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At least 523 records · Page 29
All sourcesNASA NTRSDOE OSTI
DOE OSTI2015

Hydrothermal synthesis of zinc(II)-phosphonate coordination polymers with different dimensionality (0D, 2D, 3D) and dimensionality change in the solid phase (0D→3D) induced by temperature

Three new zinc(II) coordination polymers, [Zn(HO{sub 3}PCH{sub 2}CH{sub 2}COO)(C{sub 12}H{sub 8}N{sub 2})(H{sub 2}O)] (1), [Zn{sub 3}(O{sub 3}PCH{sub 2}CH{sub 2}COO){sub 2}(C{sub 12}H{sub 8}N{sub 2})](H{sub 2}O){sub 3.40} (2) and [Zn{sub 5}(HO{sub 3}PCH{sub 2}CH{sub 2}COO){sub 2}(O{sub 3}PCH{sub 2}CH{sub 2}COO){sub 2}(C{sub 12}H{sub 8}N{sub 2}){sub 4}](H{sub 2}O){sub 0.32} (3), with different structural dimensionality (0D, 2D and 3D, respectively) have been prepared by hydrothermal synthesis, and their structures were determined by single-crystal X-ray diffraction. Compound 1 crystallizes in the monoclinic system (P2{sub 1}/c) forming discrete dimeric units bonded through H-bonds, while compounds 2 and 3 crystallize in the triclinic (P−1) and the monoclinic (C2/c) systems, respectively. Compound 3, showing three different coordination numbers (4, 5 and 6) for the zinc atoms, has also been obtained by thermal treatment of 1 (probed by high-temperature XRPD experiments). The crystalline features of these compounds, related to the coordination environments for the zinc atoms in each structure, provoke the increase of the relative fluorescence for 2 and 3, compared to the free phenanthroline. Thermal analysis (TG and DSC) and XPS studies have been also carried out for all compounds. - Graphical abstract: Three new coordination compounds of zinc with 2-carboxyethylphosphonic acid (H{sub 2}PPA) and phenanthroline have been obtained by hydrothermal synthesis. The crystalline structure depends on the different coordination environments of the zinc atoms (see two comparative Zn{sub 6}-moieties). The influence of the different coordination modes of H{sub 2}PPA with the central atom in all structures have been studied, being found new coordination modes for this ligand. Several compounds show a significant increase in relative fluorescence with respect to the free phenanthroline. - Highlights: • Compounds have been obtained modifying the reaction time and the rate of reagents. • Dimensionality and crystalline structure is a function of the zinc environments. • New coordination modes for 2-carboxyethylphosphonic acid are reported. • 3D-compound presents three different coordination environments for the zinc atoms. • Fluorescence properties are related to the structural dimensionality.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2018

A facile pathway to prepare VO{sub 2} and V{sub 2}O{sub 3} powders via a carbothermal reduction process

The development of a highly efficient and low cost production process is instrumental for the wide application of VO{sub 2} and V{sub 2}O{sub 3}. In this paper, VO{sub 2} and V{sub 2}O{sub 3} powders are successfully prepared via carbothermal reduction of V{sub 2}O{sub 5} in a flowing Ar atmosphere at 973 K and 1423 K, respectively. Compared with the traditional methods, graphite is used as a reductant, which resulted in a low cost. The experimental results show that a high temperature assists in improving the kinetic rate. The phase transformation during the low-temperature reduction process between 948 K and 973 K occurs in the following sequential order: V{sub 2}O{sub 5}→V{sub 6}O{sub 13}→VO{sub 2}. When the temperature is 1423 K or 1473 K, the phase transformation can be described as follows: V{sub 2}O{sub 5}→V{sub 3}O{sub 5}→V{sub 2}O{sub 3}. Owing to the shrink of the volume, the as-prepared VO{sub 2} and V{sub 2}O{sub 3} particles could not maintain the original micro-morphology of V{sub 2}O{sub 5}. Relative to VO{sub 2}, the as-prepared V{sub 2}O{sub 3} particles are porous. It is also concluded that the V{sub 2}O{sub 3} can be easily oxidized to VO{sub 2}, when the partial pressure of O{sub 2} is in the range of 10{sup −8} atm to 10{sup −1} atm. Therefore, a reasonable reaction temperature and reaction time are important to prepare high purity V{sub 2}O{sub 3}.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2015

Preparation of the egg membrane bandage contained the antibacterial Ag nanoparticles

Silver nanoparticles were synthesized using a rapid, single step, and completely green biosynthetic method employing aqueous aloe leaf extracts as both the reducing and capping agent. Transmission electron microscopy analysis revealed the average size of silver nanoparticles approximately 18.05 nm. Fourier transform infrared spectroscopy observation showed the estimation of two kinds of binding sites between aqueous aloe leaf and aqueous aloe leaf with silver nanoparticles. In addition, the critical roles of the concentration of silver nitrate, temperature, and reaction time in the formation of silver nanoparticles had been illustrated. Furthermore, silver nanoparticles were deposited on egg membrane bandage, forming a new egg membrane bandage that contained silver nanoparticles that exhibiting excellent antibacterial effects against Gram-negative Escherichia coli and Gram-positive Staphylococcus aureus, which was 2.5 times stronger than the commercially available bandage. - Graphical Abstract: Display Omitted.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2015

One-pot pseudomorphic crystallization of mesoporous porous silica to hierarchical porous zeolites

Hierarchically porous silica with mesopore and zeolitic micropore was synthesized via pseudomorphic crystallization under high-temperature hydrothermal treatment in the presence of cetyltrimethylammonium tosylate and tetrapropylammonium ions. A combined characterization using small-angle X-ray diffraction (XRD), nitrogen adsorption, high-resolution transmission electron microscopy (TEM), thermogravimetric analysis (TG), and elemental analysis showed that dual templates, CTA{sup +} and TPA{sup +} molecules, can work in a cooperative manner to synthesize mesoporous zeolite in a one-pot system by precisely tuning the reaction conditions, such as reaction time and temperature, and type and amount of heterometal atoms. It is found that the presence of Ti precursor is critical to the successful synthesis of such nanostructure. It not only retards the nucleation and growth of crystalline MFI domains, but also acts as nano-binder or nano-glue to favor the assembly of zeolite nanoblocks. - Graphical abstract: Display Omitted - Highlights: • A facile method to synthesize mesoporous zeolites with hierarchical porosity was presented. • It gives a new insight into keeping the balance between mesoscopic and molecular ordering in hierarchical porous materials. • A new understanding on the solid–solid transformation mechanism for the synthesis of titanosilicate zeolites was proposed.

36 MATERIALS SCIENCE↗
DOE OSTI2017

The significance of intermetallic compounds formed during interdiffusion in aluminum and magnesium dissimilar welds

Diffusion couples between Al-AA6111 and Mg-AZ31 have been used to perform a comprehensive review of the IMC phases that develop in this system, including; their growth kinetics, texture, residual stresses, and mechanical properties. The new observations made have been compared to data in the literature with the aim of providing an in-depth understanding of the detrimental effects of interfacial reaction in aluminum–magnesium dissimilar welding. Three Al–Mg binary IMC phases were identified, γ-Al{sub 12}Mg{sub 17} and β-Al{sub 3}Mg{sub 2}, as well as ε-Al{sub 30}Mg{sub 23}, which has not been previously reported in inter-diffusion studies. The β phase had the highest growth rate and became the dominant constituent of the IMC layer at longer reaction times. The ε-phase only appeared after extended heat treatment, via transformation at the Al{sub 12}Mg{sub 17}/Al{sub 3}Mg{sub 2} interface. Intrinsic diffusion coefficients of Al and Mg, calculated in the Al{sub 3}Mg{sub 2} phase, confirmed that Al is the faster diffusing species (by an order of magnitude) during IMC growth. Indentation techniques showed that all the IMC phases had extremely low toughness (1/2 ). FIB-assisted ring core milling revealed that both the β-Al{sub 3}Mg{sub 2} and γ-Al{sub 12}Mg{sub 17} phases contained large residual stresses. Their in-situ fracture toughness was consequently found to be asymmetric with lower values parallel to the joint interface. Greater tensile residual stress was measured in the β-Al{sub 3}Mg{sub 2} phase, which, combined with a lower toughness and more rapid growth kinetics, explains why it is generally the ‘weak link’ in Al–Mg dissimilar joints.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Preparation of cobalt ferrite nanoparticles via a novel solvothermal approach using divalent iron salt as precursors

Graphical abstract: CoFe{sub 2}O{sub 4} nanoparticles are obtained via solvothermal approach using Fe{sup 2+} salt as iron resource. The magnetic properties can be modified by some additives. Display Omitted Highlights: ► CoFe{sub 2}O{sub 4} nanoparticles are synthesized by a facile one-step novel solvothermal method. ► The system is firstly performed in water–glycol mixture solvent with an ordinary air surrounding. ► The ferrous ions are used as iron source without adding oxidant. ► It is firstly found the low-coercivity CoFe{sub 2}O{sub 4} nanoparticles can be obtained with the help of some additives in the synthesis system. -- Abstract: Cobalt ferrite (CoFe{sub 2}O{sub 4}) nanoparticles are synthesized by a facile novel solvothermal method. The reactions are firstly performed in water–glycol system and Fe{sup 2+} salt is used as iron source without oxidant help. Some factors influenced the reactions, including temperature, reaction time, additives, are investigated. The samples are characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), and scanning electron microscopy (SEM), respectively. The magnetic properties of some samples are detected by vibrating sample magnetometry techniques (VSM). It is firstly found that the magnetism of cobalt ferrites nanomaterials can be modified by some additives. The coercivity of CoFe{sub 2}O{sub 4} nanoparticles evidently decreases from 600 to 50 Oe in the presence of PEG-4000 in the system.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Green synthesis of silver nanoparticles from aqueous Aegle marmelos leaf extract

Graphical abstract: Silver nanoparticles capped with polyphenols present in Aegle marmelos leaf extract. Display Omitted Highlights: ► Silver nanoparticles are synthesized using Aegle marmelos leaf extract in aqueous media. ► Reduction reaction is fast and occurs at room temperature. ► The presence of polyphenols acts as in situ capping agent. -- Abstract: Synthesis of nanoparticles by green route is an emerging technique drawing more attention recently because of several advantages over the convention chemical routes. The present study reports one-pot synthesis and in situ stabilization of silver nanoparticles using Aegle marmelos leaf extract. Nanoparticles of almost uniform spherical size (∼60 nm) were synthesized within ∼25 min reaction time at room temperature. The size of particles depends on the ratio of AgNO{sub 3} and leaf extract. The crystallinity, size, and shape of the nanoparticles were characterized by X-ray diffraction, dynamic light scattering, and scanning electron microscopy respectively. The size stability was attained by the capping effect of polyphenolic tannin compound, procatacheuate in the extract. The capped polyphenols can be removed from the particle surface by simple NaOH/methanol wash. The involvement of phenolic compounds in metal ion reduction and capping were supported by UV–visible spectroscopy, infrared spectroscopy, high performance liquid chromatography, and zeta potential measurements.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2013

Synthesis and characterization of mixed phases in the Ca–Co–O system using the Pechini method

Highlights: ► We have prepared mixed Ca–Co–O phases using the Pechini method. ► Reaction times are reduced relative to conventional solid-state synthesis. ► Products have high surface area suitable for ceramic processing. ► Product composition is dictated by both kinetic and thermodynamic control. ► A revised phase diagram of the Ca–Co–O system is proposed. - Abstract: The synthesis of mixed phases in the Ca–Co–O system using the Pechini method was investigated. The phases CaCo{sub 2}O{sub 4}, Ca{sub 3}Co{sub 4}O{sub 9} and Ca{sub 3}Co{sub 2}O{sub 6}, which can be expressed in terms of the molar ratios of the binary oxides (CaO:Co{sub 2}O{sub 3}) as (1:1), (3:2) and (3:1) respectively, were obtained in pure form. Powder X-ray diffraction data showed they are comparable with materials obtained by conventional solid-state synthesis. The mild synthesis conditions of the Pechini method allowed the evolution of the Ca–Co–O phases to be studied as a function of temperature and heating time. Both variables have a strong influence on the composition of the products, indicating that both kinetic and thermodynamic factors play a role, with the former being of more importance at lower temperatures. The (1:1) phase, previously not identified in the phase diagram of the Ca–Co–O system, was obtained preferentially across the composition range below ca. 650 °C. The (3:2) phase was preferred until ca. 800 °C. At even higher temperatures, the (3:1) phase is obtained. The upper thermal stability limit of mixed phases in the Ca–Co–O system increases with the Ca:Co ratio. An updated phase diagram for the Ca–Co–O system is proposed.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Transfer of microstructure pattern of CNTs onto flexible substrate using hot press technique for sensing applications

Graphical abstract: - Highlights: • Successfully transfer of microstructure patterned CNTs on PET substrate. • Demonstrate as resistor-based NH{sub 3} gas sensor in the sub-ppm range. • Excellent photodetector having instantaneous response and recovery characteristics. • An effective technique to grow and produce flexible electronic device. - Abstract: In this work, we report the successful and efficient transfer process of two- dimensional (2-D) vertically aligned carbon nanotubes (CNTs) onto polyethylene terephthalate (PET) substrate by hot pressing method with an aim to develop flexible sensor devices. Carbon nanotubes are synthesized by cold wall thermal chemical vapor deposition using patterned SiO{sub 2} substrate under low pressure. The height of the pattern of CNTs is controlled by reaction time. The entire growth and transfer process is carried out within 30 min. Strong adhesion between the nanotube and polyethylene terephthalate substrate was observed in the post-transferred case. Raman spectroscopy and scanning electron microscope (SEM) studies are used to analyze the microstructure of carbon nanotube film before and after hot pressing. This technique shows great potential for the fabrication of flexible sensing devices. We report for the first time, the application of patterned microstructure developed by this technique in the development of gas sensor and optoelectronic device. Surface resistive mode is used for detection of ammonia (NH{sub 3}) gas in the sub-ppm range. An impressive photoconducting response is also observed in the visible wavelength. The reproducibility of the sample was checked and the results indicate the possibility of use of carbon nanotube as gas sensor, photodetector, CCDs etc.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Controllable synthesis, shape evolution, and luminescence properties of uniform and well-dispersed NaEuF{sub 4} microcrystals through hydrothermal route

Graphical abstract: Sodium europium fluorides NaEuF{sub 4} microcrystals have been prepared via a facile hydrothermal route. The possible growth mechanism and the luminescent properties of the as-prepared microcrystals have been discussed. - Highlights: • Sodium europium fluorides NaEuF{sub 4} microspheres were prepared by a facile hydrothermal route. • The as-prepared samples NaEuF{sub 4} and EuF{sub 3} exhibit respective red or orange-red emissions. • These finding may find potential applications in the fields of color display, UV laser and biomedicine. - Abstract: Sodium europium fluorides NaEuF{sub 4} microcrystals with uniform and well-dispersed shapes and dimensions have been prepared via a facile hydrothermal route using Na{sub 3}Cit as the chelating ligand and shape modifier. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), selected-area electron diffraction (SAED), energy-dispersive X-ray (EDX) and photoluminescence spectra (PL) were taken to characterize the samples. A series of controlled experiments reveal that the trisodium citrate (Na{sub 3}Cit) content, pH value of the initial solution, and reaction time have an indispensable role on the phase, size, and morphology of the as-prepared microcrystals. Based on the experimental results, the possible growth mechanism of the microcrystals prepared under different conditions was proposed. Moreover, we systematically investigated the luminescent properties of the as-prepared microcrystals with different morphologies obtained under different amounts of Na{sub 3}Cit, which have potential application in the fields of color display, UV laser and biomedicine.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Oxygen vacancy and Ce{sup 3+} ion dependent magnetism of monocrystal CeO{sub 2} nanopoles synthesized by a facile hydrothermal method

Graphical abstract: - Highlights: • Monocrystal CeO{sub 2} nanopoles are synthesized by hydrothermal method. • Suitable reaction time is beneficial for the growth CeO{sub 2} nanopoles. • As-synthesized CeO{sub 2} nanopoles show excellent RTFM. • The RTFM can be attributed to the influences of oxygen vacancies and Ce{sup 3+} ions. - Abstract: Monocrystal CeO{sub 2} nanopoles of 15–25 nm in diameter and 300–900 nm or more in length were synthesized within 100 h using hydrothermal method with CeCl{sub 3}·7H{sub 2}O as cerium source, NaOH as mineralizer, and ethylenediamine as complexant. The results of XRD and SADE analysis indicate that the as-synthesized CeO{sub 2} samples have the fluorite structure. The band gaps of CeO{sub 2} samples are 0.08–0.38 eV smaller than that of bulk CeO{sub 2}. X-ray photoelectron spectroscopy shows that the concentration of Ce{sup 3+} is higher than 20% for CeO{sub 2} samples. All the as-synthesized CeO{sub 2} samples exhibit the room temperature ferromagnetism (RTFM), and the saturation magnetization (M{sub s}) gradually increases with the increase of E{sub g} up to 2.92 eV and then decreases with E{sub g} increasing more. The highest M{sub s} of 0.167 emu/g is obtained from the CeO{sub 2} nanopoles synthesized within 100 h. The RTFM mechanism of CeO{sub 2} nanopoles has been proposed which can be mainly attributed to the influence of oxygen vacancies and Ce{sup 3+} ions.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Synthesis of the p-type semiconducting ternary oxide CuAlO{sub 2} using the Pechini method

Graphical abstract: - Highlights: • We have prepared single-phase samples of the semiconducting oxide CuAlO{sub 2} using the Pechini method. • Reaction times are reduced relative to conventional solid-state synthesis. • Products have high surface area suitable for ceramic processing. • Product composition is dictated by thermodynamic control; CuAl{sub 2}O{sub 4} is obtained preferentially at lower temperature. - Abstract: The synthesis of the delafossite phase CuAlO{sub 2} using the Pechini method was investigated. Powder X-ray diffraction data showed that pure, single-phase samples were obtained after only 3 h heating at 1100 °C. CuAl{sub 2}O{sub 4}, which contains Cu(II) rather than Cu(I), was the dominant phase between 700 and 1100 °C. Conversion to CuAlO{sub 2} is promoted by the positive entropy change associated with the evolution of oxygen. No mixed Cu–Al oxide was formed below 700 °C.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Sonochemical and hydrothermal synthesis of PbTe nanostructures with the aid of a novel capping agent

Graphical abstract: - Highlights: • PbTe nanostructures were prepared with the aid of Schiff-base compound. • Sonochemical and hydrothermal methods were employed to fabricate PbTe nanostrucrues. • The effect of preparation parameters on the morphology of PbTe was investigated. - Abstract: In this work, a new Schiff-base compound derived from 1,8-diamino-3,6-dioxaoctane and 2-hydroxy-1-naphthaldehyde marked as (2-HyNa)-(DaDo) was synthesized, characterized, and then used as capping agent for the preparation of PbTe nanostructures. To fabricate PbTe nanostructures, two different synthesis methods; hydrothermal and sonochemical routes, were applied. To further investigate, the effect of preparation parameters like reaction time and temperature in hydrothermal synthesis and sonication time in the presence of ultrasound irradiation on the morphology and purity of the final products was tested. The products were analyzed with the aid of SEM, TEM, XRD, FT-IR, and EDS. Based on the obtained results, it was found that pure cubic phased PbTe nanostructures have been obtained by hydrothermal and sonochemical approaches. Besides, SEM images showed that cubic-like and rod-like PbTe nanostructures have been formed by hydrothermal and sonochemical methods, respectively. Sonochemical synthesis of PbTe nanostructures was favorable, because the synthesis time of sonochemical method was shorter than that of hydrothermal method.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Hydrothermal synthesis and magnetic properties of CuO hollow microspheres

Graphical abstract: - Highlights: • CuO hollow microspheres were synthesized through hydrothermal route. • The possible growth mechanism was proposed according to the experimental results. • CuO hollow microspheres show an anomalous ferromagnetic behavior at 5 K and 300 K. - Abstract: In the present work, CuO hollow microspheres with the diameter about 2 μm were successfully synthesized through a facile hydrothermal method. The phase purity, morphologies and structure features of the as obtained products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and Raman spectroscopy, respectively. It was found that reaction temperature, reaction time and different volume ratios of ethanol and distilled water played important roles on the morphologies of the obtained CuO hollow microspheres. The possible formation mechanism was also proposed according to the corresponding experimental results. The magnetic properties were investigated by superconducting quantum interference device, revealing that the CuO hollow microspheres exhibited an anomalous ferromagnetic behavior at 5 K and 300 K. At the same time, the origin of the ferromagnetism in CuO hollow microspheres was also discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Effects of growth parameters on the yield and morphology of Si{sub 3}N{sub 4} microcoils prepared by chemical vapor deposition

Highlights: • CVD method was successfully applied to obtain Si{sub 3}N{sub 4} microcoils in high yield without the presence of catalyst. • The process was systematically investigated through a series of control experiments. • The effects of synthesis parameters on the yield and morphology of Si{sub 3}N{sub 4} microcoils were found. • The growth mechanism of the Si{sub 3}N{sub 4} microcoils could be explained by the different growth rates between the amorphous layer and the crystalline layer. - Abstract: In this study, we provided a reliable chemical vapor deposition (CVD) method to synthesize high-purity Si{sub 3}N{sub 4} microcoils in high yield without the presence of catalyst. The achieved products were characterized by X-ray diffraction, scanning electron microscopy, and transmission electron microscope. The results indicated that the yield and morphology of Si{sub 3}N{sub 4} products were influenced by the synthesis parameters such as reaction temperature, reaction time and gas flow rate. The particular conditions favorable to high yield synthesis of Si{sub 3}N{sub 4} microcoils were obtained through a series of control experiments. Furthermore, the growth of Si{sub 3}N{sub 4} microcoils was supposed to be in accord with vapor-solid (VS) growth process and the different growth rates between the amorphous layer and the crystalline layer were used to explain the formation of the coil geometry.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Photocatalytic reduction of aqueous mercury(II) using multi-walled carbon nanotubes/Pd-ZnO nanocomposite

Highlights: • MWCNT/Pd-ZnO were used for photocatalytic reduction of Hg{sup 2+}. • Photocatalytic reduction of Hg{sup 2+} was dependent on wt% of MWCNT, reaction time, and weight of catalyst. • Catalyst re-use revealed the present photocatalyst remain effective and active after five, cycles. - Abstract: Pd-ZnO nanocatalyst supported on multi-walled carbon nanotubes was successfully synthesized via a modified sol–gel method, and the prepared photocatalyst was used for the environmental remediation of aqueous Hg(II) via photocatalytic reduction under visible light. The prepared MWCNTs/Pd/ZnO nanocomposite photocatalyst was characterized using X-ray diffraction, Brunauer–Emmett–Teller (BET), transmission electron microscopy, and UV–vis spectra (UV–vis). The results showed that both Pd and ZnO nanoparticles were well dispersed over the MWCNTs, and a uniform nanocomposite was formed. The results also illustrated that Pd doping can eliminate the recombination of electron-hole pairs in the catalyst, and the presence of MWCNTs in ZnO composite can change surface properties to achieve sensitivity to visible light. The results demonstrated that optimum mass ratio of CNT:ZnO:Pd were 0.04:1.0:0.08, which resulted in the exceptional performance of the photocatalyst to reduce about 100% of Hg(II) in a 100 mg L solution within 30 min.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Large-scale synthesis of hierarchical-structured weissite (Cu{sub 2−x}Te) flake arrays and their catalytic properties

Graphical abstract: - Highlights: • Large-scale Cu{sub 2−x}Te flake arrays grown on copper foam were synthesized. • They possess superior catalytic efficiency on methylene blue with the assistance of H{sub 2}O{sub 2}. • The effects of preparing conditions on the growth of Cu{sub 2−x}Te flake arrays were investigated. - Abstract: Large-scale weissite (Cu{sub 2−x}Te) flake arrays with three-dimensional (3D) hierarchical structure have been successfully fabricated via a facile one-step solution-phase strategy through the reaction of tellurium powder and copper foam. At the end of the reaction Cu{sub 2−x}Te flakes were distributed evenly on the surface of a porous solid copper substrate. Field-emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM) analysis showed the abundance of flakes grown on the 3D porous copper architecture, while X-ray diffraction (XRD) and energy-dispersive X-ray spectra (EDS) were used to determine the crystal structure and phase composition of these products. A series of experiments discovered that the size and morphology of the products could be affected by some reactive parameters including the reaction time, synthesis temperature and volume ratio of absolute ethanol/deionized water. Catalysis experiments using the in situ synthesized of Cu{sub 2−x}Te flakes to catalyze the degradation of methylene blue (MB) demonstrated the strong catalytic ability of these flakes.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Rod-like nanocrystalline B-VO{sub 2}: Hydrothermal synthesis, characterization and electrochemical properties

Graphical abstract: - Highlights: • Rod-like nanocrystalline VO{sub 2}(B) was prepared by hydrothermal process. • Reaction time on the morphology has been investigated. • CV has revealed reversible redox behavior with charge–discharge cycling. • Average coulombic efficiency is upper 98%. • Energy-related applications such as cathodes in lithium batteries. - Abstract: Rod-like nanocrystalline VO{sub 2}(B) has been successfully synthesized via a simple hydrothermal process by using V{sub 2}O{sub 5} as vanadium source and 4-butylaniline H{sub 3}C–(CH{sub 2}){sub 3}–(C{sub 6}H{sub 4})–HH{sub 2} as reducing and structure directing agent. The compounds were analyzed through X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy and UV–visible spectroscopy. The VO{sub 2}(B) nanorods are up to several micrometers in length and about 80 nm in thickness with a large optical band gap of ∼2.709 eV. Thin films of VO{sub 2}(B) nanorods deposited on ITO substrates were electrochemically characterized by cyclic voltammetry. The voltammograms show reversible redox behavior with charge–discharge cycling process corresponding to the reversible lithium intercalation/deintercalation into the crystal lattice. The average coulombic efficiency to this redox processes is upper 98% during the electrochemistry measurements.

36 MATERIALS SCIENCE↗