石墨烯固体酸催化转化葡萄糖为化学品

利用氢化钠和丙磺酸内酯合成出了磺化石墨烯催化剂,采用XPS、FT-IR、TEM等方法对其进行了表征,并且对此催化剂催化葡萄糖的转化反应进行了研究．探究此催化剂在纯水中、没有添加任何有机溶剂下催化转化葡萄糖制备高附加值化学品方面的催化活性,在最优的反应条件下, 5-羟甲基糠醛(HMF)最高产率可达28.8%,产物甲酸、乳酸和HMF的总产率可达51.94%．经过5次催化反应,催化剂仍表现出相对高的催化活性,三种产物的产率依然较高,表明此种固体酸催化剂有很好的热稳定性．     

Green synthesis of biocompatiable chitosan–graphene oxide hybrid nanosheet by ultrasonication method

Ultrasound-induced synthesis of chitosan-modified nano-scale graphene oxide (CS-NGO) hybrid nanosheets, which has great potential pharmaceutical applications, in supercritical CO₂ without catalyst was presented for the first time. The preparation process does not require organic solvent and post-processing, and CO₂ easily escapes from the product. The morphology and structure of the CS-NGO, characterized using scanning electron microscopy, transmission electron microscopy, infrared spectroscopy, X-ray photoelectron spectroscopy and thermogravimetric analysis, confirms that it was combined via the amide linkage, and had excellent dispersibility and stability toward acidic and physiological aqueous solution, which implies that it could be used as a drug-carrier. The sonication power played a crucial role in inducing forming amidation, and the conversion rate increased with the sonication time. The mechanism of this reaction was explained.     

Decorating reduced graphene oxide with Co3O4 hollow spheres and their application in supercapacitor materials

In this paper, a composite of reduced graphene oxide decorated by Co₃O₄ hollow spheres (Co₃O₄/RGO composite) has been synthesized by a one-pot solvothermal method. The samples are characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), and Fourier transform infrared spectroscopy (FT-IR), Raman spectra and so on. The results demonstrate that the Co₃O₄ hollow spheres with good purity and homogenous size are absorbed onto the reduced graphene oxide sheets as spacers to prevent the aggregation of the graphene oxide sheets. Furthermore, the well electrochemical properties demonstrate that the Co₃O₄/RGO composite might have potential applications as electrode materials for supercapacitors.     

One-step simple sonochemical fabrication and photocatalytic properties of Cu2O–rGO composites

An easy, one-step synthesis of Cu₂O–reduced graphene composites (Cu₂O–rGO) was developed using a simple sonochemical route without any surfactants or templates. The morphology and structure of the Cu₂O–rGO composites were characterised using techniques such as scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, Raman spectroscopy and X-ray photoelectron spectroscopy (XPS). The results indicated that the Cu₂O sphere is approximately 200 nm in diameter and composed of small Cu₂O particles approximately 20 nm in diameter. The morphology and composition of the Cu₂O–rGO composites could be well controlled by simply changing the mole ratio of the reactants under ultrasonic irradiation. The Cu₂O–rGO composites displayed better photocatalytic performance for the degradation of methyl orange (MO) than pure Cu₂O spheres, which may have potential applications in water treatment, sensors, and energy storage.     

Ultrasound assisted synthesis of Sn nanoparticles-stabilized reduced graphene oxide nanodiscs

Sn nanoparticles-stabilized reduced graphene oxide (RGO) nanodiscs were synthesized by a sonochemical method using SnCl₂ and graphene oxide (GO) nanosheets as precursors in a polyol medium. TEM and XPS were used to characterize the Sn-stabilized RGO nanodiscs.     

Cobalt terephthalate MOF-templated synthesis of porous nano-crystalline Co3O4 by the new indirect solid state thermolysis as cathode material of asymmetric supercapacitor

In this work, two different types of Co₃O₄ nano-crystals were synthesized by (i) conventional direct solid state thermolysis of cobalt terephthalate metal-organic framework (MOF-71) and (ii) new indirect solid state thermolysis of Co(OH)₂ derived by alkaline aqueous treatment of MOF-71. The products were then characterized by X-ray diffraction technique (XRD), Fourier transforms infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), Reflection electron energy loss spectroscopy (REELS), Brunauer, Emmett, and Teller (BET), scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDX) techniques. By REELS analysis the energy band gap of MOF-71 was determined to be 3.7 eV. Further, electrochemical performance of each Co₃O₄ nanostructure was studied by the cyclic voltammetry (CV), galvanostatic charge-discharge (GCD), and electrochemical impedance spectroscopy (EIS) in a three-electrode system in KOH electrolyte. An asymmetric supercapacitor was fabricated using indirect Co₃O₄ nanoparticles as cathode and electrochemically reduced graphene oxide as anode, and the electrochemical properties were studied and showed a high energy density of 13.51 Wh kg⁻¹ along with a power density of 9775 W kg⁻¹ and good cycling stability with capacitance retention rate of 85% after 2000 cycles.     

Application of ultrasound to the synthesis of a new nanostructured Mn(II) supramolecular compound: A precursor for γ-Mn2O3 nanoparticles

A new nanostructured Mn(II) supramolecular compound [Mn(hpydcH₂)₂(H₂O)₄] (1) (hpydcH₃ = 4-hydroxy-2,6-pyridinedicarboxylic acid) has been synthesized using a sonochemical process. The structure of compound 1 was determined by single crystal X-ray diffraction and it was revealed that each hpydcH₂⁻ anionic ligand has been coordinated to Mn(II) ion in a novel monodentate fashion leaving another functional carboxylic acid group intact. Compound 1 was also characterized by scanning electron microscopy (SEM), X-ray powder diffraction (XRPD), FT-IR spectroscopy and elemental analysis. Thermal stability of compound 1 was studied by thermal gravimetric (TG) analysis and compared to that of its crystalline analogue. Subsequently, the role of concentration of the initial reactants on the size of nanostructures of compound 1, has been investigated. Compound 1 was proved to be a precursor for γ-Mn₂O₃ nanoparticles.     

Structural and magnetic properties of reduced graphene oxide-TiO2 nanoflower composite

We have focused on the structural and magnetic properties of hazardous acid free synthesis of anatase titanium dioxide (TiO₂) phase nanoflower and reduced graphene oxide-TiO₂ (rGO-TiO₂) nanocomposite using hydrothermal process. Because, strong acids free synthesis is environmental friendly and reduce overall cost of synthesized samples. In the synthesis of rGO-TiO₂, synthesized TiO₂ nanoflower and graphene oxide (GO) were used as reagents. The resulting materials have analyzed using different techniques such as, X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Raman spectroscopy and Fourier Transformation Infrared spectrophotometer for confirmation of flower like morphology, crystalline phase and chemical composition. Moreover, VSM analysis has revealed the ferromagnetism induced in the rGO-TiO₂ composite at room temperature. The values of saturation magnetization were found to be 0.002 and ~ 0.243±0.04 emu/g for TiO₂ nanoflower and rGO-TiO₂ nanocomposite, respectively. In comparison of pure TiO₂, rGO-TiO₂ exhibited larger magnetization at room temperature. This is because presences of various edge and site defects such as topological and point defects like vacancies, which create localized unpaired spins in reduced graphene oxide (rGO), induce the ferromagnetism behavior in rGO-TiO₂ nanocomposite.     

BaMnO3 nanostructures: Simple ultrasonic fabrication and novel catalytic agent toward oxygen evolution of water splitting reaction

In the current paper, the main aim is to fabricate the BaMnO₃ nanostructures via the sonochemical route. The various factor, including precursors, reaction time and power of sonication can affect the shape, size, and purity of the samples. We utilized X-ray diffraction (XRD), scanning electron microscope (SEM), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR), and X-ray energy dispersive spectroscopy (EDS) to characterize the BaMnO₃ nanostructures. The optical property of BaMnO₃ nanostructures was explored by Ultraviolet–visible spectroscopy (UV–vis) and the energy gap was suitable for catalytic activity (about 2.75 eV). Changing the precursor can affect the size, nanoparticle shape, architectures, and uniformity of the samples. We employed the BaMnO₃ nanostructures for O₂ evolution reaction as catalysts. It can observe that increasing the homogeneity of the catalysts can increase the efficiency of the Oxygen evolution reaction. The maximum amount of the O₂ evolution and the highest TOF and TON are related to nanoplate disc using barium salicylate as a precursor of barium. As a result, we can nominate the BaMnO₃ nanostructures as an effective and novel catalyst for water-splitting reaction.     

Graphene nanosheets: Ultrasound assisted synthesis and characterization

A facile sonochemical route for the synthesis of graphene nanosheets via reduction of graphene oxide (GO) has been reported. The synthesized graphene sheets are characterized using UV–vis spectra, Fourier transform infra-red (FT-IR) spectra, transmission electron microscope, X-ray photoelectron spectra (XPS) and Raman spectroscopic techniques. The UV–vis spectroscopy results showed that the absorption peak was red shifted due to the reduction of GO into graphene. FT-IR and XPS spectra revealed the removal of oxygenated functional groups in graphene after the reduction process. Raman spectra confirmed the restoration of new sp² carbon domains in graphene sheets after the reduction. The sonochemical approach for the synthesis of graphene nanosheets is relatively fast, cost-effective and efficient as compared to other methods.     

siRNA-loaded PEGylated porous silicon nanoparticles for lung cancer therapy

The BiPO₄/reduced graphene oxide (RGO) nanocomposites were prepared by a facile solvothermal approach. The prepared samples were characterized with Fourier transform infrared spectroscopy, X-ray diffraction, scanning electron microscopy, transmission electron microscopy, UV–vis diffuse reflectance spectroscopy, electrochemical impedance spectra, and Mott–Schottky and the photoluminescence spectra. A large quantity of BiPO₄ nanoparticles with sizes of ca. 150 nm were well dispersed on the RGO nanosheets. The absorbance of the BiPO₄/RGO nanocomposites is largely enhanced in the range of 400–800 nm compared with that of BiPO₄, and the BiPO₄/RGO showed better photocatalytic activities under simulated sunlight irradiation than the BiPO₄ nanocrystals.     

Sonochemical synthesis of a novel nanoscale 1D lead(II) [Pb2(L)2(I)4]n coordination Polymer,survey of temperature,reaction time parameters

One new lead(II) coordination supramolecular complex (CSC) (1D), [Pb₂(L)₂(I)₄]_n, L = C₄H₆N₂ (1-methyl imidazole), has been synthesized under different experimental conditions. Micrometric crystals (bulk) or nano-sized materials have been obtained depending on using the branch tube method or sonochemical irradiation. All materials have been characterized by scanning electron microscopy (SEM), powder X-ray diffraction (PXRD) and FT-IR spectroscopy. Single crystal X-ray analyses on complex 1 showed that Pb²⁺ ion is 4-coordinated. Topological analysis shows that the complex 1 is 2,3,5C2 net. Finally, the role of reaction time and temperature on the growth and final morphology of the structures obtained by sonochemical irradiation have been studied.     

Sonication-assisted synthesis of a new cationic zinc nitrate complex with a tetradentate Schiff base ligand: Crystal structure,Hirshfeld surface analysis and investigation of different parameters influence on morphological properties

A nanostructured cationic zinc nitrate complex with a formula of [ZnLNO₃]NO₃ (where L = (N²E,N^2′E)-N¹,N^1′-(ethane-1,2-diyl)bis(N²-((E)-3-phenylallylidene)ethane-1,2-diamine)) was prepared by sonochemical process and characterized by single crystal X-ray crystallography, scanning electron microscopy (SEM), FT-IR and NMR spectroscopy and X-ray powder diffraction (XRPD). The X-ray analysis demonstrates the formation of a cationic complex that metal center is five-coordinated by four nitrogen atom from Schiff base ligand and one oxygen atom from nitrate group. The crystal packing analysis demonstrates the essential role of the nitrate groups in the organization of supramolecular structure. The morphology and size of ultrasound-assisted synthesized zinc nitrate complex have been investigated using scanning electron microscopy (SEM) by changing parameters such as the concentration of initial reactants, the sonication power and reaction temperature. In addition the calcination of zinc nitrate complex in air atmosphere led to production of zinc oxide nanoparticles.     

Photocatalytic degradation of phenol over novel rod shaped Graphene@BiPO4 nanocomposite

Graphene@BiPO₄ nanocomposite with unique rod shape morphology of BiPO₄ has been successfully fabricated by the simple microwave assisted hydrothermal method. The crucial role of graphene oxide in the growth of rod shaped BiPO₄ crystals has been attempted to explain in this article. Graphene oxide acts as a structure-directing and morphology-controlling agent in the nucleation and growth of nanocrystals. The as prepared organic–inorganic hybrid Graphene@BiPO₄ nanocomposite photocatalyst was characterized by various techniques i.e. X-ray diffraction, scanning electron microscopy, UV–vis diffuse reflectance spectroscopy, Raman spectroscopy and photoluminescence (PL) spectroscopy. The results were promising and shown enhanced photocatalytic activity than pure BiPO₄ for phenol degradation. The effect of graphene loading on the rates of photocatalytic degradation of phenol in solution is investigated. The result shows that the optimum photocatalytic activity of Graphene@BiPO₄ composite at 5 wt% of graphene under visible light is almost three times higher than pure BiPO₄.     

Enhanced protein loading on a planar Si(111)–H surface with second generation NTA

A Si(111)–H surface was modified via a direct reaction between Si–H and 1-undecylenic acid (UA) under microwave irradiation to form molecular monolayers with terminal carboxyl groups. After esterifying carboxylic acid being esterified with N-hydroxysuccinimide (NHS), aminobutyl nitrilotriacetic acid (ANTA) was bound to the silicon surface through amidation (pH = 8.0) between its primary amino group and NHS-ester, producing nitrilotriacetic acid (NTA) anions. Then hexa-histidine tagged thioredoxin–urodilatin (his-tagged protein) and FITC-labeled hexa-histidine tagged thioredoxin–urodilatin (FITC-his-tagged protein) can be anchored after NTA was coordinated with Ni²⁺. Furthermore, the NTA-terminated chip was acidified with 0.1 M HCl and subsequently esterified with NHS and then amidated with ANTA again to produce a second generation NTA. Thus the surface density of nitrilotriacetic acid anions was improved and resultantly that of anchored proteins was also enhanced through the iterative reactions. Both multiple transmission-reflection infrared spectroscopy (MTR-IR) and fluorescence scanning measurements demonstrated a proximate 1.63 times of anchored proteins on the second generation NTA/Ni²⁺ as that on the first generation NTA/Ni²⁺ monolayer.     

Synthesis and characterization of a new nano lead(II) 0-D coordination supramolecular compound: A precursor to produce pure phase nano-sized lead(II) oxide

Nano-structure of a new 0D Pb(II) coordination supramolecular compound, [Pb₄(8-Quin)₆](ClO₄)₂(1), L = 8-HQuin = 8-hydroxyquinolin ligand has been synthesized by use of a sonochemical process and characterized by scanning electron microscopy (SEM), X-ray powder diffraction (XRPD), Fourier transform infrared spectroscopy (FTIR) and elemental analyses. The structure of compound 1 was determined by single-crystal X-ray diffraction. The single crystal X-ray data of compound 1 implies that the Pb⁺² ions are five coordinated. Each lead atom is coordinated to nitrogen and oxygen atoms of 8-hydroxyquinolin ligand. Topological analysis shows that the compound 1 is 1,2,3,4,4M12-1net. Nanoparticles of lead(II) oxide have been prepared by calcination of lead(II) coordination polymer at 500 °C that were characterized by scanning electron microscopy (SEM), X-ray powder diffraction (XRPD) and IR spectroscopy.     

A high-voltage lithium-ion battery prepared using a Sn-decorated reduced graphene oxide anode and a LiNi<Subscript>0.5</Subscript>Mn<Subscript>1.5</Subscript>O<Subscript>4</Subscript> cathode

This paper describes the preparation and characterization of a high-voltage lithium-ion battery based on Sn-decorated reduced graphene oxide and LiNi_0.5Mn_1.5O₄ as the anode and cathode active materials, respectively. The Sn-decorated reduced graphene oxide is prepared using a microwave-assisted hydrothermal synthesis method followed by reduction at high temperature of a mixture of (C₆H₅)₂SnCl₂ and graphene oxide. The so-obtained anode material is characterized by thermogravimetric analysis, X-ray diffraction, scanning electron microscopy, and electron diffraction spectroscopy. The LiNi_0.5Mn_1.5O₄ is a commercially available product. The two materials are used to prepare composite electrodes, and their electrochemical properties are investigated by galvanostatic charge/discharge cycles at various current densities in lithium cells. The electrodes are then used to assemble a high-voltage lithium-ion cell, and the cell is tested to evaluate its performance as a function of discharge rate and cycle number.     

Synthesis and characterization of nitrogen-doped TiO2 coatings on reduced graphene oxide for enhancing the visible light photocatalytic activity

Nitrogen-doped TiO₂ coatings on reduced graphene oxide were prepared via a sonochemical synthesis and hydrothermal process. The nanocomposites showed improved photocatalytic activity due to their large specific surface areas (185–447 m²/g), the presence of TiO₂ in the anatase phase, and a quenched photoluminescence peak. In particular, GN3-TiO₂ (nitrogen-doped TiO₂ coatings on rGO with 3 ml of titanium (IV) isopropoxide) exhibited the best photocatalytic efficiency and degradation rate among the materials prepared. With nitrogen-doped on the reduced graphene oxide surface, the photocatalytic activity is enhanced approximately 17.8 times compared to that of the pristine TiO₂. The dramatic enhancement of activity is attributed to the nitrogen contents and rGO effectively promoting charge-separation efficiency and providing abundant catalytically active sites to enhance the reactivity. The composites also showed improved pollutant adsorption capacity, electron–hole pair lifetime, light absorption capability, and absorbance of visible light.     

Ultrasound-assisted solid Lewis acid-catalyzed transesterification of Lesquerella fendleri oil for biodiesel synthesis

Biodiesel, a mixture of fatty acid methyl esters (FAME), is bio-renewable, non-toxic, biodegradable, and is an attractive alternative to petroleum diesel. This work studied the sonochemical transesterification of Lesquerella fendleri oil (LFO) using inexpensive solid Lewis acid (LA) catalysts with an aim to reduce environmental pollution and dependance on non-renewable fuel sources. Due to the presence of hydroxy fatty acid methyl esters (HFAME) in LFO (∼60%), in addition to producing biofuel it can also be used to generate chemically important estolides and cyclic lactones. AlCl₃, SnCl₂, and Sn(CH₃COO)₂ showed catalytic activity using direct immersion ultrasound (DI-US) among a list of LA catalysts investigated, with AlCl₃ being the best catalyst. Ultrasound increased the reaction rate by facilitating carbocation formation of glyceridic carbons. Experiments were carried out at room temperature in a solvent range from 3:1 to 18:1 methanol-to-oil molar ratio and catalyst loading from 1 wt% to 6 wt% over 10 to 60 min sonication time at 48% ultrasound amplitude (roughly 17 W/cm²). Complete conversion (>99%) was achieved in 40 min with 5 wt% AlCl₃ catalyst. A statistical regression analysis with STATA 14.0 software was performed to optimize process parameters. Chemical characterizations of the compounds were performed with nuclear magnetic resonance (NMR) spectroscopy (¹H NMR & ¹³C NMR), and % conversion of FAMEs was calculated from the ¹H NMR spectra. The fatty acid profile was determined by GC-FID and GC–MS analysis. FT-IR spectroscopic analysis and thermogravimetric analysis (TGA) were performed to investigate the infrared absorption pattern of the compound and the volatility difference between Lesquerella fendleri biodiesel and oil under nitrogen atmosphere. Results indicate that this is a fast, green, energy-efficient, sustainable, and industrially applicable method for biodiesel production from LFO.     

Sonochemical syntheses of a new nano-plate cadmium(II) coordination polymer as a precursor for the synthesis of cadmium(II) oxide nanoparticles

Nanoplates of the three-dimensional coordination polymer, {[Cd(3)(3-pyc)(4)(N(3))(2)(H(2)O)](n) (1), 3-pyc(-)=pyridine-3-carboxylate), have been synthesized by a sonochemical process and characterized by scanning electron microscopy, X-ray powder diffraction, IR spectroscopy and elemental analyses. Cadmium(II) oxide nanoparticles were prepared from thermal decomposition in oleic acid and direct calcination of compound 1 at different temperatures. The thermal stability of nano-sized compound 1 was studied by thermal gravimetric (TG) and differential thermal analyses (DTA). Results show that the size and morphology of the CdO nanoparticles are dependent upon the particles size of compound 1 and the thermolysis temperature. A decrease in the particle size of compound 1 leads to a decrease in the particle size of the CdO, while an increase in the processing temperature leads to an increase in the particle size of the produced cadmium(II) oxide nano-particles.