zhaohui; Liu, Yan'gai; Wu, Xiaowen

2018-03-01

Ti2Nb10O29 photocatalysts were successfully synthesized by three different methods. Ti2Nb10O29 fabricated by the solvothermal method (ST-TNO) exhibited unique microspheres compared to the larger irregular particles observed for the samples annealed in air (Air-TNO) and Ar (Ar-TNO). X-ray Photoelectron Spectroscopy (XPS) results revealed that a partial reduction process from Ti4+ into Ti3+ occurs in Ar-TNO, because of the introduction of oxygen defects. Ar-TNO exhibited visible-light absorption with a band gap of 2.85 eV, while the absorption edges of Air-TNO and ST-TNO were approximately 400 nm. Under UV light irradiation (λ < 420 nm), Ar-TNO exhibited a photocatalytic activity 2.1 times greater than that of Air-TNO, corresponding to the highest activity. The results indicated that the preparation method is crucial for determining the band gap and photocatalytic activity of semiconductors. Moreover, the novel semiconductor photocatalyst can be further applied for constructing the heterojunction and designing the band structure.

Nickel hydroxides and related materials: a review of their structures, synthesis and properties

PubMed Central

Hall, David S.; Lockwood, David J.; Bock, Christina; MacDougall, Barry R.

2015-01-01

This review article summarizes the last few decades of research on nickel hydroxide, an important material in physics and chemistry, that has many applications in engineering including, significantly, batteries. First, the structures of the two known polymorphs, denoted as α-Ni(OH)2 and β-Ni(OH)2, are described. The various types of disorder, which are frequently present in nickel hydroxide materials, are discussed including hydration, stacking fault disorder, mechanical stresses and the incorporation of ionic impurities. Several related materials are discussed, including intercalated α-derivatives and basic nickel salts. Next, a number of methods to prepare, or synthesize, nickel hydroxides are summarized, including chemical precipitation, electrochemical precipitation, sol–gel synthesis, chemical ageing, hydrothermal and solvothermal synthesis, electrochemical oxidation, microwave-assisted synthesis, and sonochemical methods. Finally, the known physical properties of the nickel hydroxides are reviewed, including their magnetic, vibrational, optical, electrical and mechanical properties. The last section in this paper is intended to serve as a summary of both the potentially useful properties of these materials and the methods for the identification and characterization of ‘unknown’ nickel hydroxide-based samples. PMID:25663812

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.

Na0.3WO3 nanorods: a multifunctional agent for in vivo dual-model imaging and photothermal therapy of cancer cells.

PubMed

Zhang, Yuxin; Li, Bo; Cao, Yunjiu; Qin, Jinbao; Peng, Zhiyou; Xiao, Zhiyin; Huang, Xiaojuan; Zou, Rujia; Hu, Junqing

2015-02-14

The combination of imaging diagnosis and photothermal ablation (PTA) therapy has become a potential treatment for cancer. In particular, tungsten bronzes have a number of unique properties such as broad near-infrared (NIR) absorption and a large X-ray attenuation coefficient. However, these materials have seldom been reported as an X-ray computed tomography (CT) contrast agent and a photothermal agent. Herein, we synthesized PEGylated Na(0.3)WO(3) nanorods (mean size ∼39 nm × 5 nm) by a simple one-pot solvothermal route. As we expected, the prepared PEGylated Na(0.3)WO(3) nanorods exhibit intense NIR absorption, derived from the outer d-electron of W(5+). These PEGylated Na(0.3)WO(3) nanorods also show an excellent CT imaging effect and a high HU value of 29.95 HU g L(-1) (much higher than the figure of iopamidol (19.35 HU g L(-1))), due to the intrinsic property of tungsten of large atomic number and X-ray attenuation coefficient. Furthermore, the temperature elevation and the in vivo photothermal experiment reveal that as-synthesized Na(0.3)WO(3) nanorods could be an effective photothermal agent, as they have low toxicity, high effectiveness and good photostability.

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

Singh, Paviter; Kaur, Manpreet; Singh, Bikramjeet

Boron-carbon core shell structures have been synthesized by solvo-thermal synthesis route. The synthesized material is highly pure. X-ray diffraction analysis confirms the reduction of reactants in to boron and carbon. Scanning Electron Microscopy (SEM) analysis showed that the shell is uniform with average thickness of 340 nm. Photo luminescence studies showed that the material is blue light emitting with CIE color coordinates: x=0.16085, y=0.07554.

Solvothermal synthesis of a new 3-D mixed-metal sulfide framework, (H1.33tren)[In2.67Sb1.33S8]·tren

NASA Astrophysics Data System (ADS)

Lampkin, John D.; Powell, Anthony V.; Chippindale, Ann M.

2016-11-01

A new indium(III) antimony(V) sulfide, (H1.33tren)[In2.67Sb1.33S8]·tren, has been prepared solvothermally at 433 K. The compound crystallises in the tetragonal space group I-42d (lattice parameters, a=12.6248(5) and c=19.4387(18) Å at 150 K) and contains adamantane-like T2 supertetrahedral units comprised of corner-sharing InS45- and SbS43- tetrahedra. The adamantane-like units are then linked through sulfur vertices to generate an open, 3-D framework structure containing large pores in which neutral, protonated tren (tris(2-aminoethylene)amine) molecules reside. The presence of the organic components was confirmed by solid-state 13C NMR (10 kHz), combustion and thermogravimetric analysis. The band gap, obtained from UV-vis diffuse reflectance measurements, is 2.7(2) eV. Stirring with either water or alkali-metal salt solution leads to removal of the neutral tren molecules and an 9% reduction in unit-cell volume on formation of (H1.33tren)[In2.67Sb1.33S8]·(H2O)4.

Solvothermal synthesis of TiO2 nanocrystals with {001} facets using titanic acid nanobelts for superior photocatalytic activity

NASA Astrophysics Data System (ADS)

Cao, Yuhui; Zong, Lanlan; Li, Qiuye; Li, Chen; Li, Junli; Yang, Jianjun

2017-01-01

Anatase TiO2 nanocrystals exposed with {001} facets were fabricated by solvothermal strategy in HF-C4H9OH mixed solution, using titanic acid nanobelts (TAN) as a precursor. The shape of TAN is a long flat plane with a high aspect ratio, and F- is easily adsorbed on the surface of the nanobelts, inducing a higher exposure of {001} facet of TiO2 nanoparticles during the structure reorganization. The exposed percentage of {001} facets could vary from 40 to 77% by adjusting the amount of HF. The as-prepared samples were characterized by transmission electron microscopy, N2 adsorption-desorption isotherms, X-ray diffraction, Raman spectroscopy, and X-ray photoelectron spectroscope. The photocatalytic measurement showed that TiO2 nanocrystals with 77% {001} facets exhibited much superior photocatalytic activity for photodegradation of methyl orange, methylene blue, and rhodamine B. And what's more, the mineralization rate of methyl orange was as high as 96% within 60 min. The photocatalytic enhancement is due to a large amount of the high energetic {001} facets exposing, the special truncated octahedral morphology and a stronger ability for dyes adsorption.

Controllable Synthesis of Highly Luminescent Boron Nitride Quantum Dots.

PubMed

Li, Hongling; Tay, Roland Yingjie; Tsang, Siu Hon; Zhen, Xu; Teo, Edwin Hang Tong

2015-12-22

Boron nitride quantum dots (BNQDs), as a new member of heavy metal-free quantum dots, have aroused great interest in fundamental research and practical application due to their unique physical/chemical properties. However, it is still a challenge to controllably synthesize high-quality BNQDs with high quantum yield (QY), uniform size and strong fluorescent. In this work, BNQDs have been successfully fabricated by the liquid exfoliation and the subsequent solvothermal process with respect to its facileness and easy large scale up. Importantly, BNQDs with high-quality can be controllably obtained by adjusting the synthetic parameters involved in the solvothermal process including filling factor, synthesis temperature, and duration time. Encouragingly, the as-prepared BNQDs possess strong blue luminescence with QY as high as 19.5%, which can be attributed to the synergetic effect of size, surface chemistry and edge defects. In addition, this strategy presented here provides a new reference for the controllable synthesis of other heavy metal-free QDs. Furthermore, the as-prepared BNQDs are non-toxic to cells and exhibit nanosecond-scaled lifetimes, suggesting they have great potential biological and optoelectronic applications. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Spinel Ferrite Core–Shell Nanostructures by a Versatile Solvothermal Seed-Mediated Growth Approach and Study of Their Nanointerfaces

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

Sanna Angotzi, Marco; Musinu, Anna; Mameli, Valentina

An easy, low-cost, repeatable seed-mediated growth approach in solvothermal condition has been proposed to synthesize bimagnetic spinel ferrite core–shell heterostructures in the 10–20 nm particle size range. Cobalt ferrite and manganese ferrite nanoparticles (CoFe 2O 4 and MnFe 2O 4) have been coated with isostructural spinel ferrites like maghemite/magnetite, MnFe 2O 4, and CoFe 2O 4 with similar cell parameters to create different heterostructures. The conventional study of the structure, morphology, and composition has been combined with advanced techniques in order to achieve details on the interface at the nanoscale level. Clear evidence of the heterostructure formation have been obtainedmore » (i) indirectly by comparing the 57Fe Mössbauer spectra of the core–shell samples and an ad hoc mechanical mixture and (ii) directly by mapping the nanoparticles’ chemical composition by electron energy loss spectroscopy (EELS) and energy-dispersive X-ray spectroscopy (EDX) in the scanning transmission electron microscopy mode (STEM). Additionally, chemical-sensitive electron tomography in STEM-EDX mode has been applied in order to obtain detailed 3D images with a sub-nanometer spatial resolution.« less

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.

Spinel Ferrite Core–Shell Nanostructures by a Versatile Solvothermal Seed-Mediated Growth Approach and Study of Their Nanointerfaces

DOE PAGES

Sanna Angotzi, Marco; Musinu, Anna; Mameli, Valentina; ...

2017-07-23

An easy, low-cost, repeatable seed-mediated growth approach in solvothermal condition has been proposed to synthesize bimagnetic spinel ferrite core–shell heterostructures in the 10–20 nm particle size range. Cobalt ferrite and manganese ferrite nanoparticles (CoFe 2O 4 and MnFe 2O 4) have been coated with isostructural spinel ferrites like maghemite/magnetite, MnFe 2O 4, and CoFe 2O 4 with similar cell parameters to create different heterostructures. The conventional study of the structure, morphology, and composition has been combined with advanced techniques in order to achieve details on the interface at the nanoscale level. Clear evidence of the heterostructure formation have been obtainedmore » (i) indirectly by comparing the 57Fe Mössbauer spectra of the core–shell samples and an ad hoc mechanical mixture and (ii) directly by mapping the nanoparticles’ chemical composition by electron energy loss spectroscopy (EELS) and energy-dispersive X-ray spectroscopy (EDX) in the scanning transmission electron microscopy mode (STEM). Additionally, chemical-sensitive electron tomography in STEM-EDX mode has been applied in order to obtain detailed 3D images with a sub-nanometer spatial resolution.« less

Mo0.5W0.5S2 for Q-switched pulse generation in ytterbium-doped fiber laser.

PubMed

Wang, Junli; Chen, Lei; Dou, Chenxi; Yan, Haiting; Meng, Lingjie; Wei, Zhiyi

2018-06-01

In this work, we fabricate the Mo 0.5 W 0.5 S 2 by microwave-assisted solvothermal method, and report the Q-switched Yb-doped fiber lasers (YDFL) using Mo 0.5 W 0.5 S 2 polymer film and tapered fiber as the saturable absorbers (SAs). The modulation depth and saturable intensity of the film SA are 5.63% and 6.82 MW cm -2 . The shortest pulse duration and the maximum single pulse energy are 1.22 μs and 148.8 nJ for the film SA, 1.46 μs and 339 nJ for the fiber-taper SA. To the best of our knowledge, this is the first report on the Q-switched YDFL using Mo 0.5 W 0.5 S 2 SAs.

Ultrathin rhodium nanosheets.

PubMed

Duan, Haohong; Yan, Ning; Yu, Rong; Chang, Chun-Ran; Zhou, Gang; Hu, Han-Shi; Rong, Hongpan; Niu, Zhiqiang; Mao, Junjie; Asakura, Hiroyuki; Tanaka, Tsunehiro; Dyson, Paul Joseph; Li, Jun; Li, Yadong

2014-01-01

Despite significant advances in the fabrication and applications of graphene-like materials, it remains a challenge to prepare single-layered metallic materials, which have great potential applications in physics, chemistry and material science. Here we report the fabrication of poly(vinylpyrrolidone)-supported single-layered rhodium nanosheets using a facile solvothermal method. Atomic force microscope shows that the thickness of a rhodium nanosheet is <4 Å. Electron diffraction and X-ray absorption spectroscopy measurements suggest that the rhodium nanosheets are composed of planar single-atom-layered sheets of rhodium. Density functional theory studies reveal that the single-layered Rh nanosheet involves a δ-bonding framework, which stabilizes the single-layered structure together with the poly(vinylpyrrolidone) ligands. The poly(vinylpyrrolidone)-supported single-layered rhodium nanosheet represents a class of metallic two-dimensional structures that might inspire further fundamental advances in physics, chemistry and material science.

Mo0.5W0.5S2 for Q-switched pulse generation in ytterbium-doped fiber laser

NASA Astrophysics Data System (ADS)

Wang, Junli; Chen, Lei; Dou, Chenxi; Yan, Haiting; Meng, Lingjie; Wei, Zhiyi

2018-06-01

In this work, we fabricate the Mo0.5W0.5S2 by microwave-assisted solvothermal method, and report the Q-switched Yb-doped fiber lasers (YDFL) using Mo0.5W0.5S2 polymer film and tapered fiber as the saturable absorbers (SAs). The modulation depth and saturable intensity of the film SA are 5.63% and 6.82 MW cm‑2. The shortest pulse duration and the maximum single pulse energy are 1.22 μs and 148.8 nJ for the film SA, 1.46 μs and 339 nJ for the fiber-taper SA. To the best of our knowledge, this is the first report on the Q-switched YDFL using Mo0.5W0.5S2 SAs.

Synthesis, characterization and experimental investigation of Cu-BTC as CO2 adsorbent from flue gas.

PubMed

Xie, Jiangkun; Yan, Naiqiang; Qu, Zan; Yang, Shijian

2012-01-01

Porous Cu-BTC material was synthesized by the solvothermal method. Powder X-ray diffraction (PXRD) was used to test the phase purity of the synthesized material and investigate its structural stability under the influence of flue gas components. The thermal stability of the material was determined through thermal gravimetric (TG) analysis. Scanning electron microscopy (SEM) was employed to study the microstructure of the material. Cu-BTC was demonstrated not only to have high CO2 adsorption capacity but also good selectivity of CO2 over N2 by means of packed bed tests. The adsorption capacity of Cu-BTC for CO2 was about 69 mL/g at 22 degrees C. The influence of the main flue gas components on the CO2 capacity of the material were discussed as well.

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.

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

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

Du, Pei-Yao; Liao, Sheng-Yun; Gu, Wen, E-mail: guwen68@nankai.edu.cn

2016-12-15

A 3D lanthanide MOF with formula [Sm{sub 2}(abtc){sub 1.5}(H{sub 2}O){sub 3}(DMA)]·H{sub 2}O·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. - Highlights: • A three-dimensional lanthanide metal-organic framework has been synthesized. • Complex 1 exhibits dual functional detection benzyl alcohol and benzaldehyde among different aromatic molecules. • Complex 1 displays amore » turn-on luminescence sensing with respect to ethanol among different alcohol molecules.« less

A novel mixed-metal borate with large [B12O18(OH)6]6- motif: Synthesis, structure and property

NASA Astrophysics Data System (ADS)

Wei, Li; Pan, Jie; Xue, Zhen-Zhen; Wang, Guo-Ming; Wang, Ying-Xia

2018-01-01

A new mixed-metal polyborate, Na5Li[B12O18(OH)6]·2H2O (1), has been synthesized using solvothermal method and characterized by IR spectroscopy, thermogravimetric analysis, UV-Vis spectroscopy, powder and single-crystal X-ray diffraction, respectively. It crystallizes in the trigonal space group R-3c (No. 167) with unit cell parameters of a = b = 9.6767(6) Å, c = 36.358(5) Å, and Z = 6. Its structure features unprecedented 3D framework constructed from novel honeycomb-shaped inorganic Na-O sheets with unique 12-MR sodium rings and supramolecular polyborate 2D layers of lithium-centered [B12O18(OH)6]6-. UV-Vis spectral characterization indicates that compound 1 is a wide-band-gap semiconductor.

Complexation of Sn{sub 2}Se{sub 6} with lanthanide(III) centers influenced by ethylene polyamines: Solvothermal syntheses, crystal structures, and optical properties of lanthanide selenidostannates

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

Tang, Chunying; Wang, Fang; Chen, Ruihong

Lanthanide selenidostannates (H{sub 3}O){sub n}[Ce(tepa)(μ-1κ{sup 2}:2κ{sup 2}-Sn{sub 2}Se{sub 6})]{sub n} (1), [(Yb(tepa)(μ-OH)){sub 2}(μ-1κ:2κ-Sn{sub 2}Se{sub 6})]{sub n}·nH{sub 2}O (2), [Htrien]{sub 2}[(Ln(trien)(tren)){sub 2}(μ-1κ:2κ-Sn{sub 2}Se{sub 6})][Sn{sub 2}Se{sub 6}] (Ln=Ce(3), Nd(4)) and [(Yb(dien){sub 2}){sub 2}(μ-OH){sub 2}]Sn{sub 2}Se{sub 6} (5) were solvothermally prepared in different ethylene polyamines. The Sn{sub 2}Se{sub 6} unit connects [Ce(tepa)]{sup 3+} and [(Yb(tepa)(μ-OH)){sub 2}]{sup 4+} fragments with tetradentate μ-1κ{sup 2}Se{sup 1},Se{sup 2}:2κ{sup 2}Se{sup 5},Se{sup 6} and bidentate μ-1κSe{sup 1}:2κSe{sup 5} bridging coordination modes in tepa, to form polymers 1 and 2, respectively. It joins two [Ln(trien)(tren)]{sup 3+} fragments as a μ-1κSe{sup 1}:2κSe{sup 5} ligand to form binuclear complexes 3 and 4more » in trien. Unlike the Sn{sub 2}Se{sub 6} units in 1–4 that bind with Ln(III) centers as Se-donor ligands, the Sn{sub 2}Se{sub 6} unit in 5 exists as a discrete ion. The syntheses of 1–5 show that the ethylene polyamines play an important role in the complexation of Sn{sub 2}Se{sub 6} ligand with Ln(III) centers. Compounds 1–5 exhibit optical band gaps in the range of 2.09–2.42 eV, which are influenced by the complexation of Sn{sub 2}Se{sub 6} with Ln(III) centers. - Graphical abstract: New lanthanide complexes concerning the Sn{sub 2}Se{sub 6} ligand were solvothermally prepared, and the effect of ethylene polyamines on the complexation of Sn{sub 2}Se{sub 6} with Ln(III) centers are observed. Highlights: • Lanthanide complexes concerning the selenidostannates have been solvothermally prepared in different ethylene polyamines. • A tetradentate μ-1κ{sup 2}Se{sup 1},Se{sup 2}:2κ{sup 2}Se{sup 5},Se{sup 6} and a bidentate μ-1κSe{sup 1}:2κSe{sup 5} bridging coordination modes for the Sn{sub 2}Se{sub 6} ligand is obtained. • The complexation of the Sn{sub 2}Se{sub 6} ligand with Ln(III) centers are influenced by the ethylene polyamines.« less

The Scaled-Up Synthesis of Nanostructured Ultra-High-Temperature Ceramics and Resistance Sintering of Tantalum Carbide Nanopowders and Composites

NASA Astrophysics Data System (ADS)

Kelly, James P.

Ultra-high temperature ceramics (UHTCs) are a unique class of materials with the potential to withstand harsh environments due to covalent bonding, which gives these materials high melting temperatures, although decomposition temperatures should also be considered. For example, the melting temperature of TaC is near 4000 K, but may vaporize at lower temperatures. The high melting temperatures also make them difficult to process without high pressures and temperatures and to achieve dense ceramics with a nanostructure. Such materials however are appealing for aerospace technologies. The ability to generate high density compacts and maintain a nanostructure could allow for unprecedented control and improvement to the mechanical properties. The goal of this work is to develop processes for the synthesis and consolidation of nanostructured UHTCs. A self-propagating solvothermal synthesis technique for making UHTC nanopowders is presented. The technique is fast, scalable, and requires minimal external energy input. Synthesis of transition metal boride, carbide, and nitride powders is demonstrated. TaC is synthesized using a range of synthesis conditions and characterized to determine the fundamental mechanisms controlling the nanopowder characteristics. Discussion on purification of the powders is also presented. The sintering of TaC nanopowders produced by the solvothermal synthesis method is performed by resistance sintering. The effects of temperature, heating rate, and dwell time on densification and grain growth is presented. Adequate powder processing, carbon content, volatilization, and additives are found to be critical factors affecting the densification, microstructure, and grain growth. The optimal range of carbon addition for minimizing oxygen content is determined. WC and ZrC are evaluated as additives for reducing grain growth of TaC. Secondary phases and/or solid solutions are capable of suppressing grain growth. A unified approach to solid solution chemistries to control the densification, microstructure, and properties of UHTCs in general is presented. This work has important consequences on advancing the properties of UHTCs.

In situ solvothermal growth of metal-organic framework-5 supported on porous copper foam for noninvasive sampling of plant volatile sulfides.

PubMed

Hu, Yuling; Lian, Haixian; Zhou, Langjun; Li, Gongke

2015-01-06

The present study reported on an in situ solvothermal growth method for immobilization of metal-organic framework MOF-5 on porous copper foam support for enrichment of plant volatile sulfides. The porous copper support impregnated with mother liquor of MOF-5 anchors the nucleation and growth of MOF crystallites at its surface, and its architecture of the three-dimensional channel enables accommodation of the MOF-5 crystallite seed. A continuous and well-intergrown MOF-5 layer, evidenced from scanning electron microscope imaging and X-ray diffraction, was successfully immobilized on the porous metal bar with good adhesion and high stability. Results show that the resultant MOF-5 coating was thermally stable up to 420 °C and robust enough for replicate extraction for at least 200 times. The MOF-5 bar was then applied to the headspace sorptive extraction of the volatile organic sulfur compounds in Chinese chive and garlic sprout in combination with thermal desorption-gas chromatography/mass spectrometry. It showed high extraction sensitivity and good selectivity to these plant volatile sulfides owing to the extraordinary porosity of the metal-organic framework as well as the interaction between the S-donor sites and the surface cations at the crystal edges. Several primary sulfur volatiles containing allyl methyl sulfide, dimethyl disulfide, diallyl sulfide, methyl allyl disulfide, and diallyl disulfide were quantified. Their limits of detection were found to be in the range of 0.2-1.7 μg/L. The organic sulfides were detected in the range of 6.0-23.8 μg/g with recoveries of 76.6-100.2% in Chinese chive and 11.4-54.6 μg/g with recoveries of 77.1-99.8% in garlic sprout. The results indicate the immobilization of MOF-5 on copper foam provides an efficient enrichment formats for noninvasive sampling of plant volatiles.

Solvothermal in situ synthesis of Fe{sub 3}O{sub 4}-multi-walled carbon nanotubes with enhanced heterogeneous Fenton-like activity

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

Deng, Jingheng; Wen, Xianghua, E-mail: xhwen@tsinghua.edu.cn; Wang, Qinian

Graphical abstract: After purification, the multi-wall carbon nanotubes (MWCNTs) act as seeds for Fe{sub 3}O{sub 4} nanoparticles heterogeneous nucleation. The Fe{sub 3}O{sub 4} nanoparticles with diameter range of 4.2–10.0 nm synthesized in situ on the MWCNTs under solvothermal condition. The formed nano Fe{sub 3}O{sub 4}-MWCNTs decolorized the Acid Orange II effectively via Fenton-like reaction. Highlights: ► The amount of water tunes size and size distribution of the Fe{sub 3}O{sub 4} nanoparticles (FNs). ► FNs are homogeneously coated on the multi-walled carbon nanotubes (MWCNTs). ► FNs have diameters in the range of 4.2–10.0 nm, average grain size of 7.4 nm. ►more » Fe{sub 3}O{sub 4}-MWCNTs are used as a Fenton-like catalyst to decompose Acid Orange II. ► Fe{sub 3}O{sub 4}-MWCNTs displayed a higher activity than nanometer-size Fe{sub 3}O{sub 4}. -- Abstract: Fe{sub 3}O{sub 4}-multi-walled carbon nanotubes (Fe{sub 3}O{sub 4}-MWCNTs) hybrid materials were synthesized by a solvothermal process using acid treated MWCNTs and iron acetylacetonate in a mixed solution of ethylene glycol and ultrapure water. The materials were characterized using X-ray powder diffraction, scanning and transmission electron microscopy, X-ray photoelectron spectroscopy, and vibrating sample magnetometry. The results showed that a small amount of water in the synthesis system played a role in controlling crystal phase formation, size of Fe{sub 3}O{sub 4}, and the homogeneous distribution of the Fe{sub 3}O{sub 4} nanoparticles deposited on the MWCNTs. The Fe{sub 3}O{sub 4} nanoparticles had diameters in the range of 4.2–10.0 nm. They displayed good superparamagnetism at room temperature and their magnetization was influenced by the reaction conditions. They were used as a Fenton-like catalyst to decompose Acid Orange II and displayed a higher activity than nanometer-size Fe{sub 3}O{sub 4}.« less

A series of Zn/Cd coordination polymers constructed from 1,4-naphthalenedicarboxylate and N-donor ligands: Syntheses, structures and luminescence sensing of Cr{sup 3+} in aqueous solutions

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

Hu, Dong-Cheng; Key Laboratory for Preparation and Application of Ordered Structural Materials of Guangdong Province, Shantou University, Shantou 515063; Fan, Yan

A novel series of Zn/Cd coordination polymers based on H{sub 3}L, namely, [Zn{sub 2}(HL){sub 2}(bipy){sub 2}(H{sub 2}O){sub 6}]{sub n} (1), [Zn(HL)(phen)]{sub n} (2), [Cd{sub 3}L{sub 2}(bbi){sub 3}]{sub n} (3), [Zn{sub 3}L{sub 2}(bbi){sub 3}]{sub n} (4) [(H{sub 3}L =4-[(1-carboxynaphthalen-2-yl)oxy]phthalic acid, bipy =4,4′-bipyridine, phen =1,10-phenanthroline, bbi =1,1′-(1,4-butanediyl)bis(imidazole] have been successfully synthesized by solvothermal reaction. Compound 1 possesses two diverse 1D chains constructed by different bipy coligands, which were further connected to form a 3D supramolecular architecture by hydrogen bonding interactions. Compound 2 possesses a complicated 1D chain based on secondary building unit (SBU) with binuclear Zn cluster. Compounds 3 and 4 exhibitmore » similar 2D→3D framework, which can be rationalized as (3,4,4)-connected 3D net with a Schläfli symbol of (6{sup 3}.8.10{sup 2}){sub 2}(6{sup 3}){sub 2}(6{sup 4}.8.10). In particular, compound 3 exhibited a high sensitivity for Cr{sup 3+} in aqueous solutions, which suggest that compound 3 is a promising luminescent probe for selectively sensing Cr{sup 3+}. - Graphical abstract: A series of novel Zn/Cd coordination polymers have been successfully synthesized by solvothermal reaction. The unique 3D Cd{sup 2+} polymer containing bbi as second ligand demonstrates high sensitivity for detection of toxic Cr{sup 3+} in aqueous solutions. Display Omitted - Highlights: • π-conjugated semirigid tricarboxylate ligands with naphthalene rings(H{sub 3}L) were rationally designed. • Four Zn/Cd coordination polymers based on H{sub 3}L have been successfully synthesized by solvothermal reaction. • Compound 3 is a promising luminescent probe for selectively sensing Cr{sup 3+} with high sensitivity in aqueous solutions.« less

Monodisperse Fe3O4 and γ-Fe2O3 magnetic mesoporous microspheres as anode materials for lithium-ion batteries.

PubMed

Xu, Jing-San; Zhu, Ying-Jie

2012-09-26

Monodisperse Fe(3)O(4) and γ-Fe(2)O(3) magnetic mesoporous microspheres are prepared via a surfactant-free solvothermal combined with precursor thermal transformation method. The as-prepared Fe(3)O(4) and γ-Fe(2)O(3) magnetic mesoporous microspheres have a relatively high specific surface area of 122.3 and 138.6 m(2)/g, respectively. The Fe(3)O(4) and γ-Fe(2)O(3) magnetic mesoporous microspheres are explored as the anode materials for lithium-ion batteries, and they have a high initial discharge capacity of 1307 and 1453 mA h/g, respectively, and a good reversible performance (450 mA h/g for Fe(3)O(4) and 697 mA h/g for γ-Fe(2)O(3) after 110 cycles) at the current density of 0.2C.

P-type sub-tungsten-oxide based urchin-like nanostructure for superior room temperature alcohol sensor

NASA Astrophysics Data System (ADS)

Yao, Yao; Yin, Mingli; Yan, Junqing; Liu, Shengzhong (Frank)

2018-05-01

Nanowires assembled sub-WO3 urchin-like nanostructures have been fabricated via a solvothermal method. The detailed structure and morphology features were characterized by X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM). The results reveal that the individual nanowires are grown along the [0 0 1] direction, and assembled together to form an urchin-like nanostructure. Sensing performance of the sub-WO3 was investigated toward alcohol vapor. At room temperature, the sensor devices based on the WO3-x exhibit significantly higher sensitivity comparing to that of the stoichiometric WO3. The superior sensing performance of this WO3-x sensor is ascribed to the large specific surface area and abundant oxygen vacancies. The obvious enhancement of the gas sensing property can be very useful for the future design and development of room temperature gas sensors for other volatile organic compounds.

Solution-phase synthesis of nanomaterials at low temperature

NASA Astrophysics Data System (ADS)

Zhu, Yongchun; Qian, Yitai

2009-01-01

This paper reviews the solution-phase synthesis of nanoparticles via some routes at low temperatures, such as room temperature route, wave-assisted synthesis (γ-irradiation route and sonochemical route), directly heating at low temperatures, and hydrothermal/solvothermal methods. A number of strategies were developed to control the shape, the size, as well as the dispersion of nanostructures. Using diethylamine or n-butylamine as solvent, semiconductor nanorods were yielded. By the hydrothermal treatment of amorphous colloids, Bi2S3 nanorods and Se nanowires were obtained. CdS nanowires were prepared in the presence of polyacrylamide. ZnS nanowires were obtained using liquid crystal. The polymer poly (vinyl acetate) tubule acted as both nanoreactor and template for the CdSe nanowire growth. Assisted by the surfactant of sodium dodecyl benzenesulfonate (SDBS), nickel nanobelts were synthesized. In addition, Ag nanowires, Te nanotubes and ZnO nanorod arrays could be prepared without adding any additives or templates.

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.

The preparation and degradation performance of CdS photocatalysts to methyl orange solution.

PubMed

Duan, Limei; Zhao, Weiqiang; Xu, Ling; Chen, Xiaohong; Lita, A; Liu, Zongrui

2013-03-01

In this paper, the CdS samples were prepared using thiourea or sodium sulfide as sulfur source by hydrothermal or solvothermal synthesis method, the results of XRD, TEM and SEM showed all the samples belong to hexagonal CdS nano-material with different morphologies. Using the degradation of methyl orange solution as a model reaction, the photocatalytic performance of different CdS samples was measured, and the samples prepared using thiourea as sulfur source exhibited better photocatalytic activity than those using sodium sulfide as sulfur source. The factors on degradation effect were discussed including the pH value of degradation system and the type of light source. The degradation effect of CdS samples increased with the pH value decreased, and the degradation effect was better when the methyl orange solution was irradiated under sunlight than under 250 W mercury lamp.

Hierarchical LiFePO4 with a controllable growth of the (010) facet for lithium-ion batteries.

PubMed

Guo, Binbin; Ruan, Hongcheng; Zheng, Cheng; Fei, Hailong; Wei, Mingdeng

2013-09-27

Hierarchically structured LiFePO4 was successfully synthesized by ionic liquid solvothermal method. These hierarchically structured LiFePO4 samples were constructed from nanostructured platelets with their (010) facets mainly exposed. To the best of our knowledge, facet control of a hierarchical LiFePO4 crystal has not been reported yet. Based on a series of experimental results, a tentative mechanism for the formation of these hierarchical structures was proposed. After these hierarchically structured LiFePO4 samples were coated with a thin carbon layer and used as cathode materials for lithium-ion batteries, they exhibited excellent high-rate discharge capability and cycling stability. For instance, a capacity of 95% can be maintained for the LiFePO4 sample at a rate as high as 20 C, even after 1000 cycles.

Two Co(II) compound constructed by phthalic acid and 3-Cl-phthalic acid: Synthesis, structure, and magnetic properties

NASA Astrophysics Data System (ADS)

Meng, Jun-Rong; Yao, Peng-Fei; Cui, Lian-Sheng; Gan, Yong-Le; Li, Hai-Ye; Liu, Han-Fu; Huang, Fu-Ping

2018-03-01

In this paper, we obtained two novel 2D layered cobalt coordination polymers, namely [(Co(o-BDC)]n (1) and (Co(3-Cl-o-BDC)]n (2), through solvothermal method with acetone as solvent based on phthalic acid (o-H2BDC) and 3-chloro-phthalic acid (3-Cl-o-H2BDC) respectively. Due to the steric hindrance effect of chloric substituent, the two ligands revealed different coordination modes. And cobalt centers of 1 and 2 showed CoO6 octahedral and CoO4 tetrahedral configurations respectively. As a result, 1 and 2 revealed different layered constructions: a 5-connected topology with 48.62 Schläfli symbol for 1, and a 4-connected topology with 44.62 Schläfli symbol for 2, respectively. Besides, Compound 1 and 2 reveal ferromagnetic and antiferromagnetic behaviors, respectively.

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.

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

Amine-functionalized lanthanide-doped zirconia nanoparticles: optical spectroscopy, time-resolved fluorescence resonance energy transfer biodetection, and targeted imaging.

PubMed

Liu, Yongsheng; Zhou, Shanyong; Tu, Datao; Chen, Zhuo; Huang, Mingdong; Zhu, Haomiao; Ma, En; Chen, Xueyuan

2012-09-12

Ultrasmall inorganic oxide nanoparticles doped with trivalent lanthanide ions (Ln(3+)), a new and huge family of luminescent bioprobes, remain nearly untouched. Currently it is a challenge to synthesize biocompatible ultrasmall oxide bioprobes. Herein, we report a new inorganic oxide bioprobe based on sub-5 nm amine-functionalized tetragonal ZrO(2)-Ln(3+) nanoparticles synthesized via a facile solvothermal method and ligand exchange. By utilizing the long-lived luminescence of Ln(3+), we demonstrate its application as a sensitive time-resolved fluorescence resonance energy transfer (FRET) bioprobe to detect avidin with a record-low detection limit of 3.0 nM. The oxide nanoparticles also exhibit specific recognition of cancer cells overexpressed with urokinase plasminogen activator receptor (uPAR, an important marker of tumor biology and metastasis) and thus may have great potentials in targeted bioimaging.

Effect of titanium ester on synthesizing NH2-MIL-125(Ti): Morphology changes from circular plate to octahedron and rhombic dodecahedron

NASA Astrophysics Data System (ADS)

Hu, Shen; Liu, Min; Guo, Xinwen; Kuang, Zhichong; Li, Keyan; Song, Chunshan; Zhang, Guoliang

2018-06-01

Titanium based MOF materials NH2-MIL-125 was synthesized through solvothermal method. By increasing the concentration of the reactants, the morphology of NH2-MIL-125 can be controlled from circular plate to special polyhedron. Meanwhile, the polyhedron can be modulated from octahedron to rhombic dodecahedron through changing the titanium ester of the reactants from tetraethyl titanate to tetrabutyl titanate. This is the first time to obtain NH2-MIL-125 with rhombic dodecahedron morphology. The test of acetic acid as additive on morphology changes shows that the adsorption of additives on special facets shows a more significant impact on the morphology formation. The morphology control of NH2-MIL-125 based on the modulation of the type of titanium ester, reactants concentration, and the added acetic acid concentration were detailed exhibited and explained.

Facile synthesis of uniform hierarchical composites CuO-CeO2 for enhanced dye removal

NASA Astrophysics Data System (ADS)

Xu, Pan; Niu, Helin; Chen, Jingshuai; Song, Jiming; Mao, Changjie; Zhang, Shengyi; Gao, Yuanhao; Chen, Changle

2016-12-01

The hierarchically shaped CuO-CeO2 composites were prepared through a facile solvothermal method without using any template. The as-prepared products were characterized by X-ray powder diffraction, X-ray photoelectron spectroscopy, scanning electron microscopy, transmission electron microscopy, and N2 adsorption-desorption analysis. In the characterization, we found that CuO-CeO2 composites were showed uniform size and morphology which were consisted of the secondary nanoflakes interconnected with each other. Most interestingly, the composites showed efficient performance to remove methyl blue and Congo red dyes from water with maximum adsorption capacities of 2131.24 and 1072.09 mg g-1, respectively. In addition, because of their larger surface area and the unique hierarchical structures, the adsorption performance of the CuO-CeO2 composites is much better than the materials of CuO and CeO2.

Metal-free hybrids of graphitic carbon nitride and nanodiamonds for photoelectrochemical and photocatalytic applications.

PubMed

Zhou, Li; Zhang, Huayang; Guo, Xiaochen; Sun, Hongqi; Liu, Shaomin; Tade, Moses O; Wang, Shaobin

2017-05-01

Graphitic carbon nitride (g-C 3 N 4 ) has been considered as a metal-free, cost-effective, eco-friendly and efficient catalyst for various photoelectrochemical applications. However, compared to conventional metal-based photocatalysts, its photocatalytic activity is still low because of the low mobility of carriers restricted by the polymer nature. Herein, a series of hybrids of g-C 3 N 4 (GCN) and nanodiamonds (NDs) were synthesized using a solvothermal method. The photoelectrochemical performance and photocatalytic efficiency of the GCN/NDs were investigated by means of the generation of photocurrent and photodegradation of methylene blue (MB) solutions under UV-visible light irradiations. In this study, the sample of GCN/ND-33% derived from 0.1g GCN and 0.05g NDs displayed the highest photocatalytic activity and the strongest photocurrent density. The mechanism of enhanced photoelectrochemical and photocatalytic performances was also discussed. Copyright © 2017 Elsevier Inc. All rights reserved.

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

Fu, Fang; Yao, Yuze; Wang, Haiyan

Rational and precise control of the structure and dimension of electrode materials is an efficient way to improve their electrochemical performance. In this work, solvothermal or co-precipitation method is used to synthesize lithium-rich layered oxide materials of Li1.2Mn0.56Co0.12Ni0.12O2 (LLO) with various morphologies and structures, including microspheres, microrods, nanoplates, and irregular nanoparticles. These materials exhibit strong structure- dependent electrochemical properties. The porous hierarchical structured LLO microrods exhibit the best performance, delivering a discharge capacity of 264.6 mAh g(-1) at 0.5 C with over 91% retention after 100 cycles. At a high rate of 5 C, a high discharge capacity of 173.6more » mAh g(-1) can be achieved. This work reveals the relationship between the morphologies and electrochemical properties of LLO cathode materials, and provides a feasible approach to fabricating robust and high-performance electrode materials for lithium-ion batteries.« less

Ag/BiOBr Film in a Rotating-Disk Reactor Containing Long-Afterglow Phosphor for Round-the-Clock Photocatalysis.

PubMed

Yin, Haibo; Chen, Xiaofang; Hou, Rujing; Zhu, Huijuan; Li, Shiqing; Huo, Yuning; Li, Hexing

2015-09-16

Ag/BiOBr film coated on the glass substrate was synthesized by a solvothermal method and a subsequent photoreduction process. Such a Ag/BiOBr film was then adhered to a hollow rotating disk filled with long-afterglow phosphor inside the chamber. The Ag/BiOBr film exhibited high photocatalytic activity for organic pollutant degradation owing to the improved visible-light harvesting and the separation of photoinduced charges. The long-afterglow phosphor could absorb the excessive daylight and emit light around 488 nm, activating the Ag/BiOBr film to realize round-the-clock photocatalysis. Because the Ag nanoparticles could extend the light absorbance of the Ag/BiOBr film to wavelengths of around 500 nm via a surface plasma resonance effect, they played a key role in realizing photocatalysis induced by long-afterglow phosphor.

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.

Effects of Solvent Diols on the Synthesis of ZnFe2O4 Particles and Their Use as Heterogeneous Photo-Fenton Catalysts

PubMed Central

Anchieta, Chayene Gonçalves; Cancelier, Adriano; Mazutti, Marcio Antonio; Jahn, Sérgio Luiz; Kuhn, Raquel Cristine; Gündel, Andre; Chiavone-Filho, Osvaldo; Foletto, Edson Luiz

2014-01-01

A solvothermal method was used to prepare zinc ferrite spinel oxide (ZnFe2O4) using ethylene glycol and 1,4 butanediol as solvent diols, and the influence of diols on the physical properties of ZnFe2O4 particles was investigated. The produced particles were characterized by X-ray powder diffraction (XRD), atomic force microscopy (AFM), Fourier transform infrared spectroscopy (FTIR) and nitrogen adsorption isotherms, and the catalytic activity for the organic pollutant decomposition by heterogeneous photo-Fenton reaction was investigated. Both solvents produced particles with cubic spinel structure. Microporous and mesoporous structures were obtained when ethylene glycol and 1,4 butanediol were used as diols, respectively. A higher pore volume and surface area, as well as a higher catalytic activity for the pollutant degradation were found when 1,4 butanediol was used as solvent. PMID:28788191

Effect of nitrogen-doped carbon dots on the anticorrosion properties of waterborne epoxy coatings

NASA Astrophysics Data System (ADS)

Ren, Siming; Cui, Mingjun; Zhao, Haichao; Wang, Liping

2018-06-01

In this work, nitrogen-doped carbon dots (NCDs) are prepared by solvothermal method and the effect of NCDs on the anticorrosion property of waterborne epoxy (EP) is investigated. Scanning probe microscopy results show that the size of the NCDs is about 4–6 nm. In addition, the anticorrosion property of NCD-incorporated waterborne epoxy coatings is investigated via electrochemical techniques and scanning electron microscopy. Electrochemical results demonstrate that the impedance modulus of 2.0% NCDs/EP is 364 times higher than that of blank EP after 800 h of immersion, indicating significant enhancement in the anticorrosion property of waterborne epoxy coating. The reason is that NCDs with lots of surface functional groups can connect with waterborne epoxy to suppress enlargement of the pores, and reduce the diffusion of oxygen in the coating, thus cutting off the connection between the substrate and oxygen, and delaying corrosion of the substrate.

Impedance spectroscopy study on graphene wrapped nanocrystalline V{sub 2}O{sub 5}

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

Bhaskaram, D. Surya, E-mail: dsurya.b@gmail.com; Govindaraj, G.; Cheruku, Rajesh

2016-05-23

Nanocrystalline V{sub 2}O{sub 5} was synthesized by solvothermal technique, which has potential application as electrode material in supercapacitors. The graphene oxide (GO) was prepared by modified Hummer’s method. The V{sub 2}O{sub 5}/ reduced graphene oxide (RGO) composite was synthesized using surfactant free hydrothermal technique to enhance the functionality in terms of conductivity and surface area of V{sub 2}O{sub 5}. The structural characterization was accomplished through X-ray diffraction and Raman spectroscopy. Morphology was identified by SEM and surface area of VRGO was enhanced by 8 times in comparison with V{sub 2}O{sub 5} nano particles, as confirmed through BET surface area analysis.more » Electrical characterization was done through impedance spectroscopy and the results showed decrease in sample resistance after wrapping V{sub 2}O{sub 5} with RGO.« less

Plasmon-resonance-enhanced visible-light photocatalytic activity of Ag quantum dots/TiO2 microspheres for methyl orange degradation

NASA Astrophysics Data System (ADS)

Yu, Xin; Shang, Liwei; Wang, Dongjun; An, Li; Li, Zhonghua; Liu, Jiawen; Shen, Jun

2018-06-01

We successfully prepared Ag quantum dots modified TiO2 microspheres by facile solvothermal and calcination method. The as-prepared Ag quantum dots/TiO2 microspheres were characterized by scanning electron microscope, transmission electron microscope, X-ray diffraction, X-ray photoelectron spectroscopy and UV-vis diffuse reflectance spectroscopy. The Ag quantum dots/TiO2 photocatalyst showed excellent visible light absorption and efficient photocatalytic activity for methyl orange degradation. And the sample with the molar ratio of 0.05 (Ag to Ti) showed the best visible light photocatalytic activity for methyl orange degradation, mainly because of the surface plasmon resonance (SPR) effects of Ag quantum dots to generate electron and hole pairs for enhanced visible light photocatalysis. Finally, possible visible light photocatalytic mechanism of Ag quantum dots/TiO2 microspheres for methyl orange degradation was proposed in detail.

Porous TiNb24O62 microspheres as high-performance anode materials for lithium-ion batteries of electric vehicles.

PubMed

Yang, Chao; Deng, Shengjue; Lin, Chunfu; Lin, Shiwei; Chen, Yongjun; Li, Jianbao; Wu, Hui

2016-11-10

TiNb 24 O 62 is explored as a new anode material for lithium-ion batteries. Microsized TiNb 24 O 62 particles (M-TiNb 24 O 62 ) are fabricated through a simple solid-state reaction method and porous TiNb 24 O 62 microspheres (P-TiNb 24 O 62 ) are synthesized through a facile solvothermal method for the first time. TiNb 24 O 62 exhibits a Wadsley-Roth shear structure with a structural unit composed of a 3 × 4 octahedron-block and a 0.5 tetrahedron at the block-corner. P-TiNb 24 O 62 with an average sphere size of ∼2 μm is constructed by nanoparticles with an average size of ∼100 nm, forming inter-particle pores with a size of ∼8 nm and inter-sphere pores with a size of ∼55 nm. Such desirable porous microspheres are an ideal architecture for enhancing the electrochemical performances by shortening the transport distance of electrons/Li + -ions and increasing the reaction area. Consequently, P-TiNb 24 O 62 presents outstanding electrochemical performances in terms of specific capacity, rate capability and cyclic stability. The reversible capacities of P-TiNb 24 O 62 are, respectively, as large as 296, 277, 261, 245, 222, 202 and 181 mA h g -1 at 0.1, 0.5, 1, 2, 5, 10 and 20 C, which are obviously larger than those of M-TiNb 24 O 62 (258, 226, 210, 191, 166, 147 and 121 mA h g -1 ). At 10 C, the capacity of P-TiNb 24 O 62 still remains at 183 mA h g -1 over 500 cycles with a decay of only 0.02% per cycle, whereas the corresponding values of M-TiNb 24 O 62 are 119 mA h g -1 and 0.04%. These impressive results indicate that P-TiNb 24 O 62 can be a promising anode material for lithium-ion batteries of electric vehicles.

Solvothermal syntheses, structures, and magnetic properties of three cobalt coordination polymers constructed from naphthalene-1,4-dicarboxylic acid and bis(imidazole) linkers

NASA Astrophysics Data System (ADS)

Dong, Jun-Liang; He, Kun-Huan; Wang, Duo-Zhi; Zhang, Ying-Hui; Wang, Dan-Hong

2018-07-01

Three new Co(II) coordination polymers with formulas of {[Co2(L1)(1,4-NDC)2]·3H2O}n (1), [Co3(L2)2(HCOO)2(1,4-NDC)2]n (2) and [Co2(L2)(μ3-OH)(1,4-NDC)1.5]n (3) (1,4-H2NDC = Naphthalene-1,4-dicarboxylic acid, L1 = di(1H-imidazol-1-yl)methane, L2 = 1,4-di(1H-imidazol-1-yl)benzene) were solvothermal synthesized from 1,4-H2NDC with the aid of three different length-controllable auxiliary ligands and fully characterized. Their structures are determined by single-crystal X-ray diffraction, IR spectra, elemental analysis, powder X-ray diffraction and thermogravimetric analysis. Complexes 1 and 3 display 3D framework structures, corresponding to a 6-connected (412·63) net, a 8-connected (424·5·63) net, respectively. However, it is noteworthy that the complex 1 displays a 2-fold interpenetrating framework structure, complex 3 possesses a self-interpenetrating framework structure. Complex 2 displays 2D 4-connected undulating plane net structure. Moreover, magnetic studies indicate antiferromagnetic interactions between the Co(II) ions in the four complexes.

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

Facile solvothermal synthesis of NaTi2(PO4)3/C porous plates as electrode materials for high-performance sodium ion batteries

NASA Astrophysics Data System (ADS)

Huang, Zhifeng; Liu, Li; Yi, Lingguang; Xiao, Wei; Li, Min; Zhou, Qian; Guo, Guoxiong; Chen, Xiaoying; Shu, Hongbo; Yang, Xiukang; Wang, Xianyou

2016-09-01

NaTi2(PO4)3/C porous plates have been successfully synthesized via solvothermal approach with ammonia as inductive agent combined in-situ carbon coating. It reveals that the inductive agent plays a critical role in morphology-controllable fabrication. The morphology, structure, and electrochemical properties of NaTi2(PO4)3/C composites with multilayered plates, single-layered plate, porous multilayered plates all have been investigated, which are prepared by using urea, triethylamine, and ammonia, respectively. Among these samples, NaTi2(PO4)3/C porous multilayered plates with ammonia addition exhibit the best electrochemical properties due to their unique mesoporous structure. NaTi2(PO4)3/C porous multilayered plates deliver an initial specific capacity of 125 and 110 mAh g-1 at 0.1 and 1 C, respectively. Furthermore, NaTi2(PO4)3/C porous multilayered plates show a good rate capability, whose capacity and corresponding capacity retention reach 85 mAh g-1 and 82.4%, respectively, after 120 cycles under the high rate of 10 C. The excellent results indicate that the NaTi2(PO4)3/C porous multilayered plates are a promising electrode candidate for sodium ion battery.

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.

Optical and structural properties of Mo-doped NiTiO3 materials synthesized via modified Pechini methods

NASA Astrophysics Data System (ADS)

Pham, Thanh-Truc; Kang, Sung Gu; Shin, Eun Woo

2017-07-01

In this study, molybdenum (Mo)-doped nickel titanate (NiTiO3) materials were successfully synthesized as a function of Mo content through a modified Pechini method followed by a solvothermal treatment process. Various characterization methods were employed to investigate the optical and structural properties of the materials. XRD patterns clearly showed that the NiTiO3 structure maintained a single phase with no observed crystalline structure transformations, even after the addition of 10 wt.% Mo. In the Raman spectra and XRD patterns, peak positions shifted with a change in Mo content, confirming that the NiTiO3 lattice was doped with Mo. On the other hand, Mo doping of NiTiO3 materials changed their optical properties. DRS-UV demonstrated that the addition of Mo increased photon absorption within the UV region. Relaxation processes were inhibited by Mo doping, which was evident in the PL spectra. Structural properties of the prepared materials were studied via FE-SEM and HR-TEM. The measured surface area increased proportionally with Mo content due to a reduction in grain size of the materials.

Fully Printed Organic-Inorganic Nanocomposites for Flexible Thermoelectric Applications.

PubMed

Ou, Canlin; Sangle, Abhijeet L; Datta, Anuja; Jing, Qingshen; Busolo, Tommaso; Chalklen, Thomas; Narayan, Vijay; Kar-Narayan, Sohini

2018-06-13

Thermoelectric materials, capable of interconverting heat and electricity, are attractive for applications in thermal energy harvesting as a means to power wireless sensors, wearable devices, and portable electronics. However, traditional inorganic thermoelectric materials pose significant challenges due to high cost, toxicity, scarcity, and brittleness, particularly when it comes to applications requiring flexibility. Here, we investigate organic-inorganic nanocomposites that have been developed from bespoke inks which are printed via an aerosol jet printing method onto flexible substrates. For this purpose, a novel in situ aerosol mixing method has been developed to ensure uniform distribution of Bi 2 Te 3 /Sb 2 Te 3 nanocrystals, fabricated by a scalable solvothermal synthesis method, within a poly(3,4-ethylenedioxythiophene) polystyrene sulfonate matrix. The thermoelectric properties of the resulting printed nanocomposite structures have been evaluated as a function of composition, and the power factor was found to be maximum (∼30 μW/mK 2 ) for a nominal loading fraction of 85 wt % Sb 2 Te 3 nanoflakes. Importantly, the printed nanocomposites were found to be stable and robust upon repeated flexing to curvatures up to 300 m -1 , making these hybrid materials particularly suitable for flexible thermoelectric applications.

Acetone gas sensor based on NiO/ZnO hollow spheres: Fast response and recovery, and low (ppb) detection limit.

PubMed

Liu, Chang; Zhao, Liupeng; Wang, Boqun; Sun, Peng; Wang, Qingji; Gao, Yuan; Liang, Xishuang; Zhang, Tong; Lu, Geyu

2017-06-01

NiO/ZnO composites were synthesized by decorating numerous NiO nanoparticles on the surfaces of well dispersed ZnO hollow spheres using a facile solvothermal method. Various kinds of characterization methods were utilized to investigate the structures and morphologies of the hybrid materials. The results revealed that the NiO nanoparticles with a size of ∼10nm were successfully distributed on the surfaces of ZnO hollow spheres in a discrete manner. As expected, the NiO/ZnO composites demonstrated dramatic improvements in sensing performances compared with pure ZnO hollow spheres. For example, the response of NiO/ZnO composites to 100ppm acetone was ∼29.8, which was nearly 4.6 times higher than that of primary ZnO at 275°C, and the response/recovery time were 1/20s, respectively. Meanwhile, the detection limit could extend down to ppb level. The likely reason for the improved gas sensing properties was also proposed. Copyright © 2017 Elsevier Inc. All rights reserved.

Reduced graphene oxide-TiO2 nanocomposite as a promising visible-light-active photocatalyst for the conversion of carbon dioxide

NASA Astrophysics Data System (ADS)

Tan, Lling-Lling; Ong, Wee-Jun; Chai, Siang-Piao; Mohamed, Abdul Rahman

2013-11-01

Photocatalytic reduction of carbon dioxide (CO2) into hydrocarbon fuels such as methane is an attractive strategy for simultaneously harvesting solar energy and capturing this major greenhouse gas. Incessant research interest has been devoted to preparing graphene-based semiconductor nanocomposites as photocatalysts for a variety of applications. In this work, reduced graphene oxide (rGO)-TiO2 hybrid nanocrystals were fabricated through a novel and simple solvothermal synthetic route. Anatase TiO2 particles with an average diameter of 12 nm were uniformly dispersed on the rGO sheet. Slow hydrolysis reaction was successfully attained through the use of ethylene glycol and acetic acid mixed solvents coupled with an additional cooling step. The prepared rGO-TiO2 nanocomposites exhibited superior photocatalytic activity (0.135 μmol gcat -1 h-1) in the reduction of CO2 over graphite oxide and pure anatase. The intimate contact between TiO2 and rGO was proposed to accelerate the transfer of photogenerated electrons on TiO2 to rGO, leading to an effective charge anti-recombination and thus enhancing the photocatalytic activity. Furthermore, our photocatalysts were found to be active even under the irradiation of low-power energy-saving light bulbs, which renders the entire process economically and practically feasible.

Cobalt- and Cadmium-Based Metal-Organic Frameworks as High-Performance Anodes for Sodium Ion Batteries and Lithium Ion Batteries.

PubMed

Dong, Caifu; Xu, Liqiang

2017-03-01

Two multifunctional metal-organic frameworks (MOFs) with the same coordination mode, [Co(L)(H 2 O)] n ·2nH 2 O [defined as "Co(L) MOF"] and [Cd(L)(H 2 O)] n ·2nH 2 O [defined as "Cd(L) MOF"] (L = 5-aminoisophthalic acid) have been fabricated via a simple and versatile scalable solvothermal approach at 85 °C for 24 h. The relationship between the structure of the electrode materials (especially the coordination water and different metal ions) and the electrochemical properties of MOFs have been investigated for the first time. And then the possible electrochemical mechanisms of the electrodes have been studied and proposed. In addition, MOFs/RGO hybrid materials were prepared via ball milling, which demonstrated better electrochemical performances than those of individual Co(L) MOF and Cd(L) MOF. For example, when Co(L) MOF/RGO was applied as anode for sodium ion batteries (SIBs), it retained 206 mA h g -1 after 330 cycles at 500 mA g -1 and 1185 mA h g -1 could be obtained after 50 cycles at 100 mA g -1 for lithium-ion batteries (LIBs). The high-discharge capacity, excellent cyclic stability combined with the facile synthesis procedure enable Co(L) MOF- and Cd(L) MOF-based materials to be prospective anode materials for SIBs and LIBs.

S-TiO2/S-reduced graphene oxide for enhanced photoelectrochemical water splitting

NASA Astrophysics Data System (ADS)

Elbakkay, Mohamed H.; El Rouby, Waleed M. A.; El-Dek, S. I.; Farghali, Ahmed A.

2018-05-01

Sulfur-doped titanium oxide on the surface of sulfur-doped reduced graphene oxide nanocomposites (S-TiO2/S-RGO) were successfully synthesized for the first time through a simple low cost solvothermal reaction process. The sulfur doping was detected in both TiO2 matrix and carbon framework structure of reduced graphene oxide using X-ray photoelectron spectroscopy (XPS) and Energy-dispersive X-ray spectroscopy (EDX). Cross-sectional AFM analysis of S-RGO nanosheets reveals a thickness of 0.51 nm which is much thinner than those previously reported of heteroatom doped-RGO, confirming the single-layer feature. When the as-prepared (S-TiO2/S-RGO) nanocomposites are utilized as photoanodes for photoelectrochemical (PEC) water splitting, they exhibited an enhanced photoelectrochemical performance and long-term stability. The photocurrent density of S-TiO2/S-RGO(0.2) photoanode revealed 3.36 mA/cm2 at 1 V vs Ag/AgCl which is considered 3 times compared to bare synthesized TiO2. This improvement in the photocurrent density was attributed to the increased separation rate of photogenerated electrons and holes and efficient visible light harvesting as a result of the successful combination of the S-TiO2 and the S-RGO in the same nanocomposite photoanode. This promising result presents a new approach for the synthesis of high-efficient future metal-free photoelectrocatalysts.

Solvothermal synthesis of Fe{sub 7}C{sub 3} and Fe{sub 3}C nanostructures with phase and morphology control

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

Williams, Brent; Clifford, Dustin; Carpenter, Everett E., E-mail: aelgendy@vcu.edu, E-mail: ecarpenter2@vcu.edu

A phase transition, from orthorhombic Fe{sub 3}C to hexagonal Fe{sub 7}C{sub 3}, was observed using a wet synthesis mediated by hexadecyltrimethylammonium chloride (CTAC). In this study, CTAC has been shown to control carbide phase, morphology, and size of the iron carbide nanostructures. Fe{sub 7}C{sub 3} hexagonal prisms were formed with an average diameter of 960 nm, the thickness of 150 nm, and Fe{sub 3}C nanostructures with an approximate size of 50 nm. Magnetic studies show ferromagnetic behavior with M{sub s} of 126 emu/g, and H{sub c} of 170 Oe with respect to Fe{sub 7}C{sub 3} and 95 emu/g and 590 Oe with respect to Fe{sub 3}C. Themore » thermal studies using high temperature x-ray diffraction show stability of Fe{sub 7}C{sub 3} up to 500 °C. Upon slow cooling, the Fe{sub 7}C{sub 3} phase is recovered with an intermediate oxide phase occurring around 300 °C. This study has demonstrated a simple route in synthesizing iron carbides for an in depth magnetic study and crystal phase transition study of Fe{sub 7}C{sub 3} at elevated temperatures.« less

Reduced graphene oxide-TiO2 nanocomposite as a promising visible-light-active photocatalyst for the conversion of carbon dioxide.

PubMed

Tan, Lling-Lling; Ong, Wee-Jun; Chai, Siang-Piao; Mohamed, Abdul Rahman

2013-11-06

Photocatalytic reduction of carbon dioxide (CO2) into hydrocarbon fuels such as methane is an attractive strategy for simultaneously harvesting solar energy and capturing this major greenhouse gas. Incessant research interest has been devoted to preparing graphene-based semiconductor nanocomposites as photocatalysts for a variety of applications. In this work, reduced graphene oxide (rGO)-TiO2 hybrid nanocrystals were fabricated through a novel and simple solvothermal synthetic route. Anatase TiO2 particles with an average diameter of 12 nm were uniformly dispersed on the rGO sheet. Slow hydrolysis reaction was successfully attained through the use of ethylene glycol and acetic acid mixed solvents coupled with an additional cooling step. The prepared rGO-TiO2 nanocomposites exhibited superior photocatalytic activity (0.135 μmol gcat-1 h-1) in the reduction of CO2 over graphite oxide and pure anatase. The intimate contact between TiO2 and rGO was proposed to accelerate the transfer of photogenerated electrons on TiO2 to rGO, leading to an effective charge anti-recombination and thus enhancing the photocatalytic activity. Furthermore, our photocatalysts were found to be active even under the irradiation of low-power energy-saving light bulbs, which renders the entire process economically and practically feasible.

A Gel-Polymer Sn-C/LiMn0.5Fe0.5PO4 Battery Using a Fluorine-Free Salt.

PubMed

Di Lecce, Daniele; Fasciani, Chiara; Scrosati, Bruno; Hassoun, Jusef

2015-09-30

Safety and environmental issues, because of the contemporary use of common liquid electrolytes, fluorinated salts, and LiCoO2-based cathodes in commercial Li-ion batteries, might be efficiently mitigated by employing alternative gel-polymer battery configurations and new electrode materials. Herein we study a lithium-ion polymer cell formed by combining a LiMn0.5Fe0.5PO4 olivine cathode, prepared by simple solvothermal pathway, a nanostructured Sn-C anode, and a LiBOB-containing PVdF-based gel electrolyte. The polymer electrolyte, here analyzed in terms of electrochemical stability by impedance spectroscopy (EIS) and voltammetry, reveals full compatibility for cell application. The LiBOB electrolyte salt and the electrochemically delithiaded Mn0.5Fe0.5PO4 have a higher thermal stability compared to conventional LiPF6 and Li0.5CoO2, as confirmed by thermogravimetric analysis (TGA) and by galvanostatic cycling at high temperature. LiMn0.5Fe0.5PO4 and Sn-C, showing in lithium half-cell a capacity of about 120 and 350 mAh g(-1), respectively, within the gelled electrolyte configuration are combined in a full Li-ion polymer battery delivering a stable capacity of about 110 mAh g(-1), with working voltage ranging from 2.8 to 3.6 V.

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

1,2,3-triazolate-bridged tetradecametallic transition metal clusters [M14(L)6O6(OMe)18X6] (M=FeIII, CrIII and VIII/IV) and related compounds: ground-state spins ranging from S=0 to S=25 and spin-enhanced magnetocaloric effect.

PubMed

Shaw, Rachel; Laye, Rebecca H; Jones, Leigh F; Low, David M; Talbot-Eeckelaers, Caytie; Wei, Qiang; Milios, Constantinos J; Teat, Simon; Helliwell, Madeleine; Raftery, James; Evangelisti, Marco; Affronte, Marco; Collison, David; Brechin, Euan K; McInnes, Eric J L

2007-06-11

We report the synthesis, by solvothermal methods, of the tetradecametallic cluster complexes [M14(L)6O6(OMe)18Cl6] (M=FeIII, CrIII) and [V14(L)6O6(OMe)18Cl6-xOx] (L=anion of 1,2,3-triazole or derivative). Crystal structure data are reported for the {M14} complexes [Fe14(C2H2N3)6O6(OMe)18Cl6], [Cr14(bta)6O6(OMe)18Cl6] (btaH=benzotriazole), [V14O6(Me2bta)6(OMe)18Cl6-xOx] [Me2btaH=5,6-Me2-benzotriazole; eight metal sites are VIII, the remainder are disordered between {VIII-Cl}2+ and {VIV=O}2+] and for the distorted [FeIII14O9(OH)(OMe)8(bta)7(MeOH)5(H2O)Cl8] structure that results from non-solvothermal synthetic methods, highlighting the importance of temperature regime in cluster synthesis. Magnetic studies reveal the {Fe14} complexes to have ground state electronic spins of S

Photocatalytic wastewater purification with simultaneous hydrogen production using MoS2 QD-decorated hierarchical assembly of ZnIn2S4 on reduced graphene oxide photocatalyst.

PubMed

Zhang, Shuqu; Wang, Longlu; Liu, Chengbin; Luo, Jinming; Crittenden, John; Liu, Xia; Cai, Tao; Yuan, Jili; Pei, Yong; Liu, Yutang

2017-09-15

It is attractive to photocatalytically purify wastewater and simultaneously convert solar energy into clean hydrogen energy. However, it is still a challenge owing to the relatively low photocatalytic efficiency of photocatalysts. In this study, we synthesized a molybdenum disulfide (MoS 2 ) quantum dot-decorated 3D nanoarchitecture (MoS 2 QDs) of indium zinc sulfide (ZnIn 2 S 4 ) and reduced grapheme oxide (MoS 2 QDs@ZnIn 2 S 4 @RGO) photocatalyst using a simple solvothermal method. The RGO promotes the electron transfer, and the highly dispersed MoS 2 QDs provides numerous catalytic sites. The photocatalytic purification of rhodamine B (RhB), eosin Y (EY), fulvic acid (FA), methylene blue (MB) and p-nitrophenol (PNP) in simulated wastewaters were further tested. The degradation efficiencies and TOC removal were 91% and 75% for PNP, 92.2% and 72% for FA, 98.5% and 80% for MB, 98.6% and 84% for EY, and 98.8% and 88% for RhB, respectively (C organics  = 20 mg/L, C catalyst  = 1.25 g/L, t = 12 h, I light  = 3.36 × 10 -5  E L -1  s -1 ). Among these tests, the highest hydrogen production was achieved (45 μmol) during RhB degradation. Both experimental and calculational results prove that lower LUMO (lowest unoccupied molecular orbit) level of organic molecules was available for transferring electrons to catalysts, resulting in more efficient hydrogen production. Significantly, the removal efficiencies of natural organic substances in actual river water reached 76.3-98.4%, and COD reduced from 32 to 16 mg/L with 13.8 μmol H 2 production after 12 h. Copyright © 2017 Elsevier Ltd. All rights reserved.

Fullerene-Like Nickel Oxysulfide Hollow Nanospheres as Bifunctional Electrocatalysts for Water Splitting.

PubMed

Liu, Junli; Yang, Yong; Ni, Bing; Li, Haoyi; Wang, Xun

2017-02-01

Fullerene-like nickel oxysulfide hollow nanospheres with ≈50 nm are constructed by in situ growth on the surface of nickel foam by taking advantage of solvothermal reaction. The as-prepared composite exhibits exhilaratingly high HER and OER performance in 1 m KOH, which opens up a very promising aspect for non-noble metal chalcogenides as bifunctional electrocatalysts. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Constructing CrIII-centered heterometallic complexes: [NiCrIII] and [CoCrIII] wheels.

PubMed

Kakaroni, Foteini E; Collet, Alexandra; Sakellari, Eirini; Tzimopoulos, Demetrios I; Siczek, Milosz; Lis, Tadeusz; Murrie, Mark; Milios, Constantinos J

2017-12-19

The solvothermal reaction between Cr(acac) 3 , MCl 2 ·6H 2 O (M = Ni, Co) and 2-hydroxy-4-methyl-6-phenyl-pyridine-3-amidoxime (H 2 L), under basic conditions, led to the synthesis of the heterometallic heptanuclear clusters [MCr(HL zw ) 6 (HL) 6 ]·3Cl (M = Ni, 1; Co, 2), with the nickel analogue displaying an S = 9/2 spin ground-state.

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

Defect-Controlled Preparation of UiO-66 Metal-Organic Framework Thin Films with Molecular Sieving Capability.

PubMed

Zhang, Caiqin; Zhao, Yajing; Li, Yali; Zhang, Xuetong; Chi, Lifeng; Lu, Guang

2016-01-01

Metal-organic framework (MOF) UiO-66 thin films are solvothermally grown on conducting substrates. The as-synthesized MOF thin films are subsequently dried by a supercritical process or treated with polydimethylsiloxane (PDMS). The obtained UiO-66 thin films show excellent molecular sieving capability as confirmed by the electrochemical studies for redox-active species with different sizes. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Solvothermal Vapor Annealing of Lamellar Poly(styrene)-block-poly(d,l-lactide) Block Copolymer Thin Films for Directed Self-Assembly Application.

PubMed

Cummins, Cian; Mokarian-Tabari, Parvaneh; Andreazza, Pascal; Sinturel, Christophe; Morris, Michael A

2016-03-01

Solvothermal vapor annealing (STVA) was employed to induce microphase separation in a lamellar forming block copolymer (BCP) thin film containing a readily degradable block. Directed self-assembly of poly(styrene)-block-poly(d,l-lactide) (PS-b-PLA) BCP films using topographically patterned silicon nitride was demonstrated with alignment over macroscopic areas. Interestingly, we observed lamellar patterns aligned parallel as well as perpendicular (perpendicular microdomains to substrate in both cases) to the topography of the graphoepitaxial guiding patterns. PS-b-PLA BCP microphase separated with a high degree of order in an atmosphere of tetrahydrofuran (THF) at an elevated vapor pressure (at approximately 40-60 °C). Grazing incidence small-angle X-ray scattering (GISAXS) measurements of PS-b-PLA films reveal the through-film uniformity of perpendicular microdomains after STVA. Perpendicular lamellar orientation was observed on both hydrophilic and relatively hydrophobic surfaces with a domain spacing (L0) of ∼32.5 nm. The rapid removal of the PLA microdomains is demonstrated using a mild basic solution for the development of a well-defined PS mask template. GISAXS data reveal the through-film uniformity is retained following wet etching. The experimental results in this article demonstrate highly oriented PS-b-PLA microdomains after a short annealing period and facile PLA removal to form porous on-chip etch masks for nanolithography application.

Development of CdS Nanostructures by Thermal Decomposition of Aminocaproic Acid-Mixed Cd-Thiourea Complex Precursor: Structural, Optical and Photocatalytic Characterization.

PubMed

Patel, Jayesh D; Mighri, Frej; Ajji, Abdellah; Chaudhuri, Tapas K

2015-04-01

The present work deals with two different CdS nanostructures produced via hydrothermal and solvothermal decompositions of aminocaproic acid (ACA)-mixed Cd-thiourea complex precursor at 175 °C. Both nanostructures were extensively characterized for their structural, morphological and optical properties. The powder X-ray diffraction characterization showed that the two CdS nanostructures present a wurtzite morphology. Scanning electron microscopy and energy-dispersive X-ray characterizations revealed that the hydrothermal decomposition produced well-shaped CdS flowers composed of six dendritic petals, and the solvothermal decomposition produced CdS microspheres with close stoichiometric chemical composition. The UV-vis absorption and photoluminescence spectra of CdS dendritic flowers and microsphere nanostructures showed that both nanostructures present a broad absorption between 200 and 700 nm and exhibit strong green emissions at 576 and 520 nm upon excitations at 290 nm and 260 nm, respectively. The transmission electron microscopy (TEM) and Brunauer-Emmett-Teller (BET) characterizations confirmed that CdS microspheres were mesoporous and were composed of small nanocrystals. A possible growth mechanism in the formation of the CdS nanostructures was proposed based on morphology evolution as a function of the reaction time. Furthermore, the as-synthesized CdS nanostructures were found to exhibit highly efficient photocatalytic activities for the degradation of methyl orange (MeO) and rhodamine B (RhB) dyes.

Facile solvothermal synthesis of mesostructured Fe3O4/chitosan nanoparticles as delivery vehicles for pH-responsive drug delivery and magnetic resonance imaging contrast agents.

PubMed

Zhao, Guanghui; Wang, Jianzhi; Peng, Xiaomen; Li, Yanfeng; Yuan, Xuemei; Ma, Yingxia

2014-02-01

We report a facile fabrication of a host-metal-guest coordination-bonding system in a mesostructured Fe3O4/chitosan nanoparticle that can act as a pH-responsive drug-delivery system. The mesostructured Fe3O4/chitosan was synthesized by a solvothermal approach with iron(III) chloride hexahydrate as a precursor, ethylene glycol as a reducing agent, ammonium acetate as a porogen, and chitosan as a surface-modification agent. Subsequently, doxorubicin (DOX), acting as a model drug (guest), was loaded onto the mesostructured Fe3O4/chitosan nanoparticles, with chitosan acting as a host molecule to form the NH2-Zn(II)-DOX coordination architecture. The release of DOX can be achieved through the cleavage of coordination bonds that are sensitive to variations in external pH under weakly acidic conditions. The pH-responsive nature of the nanoparticles was confirmed by in vitro releases and cell assay tests. Furthermore, the relaxation efficiency of the nanoparticles as high-performance magnetic resonance imaging contrast agents was also investigated. Experimental results confirm that the synthesized mesostructured Fe3O4/chitosan is a smart nanovehicle for drug delivery owing to both its pH-responsive nature and relaxation efficiency. Copyright © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Size control mechanism of ZnO nanoparticles obtained in microwave solvothermal synthesis

NASA Astrophysics Data System (ADS)

Wojnarowicz, Jacek; Chudoba, Tadeusz; Koltsov, Iwona; Gierlotka, Stanislaw; Dworakowska, Sylwia; Lojkowski, Witold

2018-02-01

The aim of the paper is to explain the mechanism of zinc oxide (ZnO) nanoparticle (NP) size control, which enables the size control of ZnO NPs obtained in microwave solvothermal synthesis (MSS) within the size range between circa 20 and 120 nm through the control of water content in the solution of zinc acetate in ethylene glycol. Heavy water was used in the tests. The mechanism of ZnO NPs size control was explained, discussed and experimentally verified. The discovery and investigation of this mechanism was possible by tracking the fate of water molecules during the whole synthesis process. All the synthesis products were identified. It was indicated that the MSS of ZnO NPs proceeded through the formation and conversion of intermediates such as Zn5(OH)8(CH3COO)2 · xH2O. Esters and H2O were the by-products of the MSS reaction of ZnO NPs. We justified that the esterification reaction is the decisive stage that is a prerequisite of the formation of ZnO NPs. The following parameters of the obtained ZnO NPs and of the intermediate were determined: pycnometric density, specific surface area, phase purity, average particles size, particles size distribution and chemical composition. The ZnO NPs morphology and structure were determined using scanning electron microscopy.

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.

Hierarchical flower-like nickel(II) oxide microspheres with high adsorption capacity of Congo red in water.

PubMed

Zheng, Yingqiu; Zhu, Bicheng; Chen, Hua; You, Wei; Jiang, Chuanjia; Yu, Jiaguo

2017-10-15

Monodispersed hierarchical flower-like nickel(II) oxide (NiO) microspheres were fabricated by a facile solvothermal reaction with the assistance of ethanolamine and a subsequent calcination process. The as-synthesized samples were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, nitrogen adsorption-desorption isotherms, zeta potential measurement and Fourier transform infrared spectroscopy. Flower-like nickel(II) hydroxide microspheres with uniform diameters of approximate 6.3μm were obtained after the solvothermal reaction. After heat treatment at 350°C, the crystal phase transformed to NiO, but the hierarchical porous structure was maintained. The as-prepared microspheres exhibited outstanding performance for the adsorption of Congo red (CR), an anionic organic dye, from aqueous solution at circumneutral pH. The pseudo-second-order model can make a good description of the adsorption kinetics, while Langmuir model could well express the adsorption isotherms, with calculated maximum CR adsorption capacity of 534.8 and 384.6mgg -1 , respectively, for NiO and Ni(OH) 2 . The adsorption mechanism of CR onto the as-synthesized samples can be mainly attributed to electrostatic interaction between the positively charged sample surface and the anionic CR molecules. The as-prepared NiO microspheres are a promising adsorbent for CR removal in water treatment. Copyright © 2017 Elsevier Inc. All rights reserved.

Sonochemical Assisted Solvothermal Synthesis of Gallium Oxynitride Nanosheets and their Solar-Driven Photoelectrochemical Water-Splitting Applications.

PubMed

Iqbal, Naseer; Khan, Ibrahim; Yamani, Zain H; Qurashi, Ahsanullhaq

2016-08-26

Gallium oxynitride (GaON) nanosheets for photoelectrochemical (PEC) analysis are synthesized via direct solvothermal approach. Their FE-SEM revealed nanosheets morphology of GaON prepared at a reaction time of 24 hours at 180 °C. The elemental composition and mapping of Ga, O and N are carried out through electron dispersive X-ray spectroscopy (EDX). The cubic structure of GaON nanosheets is elucidated by X-ray diffraction (XRD)analysis. The X-ray Photoelectron Spectroscopy (XPS) further confirms Ga, O and N in their respective ratios and states. The optical properties of GaON nanosheets are evaluated via UV-Visible, Photoluminescence (PL) and Raman spectroscopy's. The band gap energy of ~1.9 eV is calculated from both absorption and diffused reflectance spectroscopy's which showed stronger p-d repulsions in the Ga (3d) and N (2p) orbitals. This effect and chemical nitridation caused upward shift of valence band and band gap reduction. The GaON nanosheets are investigated for PEC studies in a standard three electrode system under 1 Sun irradiation in 0.5 M Na2SO4. The photocurrent generation, oxidation and reduction reactions during the measurements are observed by Chronoampereometry, linear sweep Voltametry (LSV) and Cyclic Voltametry (CV) respectively. Henceforward, these GaON nanosheets can be used as potential photocatalyts for solar water splitting.

Sonochemical Assisted Solvothermal Synthesis of Gallium Oxynitride Nanosheets and their Solar-Driven Photoelectrochemical Water-Splitting Applications

PubMed Central

Iqbal, Naseer; Khan, Ibrahim; Yamani, Zain H.; Qurashi, Ahsanullhaq

2016-01-01

Gallium oxynitride (GaON) nanosheets for photoelectrochemical (PEC) analysis are synthesized via direct solvothermal approach. Their FE-SEM revealed nanosheets morphology of GaON prepared at a reaction time of 24 hours at 180 °C. The elemental composition and mapping of Ga, O and N are carried out through electron dispersive X-ray spectroscopy (EDX). The cubic structure of GaON nanosheets is elucidated by X-ray diffraction (XRD)analysis. The X-ray Photoelectron Spectroscopy (XPS) further confirms Ga, O and N in their respective ratios and states. The optical properties of GaON nanosheets are evaluated via UV-Visible, Photoluminescence (PL) and Raman spectroscopy’s. The band gap energy of ~1.9 eV is calculated from both absorption and diffused reflectance spectroscopy’s which showed stronger p-d repulsions in the Ga (3d) and N (2p) orbitals. This effect and chemical nitridation caused upward shift of valence band and band gap reduction. The GaON nanosheets are investigated for PEC studies in a standard three electrode system under 1 Sun irradiation in 0.5 M Na2SO4. The photocurrent generation, oxidation and reduction reactions during the measurements are observed by Chronoampereometry, linear sweep Voltametry (LSV) and Cyclic Voltametry (CV) respectively. Henceforward, these GaON nanosheets can be used as potential photocatalyts for solar water splitting. PMID:27561646

Solvothermal synthesis of InP quantum dots and their enhanced luminescent efficiency by post-synthetic treatments.

PubMed

Byun, Ho-June; Lee, Ju Chul; Yang, Heesun

2011-03-01

InP quantum dots (QDs) were solvothermally synthesized by using a greener phosphorus source of P(N(CH(3))(2))(3) instead of highly toxic P(TMS)(3) widely used, and subsequently subjected to a size-sorting processing. While as-grown QDs showed an undetectably low emission intensity, post-synthetic treatments such as photo-etching, photo-radiation, and photo-assisted ZnS shell coating gave rise to a substantial increase in emission efficiency due to the effective removal and passivation of surface states. The emission efficiency of the photo-etched QDs was further enhanced by a consecutive UV photo-radiation, attributable to the photo-oxidation at QD surface. Furthermore, a relatively thick ZnS shell on the surface of InP QDs that were surface-modified with hydrophilic ligands beforehand was photochemically generated in an aqueous solution at room temperature. The resulting InP/ZnS core/shell QDs, emitting from blue to red wavelengths, were more efficient than the above photo-treated InP QDs, and their luminescent properties (emission bandwidth and quantum yield) were comparable to those of InP QDs synthesized with P(TMS)(3). Structural, size, and compositional analyses on InP/ZnS QDs were also conducted to elucidate their core/shell structure. Copyright © 2010 Elsevier Inc. All rights reserved.

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.

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.

ZnO twin-cones: synthesis, photoluminescence, and catalytic decomposition of ammonium perchlorate.

PubMed

Sun, Xuefei; Qiu, Xiaoqing; Li, Liping; Li, Guangshe

2008-05-19

ZnO twin-cones, a new member to the ZnO family, were prepared directly by a solvothermal method using a mixed solution of zinc nitrate and ethanol. The reaction and growth mechanisms of ZnO twin-cones were investigated by X-ray diffraction, UV-visible spectra, infrared and ion trap mass spectra, and transmission electron microscopy. All as-prepared ZnO cones consisted of tiny single crystals with lengths of several micrometers. With prolonging of the reaction time from 1.5 h to 7 days, the twin-cone shape did not change at all, while the lattice parameters increased slightly and the emission peak of photoluminescence shifted from the green region to the near orange region. ZnO twin-cones are also explored as an additive to promote the thermal decomposition of ammonium perchlorate. The variations of photoluminescence spectra and catalytic roles in ammonium perchlorate decomposition were discussed in terms of the defect structure of ZnO twin-cones.

Hierarchical Nanostructures of Metal-Organic Frameworks Applied in Gas Separating ZIF-8-on-ZIF-67 Membranes.

PubMed

Knebel, Alexander; Wulfert-Holzmann, Paul; Friebe, Sebastian; Pavel, Janet; Strauß, Ina; Mundstock, Alexander; Steinbach, Frank; Caro, Jürgen

2018-04-17

Membranes from metal-organic frameworks (MOFs) are highly interesting for industrial gas separation applications. Strongly improved performances for carbon capture and H 2 purification tasks in MOF membranes are obtained by using highly reproducable and very accuratly, hierarchically grown ZIF-8-on-ZIF-67 (ZIF-8@ZIF-67) nanostructures. To forgo hardly controllable solvothermal synthesis, particles and layers are prepared by self-assembling methods. It was possible for the first time to confirm ZIF-8-on-ZIF-67 membrane growth on rough and porous ceramic supports using the layer-by-layer deposition. Additionally, hierarchical particles are made in a fast RT synthesis with high monodispersity. Characterization of the hierarchical and epitaxial grown layers and particles is performed by SEM, TEM, EDXM and gas permeation. The system ZIF-8@ZIF-67 shows a nearly doubled H 2 /CO 2 separation factor, regardless of whether neat membrane or mixed-matrix-membrane in comparison to other MOF materials. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Magnetoresistance behavior in nanobulk assembled Bi2Se3 topological insulator

NASA Astrophysics Data System (ADS)

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

2018-05-01

Temperature and magnetic field dependent magnetoresistance (MR) including structural, morphological studies of Bi2Se3 nanoflower like structure synthesized by microwave assisted solvothermal method has been investigated. Powder X-ray diffraction (XRD) has confirmed the formation of single phase. Morphology of the material shows nanoflower kind of structures with edge to edge size of around 4 µm and such occurrences are quite high. The temperature dependent resistance invokes a metallic behavior up to a certain lower temperature, below which it follows -ln(T) behavior that has been elucidated in literature using electron-electron interaction and weak anti-localization effects. High temperature magnetoresistance is consistent with parabolic field dependence indicating a classical magnetoresistance in metals as a result of Lorenz force. In low temperature regime magnetoresistance as a function of magnetic field at different temperatures obeys power law near low field which indicates a three dimensional weak-antilocalization. A linear magnetoresistance at low temperature and high magnetic field shows the domination of surface state conduction.

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.

Sonochemical synthesis and structural characterization of a new Zn(II) nanoplate metal-organic framework with removal efficiency of Sudan red and Congo red.

PubMed

Abdollahi, Nasrin; Masoomi, Mohammad Yaser; Morsali, Ali; Junk, Peter C; Wang, Jun

2018-07-01

A 3-D Zn(II) based metal-organic framework (MOF) of [Zn 4 (oba) 3 (DMF) 2 ] was synthesized using the nonlinear dicarboxylate ligand, 4,4'-oxybis(benzoic acid) (H 2 oba) via sonochemical and solvothermal routes. IR spectroscopy, single-crystal X-ray crystallography, scanning electron microscopy, and X-ray powder diffraction were used to characterize these MOF samples. The effect of different times of irradiation and various concentrations of primary reagents were experimented for obtaining monotonous morphology. The results show that uniform nanoplates can be achieved by increasing the time of irradiation and decreasing the concentration. N 2 adsorption was applied to examine the effect of synthesis method on porosity of the framework. Also Congo red and Sudan red dyes were employed to explore the efficiency of this MOF in removal of the dye pollutants. Copyright © 2018 Elsevier B.V. All rights reserved.

Monodisperse Zn-doped Fe3O4 formation and photo-Fenton activity for degradation of rhodamine B in water

NASA Astrophysics Data System (ADS)

Cen, Huoshi; Nan, Zhaodong

2018-10-01

Zn-doped Fe3O4 can be used as a catalyst in the photo-Fenton process to degrade dye molecules dissolved in water, in which cluster-shaped Zn-doped Fe3O4 (CSZnFe) was synthesized. To enhance the catalytic activity, monodisperse Zn-doped Fe3O4 (MZnFe) was facilely synthesized by a modified solvothermal method through replacement of sodium acetate by urea as a base. The particle size of MZnFe was about 9-16 nm. MZnFe exhibits a larger surface area and higher photo-Fenton catalytic activity for degradation of rhodamine B in water than CSZnFe. Additionally, MZnFe exhibits high saturation magnetization (about 80 emu/g), which is very convenient for separation of MZnFe from solution by a magnet. The growth processes for MZnFe were proposed on the basis of results from in situ calorimetry and other techniques, which indicated different formation mechanisms for MZnFe and CSZnFe.

A novel synthesis of SrCO3-SrTiO3 nanocomposites with high photocatalytic activity

NASA Astrophysics Data System (ADS)

Márquez-Herrera, A.; Ovando-Medina, Víctor M.; Castillo-Reyes, Blanca E.; Meléndez-Lira, M.; Zapata-Torres, M.; Saldaña, N.

2014-12-01

The results of the production and characterization of SrCO3-SrTiO3 nanocomposites as a promising candidate for efficient photocatalysts are reported. The production is based on a novelty route employing the solvothermal method with strontium chloride and titanium (IV) butoxide as the precursor solutions. The effect on the properties of the nanocomposites due to changes in the content of SrCO3 and SrTiO3 is reported. The as-prepared materials were tested in the photodegradation of methylene blue dye in aqueous solutions under the solar light. The reported route allows the production of SrCO3-SrTiO3 nanocomposites with particle sizes ranging between 18 and 29 nm. The SrCO3-SrTiO3 nanocomposites obtained with 19 % of SrCO3 phase and 81 % of SrTiO3 (M10) can achieve 94 and 97 % of dye photodegradation after 30 and 120 min, respectively.

Enhanced Photoelectrocatalytic Activity of BiOI Nanoplate-Zinc Oxide Nanorod p-n Heterojunction.

PubMed

Kuang, Pan-Yong; Ran, Jing-Run; Liu, Zhao-Qing; Wang, Hong-Juan; Li, Nan; Su, Yu-Zhi; Jin, Yong-Gang; Qiao, Shi-Zhang

2015-10-19

The development of highly efficient and robust photocatalysts has attracted great attention for solving the global energy crisis and environmental problems. Herein, we describe the synthesis of a p-n heterostructured photocatalyst, consisting of ZnO nanorod arrays (NRAs) decorated with BiOI nanoplates (NPs), by a facile solvothermal method. The product thus obtained shows high photoelectrochemical water splitting performance and enhanced photoelectrocatalytic activity for pollutant degradation under visible light irradiation. The p-type BiOI NPs, with a narrow band gap, not only act as a sensitizer to absorb visible light and promote electron transfer to the n-type ZnO NRAs, but also increase the contact area with organic pollutants. Meanwhile, ZnO NRAs provide a fast electron-transfer channel, thus resulting in efficient separation of photoinduced electron-hole pairs. Such a p-n heterojunction nanocomposite could serve as a novel and promising catalyst in energy and environmental applications. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

W18O49 nanowires assembled on carbon felt for application to supercapacitors

NASA Astrophysics Data System (ADS)

Jung, Jinjoo; Kim, Do Hyung

2018-03-01

For supercapacitor applications, W18O49 nanowires have been extensively grown on graphitic carbon felt using a facile solvothermal method. The diameter and length of the nanowires are about 7 and 300 nm, respectively. The nanowires consist of monoclinic W18O49 grown along the [010] direction, as shown by TEM and XRD analyses. The W18O49 nanowires, assembled on carbon felt, exhibit a high capacity of 588.33 F/g at a current density of 1 A/g together with an excellent cycle performance, and a low internal resistance during the electrochemical tests. This outstanding performance may originate from the three-dimensional porous nanostructure of these W18O49 nanowires, which leads to a reduction in the resistance and fast reaction kinetics due to the high specific surface area and electrolyte accessibility. Furthermore, sufficient oxygen deficiencies of the substoichiometric tungsten oxide can also contribute to the electrochemical activity, which can be confirmed by comparison of CV and EIS data with WO3 nanowires.

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.

Room-temperature H2S Gas Sensor Based on Au-doped ZnFe2O4 Yolk-shell Microspheres.

PubMed

Yan, Yin; Nizamidin, Patima; Turdi, Gulmira; Kari, Nuerguli; Yimit, Abliz

2017-01-01

Room-temperature type H 2 S sensing devices that use Au-doped ZnFe 2 O 4 yolk-shell microspheres as the active material have been fabricated using a solvothermal method as well as subsequent annealing and a chemical etching process. The samples are characterized using X-ray diffraction (XRD), energy-dispersive X-ray spectroscopy (EDS), field-emission scanning electron microscopy (FESEM), and X-ray photoelectron spectroscopy (XPS). The results demonstrate that the doping of Au does not change the spinel structure of the products, which were yolk-shell microspheres, while the particle size varied with the Au doping concentration. Also, the as-fabricated sensor device exhibited excellent selectivity toward H 2 S gas at the room temperature; the gas-sensing property of 2 wt% Au-doped ZnFe 2 O 4 microspheres was the best. The Au-doped ZnFe 2 O 4 yolk-shell microspheres can be promising as a sensing material for H 2 S gas detecting at room temperature.

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

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.

Effects of morphology and chemical doping on electrochemical properties of metal hydroxides in pseudocapacitors.

PubMed

Lee, Gyeonghee; Varanasi, Chakrapani V; Liu, Jie

2015-02-21

It is well known that both the structural morphology and chemical doping are important factors that affect the properties of metal hydroxide materials in electrochemical energy storage devices. In this work, an effective method to tailor the morphology and chemical doping of metal hydroxides is developed. It is shown that the morphology and the degree of crystallinity of Ni(OH)2 can be changed by adding glucose in the ethanol-mediated solvothermal synthesis. Ni(OH)2 produced in this manner exhibited an increased specific capacitance, which is partially attributed to its increased surface area. Interestingly, the effect of morphology on cobalt doped-Ni(OH)2 is found to be more effective at low cobalt contents than at high cobalt contents in terms of improving the electrochemical performance. This result reveals the existence of competitive effects between chemical doping and morphology change. These findings will provide important insights to design effective materials for energy storage devices.

Isostructural 1D coordination polymers of Zn(II), Cd(II) and Cu(II) with phenylpropynoic acid and DABCO as organic linkers

NASA Astrophysics Data System (ADS)

Saravanakumar, Rajendran; Varghese, Babu; Sankararaman, Sethuraman

2014-11-01

Using phenylpropynoic acid (PPA) and 1,4-diazabicyclo[2.2.2]octane (DABCO) as organic spacers, isostructural coordination polymers of Zn(II), Cd(II) and Cu(II) were synthesized by solvothermal method and structurally characterized using single crystal XRD, powder XRD, 13C CP-MAS NMR spectroscopy. Single crystal XRD data revealed four PPA units coordinating with two metal ions forming a paddle wheel secondary building unit (SBU). The paddle wheel units are connected through coordination of DABCO nitrogen to the metal centers from the axial positions leading to the formation of the 1D coordination polymers along the c axis. Intermolecular π stacking and Csbnd H…π interactions between the adjacent polymer chains convert the 1D coordination polymer into an interesting 3D network with the Csbnd H…π bonds running along the crystallographic a and b axes. Thermal and nitrogen adsorption studies of these coordination polymers are reported.

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.

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.

High-rate synthesis of Cu-BTC metal-organic frameworks.

PubMed

Kim, Ki-Joong; Li, Yong Jun; Kreider, Peter B; Chang, Chih-Hung; Wannenmacher, Nick; Thallapally, Praveen K; Ahn, Ho-Geun

2013-12-21

The reaction conditions for the synthesis of Cu-BTC (BTC = benzene-1,3,5-tricarboxylic acid) were elucidated using a continuous-flow microreactor-assisted solvothermal system to achieve crystal size and phase control. A high-rate synthesis of Cu-BTC metal-organic frameworks with a BET surface area of more than 1600 m(2) g(-1) (Langmuir surface area of more than 2000 m(2) g(-1)) and with a 97% production yield could be achieved with a total reaction time of 5 minutes.

Four unexpected lanthanide coordination polymers involving in situ reaction of solvent N, N-Dimethylformamide

NASA Astrophysics Data System (ADS)

Jin, Jun-Cheng; Tong, Wen-Quan; Fu, Ai-Yun; Xie, Cheng-Gen; Chang, Wen-Gui; Wu, Ju; Xu, Guang-Nian; Zhang, Ya-Nan; Li, Jun; Li, Yong; Yang, Peng-Qi

2015-05-01

Four unexpected 2D lanthanide coordination polymers have been synthesized through in situ reactions of DMF solvent under solvothermal conditions. The isostructural complexes 1-3 contain four types of 21 helical chains. While the Nd(III) ions are bridged through μ2-HIDC2- and oxalate to form a 2D sheet along the bc plane without helical character in 4. Therefore, complex 1 exhibits bright red solid-state phosphorescence upon exposure to UV radiation at room temperature.

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.

An effective approach to study the biocompatibility of Fe3O4 nanoparticles, graphene and their nanohybrid composite

NASA Astrophysics Data System (ADS)

Singh, Ashwani Kumar; Singh, Pallavi; Verma, Rajiv Kumar; Yadav, Suresh; Singh, Kedar; Srivastava, Amit

2018-02-01

The present manuscript describes a simple, facile and effective solvothermal route to synthesize Fe3O4 nanoparticles (Fe3O4 NPs), reduced graphene oxide nanosheets (rGO NSs) and Fe3O4/reduced graphene oxide nanohybrid composite (Fe3O4/rGO nanohybrid composite) and subsequently examines their comparative biocompatibilities. The as-obtained Fe3O4 NPs, rGO NSs and Fe3O4/rGO nanohybrid composite have been characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and Raman spectroscopy. The XRD studies and scanning electron microscope confirmed the proper phase formation and the surface morphology of the as-synthesized products, respectively. The Raman spectra of Fe3O4 NPs show the strongest peak at 673 cm-1 which can be assigned to A1g peak of bare Fe3O4 NPs and it complements the XRD studies. Furthermore, the increment in the I D/I G ratio in the Fe3O4/rGO nanohybrid composite suggests the creation of defects in graphene sheets due to strain caused by Fe3O4 NPs. The biocompatibility of these samples has been tested using Lung cancer cell line H1299 through MTT assay. The MTT assay reveals that the nanohybrid composite endows more biocompatible and effectiveness than rGO NSs and Fe3O4 NPs individually, as anti-proliferative agent for cancer treatment.

A novel strategy to construct Janus metallamacrocycles with both a Ru-arene face and an imidazolium face.

PubMed

Li, Ji; Zhang, Peipei; Xu, Yan; Su, Zhi; Qian, Yong; Li, Shunli; Yu, Tao; Sadler, Peter J; Liu, Hong-Ke

2017-11-28

The bottom-up construction of highly functional metallamacrocycles from simple building blocks is a challenge of much current interest. We have used solvothermal reactions of a bifunctional p-bitmb ligand with [Ru(arene)X 2 ] 2 in CH 2 Cl 2 or CH 2 Br 2 to generate the novel mononuclear metallamacrocyclic [RuX(arene)L 2 CH 2 ]X 3 complexes 1-3 (1, arene = p-cym, X = Cl; 2, arene = bip, X = Cl; 3, arene = p-cym, X = Br), which were characterized by various techniques. These complexes are "bowl-like" and have two faces: one coordinative Ru centre (arene)Ru(N,N)X bridged by L (L = 1,4-bis(imidazol-1-ylmethyl)-2,3,5,6-tetramethylbenzene, p-bitmb) to a dipositive bis-imidazolinium centre. Cl - or Br - anions can be trapped inside the cavity of the "bowl-like" structure, forming H-bonds with the backbone. Experimental (NMR and ESI-MS) and computational (DFT calculations) studies show that the source of the bridging -CH 2 - group is the dihalogenated solvent (CH 2 Cl 2 or CH 2 Br 2 ) that links the two arms of an initially formed non-cyclic complex (arene)RuX 2 L 2 by a mechanism of nucleophilic substitution. Optimization of the reaction conditions afforded the macrocyclic complexes in almost quantitative yields. The applications of these complexes as anti-proliferative agents towards cancer cells and for selective anion sensing have been explored.

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.

Octahedron Fe3O4 particles supported on 3D MWCNT/graphene foam: In-situ method and application as a comprehensive microwave absorption material

NASA Astrophysics Data System (ADS)

Shi, Luolin; Zhao, Yan; Li, Ye; Han, Xiao; Zhang, Tong

2017-09-01

In this work, we used in-situ method to directly prepare a novel structure consisting of well-distributed octahedron Fe3O4 particles, porous graphene foam (GF) and fibrous multiwalled carbon nanotube (MWCNT): started with an intense stir to anchor Fe3+ on the surfaces of graphene oxide and oxided MWCNT, followed by solvothermal reaction to synthesize 3D lightweight Fe3O4/MWCNT/GF hybrids with high performance microwave absorption (MA). The maximum Reflection Loss (RL) value of -35.30 dB and 9.01 GHz bandwidth with RL below -10 dB detected with the thickness of 3.0 mm are achieved by Fe3O4/MWCNT/GF with an ultralow bulk density of 5.0 mg cm-3, of which the Specific Microwave Absorption Performance is much higher than most available MA materials reported. Impedance matching, high loss characteristic, interfacial polarization and polarization relaxation significantly improve MA properties, which serves as a guide for fabricating comprehensive MA materials enjoying numerous advantages of high RL value, broad bandwidth, low density and thin thickness.

Synthesis, characterization and adsorptive performance of MgFe2O4 nanospheres for SO2 removal.

PubMed

Zhao, Ling; Li, Xinyong; Zhao, Qidong; Qu, Zhenping; Yuan, Deling; Liu, Shaomin; Hu, Xijun; Chen, Guohua

2010-12-15

A type of uniform Mg ferrite nanospheres with excellent SO(2) adsorption capacity could be selectively synthesized via a facile solvothermal method. The size of the MgFe(2)O(4) nanospheres was controlled to be 300-400 nm in diameter. The structural, textural, and surface properties of the adsorbent have been fully characterized by a variety of techniques (Brunauer-Emmett-Teller, BET; X-ray diffraction analysis, XRD; scanning electron microscopy, SEM; and energy-dispersive X-ray spectroscopy, EDS). The valence states and the surface chemical compositions of MgFe(2)O(4) nanospheres were further identified by X-ray photoelectron spectroscopy (XPS). The behaviors of SO(2) oxidative adsorption on MgFe(2)O(4) nanospheres were studied using Fourier transform infrared spectroscopy (FTIR). Both the sulfite and sulfate species could be formed on the surface of MgFe(2)O(4). The adsorption equilibrium isotherm of SO(2) was analyzed using a volumetric method at 298 K and 473 K. The results indicate that MgFe(2)O(4) nanospheres possess a good potential as the solid-state SO(2) adsorbent for applications in hot fuel gas desulfurization. Copyright © 2010 Elsevier B.V. All rights reserved.

Ultrathin nickel hydroxide nanosheet arrays grafted biomass-derived honeycomb-like porous carbon with improved electrochemical performance as a supercapacitive material

NASA Astrophysics Data System (ADS)

Nagaraju, Goli; Cha, Sung Min; Yu, Jae Su

2017-03-01

Three-dimensional hierarchical honeycomb-like activated porous carbon pillared ultrathin Ni(OH)2 nanosheets (Ni(OH)2 NSs@HAPC) for use as supercapacitor materials were facilely synthesized. With an aid of pine cone flowers as a biomass source, HAPC conducting scaffolds were prepared by the alkali treatment and pyrolysis methods under an inert gas atmosphere. Subsequently, the Ni(OH)2 NSs were synthesized evenly on the surface of HAPC via a solvothermal method. The resulting HAPC and Ni(OH)2 NSs@HAPC composite materials offered free pathways for effective diffusion of electrolyte ions and fast transportation of electrons when employed as an electrode material. The Ni(OH)2 NSs@HAPC composite electrode exhibited excellent electrochemical properties including a relatively high specific capacitance (Csp) value of ~ 916.4 F/g at 1 A/g with good cycling stability compared to the pristine HAPC and Ni(OH)2 NSs electrodes. Such bio-friendly derived carbon-based materials with transition metal hydroxide/oxide composite materials could be a promising approach for high-performance energy storage devices because of their advantageous properties of cost effectiveness and easy availability.

Synthesis and characterization of α-MoO{sub 3} nanobelt composite positive electrode materials for lithium battery application

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

Nadimicherla, Reddeppa; State Key Laboratory of Advanced Technology for Materials Synthesis and Processing, and School of Materials Science and Engineering, Wuhan University of Technology, Wuhan 430070; Chen, Wen

2015-06-15

Graphical abstract: (a) TEM image of MoO{sub 3}/PEO nanobelts composite, (b) CV curves of MoO{sub 3}/PEO nanobelts composite. - Highlights: • α-MoO{sub 3} and PEO surfactant MoO{sub 3} nanobelts were synthesized by solvothermal method. • The capacity retention of 12.5 wt% PEO surfactant MoO{sub 3} nanobelts is 88.78%. • The specific capacity of 12.5 wt% PEO surfactant MoO{sub 3} nanobelts is 352 mAh g{sup −1}. • MoO{sub 3}/PEO nanobelts composite material demonstrates good cycling stability as cathode. - Abstract: α-MoO{sub 3} and PEO surfactant MoO{sub 3} nanobelts were synthesized by a solvothermal method. The morphology and nanostructure of samples weremore » characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Bare α-MoO{sub 3} and 12.5 wt% PEO surfactant MoO{sub 3} nanobelts have an initial specific capacities of 279 and 352 mAh g{sup −1}, respectively, at constant current density 30 mA g{sup −1} with potential range of 1.5–4.0 V vs. Li/Li{sup +}. While MoO{sub 3} is modified by the intercalation of PEO, it is effectively shielded against electrostatic interaction between the MoO{sub 3} interlayer and Li{sup +} ions. We reported positive material, a nanocomposite of MoO{sub 3} coated with polyethylene oxide. It presents good cycling stability due to existence of the conductive and protective polyethylene oxide coating and the nanobelt morphology of MoO{sub 3}. The polyethylene oxide acts as a conducting matrix, a binder and an active material, as well as a volume change buffer agent, which holds the MoO{sub 3} particles in place during the discharge cycles. The cyclic voltammograms of the 12.5 wt% PEO surfactant MoO{sub 3} nanobelt composite displayed better cyclic performance compared with pure MoO{sub 3} nanobelts. The specific capacity of the pure MoO{sub 3} nanobelts and 12.5 wt% PEO surfactant MoO{sub 3} nanobelts exhibit as 199 mAh g{sup −1} and 225 mAh g{sup −1}, respectively, after 9 cycles, suggesting that the stability of surfactant material is worthy.« less

Synthesis of three-dimensional reduced graphene oxide layer supported cobalt nanocrystals and their high catalytic activity in F-T CO2 hydrogenation

NASA Astrophysics Data System (ADS)

He, Fei; Niu, Na; Qu, Fengyu; Wei, Shuquan; Chen, Yujin; Gai, Shili; Gao, Peng; Wang, Yan; Yang, Piaoping

2013-08-01

The reduced graphene oxide (rGO) supported cobalt nanocrystals have been synthesized through an in situ crystal growth method using Co(acac)2 under solvothermal conditions by using DMF as the solvent. By carefully controlling the reaction temperature, the phase transition of the cobalt nanocrystals from the cubic phase to the hexagonal phase has been achieved. Moreover, the microscopic structure and morphology as well as the reduction process of the composite have been investigated in detail. It is found that oxygen-containing functional groups on the graphene oxide (GO) can greatly influence the formation process of the Co nanocrystals by binding the Co2+ cations dissociated from the Co(acac)2 in the initial reaction solution at 220 °C, leading to the 3D reticular structure of the composite. Furthermore, this is the first attempt to use a Co/rGO composite as the catalyst in the F-T CO2 hydrogenation process. The catalysis testing results reveal that the as-synthesized 3D structured composite exhibits ideal catalytic activity and good stability, which may greatly extend the scope of applications for this kind of graphene-based metal hybrid material.The reduced graphene oxide (rGO) supported cobalt nanocrystals have been synthesized through an in situ crystal growth method using Co(acac)2 under solvothermal conditions by using DMF as the solvent. By carefully controlling the reaction temperature, the phase transition of the cobalt nanocrystals from the cubic phase to the hexagonal phase has been achieved. Moreover, the microscopic structure and morphology as well as the reduction process of the composite have been investigated in detail. It is found that oxygen-containing functional groups on the graphene oxide (GO) can greatly influence the formation process of the Co nanocrystals by binding the Co2+ cations dissociated from the Co(acac)2 in the initial reaction solution at 220 °C, leading to the 3D reticular structure of the composite. Furthermore, this is the first attempt to use a Co/rGO composite as the catalyst in the F-T CO2 hydrogenation process. The catalysis testing results reveal that the as-synthesized 3D structured composite exhibits ideal catalytic activity and good stability, which may greatly extend the scope of applications for this kind of graphene-based metal hybrid material. Electronic supplementary information (ESI) available. See DOI: 10.1039/c3nr03038e

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.

Improvement of the BiOI photocatalytic activity optimizing the solvothermal synthesis

NASA Astrophysics Data System (ADS)

Mera, Adriana C.; Moreno, Yanko; Contreras, David; Escalona, Nestor; Meléndrez, Manuel F.; Mangalaraja, Ramalinga Viswanathan; Mansilla, Héctor D.

2017-01-01

BiOI nanostructured microspheres were obtained from the solvothermal synthesis route in the presence of ethylene glycol and KI as solvent and source of iodide, respectively. Optimal conditions for the synthesis were obtained by using multivariate analysis and choosing the photocatalytic oxidation rate constant of 3,4,5-trihydroxybenzoic acid (gallic acid) as response factor under simulated solar radiation. Response surface methodology (RSM) was used to determine the optimum values of the reaction time and temperature which were 18 h and 126 °C, respectively, to obtain the most active catalyst. In addition, BiOI synthesis using ionic liquid 1-butyl-3-methylimidazolium iodide ([bmim]I) as iodide source was also carried out for the comparison of microstructure and its photocatalytic efficiency. The obtained BiOI nanostructures were characterized by scanning electron microscopy (SEM) attached with energy dispersive spectrometer (EDS), nitrogen adsorption, X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), thermogravimetry (TG), Fourier transform infrared (FTIR) spectrometry, diffuse reflectance spectroscopy (DRS) and cyclic voltammetry (CV) analyses for their changes in morphological and structural behaviors. It was observed that the synthesis temperature of BiOI nanostructures strongly influenced the morphology, crystalline phase, surface area and electrochemical behavior, and thus affecting the photocatalytic efficiency. The higher photocatalytic removal of gallic acid (60%) was reached within 30 min of irradiation with UV-A on microspheres obtained with ionic liquid. The (1 1 0) crystal phase of BiOI influenced the photocatalytic efficiency.

Ionic liquid-assisted preparation of square-shaped Y{sub 2}O{sub 3} nanoplates

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

Wang, Lei; Fang, Hao; Xu, Hualan

Highlights: • Y{sub 4}O(OH){sub 9}(NO{sub 3}) nanosheets were prepared by an ionic liquid-assisted mixed solvothermal route. • Y{sub 2}O{sub 3} nanosheets were obtained after calcining the Y{sub 4}O(OH){sub 9}(NO{sub 3}) nanosheets. • The Y{sub 2}O{sub 3} nanosheets are with length of about 300 nm and thickness of several nanometers. - Abstract: Uniform square-shaped Y{sub 4}O(OH){sub 9}(NO{sub 3}) nanoplates with side length of about 300 nm and thickness of tens of nanometers have been successfully prepared by an ionic liquid-assisted mixed solvothermal route. Y{sub 2}O{sub 3} nanoplates with similar size were obtained after calcining the Y{sub 4}O(OH){sub 9}(NO{sub 3}) nanoplates atmore » 800 °C. The products were analyzed by powder X-ray diffraction (XRD), thermogravimetric analysis (TG), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high resolution TEM (HRTEM), and electron diffraction (ED). The effects of reaction time, composition of solvents, and the molar ratio of reagents on the morphology of the products have been investigated. The possible formation mechanism of the Y{sub 4}O(OH){sub 9}(NO{sub 3}) nanoplates was also discussed. Y{sub 2}O{sub 3}:Eu{sup 3+} nanoplates were also synthesized and their photoluminescent properties were examined.« less

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.

A template-free solvothermal synthesis and photoluminescence properties of multicolor Gd2O2S:xTb3+, yEu3+ hollow spheres

NASA Astrophysics Data System (ADS)

Sang, Xiaotong; Xu, Guangxi; Lian, Jingbao; Wu, Nianchu; Zhang, Xue; He, Jiao

2018-06-01

The multicolor Gd2O2S:xTb3+, yEu3+ hollow spheres were successfully synthesized via a template-free solvothermal route without the use of surfactant from commercially available Ln (NO3)3·6H2O (Ln = Gd, Tb and Eu), absolute ethanol, ethanediamine and sublimed sulfur as the starting materials. The phase, structure, particle morphology and photoluminescence (PL) properties of the as-obtained products were investigated by X-ray diffraction (XRD), fourier transform infrared spectroscopy (FT-IR), field emission scanning electron microscopy (FE-SEM) and photoluminescence spectra. The influence of synthetic time on phase, structure and morphology was systematically investigated and discussed. The possible formation mechanism depending on synthetic time t for the Gd2O2S phase has been presented. These results demonstrate that the Gd2O2S hollow spheres could be obtained under optimal condition, namely solvothermal temperature T = 220 °C and synthetic time t = 16 h. The as-obtained Gd2O2S sample possesses hollow sphere structure, which has a typical size of about 2.5 μm in diameter and about 0.5 μm in shell thickness. PL spectroscopy reveals that the strongest emission peak for the Gd2O2S:xTb3+ and the Gd2O2S:yEu3+ samples is located at 545 nm and 628 nm, corresponding to 5D4→7F5 transitions of Tb3+ ions and 5D0→7F2 transitions of Eu3+ ions, respectively. The quenching concentration of Tb3+ ions and Eu3+ ions is 7%. In the case of Tb3+ and Eu3+ co-doped samples, when the concentration of Tb3+ or Eu3+ ions is 7%, the optimum concentration of Eu3+ or Tb3+ ions is determined to be 1%. Under 254 nm ultraviolet (UV) light excitation, the Gd2O2S:7%Tb3+, the Gd2O2S:7%Tb3+,1%Eu3+ and the Gd2O2S:7%Eu3+ samples give green, yellow and red light emissions, respectively. And the corresponding CIE coordinates vary from (0.3513, 0.5615), (0.4120, 0.4588) to (0.5868, 0.3023), which is also well consistent with their luminous photographs.

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

I2-induced SC-SC transformation within two-dimensional Zn(ii)-triazole framework: an ideal detector of cyano-containing molecules.

PubMed

Wang, Ying; Yi, Jin-Min; Zhang, Meng-Yuan; Xu, Ping; Zhao, Xiao-Jun

2016-02-21

A novel interpenetrated 2D + 2D → 2D architechture {[Zn(BTPS)(TPA)]·1.5DMF·H2O}n () has been constructed under solvothermal conditions. Interestingly, I2-induced single-crystal-to-single-crystal transformation to {[Zn(BTPS)(I)(TPA)1.5]·1.5H2O}n () showed a 2D + 1D → 2D array. Luminescent properties indicated that represents the first example of selective recognition toward cyano-containing molecules.

Photoluminescent carbon dots based on a rare 3D inorganic-organic hybrid cadmium borate crystal.

PubMed

Zhou, Kang; Zhang, Wen-Jin; Luo, Yuan-Zhang; Pan, Chun-Yang

2018-05-17

A 3D inorganic-organic hybridized skeleton cadmium borate [Cden][B5O8(OH)] (1) (en = ethylenediamine) has been solvothermally synthesized. By calcining it, specific shape carbon dots (C-dots) with abundant free radicals were observed. In addition, C-dots in the ethanol phase exhibited variable photoluminescence and showed rare turn on or off effects to Cr3+ ions and CdSe/ZnS quantum dots, but only a turn on effect to Cs+ ions and a turn off effect to CsPbBr3 quantum dots.

Continuous Solvothermal Synthesis and Surface Treatment for Improved and Scalable Processing of Ultra High Temperature Ceramic (UHTC) Nanopowders

DTIC Science & Technology

2017-06-13

with homogeneous nonagglomerated nanoparticles,20 smudge- and stain -resistant coatings, antibody bonding to phosphor particles, and more. A series...2 BBn + 11.0 Na (in benzene) --- ZrB2 + 4 NaCl + 6 NaBr (1) (2) In a typical experiment, the reactor is charged with 5 grams of anhydrous ZrCl4...21.5 mmol), 0.471 grams of boron (43.5 mmol), 2.35 grams of sodium metal (102.3 mmol) and 100 ml of anhydrous benzene in a controlled atmosphere

Two-dimensional ultra-thin SiO(x) (0 < x < 2) nanosheets with long-term cycling stability as lithium ion battery anodes.

PubMed

Sun, Lin; Su, Tingting; Xu, Lei; Liu, Meipin; Du, Hong-Bin

2016-03-21

Ultra-thin SiO(x) (0 < x < 2) nanosheets were obtained via a convenient solvothermal route from a Zintl compound CaSi2. After carbon coating, the SiOx@C nanosheet anodes exhibit high capacity, good rate and superior cycling performance for high-capacity lithium ion battery applications. The specific capacity can be maintained as high as 760 mA h g(-1) with almost no capacity decay after 400 cycles at a current density of 0.5 A g(-1).

Sol-Gel Processing of MgF₂ Antireflective Coatings.

PubMed

Löbmann, Peer

2018-05-02

There are different approaches for the preparation of porous antireflective λ/4 MgF₂ films from liquid precursors. Among these, the non-aqueous fluorolytic synthesis of precursor solutions offers many advantages in terms of processing simplicity and scalability. In this paper, the structural features and optical performance of the resulting films are highlighted, and their specific interactions with different inorganic substrates are discussed. Due to their excellent abrasion resistance, coatings have a high potential for applications on glass. Using solvothermal treatment of precursor solutions, also the processing of thermally sensitive polymer substrates becomes feasible.

Synthesis and Characterization of Functionalized Metal-organic Frameworks

PubMed Central

Karagiaridi, Olga; Bury, Wojciech; Sarjeant, Amy A.; Hupp, Joseph T.; Farha, Omar K.

2014-01-01

Metal-organic frameworks have attracted extraordinary amounts of research attention, as they are attractive candidates for numerous industrial and technological applications. Their signature property is their ultrahigh porosity, which however imparts a series of challenges when it comes to both constructing them and working with them. Securing desired MOF chemical and physical functionality by linker/node assembly into a highly porous framework of choice can pose difficulties, as less porous and more thermodynamically stable congeners (e.g., other crystalline polymorphs, catenated analogues) are often preferentially obtained by conventional synthesis methods. Once the desired product is obtained, its characterization often requires specialized techniques that address complications potentially arising from, for example, guest-molecule loss or preferential orientation of microcrystallites. Finally, accessing the large voids inside the MOFs for use in applications that involve gases can be problematic, as frameworks may be subject to collapse during removal of solvent molecules (remnants of solvothermal synthesis). In this paper, we describe synthesis and characterization methods routinely utilized in our lab either to solve or circumvent these issues. The methods include solvent-assisted linker exchange, powder X-ray diffraction in capillaries, and materials activation (cavity evacuation) by supercritical CO2 drying. Finally, we provide a protocol for determining a suitable pressure region for applying the Brunauer-Emmett-Teller analysis to nitrogen isotherms, so as to estimate surface area of MOFs with good accuracy. PMID:25225784

A multi-controlled drug delivery system based on magnetic mesoporous Fe3O4 nanopaticles and a phase change material for cancer thermo-chemotherapy

NASA Astrophysics Data System (ADS)

Zhang, Qi; Liu, Jian; Yuan, Kunjie; Zhang, Zhengguo; Zhang, Xiaowen; Fang, Xiaoming

2017-10-01

Herein a novel multi-controlled drug release system for doxorubicin (DOX) was developed, in which monodisperse mesoporous Fe3O4 nanoparticles were combined with a phase change material (PCM) and polyethylene glycol 2000 (PEG2000). It is found that the PCM/PEG/DOX mixture containing 20% PEG could be dissolved into water at 42 °C. The mesoporous Fe3O4 nanoparticles prepared by the solvothermal method had sizes of around 25 nm and exhibited a mesoporous microstructure. A simple solvent evaporation process was employed to load the PCM/PEG/DOX mixture on the mesoporous Fe3O4 nanoparticles completely. In the Fe3O4@PCM/PEG/DOX system, the pores of the Fe3O4 nanoparticles were observed to be filled with the mixture of PCM/PEG/DOX. The Fe3O4@PCM/PEG/DOX system showed a saturation magnetization value of 50.0 emu g-1, lower than 71.1 emu g-1 of the mesoporous Fe3O4 nanoparticles, but it was still high enough for magnetic targeting and hyperthermia application. The evaluation on drug release performance indicated that the Fe3O4@PCM/PEG/DOX system achieved nearly zero release of DOX in vitro in body temperature, while around 80% of DOX could be released within 1.5 h at the therapeutic threshold of 42 °C or under the NIR laser irradiation for about 4 h. And a very rapid release of DOX was achieved by this system when applying an alternating magnetic field. By comparing the systems with and without PEG2000, it is revealed that the presence of PEG2000 makes DOX easy to be released from 1-tetradecanol to water, owing to its functions of increasing the solubility of DOX in 1-tetradecanol as well as decreasing the surface tension between water and 1-tetradecanol. The novel drug release system shows great potential for the development of thermo-chemotherapy of cancer treatment.

Core-shell indium (III) sulfide@metal-organic framework nanocomposite as an adsorbent for the dispersive solid-phase extraction of nitro-polycyclic aromatic hydrocarbons.

PubMed

Jia, Yuqian; Zhao, Yanfang; Zhao, Mei; Wang, Zhenhua; Chen, Xiangfeng; Wang, Minglin

2018-05-25

A core-shell discoid shaped indium (III) sulfide@metal-organic framework (MIL-125(Ti)) nanocomposite was synthesized by a solvothermal method and explored as an adsorbent material for dispersive solid-phase extraction (d-SPE). The as-synthesized sorbent was characterized by scanning electron microscopy, energy-dispersive spectroscopy, transmission electron microscopy, powder X-ray diffraction, N 2 adsorption-desorption analysis, and Fourier transform infrared spectroscopy. The extraction performance was evaluated by the d-SPE of 16 nitro-polycyclic aromatic hydrocarbons (NPAHs) from water samples. The analysis was carried out by gas chromatography (GC) coupled with triple quadruple mass spectrometer in negative chemical ionization (NCI) mode. The selected ion monitoring (SIM) was used in the quantification of the target NPAHs. Extraction factors affecting the d-SPE, including the ionic strength, extraction temperature, and extraction time were optimized by the response surface methodology. The developed d-SPE method showed good linear correlations from 10 to 1000 ng L -1 (r > 0.99), low detection limits (2.9-83.0 ng L -1 ), satisfactory repeatability (relative standard deviation of <10%, n = 6), and acceptable recoveries (71.3%-112.2%) for water samples. The developed method was used for the food and environmental sample analysis. The results demonstrated that the method could be used for sample preparation of trace NPAHs in real samples. Copyright © 2018. Published by Elsevier B.V.

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.

Fabrication of functional hollow microspheres constructed from MOF shells: Promising drug delivery systems with high loading capacity and targeted transport

PubMed Central

Gao, Xuechuan; Hai, Xiao; Baigude, Huricha; Guan, Weihua; Liu, Zhiliang

2016-01-01

An advanced multifunctional, hollow metal-organic framework (MOF) drug delivery system with a high drug loading level and targeted delivery was designed and fabricated for the first time and applied to inhibit tumour cell growth. This hollow MOF targeting drug delivery system was prepared via a simple post-synthetic surface modification procedure, starting from hollow ZIF-8 successfully obtained for the first time via a mild phase transformation under solvothermal conditions. As a result, the hollow ZIF-8 exhibits a higher loading capacity for the model anticancer drug 5-fluorouracil (5-FU). Subsequently, 5-FU-loaded ZIF-8 was encapsulated into polymer layers (FA-CHI-5-FAM) with three components: a chitosan (CHI) backbone, the imaging agent 5-carboxyfluorescein (5-FAM), and the targeting reagent folic acid (FA). Thus, an advanced drug delivery system, ZIF-8/5-FU@FA-CHI-5-FAM, was fabricated. A cell imaging assay demonstrated that ZIF-8/5-FU@FA-CHI-5-FAM could target and be taken up by MGC-803 cells. Furthermore, the as-prepared ZIF-8/5-FU@FA-CHI-5-FAM exhibited stronger cell growth inhibitory effects on MGC-803 cells because of the release of 5-FU, as confirmed by a cell viability assay. In addition, a drug release experiment in vitro indicated that ZIF-8/5-FU@FA-CHI-5-FAM exhibited high loading capacity (51%) and a sustained drug release behaviour. Therefore, ZIF-8/5-FU@FA-CHI-5-FAM could provide targeted drug transportation, imaging tracking and localized sustained release. PMID:27876876

Self-sacrifice Template Formation of Hollow Hetero-Ni7S6/Co3S4 Nanoboxes with Intriguing Pseudo-capacitance for High-performance Electrochemical Capacitors

PubMed Central

Hua, Hui; Liu, Sijia; Chen, Zhiyi; Bao, Ruiqi; Shi, Yaoyao; Hou, Linrui; Pang, Gang; Hui, Kwun Nam; Zhang, Xiaogang; Yuan, Changzhou

2016-01-01

Herein, we report a simple yet efficient self-sacrifice template protocol to smartly fabricate hollow hetero-Ni7S6/Co3S4 nanoboxes (Ni-Co-S NBs). Uniform nickel cobalt carbonate nanocubes are first synthesized as the precursor via solvothermal strategy, and subsequently chemically sulfidized into hollow heter-Ni-Co-S NBs through anion-exchange process. When evaluated as electrode for electrochemical capacitors (ECs), the resultant hetero-Ni-Co-S NBs visually exhibit attractive pesudo-capacitance in KOH just after continuously cyclic voltammetry (CV) scanning for 100 cycles. New insights into the underlying energy-storage mechanism of the hollow hetero-Ni-Co-S electrode, based on physicochemical characterizations and electrochemical evaluation, are first put forward that the electrochemically induced phase transformation gradually occurrs during CV sweep from the hetero-Ni-Co-S to bi-component-active NiOOH and CoOOH, which are the intrinsic charge-storage phases for the appealing Faradaic capacitance (~677 F g−1 at 4 A g−1) of hollow Ni-Co-S NBs at high rates after cycling. When further coupled with negative activated carbon (AC), the AC//hetero-Ni-Co-S asymmetric device with extended electrochemical window of 1.5 V demonstrates high specific energy density of ~31 Wh kg−1. Of significance, we strongly envision that hollow design concept and new findings here hold great promise for enriching synthetic methodologies, and electrochemistry of complex metal sulfides for next-generation ECs. PMID:26865246

Organosilane-functionalized graphene quantum dots and their encapsulation into bi-layer hollow silica spheres for bioimaging applications.

PubMed

Wen, Ting; Yang, Baocheng; Guo, Yanzhen; Sun, Jing; Zhao, Chunmei; Zhang, Shouren; Zhang, Miao; Wang, Yonggang

2014-11-14

Graphene quantum dots (GQDs) represent an important class of luminescent quantum dots owing to their low toxicity and superior biocompatibility. Chemical functionalization of GQDs and subsequent combination with other materials further provide attractive techniques for advanced bioapplications. Herein, we report the facile fabrication of fluorescent organosilane-functionalized graphene quantum dots (Si-GQDs) and their embedding into mesoporous hollow silica spheres as a biolabel for the first time. Well-proportioned Si-GQDs with bright and excitation dependent tunable emissions in the visible region were obtained via a simple and economical solvothermal route adopting graphite oxide as a carbon source and 3-(2-aminoethylamino)-propyltrimethoxysilane as a surface modifier. The as-synthesized Si-GQDs can be well dispersed and stored in organic solvents, easily manufactured into transparent film and bulk form, and particularly provide great potential to be combined with other materials. As a proof-of-principle experiment, we demonstrate the successful incorporation of Si-GQDs into hollow mesoporous silica spheres and conduct preliminary cellular imaging experiments. Interestingly, the Si-GQDs not only serve as fluorescent chromophores in the composite material, but also play a crucial role in the formation of mesoporous hollow silica spheres with a distinctive bi-layer architecture. The layer thickness and optical properties can be precisely controlled by simply adjusting the silane coupling agent addition procedure in the preparation process. Our demonstration of low-cost Si-GQDs and their encapsulation into multifunctional composites may expand the applications of carbon-based nanomaterials for future biomedical imaging and other optoelectronic applications.

Self-sacrifice Template Formation of Hollow Hetero-Ni7S6/Co3S4 Nanoboxes with Intriguing Pseudo-capacitance for High-performance Electrochemical Capacitors

NASA Astrophysics Data System (ADS)

Hua, Hui; Liu, Sijia; Chen, Zhiyi; Bao, Ruiqi; Shi, Yaoyao; Hou, Linrui; Pang, Gang; Hui, Kwun Nam; Zhang, Xiaogang; Yuan, Changzhou

2016-02-01

Herein, we report a simple yet efficient self-sacrifice template protocol to smartly fabricate hollow hetero-Ni7S6/Co3S4 nanoboxes (Ni-Co-S NBs). Uniform nickel cobalt carbonate nanocubes are first synthesized as the precursor via solvothermal strategy, and subsequently chemically sulfidized into hollow heter-Ni-Co-S NBs through anion-exchange process. When evaluated as electrode for electrochemical capacitors (ECs), the resultant hetero-Ni-Co-S NBs visually exhibit attractive pesudo-capacitance in KOH just after continuously cyclic voltammetry (CV) scanning for 100 cycles. New insights into the underlying energy-storage mechanism of the hollow hetero-Ni-Co-S electrode, based on physicochemical characterizations and electrochemical evaluation, are first put forward that the electrochemically induced phase transformation gradually occurrs during CV sweep from the hetero-Ni-Co-S to bi-component-active NiOOH and CoOOH, which are the intrinsic charge-storage phases for the appealing Faradaic capacitance (~677 F g-1 at 4 A g-1) of hollow Ni-Co-S NBs at high rates after cycling. When further coupled with negative activated carbon (AC), the AC//hetero-Ni-Co-S asymmetric device with extended electrochemical window of 1.5 V demonstrates high specific energy density of ~31 Wh kg-1. Of significance, we strongly envision that hollow design concept and new findings here hold great promise for enriching synthetic methodologies, and electrochemistry of complex metal sulfides for next-generation ECs.

Self-sacrifice Template Formation of Hollow Hetero-Ni7S6/Co3S4 Nanoboxes with Intriguing Pseudo-capacitance for High-performance Electrochemical Capacitors.

PubMed

Hua, Hui; Liu, Sijia; Chen, Zhiyi; Bao, Ruiqi; Shi, Yaoyao; Hou, Linrui; Pang, Gang; Hui, Kwun Nam; Zhang, Xiaogang; Yuan, Changzhou

2016-02-11

Herein, we report a simple yet efficient self-sacrifice template protocol to smartly fabricate hollow hetero-Ni7S6/Co3S4 nanoboxes (Ni-Co-S NBs). Uniform nickel cobalt carbonate nanocubes are first synthesized as the precursor via solvothermal strategy, and subsequently chemically sulfidized into hollow heter-Ni-Co-S NBs through anion-exchange process. When evaluated as electrode for electrochemical capacitors (ECs), the resultant hetero-Ni-Co-S NBs visually exhibit attractive pesudo-capacitance in KOH just after continuously cyclic voltammetry (CV) scanning for 100 cycles. New insights into the underlying energy-storage mechanism of the hollow hetero-Ni-Co-S electrode, based on physicochemical characterizations and electrochemical evaluation, are first put forward that the electrochemically induced phase transformation gradually occurrs during CV sweep from the hetero-Ni-Co-S to bi-component-active NiOOH and CoOOH, which are the intrinsic charge-storage phases for the appealing Faradaic capacitance (~677 F g(-1) at 4 A g(-1)) of hollow Ni-Co-S NBs at high rates after cycling. When further coupled with negative activated carbon (AC), the AC//hetero-Ni-Co-S asymmetric device with extended electrochemical window of 1.5 V demonstrates high specific energy density of ~31 Wh kg(-1). Of significance, we strongly envision that hollow design concept and new findings here hold great promise for enriching synthetic methodologies, and electrochemistry of complex metal sulfides for next-generation ECs.

MnO2-x nanosheets on stainless steel felt as a carbon- and binder-free cathode for non-aqueous lithium-oxygen batteries

NASA Astrophysics Data System (ADS)

Wei, Z. H.; Zhao, T. S.; Zhu, X. B.; Tan, P.

2016-02-01

Manganese dioxide (MnO2) has been recognized as an effective catalyst for the oxygen reduction and oxygen evolution reactions in non-aqueous lithium-oxygen batteries. However, a further improvement in battery performance with the MnO2 catalyst is limited by its low electronic conductivity and catalytic activity, which strongly depend on the morphology and composition. In this work, we develop a carbon- and binder-free MnO2-x nanosheets/stainless steel (SS) cathode via a simple and effective electrodeposition-solvothermal route. The created Mn(III) and oxygen vacancy in MnO2-x nanosheets allows an significant increase in the electronic conductivity and catalytic activity. It is experimentally shown that the use of the present nanostructure MnO2-x/SS cathode in a non-aqueous lithium-oxygen battery results in a rechargeable specific capacity of 7300 mAh g-1 at a current density of 200 mA g-1, which is 39% higher than that with the MnO2/SS cathode. In addition, the specific capacities at 400 mA g-1 and 800 mA g-1 reach 5249 mAh g-1 and 2813 mAh g-1, respectively, which are over 30% higher than that with the MnO2/SS cathode. Furthermore, the discharge/charge cycle test shows no degradation for 120 cycles. All the results show that the present nanostructure MnO2-x/SS cathode is a promising candidate for high-performance lithium-oxygen batteries.

In situ growth of TiO2 in interlayers of expanded graphite for the fabrication of TiO2-graphene with enhanced photocatalytic activity.

PubMed

Jiang, Baojiang; Tian, Chungui; Zhou, Wei; Wang, Jianqiang; Xie, Ying; Pan, Qingjiang; Ren, Zhiyu; Dong, Youzhen; Fu, Dan; Han, Jiale; Fu, Honggang

2011-07-18

We present a facile route for the preparation of TiO(2)-graphene composites by in situ growth of TiO(2) in the interlayer of inexpensive expanded graphite (EG) under solvothermal conditions. A vacuum-assisted technique combined with the use of a surfactant (cetyltrimethylammonium bromide) plays a key role in the fabrication of such composites. Firstly, the vacuum environment promotes full infusion of the initial solution containing Ti(OBu)(4) and the surfactant into the interlayers of EG. Subsequently, numerous TiO(2) nanoparticles uniformly grow in situ in the interlayers with the help of the surfactant, which facilitates the exfoliation of EG under the solvothermal conditions in ethanol, eventually forming TiO(2)-graphene composites. The as-prepared samples have been characterized by Raman and FTIR spectroscopies, SEM, TEM, AFM, and thermogravimetic analysis. It is shown that a large number of TiO(2) nanoparticles homogeneously cover the surface of high-quality graphene sheets. The graphene exhibits a multi-layered structure (5-7 layers). Notably, the TiO(2)-graphene composite (only 30 wt % of which is TiO(2)) synthesized by subsequent thermal treatment at high temperature under nitrogen shows high photocatalytic activity in the degradation of phenol under visible and UV lights in comparison with bare Degussa P25. The enhanced photocatalytic performance is attributed to increased charge separation, improved light absorbance and light absorption width, and high adsorptivity for pollutants. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Templating Influence of Molecular Precursors on Pr(OH)3 Nanostructures.

PubMed

Hemmer, Eva; Cavelius, Christian; Huch, Volker; Mathur, Sanjay

2015-07-06

Four new praseodymium alkoxo and amido compounds ([Pr3(μ3-OtBu)2(μ2-OtBu)3(OtBu)4(HOtBu)2] (1), [Pr{OC(tBu)3}3(THF)] (2), [PrCl{N(SiMe3)2}2(THF)]2 (3), and [PrCl{OC(tBu)3}2(THF)]2 (4)) were synthesized and structurally characterized by single-crystal X-ray diffraction analysis. Application of these compounds in solvothermal synthesis of praseodymium oxide/hydroxide nanostructures showed their templating influence on the morphology and phase composition of the resulting solid-state materials. Differential reactivity of the chosen alkoxide ligands toward water and the different arrangements of metal-oxygen units in the studied precursor compounds strongly influenced the kinetics of hydrolysis and cross-condensation reactions as manifested in the morphological changes and phase composition of the final products. Thermal decomposition studies of 1-4 confirmed their conversion into the corresponding oxide phases. Activation of compounds 1, 2, and 4 by either a base or a stoichiometric amount of water showed the distinct influence of their chemical configuration on the obtained nanopowders: whereas 1 solely produced nanorods of Pr(OH)3, 2 predominantly formed a mixture of rod-shaped and spherical particles. The solvothermal decomposition of 4 resulted in Pr(OH)2Cl or PrOCl due to the presence of Cl ligands in the molecular precursor. The resultant materials were thoroughly characterized to demonstrate the relationship between precursor chemistry and the processing parameters that are clearly manifested in the morphology and phase of the final ceramics.

Green synthesis of CuInS2/ZnS core-shell quantum dots by facile solvothermal route with enhanced optical properties

NASA Astrophysics Data System (ADS)

Jindal, Shikha; Giripunje, Sushama M.; Kondawar, Subhash B.; Koinkar, Pankaj

2018-03-01

We report an eco-friendly green synthesis of highly luminescent CuInS2/ZnS core-shell quantum dots (QDs) with average particle size ∼ 3.9 nm via solvothermal process. The present study embodies the intensification of CuInS2/ZnS QDs properties by the shell growth on the CuInS2 QDs. The as-prepared CuInS2 core and CuInS2/ZnS core-shell QDs have been characterized using a range of optical and structural techniques. By adopting a low temperature growth of CuInS2 core and high temperature growth of CuInS2/ZnS core-shell growth, the tuning of absorption and photoluminescence emission spectra were observed. Optical absorption and photoluminescence spectroscopy probe the effect of ZnS passivation on the electronic structure of the CuInS2 dots. In addition, QDs have been scrutinized using ultra violet photoelectron spectroscopy (UPS) to explore their electronic band structure. The band level positions of CuInS2 and CuInS2/ZnS QDs suffices the demand of non-toxic acceptor material for electronic devices. The variation in electronic energy levels of CuInS2 core with the coating of wide band gap ZnS shell influence the removal of trap assisted recombination on the surface of the core. QDs exhibited tunable emission from red to orange region. These studies reveal the feasibility of QDs in photovoltaic and light emitting diodes.

Paramagnetism of cobalt-doped ZnO nanoparticles obtained by microwave solvothermal synthesis.

PubMed

Wojnarowicz, Jacek; Kusnieruk, Sylwia; Chudoba, Tadeusz; Gierlotka, Stanislaw; Lojkowski, Witold; Knoff, Wojciech; Lukasiewicz, Malgorzata I; Witkowski, Bartlomiej S; Wolska, Anna; Klepka, Marcin T; Story, Tomasz; Godlewski, Marek

2015-01-01

Zinc oxide nanopowders doped with 1-15 mol % cobalt were produced by the microwave solvothermal synthesis (MSS) technique. The obtained nanoparticles were annealed at 800 °C in nitrogen (99.999%) and in synthetic air. The material nanostructure was investigated by means of the following techniques: X-ray diffraction (XRD), helium pycnometry density, specific surface area (SSA), inductively coupled plasma optical emission spectrometry (ICP-OES), extended X-ray absorption fine structure (EXAFS) spectroscopy, scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS) and with magnetometry using superconducting quantum interference device (SQUID). Irrespective of the Co content, nanoparticles in their initial state present a similar morphology. They are composed of loosely agglomerated spherical particles with wurtzite-type crystal structure with crystallites of a mean size of 30 nm. Annealing to temperatures of up to 800 °C induced the growth of crystallites up to a maximum of 2 μm in diameter. For samples annealed in high purity nitrogen, the precipitation of metallic α-Co was detected for a Co content of 5 mol % or more. For samples annealed in synthetic air, no change of phase structure was detected, except for precipitation of Co3O4 for a Co content of 15 mol %. The results of the magentometry investigation indicated that all as-synthesized samples displayed paramagnetic properties with a contribution of anti-ferromagnetic coupling of Co-Co pairs. After annealing in synthetic air, the samples remained paramagnetic and samples annealed under nitrogen flow showed a magnetic response under the influences of a magnetic field, likely related to the precipitation of metallic Co in nanoparticles.

Unique and facile solvothermal synthesis of mesoporous WO3 using a solid precursor and a surfactant template as a photoanode for visible-light-driven water oxidation

PubMed Central

2014-01-01

Mesoporous tungsten trioxide (WO3) was prepared from tungstic acid (H2WO4) as a tungsten precursor with dodecylamine (DDA) as a template to guide porosity of the nanostructure by a solvothermal technique. The WO3 sample (denoted as WO3-DDA) prepared with DDA was moulded on an electrode to yield efficient performance for visible-light-driven photoelectrochemical (PEC) water oxidation. Powder X-ray diffraction (XRD) data of the WO3-DDA sample calcined at 400°C indicate a crystalline framework of the mesoporous structure with disordered arrangement of pores. N2 physisorption studies show a Brunauer-Emmett-Teller (BET) surface area up to 57 m2 g-1 together with type IV isotherms and uniform distribution of a nanoscale pore size in the mesopore region. Scanning electron microscopy (SEM) images exhibit well-connected tiny spherical WO3 particles with a diameter of ca. 5 to 20 nm composing the mesoporous network. The WO3-DDA electrode generated photoanodic current density of 1.1 mA cm-2 at 1.0 V versus Ag/AgCl under visible light irradiation, which is about three times higher than that of the untemplated WO3. O2 (1.49 μmol; Faraday efficiency, 65.2%) was evolved during the 1-h photoelectrolysis for the WO3-DDA electrode under the conditions employed. The mesoporous electrode turned out to work more efficiently for visible-light-driven water oxidation relative to the untemplated WO3 electrode. PMID:25313301

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.

Novel Nano Boehmite prepared by Solvothermal reaction of aluminum hydroxide gel in Monoethanolamine

NASA Astrophysics Data System (ADS)

Ohta, Yasuhiro; Hayakawa, Tomokatsu; Inomata, Tomohiko; Ozawa, Tomohiro; Masuda, Hideki

2017-07-01

Solvothermal reaction of aluminum hydroxide gel (AHG) in monoethanolamine (MEA) was studied at several temperatures (100, 120, 150, and 200 °C) in several reaction times (2, 3, 4, 5, 6, and 13 h). The reaction product prepared at a low temperature of 120 °C in the reaction time more than 6 h gave a blue photoluminescence nanoboehmite intercalated with monoethanolamine derivatives (BM-MEA) in the colloidal solution, which showed a photoluminescence emission centered at 420 nm with an excitation of 360 nm. The powdery samples recovered from the reaction products were characterized by using elemental analysis, XRD analysis, IR spectroscopy, thermogravimetric (TG)-DTA, 13C and 27Al CP/MAS NMR spectroscopies, N2 gas adsorption/desorption isotherm, SEM and TEM images, and photoluminescence spectroscopy. The X-ray diffraction revealed that the basal space in BM-MEA was expanded from 0.61 to 1.2 nm by intercalation of MEA derivatives to boehmite, and the IR and 13C CP/MAS NMR spectra determined that the intercalated MEA derivatives are protonated- and carbamate-substituted MEAs, which are formed in the layers through a covalent bond with Al-OH groups on boehmite surface. The empirical formula of BM-MEA was estimated to be AlO(OH)0.82(OCH2CH2NH3 +)0.05(OCH2CH2NHCOO-)0.13 on the basis of the elemental TG-DTA and IR spectral analyses. We discuss the reaction mechanism of a unique blue photoluminescence BM-MEA formed by proceeding in CO2-H2O-alkanolamine system.

Hierarchical heterostructures of p-type bismuth oxychloride nanosheets on n-type zinc ferrite electrospun nanofibers with enhanced visible-light photocatalytic activities and magnetic separation properties.

PubMed

Sun, Yucong; Shao, Changlu; Li, Xinghua; Guo, Xiaohui; Zhou, Xuejiao; Li, Xiaowei; Liu, Yichun

2018-04-15

P-type bismuth oxychloride (p-BiOCl) nanosheets were uniformly grown on n-type zinc ferrite (n-ZnFe 2 O 4 ) electrospun nanofibers via a solvothermal technique to form hierarchical heterostructures of p-BiOCl/n-ZnFe 2 O 4 (p-BiOCl/n-ZnFe 2 O 4 H-Hs). The density and loading amounts of the BiOCl nanosheets with exposed {0 0 1} facets were easily controlled by adjusting the reactant concentration in the solvothermal process. The p-BiOCl/n-ZnFe 2 O 4 H-Hs exhibited enhanced visible-light photocatalytic activities for the degradation of Rhodamine B (RhB). The apparent first-order rate of the p-BiOCl/n-ZnFe 2 O 4 H-Hs and its normalized constant were about 12.6- and 8-fold higher than pure ZnFe 2 O 4 nanofibers. This suggests that both the improved charge separation efficiency from the uniform p-n heterojunctions and the enlarged active surface sites from the hierarchical structures increase the photocatalytic performances. Furthermore, the p-BiOCl/n-ZnFe 2 O 4 H-Hs could be efficiently separated from the solution with an external magnetic field via the ferromagnetic behavior of ZnFe 2 O 4 nanofibers. The magnetic p-BiOCl/n-ZnFe 2 O 4 H-Hs with enhanced visible-light photocatalytic performances might have potential applications in water treatment. Copyright © 2018. Published by Elsevier Inc.

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.

Thermal oxidation synthesis hollow MoO{sub 3} microspheres and their applications in lithium storage and gas-sensing

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

Zhao, Xinyu; School of Petrochemical Engineering, Shenyang University of Technology, Liaoyang 111003; Cao, Minhua, E-mail: caomh@bit.edu.cn

2013-06-01

Graphical abstract: MoO{sub 3} hollow microspheres were synthesized via a facile and template-free solvothermal route and subsequent heat treatment in air. The MoO{sub 3} hollow microspheres exhibit an improved lithium storage and gas-sensing performance. Highlights: ► Hollow MoO{sub 3} microspheres were synthesized by thermal oxidation of hollow MoO{sub 2}. ► The MoO{sub 3} hollow microspheres have a relatively high specific surface area. ► The MoO{sub 3} hollow microspheres exhibit improved lithium storage performance. ► The MoO{sub 3} hollow microspheres show good responses to ammonia gas. - Abstract: In this paper, MoO{sub 3} hollow microspheres were synthesized via a facile andmore » template-free solvothermal route and subsequent heat treatment in air. The MoO{sub 3} hollow microspheres have a relatively high specific surface area, and with such a feature, the as-synthesized MoO{sub 3} hollow microspheres have potential applications in Li-ion battery and gas-sensor. When tested as a Li-storage anode material, the MoO{sub 3} hollow microspheres show a higher discharge capacity of 1377.1 mA h g{sup −1} in the first discharge and a high reversible capacity of 780 mA h g{sup −1} after 100 cycles at a rate of 1 C. Furthermore, as a gas sensing material, the MoO{sub 3} hollow microspheres exhibit an improved sensitivity and short response/recovery time to trace levels of ammonia gas.« less

Highly Sensitive Detection of UV Radiation Using a Uranium Coordination Polymer.

PubMed

Liu, Wei; Dai, Xing; Xie, Jian; Silver, Mark A; Zhang, Duo; Wang, Yanlong; Cai, Yawen; Diwu, Juan; Wang, Jian; Zhou, Ruhong; Chai, Zhifang; Wang, Shuao

2018-02-07

The accurate detection of UV radiation is required in a wide range of chemical industries and environmental or biological related applications. Conventional methods taking advantage of semiconductor photodetectors suffer from several drawbacks such as sophisticated synthesis and manufacturing procedure, not being able to measure the accumulated UV dosage as well as high defect density in the material. Searching for new strategies or materials serving as precise UV dosage sensor with extremely low detection limit is still highly desirable. In this work, a radiation resistant uranium coordination polymer [UO 2 (L)(DMF)] (L = 5-nitroisophthalic acid, DMF = N,N-dimethylformamide, denoted as compound 1) was successfully synthesized through mild solvothermal method and investigated as a unique UV probe with the detection limit of 2.4 × 10 -7 J. On the basis of the UV dosage dependent luminescence spectra, EPR analysis, single crystal structure investigation, and the DFT calculation, the UV-induced radical quenching mechanism was confirmed. Importantly, the generated radicals are of significant stability which offers the opportunity for measuring the accumulated UV radiation dosage. Furthermore, the powder material of compound 1 was further upgraded into membrane material without loss in luminescence intensity to investigate the real application potentials. To the best of our knowledge, compound 1 represents the most sensitive coordination polymer based UV dosage probe reported to date.

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

Simple Test Functions in Meshless Local Petrov-Galerkin Methods

NASA Technical Reports Server (NTRS)

Raju, Ivatury S.

2016-01-01

Two meshless local Petrov-Galerkin (MLPG) methods based on two different trial functions but that use a simple linear test function were developed for beam and column problems. These methods used generalized moving least squares (GMLS) and radial basis (RB) interpolation functions as trial functions. These two methods were tested on various patch test problems. Both methods passed the patch tests successfully. Then the methods were applied to various beam vibration problems and problems involving Euler and Beck's columns. Both methods yielded accurate solutions for all problems studied. The simple linear test function offers considerable savings in computing efforts as the domain integrals involved in the weak form are avoided. The two methods based on this simple linear test function method produced accurate results for frequencies and buckling loads. Of the two methods studied, the method with radial basis trial functions is very attractive as the method is simple, accurate, and robust.

Highly efficient removal of pathogenic bacteria with magnetic graphene composite.

PubMed

Zhan, Sihui; Zhu, Dandan; Ma, Shuanglong; Yu, Wenchao; Jia, Yanan; Li, Yi; Yu, Hongbing; Shen, Zhiqiang

2015-02-25

Magnetic Fe3O4/graphene composite (abbreviated as G-Fe3O4) was synthesized successfully by solvothermal method to effectively remove both bacteriophage and bacteria in water, which was tested by HRTEM, XRD, BET, XPS, FTIR, CV, magnetic property and zeta-potential measurements. Based on the result of HRTEM, the single-sheet structure of graphene oxide and the monodisperse Fe3O4 nanoparticles on the surface of graphene can be observed obviously. The G-Fe3O4 composite were attractive for removing a wide range of pathogens including not only bacteriophage ms2, but also various bacteria such as S. aureus, E. coli, Salmonella, E. Faecium, E. faecalis, and Shigella. The removal efficiency of E. coli for G-Fe3O4 composite can achieve 93.09%, whereas it is only 54.97% with pure Fe3O4 nanoparticles. Moreover, a detailed verification test of real water samples was conducted and the removal efficiency of bacteria in real water samples with G-Fe3O4 composite can also reach 94.8%.

Single-crystalline dendritic bimetallic and multimetallic nanocubes.

PubMed

Kuang, Yun; Zhang, Ying; Cai, Zhao; Feng, Guang; Jiang, Yingying; Jin, Chuanhong; Luo, Jun; Sun, Xiaoming

2015-12-01

Developing facial synthetic routes for fabrication of multimetallic nanocatalysts with open porous morphology, tunable composition and tailored crystalline structure is a big challenge for fabrication of low-cost electrocatalysts. Here we report on the synthesis of single-crystalline dendritic bimetallic and multimetallic nanocubes via a solvothermal co-reduction method. These cubes show highly porous, complex 3D inner connections but single-crystalline structure. Tuning the reduction kinetics of metal precursors and introducing galvanic reaction at the active sites during growth were believed to be the keys for the formation of such unique nanostructure. Electro-catalytic oxygen reduction (ORR) and methanol oxidation (MOR) on these catalysts showed dramatic enhancements for both cathodic and anodic electrocatalysis in fuel cells, which were attributed to their unique morphology and crystalline structure, as well as synergetic effect of the multi-metallic components. This work uncovers the formation mechanism of such complex single-crystalline dendritic multimetallic nanocrystals and offers a promising synthetic strategy for geometric and crystalline control of multimetallic nanocrystals with tailored physical and chemical properties, which will benefit the development of clean energy.

Template-free synthesis of novel SnS2 array and its superior performances for lithium ion battery

NASA Astrophysics Data System (ADS)

Zhu, Anquan; Qiao, Lulu; Tan, Pengfei; Ma, Yongjin; Liu, Yi; Pan, Jun

2018-05-01

A kind of novel three-dimensional SnS2 array was fabricated by an ethylenediamine (EDA) assisting low-temperature solvothermal method. It was observed that as-obtained SnS2 array was composed of numerous SnS2 nanosheets with the thickness of about 22 nm. When used as lithium ion batteries (LIBs) anode, the SnS2 array displayed remarkable capacities on rate and cycling performances, delivering the rates with reversible capacities of 763.3, 658.6, 593.6, 554.4 and 450.3 mAh g-1 at the current densities of 0.2, 0.5, 1, 2 and 5 A g-1, respectively. Moreover, the satisfactory cycling performance was also disclosed, remaining capacity of 547.8 mAh g-1 after 100th cycle at 0.2 A g-1, better than some reported pure SnS2 nanostructures. Based on the characterization and experimental results, the reasons of such superior electrochemical performances were determined and elaborated. It means that the SnS2 array possesses promising potential on the renewable energy field.

Thermal annealing effect on structural and thermoelectric properties of hexagonal Bi2Te3 nanoplate thin films by drop-casting technique

NASA Astrophysics Data System (ADS)

Hosokawa, Yuichi; Wada, Kodai; Tanaka, Masaki; Tomita, Koji; Takashiri, Masayuki

2018-02-01

High-purity hexagonal bismuth telluride (Bi2Te3) nanoplates were prepared by a solvothermal synthesis method, followed by the fabrication of nanoplate thin films by the drop-casting technique. The Bi2Te3 nanoplates exhibited a single-crystalline phase with a rhombohedral crystal structure. The nanoplates had a flat surface with edge sizes ranging from 500 to 2000 nm (average size of 1000 nm) and a thickness of less than 50 nm. The resulting Bi2Te3 nanoplate thin films were composed of well-aligned hexagonal nanoplates along the surface direction with an approximate film thickness of 40 µm. To tightly connect the nanoplates together within the thin films, thermal annealing was performed at different temperatures. We found that the thermoelectric properties, especially the Seebeck coefficient, were very sensitive to the annealing temperature. Finally, the optimum annealing temperature was determined to be 250 °C and the Seebeck coefficient and power factor were -300 µV/K and 3.5 µW/(cm·K2), respectively.

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.

Potential effect of CuInS2/ZnS core-shell quantum dots on P3HT/PEDOT:PSS heterostructure based solar cell

NASA Astrophysics Data System (ADS)

Jindal, Shikha; Giripunje, S. M.

2018-07-01

Nanostructured quantum dots (QDs) are quite promising in the solar cell application due to quantum confinement effect. QDs possess multiple exciton generation and large surface area. The environment friendly CuInS2/ZnS core-shell QDs were prepared by solvothermal method. Thus, the 3 nm average sized CuInS2/ZnS QDs were employed in the bulk heterojunction device and the active blend layer consisting of the P3HT and CuInS2/ZnS QDs was investigated. The energy level information of CuInS2/ZnS QDs as an electron acceptor was explored by ultra violet photoelectron spectroscopy. Bulk heterojunction hybrid device of ITO/PEDOT:PSS/P3HT: (CuInS2/ZnS QDs)/ZnO/Ag was designed by spin coating approach and its electrical characterization was investigated by solar simulator. Current density - voltage characteristics shows the enhancement in power conversion efficiency with increasing concentration of CuInS2/ZnS QDs in bulk heterojunction device.

Heterogeneous photo-Fenton processes using graphite carbon coating hollow CuFe2O4 spheres for the degradation of methylene blue

NASA Astrophysics Data System (ADS)

Guo, Xiaojun; Wang, Kebai; Li, Dai; Qin, Jiabin

2017-10-01

The novel graphite carbon coating hollow CuFe2O4 spheres were fabricated through solvothermal method and characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and Raman spectra, etc. The catalytic performance of the graphite carbon coating hollow CuFe2O4 spheres was evaluated in photo-Fenton-like degradation of methylene blue (MB) using H2O2 as a green oxidant under light irradiation (λ > 400 nm). The results demonstrated that the hollow CuFe2O4 spheres with graphite carbon coating exhibited superior catalytic activity. In the preparation process of catalyst, the addition of glucose was very important to its catalytic performance. Photoresponse analysis of the typical samples proved that CuFe2O4@graphite carbon core-shell hollow spheres possessed excellent photocurrent response and lower electrochemical impedance. In addition, a possible mechanism for photocatalytic degradation of MB had been presumed. Moreover, after five regeneration cycles, the graphite carbon coating hollow CuFe2O4 spheres still exhibited better properties.

An efficient dye-sensitized BiOCl photocatalyst for air and water purification under visible light irradiation.

PubMed

Li, Guisheng; Jiang, Bo; Xiao, Shuning; Lian, Zichao; Zhang, Dieqing; Yu, Jimmy C; Li, Hexing

2014-08-01

A photosensitized BiOCl catalyst was found to be effective for photocatalytic water purification and air remediation under visible light irradiation (λ > 420 nm). Prepared by a solvothermal method, the BiOCl crystals possessed a 3D hierarchical spherical structure with the highly active facets exposed. When sensitized by Rhodamine B (RhB), the photocatalyst system was more active than N-doped TiO2 for breaking down 4-chlorophenol (4-CP, 200 ppm) and nitric monoxide (NO, 500 ppb). The high activity could be attributed to the hierarchical structure (supplying feasible reaction tunnels for adsorption and transition of reactants or products) and the efficient exposure of the {001} facets. The former provides an enriched oxygen atom density that promotes adsorption of cationic dye RhB, and creates an oxygen vacancy state. The HO˙ and ˙O2(-) radicals produced from the injected electrons from the excited dye molecule (RhB*) into the conduction band of BiOCl were responsible for the excellent photocatalytic performance of the RhB-BiOCl system.

Cubic sub-20 nm NaLuF(4)-based upconversion nanophosphors for high-contrast bioimaging in different animal species.

PubMed

Yang, Tianshe; Sun, Yun; Liu, Qian; Feng, Wei; Yang, Pengyuan; Li, Fuyou

2012-05-01

A new upconversion luminescence (UCL) nanophosphors based on host matrix of cubic NaLuF(4) with bright luminescence have been synthesized by a solvothermal method, facilitate the nanocrystals potential candidates for imaging in vivo, especially large-animals. The sub-20 nm NaLuF(4) co-doped Yb(3+) and Er(3+) (Tm(3+)) showed about 10-fold stronger UCL emission than that of corresponding hexagonal NaYF(4)-based nanocrystals with a 20 nm diameter. Near-infrared to near-infrared (NIR-to-NIR) UCL emission of PAA-coated NaLuF(4):20%Yb,1%Tm (PAA-Lu(Tm)) can penetrate >1.5 cm tissue of pork with high contrast. Based on super-strong UCL emission and deep penetration, PAA-Lu(Tm) as optical bioprobe has been demonstrated by in vivo UCL imaging of a normal black mouse, even rabbit with excellent signal-to-noise ratio. Furthermore, such cubic NaLuF(4)-based nanophosphor was applied in lymph node imaging of live Kunming mouse with rich white fur. Copyright © 2012 Elsevier Ltd. All rights reserved.

Selective sensing of two novel coordination polymers based on tris(4-carboxylphenyl)phosphine oxide for organic molecules and Fe3+ and Hg2+ ions

NASA Astrophysics Data System (ADS)

Huo, Liangqin; Zhang, Jie; Gao, Lingling; Wang, Xiaoqing; Fan, Liming; Fang, Kegong; Hu, Tuoping

2017-12-01

Two novel coordination polymers, formulated as {[Zn(HTPO)(bib)]·4H2O}n (1), {[Cu3(TPO)2 (bib)3]·2DMF·0.5EtOH·0.5H2O}n (2) (H3TPO = tris(4-carboxylphenyl)phosphine oxide; bib = 1,4-bis(1H-imidazol-4-yl) benzene), have been synthesized under solvothermal method and characterized by single-crystal X-ray diffraction, elemental analysis (EA), IR spectra, thermogravimetric (TG) analysis, powder X-ray diffraction (PXRD). Structural analysis reveals that complex 1 is a 2D 4-connected sheet with an intriguing 2D + 2D→2D network. Complex 2 displays a 3D 3,4-connected net with the point symbol of {103}2{106}3. Furthermore, the photoluminescence properties of 1 and 2 were investigated in the solid state and various solvent emulsions, the results show that 1 and 2 have better fluorescent recognition for organic molecules, Fe3+ and Hg2+ ions.

A silicon nanowire-reduced graphene oxide composite as a high-performance lithium ion battery anode material.

PubMed

Ren, Jian-Guo; Wang, Chundong; Wu, Qi-Hui; Liu, Xiang; Yang, Yang; He, Lifang; Zhang, Wenjun

2014-03-21

Toward the increasing demands of portable energy storage and electric vehicle applications, silicon has been emerging as a promising anode material for lithium-ion batteries (LIBs) owing to its high specific capacity. However, serious pulverization of bulk silicon during cycling limits its cycle life. Herein, we report a novel hierarchical Si nanowire (Si NW)-reduced graphene oxide (rGO) composite fabricated using a solvothermal method followed by a chemical vapor deposition process. In the composite, the uniform-sized [111]-oriented Si NWs are well dispersed on the rGO surface and in between rGO sheets. The flexible rGO enables us to maintain the structural integrity and to provide a continuous conductive network of the electrode, which results in over 100 cycles serving as an anode in half cells at a high lithium storage capacity of 2300 mA h g(-1). Due to its [111] growth direction and the large contact area with rGO, the Si NWs in the composite show substantially enhanced reaction kinetics compared with other Si NWs or Si particles.

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.